阅读说明：本技术 一种乙酸乙酯的生产设备及乙酸乙酯生产方法 (Production equipment and production method of ethyl acetate ) 是由 李波 李森兰 王利亚 贾若钦 谭庚 于 2020-11-16 设计创作，主要内容包括：一种乙酸乙酯的生产设备及生产方法,该生产设备包括由上圆台段、圆柱段和下圆台段组成的分反罐,分反罐内设有催化剂隔离器,圆柱段外壁上设有多个切向进料的进料喷嘴管和多个切向进液的循环反应流体进口；上圆台段顶部设有气体采集分离管,并通过不同的切向出口分别和水蒸气收集装置、乙醛蒸汽回流管连接；下圆台段底部设有收集管,收集管以不同位置的切向出口分别和乙酸乙酯收集装置、沉渣收集装置和循环反应流体收集装置连接,乙醛蒸汽回流管通过循环反应流体收集装置与分反罐连接。利用该设备的生产方法可以将水及副产物排出分反罐,增大催化剂浓度量,提高了反应速率,还可以利用反应热对乙醛进行预热,降低冷耗,从而降低生产成本。(A production facility and production method of ethyl acetate, this production facility includes dividing the anti-tank composed of upper round platform section, cylindrical section and lower round platform section, divide and is equipped with the catalyst isolator in the anti-tank, there are a plurality of feeding nozzle pipes and a plurality of circulating reaction fluid inlets of the tangential feed liquor on the outer wall of cylindrical section of tangential feed; the top of the upper round platform section is provided with a gas collecting and separating pipe which is respectively connected with a water vapor collecting device and an acetaldehyde vapor return pipe through different tangential outlets; the bottom of the lower round platform section is provided with a collecting pipe, the collecting pipe is respectively connected with an ethyl acetate collecting device, a sediment collecting device and a circulating reaction fluid collecting device through tangential outlets at different positions, and an acetaldehyde steam return pipe is connected with a reverse separating tank through the circulating reaction fluid collecting device. The production method using the equipment can discharge water and byproducts out of the reaction tank, increase the concentration of the catalyst, improve the reaction rate, preheat acetaldehyde by using reaction heat, and reduce the cold consumption, thereby reducing the production cost.)

1. The ethyl acetate production equipment comprises a reverse separation tank, wherein a tank body of the reverse separation tank is divided into an upper circular table section, a cylindrical section and a lower circular table section from top to bottom, a cooling jacket and a heat insulation layer are arranged on the outer wall of the tank body of the reverse separation tank, and a liquid level meter is further connected to one side of the cylindrical section; the method is characterized in that: a catalyst isolator is arranged in the sub-reaction tank to retain the catalyst in the sub-reaction tank; a plurality of feeding nozzle pipes and a plurality of circulating reaction fluid inlets are arranged on the outer wall of the cylindrical section at the part corresponding to the height of the catalyst isolator, and the plurality of feeding nozzle pipes and the plurality of circulating reaction fluid inlets are uniformly arranged along the circumferential direction of the cylindrical section and can feed materials tangentially or feed liquid tangentially; the top of the upper circular table section is provided with a gas collecting and separating pipe, and the gas collecting and separating pipe is connected with a water vapor collecting device through a water vapor outlet and is connected with an acetaldehyde vapor return pipe through an acetaldehyde vapor outlet; the bottom of the lower circular table section is provided with a collecting pipe, and tangential openings respectively connected with an ethyl acetate collecting device, a sediment collecting device and a circulating reaction fluid collecting device are formed in different positions of the collecting pipe; the circulating reaction fluid collecting device comprises a circulating reaction fluid collecting device arranged in the separating and reacting tank, and the reaction fluid collected by the circulating reaction fluid collecting device returns to the separating and reacting tank again through a plurality of flow dividing pipes on the circulating reaction fluid collecting device and the circulating reaction fluid inlet to participate in the reaction; the inlet ends of the feeding nozzle pipes are connected with heat exchangers, wherein one part of the heat exchangers are connected with a pipeline of the ethyl acetate collecting device so that the collected ethyl acetate can preheat one part of acetaldehyde entering the reaction separating tank, and the other part of the heat exchangers are correspondingly connected with the shunt pipes of the circulating reaction fluid collecting device one by one so that the collected reaction fluid can preheat the other part of acetaldehyde entering the reaction separating tank; the circulating reaction fluid collecting device is also connected with the acetaldehyde vapor return pipe to realize the return of the acetaldehyde vapor to the separating and returning tank.

2. The apparatus for producing ethyl acetate according to claim 1, wherein: the catalyst isolator comprises an annular baffle plate and a cylindrical barrel with openings at two ends, the outer edge of the annular baffle plate is fixed at the upper part of the lower circular table section, and the inner edge of the annular baffle plate is fixedly connected with the opening at the bottom of the cylindrical barrel.

3. The apparatus for producing ethyl acetate according to claim 1, wherein: the collecting pipes comprise a first collecting pipe, a second collecting pipe and a third collecting pipe, wherein the pipe diameters of the first collecting pipe, the second collecting pipe and the third collecting pipe are sequentially increased; the upper end of the third collecting pipe is fixedly connected with the lower end of the lower circular table section, the second collecting pipe is sleeved in the third collecting pipe, the distance from the upper edge of the second collecting pipe to the bottom surface of the third collecting pipe is larger than the size of a tangential opening at a corresponding position on the third collecting pipe, and the length of the second collecting pipe exposed from the bottom surface of the third collecting pipe is larger than the size of the tangential opening at the corresponding position on the second collecting pipe; the pipe orifice of the first collecting pipe is in butt joint with the pipe orifice of the bottom surface of the second collecting pipe, the bottom surface of the first collecting pipe is closed, and a tangential opening is formed in the side surface of the first collecting pipe; the sediment collecting device is connected with a tangential opening of the third collecting pipe; the ethyl acetate collecting device is connected with the tangential opening of the second collecting pipe; the inlet end of the circulating reaction fluid collecting device is connected with the tangential opening of the first collecting pipe.

4. The apparatus for producing ethyl acetate according to claim 3, wherein: the second collecting pipe consists of an upper section and a lower section, the top of the upper section is provided with an outward-expanded bell mouth, the outer pipe wall of the bottom of the upper section is provided with an external thread screwed with the pipe orifice at the bottom of the third collecting pipe, the top of the lower section is detachably connected with the bottom surface of the third collecting pipe, and the pipe orifice at the bottom of the lower section is provided with an internal thread for connecting with a circulating reaction fluid collecting pipe of the circulating reaction fluid collecting device; and the upper part of the third collecting pipe is provided with a bell mouth which is in butt joint with the bottom end of the lower round platform section.

5. The apparatus for producing ethyl acetate according to claim 4, wherein: the circulating reaction fluid collecting pipe is sleeved with a first blocking disc and a second blocking disc, a first collecting seam is reserved between the edge of the first blocking disc and the pipe wall of the bell mouth of the third collecting pipe, a second collecting seam is reserved between the edge of the second blocking disc and the inner wall of the bell mouth of the upper section of the second collecting pipe, a third collecting seam is reserved between the upper edge of the bell mouth of the upper section of the second collecting pipe and the pipe wall of the third collecting pipe, a plurality of backflow ports are respectively arranged between the first blocking disc and the circulating reaction fluid collecting pipe and between the second blocking disc and the circulating reaction fluid collecting pipe, and a separation cavity is arranged between the two blocking discs.

6. The apparatus for producing ethyl acetate according to claim 1, wherein: the circulating reaction fluid collecting device comprises a circulating reaction fluid collecting pipe, a collecting funnel, an upper disc and a lower disc, wherein the upper edge of the collecting funnel is fixedly connected with the lower disc, the lower end of the collecting funnel is inserted into the circulating reaction fluid collecting pipe, and the circulating reaction fluid collecting pipe penetrates through the cylindrical barrel of the catalyst isolator; the upper disc is attached to and arranged above the lower disc, and the upper disc and the lower disc are coaxially arranged; the upper disc and the lower disc are respectively provided with a strip-shaped through hole with respective axes as symmetric centers, the radius of the strip-shaped through hole is gradually increased along the radial direction of the disc, the strip-shaped through hole on the upper disc and the strip-shaped through hole on the lower disc are mutually mirror images by the axial surface of the disc, and the strip-shaped through hole on the upper disc and the strip-shaped through hole on the lower disc can be superposed to form a circulating reaction fluid acquisition port; the upper disc and the lower disc are connected with a circulating reaction fluid collecting and adjusting device arranged at the top of the sub-reaction tank, and can rotate relatively and move axially synchronously under the driving of the circulating reaction fluid collecting and adjusting device so as to adjust the spatial position of the circulating reaction fluid collecting port.

7. The apparatus for producing ethyl acetate according to claim 6, wherein: the circulating reaction fluid collecting and adjusting device is arranged above the gas collecting and separating pipe through a bracket, and also comprises an inner transmission rod and an outer transmission rod which can rotate relatively and move axially synchronously, an axial movement driving mechanism and a rotating mechanism; the inner transmission rod is sleeved in the rod cavity of the outer transmission rod, the lower end of the inner transmission rod extends out of the central hole of the upper disc and then penetrates through the central hole of the lower disc to be fixed in the center of the lower disc, and the lower end of the outer transmission rod is fixed on the upper surface of the upper disc.

8. The apparatus for producing ethyl acetate according to claim 7, wherein: the upper end of the inner transmission rod is provided with an outer thread section extending out of the outer transmission rod, the outer thread section is in key connection with the bracket so that the inner transmission rod can only axially move, the outer thread section is also in threaded connection with a central hole of a first worm wheel, the first worm wheel is rotatably arranged at the top of the bracket, a first worm which is in matched connection with the first worm wheel is horizontally arranged at the top of the bracket, and the first worm is connected with an axial movement driving mechanism; a second worm wheel is sleeved outside the outer transmission rod and is in rotating connection with the guide rail buckle, a second worm which is in matching connection with the second worm wheel is horizontally arranged on the guide rail buckle, the second worm is driven by the rotating mechanism to rotate, and the guide rail buckle is slidably arranged on the vertical guide rail of the support; the rod body below the external thread section on the inner transmission rod is also provided with a positioning pin which is propped against the shaft sealing element on the upper surface of the guide rail fastener.

9. The apparatus for producing ethyl acetate according to claim 1, wherein: the gas collecting and separating pipe comprises an inner pipe and an outer pipe which are mutually nested and extend into the upper round platform section of the sub-reverse tank, the top of the outer pipe is connected with the inner pipe, and the lower part of the outer pipe is connected with the top opening of the upper round platform section of the sub-reverse tank; the pipe orifice at the bottom of the inner pipe is a water vapor collecting orifice, the upper part of the inner pipe extends out of the outer pipe, the extending part is provided with the water vapor outlet, and a gap is reserved between the part of the inner pipe extending into the outer pipe and the outer pipe to be used as an acetaldehyde vapor annular channel; the side surface of the outer pipe is provided with an acetaldehyde steam outlet communicated with the acetaldehyde steam annular channel.

10. A method for producing ethyl acetate, characterized in that the method is carried out by using the apparatus for producing ethyl acetate according to any one of claims 1 to 9, and comprises the steps of:

closing a discharge valve of a two-way tank, an ethyl acetate steam switch valve connected with a second collecting pipe, a reflux switch valve and a reaction liquid sampling valve in a sediment collecting device and an acetaldehyde steam sampling valve in the acetaldehyde steam collecting device; the other valves are all in an open state;

setting working parameters of a pressure measuring and controlling instrument, a reaction temperature measuring and controlling instrument, an acetaldehyde flow measuring and controlling instrument, a circulating reaction fluid flow measuring and controlling instrument, an acetaldehyde steam flow measuring and controlling instrument, an ethyl acetate steam flow measuring and controlling instrument and a cooling water flow measuring and controlling instrument through a control cabinet, wherein the temperature set value of the reaction temperature measuring and controlling instrument is (79 +/-0.5) DEG C; then adjusting the spatial position of a circulating reaction fluid collecting port;

connecting a sampling valve in the circulating reaction fluid collecting device with a nitrogen container, introducing nitrogen into the equipment, starting each centrifugal fan respectively connected with each circulating reaction fluid inlet to discharge air and water vapor in the equipment, wherein the discharge of the air is subject to no detection of oxygen, then closing the sampling valve, and disconnecting the sampling valve from the nitrogen container;

step four, starting a cooling water pump, starting each plunger pump, pumping catalyst solution required by the reaction into the sub-tank through the plunger pump, closing the plunger pump after the liquid level in the sub-tank reaches a set height, connecting an inlet pipe of the plunger pump with a corresponding acetaldehyde storage tank, restarting the plunger pump, pumping acetaldehyde into the sub-tank, and producing ethyl acetate;

step five, gradually adjusting the temperature set value of the reaction temperature measuring and controlling instrument to (101 +/-0.5) DEG C along with the progress of the reaction; when the temperature value measured by the reaction temperature measuring and controlling instrument is stable, the flow of the ethyl acetate steam flow measuring and controlling instrument is an initial set value, and the cooling water pump is intermittently started and stopped, the reaction system reaches a stable state, the ethyl acetate content measuring instrument is observed, and when the reading of the ethyl acetate content measuring instrument is higher than 99%, the ethyl acetate product is collected.

Technical Field

The invention belongs to the technical field of chemical industry, and particularly relates to production equipment for producing ethyl acetate by using acetaldehyde and a production method for producing ethyl acetate by using the production equipment.

Background

Ethyl acetate is a common basic chemical raw material and has wide application in the chemical field. The earliest synthesis method was the production of acetic acid by the reaction of concentrated sulfuric acid catalyzed by ethanol. However, the method has the disadvantages of serious corrosion to equipment, low yield, more byproducts and relatively difficult product purification. Therefore, a phosphomolybdic acid-catalyzed acetic acid-ethanol synthesis method, an ethanol dehydrogenation-oxidation method, an acetic acid-ethylene addition method and an aluminum triethoxide-catalyzed acetaldehyde production method are successively developed. The catalyst has high price and volatile effect, the reaction temperature and pressure are high, the equipment investment is large, the investment is minimum, the production cost is minimum and the corrosion to the equipment is minimum compared with the former three. However, although the catalyst of the fourth step is easy to prepare and has a high acetaldehyde conversion rate, aluminum triethoxide dissolves in ethyl acetate, and water must be added to destroy the catalyst to obtain ethyl acetate, thereby converting the catalyst into aluminum hydroxide, which is a solid waste that is almost useless. The catalyst of aluminum triethoxide (actually containing a small amount of ferric chloride, zinc chloride and the like and metal aluminum powder) is about 10 percent (w) of the acetaldehyde of the raw material, so that a great amount of metal aluminum is necessarily consumed to produce the catalyst. The other raw material ethanol of the aluminum triethoxide has larger loss of ethanol and ethyl acetate because the ethanol is easily dissolved in water when the aluminum triethoxide is destroyed by hydrolysis. The ethanol and water remaining in the ethyl acetate organic phase also increase the difficulty of rectification and purification of ethyl acetate and affect the yield of ethyl acetate. In addition, acetaldehyde, which is a raw material for producing acetaldehyde, is active chemically and has a too low boiling point (20.8 ℃), and the reaction temperature for producing ethyl acetate from acetaldehyde is below 20 ℃ and lower than room temperature, so that the raw material and the reaction heat are cooled (conversely, if the reaction heat is utilized, the reaction heat is higher than the room temperature), and a large amount of cold energy is consumed. How to make it longer and avoid it shorter is necessary to make a lot of work on production equipment and preparation technology. The invention designs a set of reaction equipment aiming at the problem and can better solve the existing problem.

Disclosure of Invention

The invention aims to provide a new ethyl acetate production device and a corresponding production method aiming at the defects of the current equipment and process technology for producing ethyl acetate by catalyzing acetaldehyde reaction with aluminum triethoxide, so as to further reduce the production cost and realize the aim of clean production of ethyl acetate.

In order to achieve the purpose, the invention adopts the technical scheme that: the ethyl acetate production equipment comprises a reverse separation tank, wherein a tank body of the reverse separation tank is divided into an upper circular table section, a cylindrical section and a lower circular table section from top to bottom, a cooling jacket and a heat insulation layer are arranged on the outer wall of the tank body of the reverse separation tank, and a liquid level meter is further connected to one side of the cylindrical section; a catalyst isolator is arranged in the sub-reaction tank to retain the catalyst in the sub-reaction tank; a plurality of feeding nozzle pipes and a plurality of circulating reaction fluid inlets are arranged on the outer wall of the cylindrical section at the part corresponding to the height of the catalyst isolator, and the plurality of feeding nozzle pipes and the plurality of circulating reaction fluid inlets are uniformly arranged along the circumferential direction of the cylindrical section and can feed materials tangentially or feed liquid tangentially; the top of the upper circular table section is provided with a gas collecting and separating pipe, and the gas collecting and separating pipe is connected with a water vapor collecting device through a water vapor outlet and is connected with an acetaldehyde vapor return pipe through an acetaldehyde vapor outlet; the bottom of the lower circular table section is provided with a collecting pipe, and tangential openings respectively connected with an ethyl acetate collecting device, a sediment collecting device and a circulating reaction fluid collecting device are formed in different positions of the collecting pipe; the circulating reaction fluid collecting device comprises a circulating reaction fluid collecting device arranged in the separating and reacting tank, and the reaction fluid collected by the circulating reaction fluid collecting device returns to the separating and reacting tank again through a plurality of flow dividing pipes on the circulating reaction fluid collecting device and the circulating reaction fluid inlet to participate in the reaction; the inlet ends of the feeding nozzle pipes are connected with heat exchangers, wherein one part of the heat exchangers are connected with a pipeline of the ethyl acetate collecting device so that the collected ethyl acetate can preheat one part of acetaldehyde entering the reaction separating tank, and the other part of the heat exchangers are correspondingly connected with the shunt pipes of the circulating reaction fluid collecting device one by one so that the collected reaction fluid can preheat the other part of acetaldehyde entering the reaction separating tank; the circulating reaction fluid collecting device is also connected with the acetaldehyde vapor return pipe to realize the return of the acetaldehyde vapor to the separating and returning tank.

The catalyst isolator comprises an annular baffle plate and a cylindrical barrel with openings at two ends, the outer edge of the annular baffle plate is fixed at the upper part of the lower circular table section, and the inner edge of the annular baffle plate is fixedly connected with the opening at the bottom of the cylindrical barrel.

The collecting pipes comprise a first collecting pipe, a second collecting pipe and a third collecting pipe, wherein the pipe diameters of the first collecting pipe, the second collecting pipe and the third collecting pipe are sequentially increased; the upper end of the third collecting pipe is fixedly connected with the lower end of the lower circular table section, the second collecting pipe is sleeved in the third collecting pipe, the distance from the upper edge of the second collecting pipe to the bottom surface of the third collecting pipe is larger than the size of a tangential opening at a corresponding position on the third collecting pipe, and the length of the second collecting pipe exposed from the bottom surface of the third collecting pipe is larger than the size of the tangential opening at the corresponding position on the second collecting pipe; the pipe orifice of the first collecting pipe is in butt joint with the pipe orifice of the bottom surface of the second collecting pipe, the bottom surface of the first collecting pipe is closed, and a tangential opening is formed in the side surface of the first collecting pipe; the sediment collecting device is connected with a tangential opening of the third collecting pipe; the ethyl acetate collecting device is connected with the tangential opening of the second collecting pipe; the inlet end of the circulating reaction fluid collecting device is connected with the tangential opening of the first collecting pipe.

The second collecting pipe consists of an upper section and a lower section, the top of the upper section is provided with an outward-expanded bell mouth, the outer pipe wall of the bottom of the upper section is provided with an external thread screwed with the pipe orifice at the bottom of the third collecting pipe, the top of the lower section is detachably connected with the bottom surface of the third collecting pipe, and the pipe orifice at the bottom of the lower section is provided with an internal thread for connecting with a circulating reaction fluid collecting pipe of the circulating reaction fluid collecting device; and the upper part of the third collecting pipe is provided with a bell mouth which is in butt joint with the bottom end of the lower round platform section.

The circulating reaction fluid collecting pipe is sleeved with a first blocking disc and a second blocking disc, a first collecting seam is reserved between the edge of the first blocking disc and the pipe wall of the bell mouth of the third collecting pipe, a second collecting seam is reserved between the edge of the second blocking disc and the inner wall of the bell mouth of the upper section of the second collecting pipe, a third collecting seam is reserved between the upper edge of the bell mouth of the upper section of the second collecting pipe and the pipe wall of the third collecting pipe, a plurality of backflow ports are respectively arranged between the first blocking disc and the circulating reaction fluid collecting pipe and between the second blocking disc and the circulating reaction fluid collecting pipe, and a separation cavity is arranged between the two blocking discs.

The circulating reaction fluid collecting device comprises a circulating reaction fluid collecting pipe, a collecting funnel, an upper disc and a lower disc, wherein the upper edge of the collecting funnel is fixedly connected with the lower disc, the lower end of the collecting funnel is inserted into the circulating reaction fluid collecting pipe, and the circulating reaction fluid collecting pipe penetrates through the cylindrical barrel of the catalyst isolator; the upper disc is attached to and arranged above the lower disc, and the upper disc and the lower disc are coaxially arranged; the upper disc and the lower disc are respectively provided with a strip-shaped through hole with respective axes as symmetric centers, the radius of the strip-shaped through hole is gradually increased along the radial direction of the disc, the strip-shaped through hole on the upper disc and the strip-shaped through hole on the lower disc are mutually mirror images by the axial surface of the disc, and the strip-shaped through hole on the upper disc and the strip-shaped through hole on the lower disc can be superposed to form a circulating reaction fluid acquisition port; the upper disc and the lower disc are connected with a circulating reaction fluid collecting and adjusting device arranged at the top of the sub-reaction tank, and can rotate relatively and move axially synchronously under the driving of the circulating reaction fluid collecting and adjusting device so as to adjust the spatial position of the circulating reaction fluid collecting port.

The circulating reaction fluid collecting and adjusting device is arranged above the gas collecting and separating pipe through a bracket, and also comprises an inner transmission rod and an outer transmission rod which can rotate relatively and move axially synchronously, an axial movement driving mechanism and a rotating mechanism; the inner transmission rod is sleeved in the rod cavity of the outer transmission rod, the lower end of the inner transmission rod extends out of the central hole of the upper disc and then penetrates through the central hole of the lower disc to be fixed in the center of the lower disc, and the lower end of the outer transmission rod is fixed on the upper surface of the upper disc.

The upper end of the inner transmission rod is provided with an outer thread section extending out of the outer transmission rod, the outer thread section is in key connection with the bracket so that the inner transmission rod can only axially move, the outer thread section is also in threaded connection with a central hole of a first worm wheel, the first worm wheel is rotatably arranged at the top of the bracket, a first worm which is in matched connection with the first worm wheel is horizontally arranged at the top of the bracket, and the first worm is connected with an axial movement driving mechanism; a second worm wheel is sleeved outside the outer transmission rod and is in rotating connection with the guide rail buckle, a second worm which is in matching connection with the second worm wheel is horizontally arranged on the guide rail buckle, the second worm is driven by the rotating mechanism to rotate, and the guide rail buckle is slidably arranged on the vertical guide rail of the support; the rod body below the external thread section on the inner transmission rod is also provided with a positioning pin which is propped against the shaft sealing element on the upper surface of the guide rail fastener.

The gas collecting and separating pipe comprises an inner pipe and an outer pipe which are mutually nested and extend into the upper round platform section of the sub-reverse tank, the top of the outer pipe is connected with the inner pipe, and the lower part of the outer pipe is connected with the top opening of the upper round platform section of the sub-reverse tank; the pipe orifice at the bottom of the inner pipe is a water vapor collecting orifice, the upper part of the inner pipe extends out of the outer pipe, the extending part is provided with the water vapor outlet, and a gap is reserved between the part of the inner pipe extending into the outer pipe and the outer pipe to be used as an acetaldehyde vapor annular channel; the side surface of the outer pipe is provided with an acetaldehyde steam outlet communicated with the acetaldehyde steam annular channel.

A production method of ethyl acetate is carried out by utilizing the production equipment of ethyl acetate, and comprises the following steps:

closing a discharge valve of a two-way tank, an ethyl acetate steam switch valve connected with a second collecting pipe, a reflux switch valve and a reaction liquid sampling valve in a sediment collecting device and an acetaldehyde steam sampling valve in the acetaldehyde steam collecting device; the other valves are all in an open state;

setting working parameters of a pressure measuring and controlling instrument, a reaction temperature measuring and controlling instrument, an acetaldehyde flow measuring and controlling instrument, a circulating reaction fluid flow measuring and controlling instrument, an acetaldehyde steam flow measuring and controlling instrument, an ethyl acetate steam flow measuring and controlling instrument and a cooling water flow measuring and controlling instrument through a control cabinet, wherein the temperature set value of the reaction temperature measuring and controlling instrument is (79 +/-0.5) DEG C; then adjusting the spatial position of a circulating reaction fluid collecting port;

connecting a sampling valve in the circulating reaction fluid collecting device with a nitrogen container, introducing nitrogen into the equipment, starting each centrifugal fan respectively connected with each circulating reaction fluid inlet to discharge air and water vapor in the equipment, wherein the discharge of the air is subject to no detection of oxygen, then closing the sampling valve, and disconnecting the sampling valve from the nitrogen container;

step four, starting a cooling water pump, starting each plunger pump, pumping catalyst solution required by the reaction into the sub-tank through the plunger pump, closing the plunger pump after the liquid level in the sub-tank reaches a set height, connecting an inlet pipe of the plunger pump with a corresponding acetaldehyde storage tank, restarting the plunger pump, pumping acetaldehyde into the sub-tank, and producing ethyl acetate;

step five, gradually adjusting the temperature set value of the reaction temperature measuring and controlling instrument to (101 +/-0.5) DEG C along with the progress of the reaction; when the temperature value measured by the reaction temperature measuring and controlling instrument is stable, the flow of the ethyl acetate steam flow measuring and controlling instrument is an initial set value, and the cooling water pump is intermittently started and stopped, the reaction system reaches a stable state, the ethyl acetate content measuring instrument is observed, and when the reading of the ethyl acetate content measuring instrument is higher than 99%, the ethyl acetate product is collected.

The basic principle of the operation of the knock-out drum can be described as follows.

Setting: the initial flow rate of the fluid entering the reverse separating tank is v₁Angular velocity of ω₁The radius of the middle cylindrical section of the sub-tank is R, the radius of the collecting seam of the lower circular table section is R, the mass of the fluid mass point is m, and the linear velocity at the inner edge of the collecting seam is v₂Angular velocity of ω₂. If the friction resistance is not considered temporarily, or the friction resistance is considered at the same time, and after the system reaches stable dynamic balance, the driving force generated by the fluid conveying power is opposite to the direction of the friction force and equal in magnitude, namely the resultant force borne by the fluid mass point is zero, namely the principle of angular momentum conservation is followed:

L＝mR²ω₁＝mr²ω₂fixed value (1)

Or L ═ mv₁R＝mv₂r is a constant value (2)

Where L is the angular momentum of the fluid particles.

From the formula₂/ω₁＝(R/r)² (3)

V is obtained from₂/v₁＝R/r (4)

From the centripetal force formula: f_{Separation device}＝F_{To the direction of}＝ma＝mω²r＝mv²R, can know

The centrifugal force of the fluid particles on the inner side wall of the middle cylindrical section of the reverse separating tank is as follows:

the centrifugal force of the fluid particles at the collection slit is:

Then

for the invention, because R is dozens to hundreds times of R and even higher, omega can be known by formula III₂Is omega₁Several tens or several hundreds of square times of (v) is given by the formula₂Is v₁Dozens or hundreds times of the formula (V), F_{2 from}Is F_{1 from}The cubic times of dozens or hundreds, the invention fully utilizes the multiplication of the 'minute reaction tank' on the fluid rotating speed, the linear speed and the centrifugal force.

It can be seen that the centripetal force (centrifugal force) and centripetal acceleration of the fluid from the inlet to the collection slit are both greatly increased to the initial (R/R)³And (4) doubling.Thus, for a given v₁R, when R → infinity, then v₂、ω₂、F_{2 from}、a₂About infinity, where F is_{2 from}、a₂The fastest rate of change.

The main reaction of acetaldehyde in the presence of aluminum triethoxide (synthesized by traditional method, including small amount of ferric chloride, aluminum powder and absolute ethyl alcohol) to produce ethyl acetate is:

the side reaction is Al (OCH)₂CH₃)₃+3H₂O→Al(OH)₃+3CH₃CH₂OH (7)

CH₃CHO+2CH₃CH₂OH→CH₃CH(OCH₂CH₃)₂+H₂O (8)

In the above formula, (7) water in the formula is derived from trace water carried by raw materials and (8) water generated by the formula, and another source of ethanol in the formula (8) is ethanol which is not completely reacted in the preparation of aluminum triethoxide. Therefore, the process for producing ethyl acetate by the traditional acetaldehyde catalysis method and the process must have acetal by-products. The invention is characterized in that the water can be separated and discharged in time, thus not only reducing the hydrolysis amount of the aluminum triethoxide, namely reducing the amount of byproducts, but also leaving the aluminum triethoxide in the reaction tank to play the catalytic role continuously, and only needing to supplement a little aluminum triethoxide, thereby greatly reducing the amount of the aluminum triethoxide brought into the ethanol.

The dynamic energy balance and material balance of the present invention were analyzed as follows.

When the driving force generated by the fluid conveying power and the friction force are opposite in direction and equal in magnitude, and the materials of the sub-reaction tank are not fed in and out, namely the resultant external force borne by fluid particles is zero, the state of the sub-reaction tank can meet the law of conservation of angular momentum, but the state is only an 'ideal state'. Because the linear speed difference of the inlet and outlet branch reaction tanks is large, the kinetic energy brought by reactants can be almost ignored. Therefore, to maintain the "resultant external force" of the partial-reaction tank to be zero, some "low linear velocity fluid" must be taken out of the partial-reaction tank, and the linear velocity of the fluid must be increased to provide the partial-reaction tank with the kinetic energy lost by the discharged product. The circulating reaction fluid collecting device of the sub-anti-tank comprises the centrifugal fan which can continuously provide energy for the rotating fluid of the sub-anti-tank, so that the balance of input and output of dynamic energy in the sub-anti-tank is ensured.

The gas collecting port arranged at the upper part of the anti-separation tank and the collecting slot arranged at the lower part of the anti-separation tank have much smaller resistance to rotating fluid than the outlet pipe of the traditional cyclone separation tank. The fluids with different densities in the separating and reversing tank of the invention respectively flow out tangentially along the side wall of the collecting pipe, and part of kinetic energy of the circulating reaction fluid can be recovered and utilized by the circulating reaction fluid collecting device.

Compared with the existing chemical equipment, the invention has the beneficial effects that:

1. the reaction system is operated in a fully sealed way, only a small amount of water and a small amount of perfume acetal are discharged, and the yield of the main product ethyl acetate is higher than that of the traditional process.

2. The reaction system is separated from the trace water in time, so that the catalyst is prevented from being damaged by hydrolysis, and the catalyst can be left in the reaction separating tank to play a role continuously, thereby greatly reducing the using amount of the catalyst and saving the catalyst treatment and distillation processes.

3. Compared with the traditional ethyl acetate production process, the invention improves the reaction temperature (100 ℃, which is far higher than the temperature below 20 ℃ in the prior art), and can ensure that the reactant acetaldehyde firstly passes through the catalyst solution with higher concentration at the position of the catalyst isolator when entering the reaction tank, thereby greatly improving the reaction rate and greatly improving the productivity of the unit volume of the equipment.

4. The reaction heat is fully utilized, the cooling efficiency is greatly improved, and the cooling consumption is greatly reduced.

Drawings

FIG. 1 is a schematic diagram of the main structure of the present invention;

FIG. 2 is a top view of the circulation loop, feed system and the distributor tank connected together;

FIG. 3 is a schematic view of the connection of the separating and returning tank and the sediment tank;

FIG. 4 is an enlarged view of the top A of the reverse tank of FIG. 1;

FIG. 5 is an enlarged view at B in FIG. 4;

FIG. 6 is an enlarged view at C of FIG. 1;

FIG. 7 is a schematic view of the mating relationship of the upper and lower disks of FIG. 6;

FIG. 8 is an enlarged view taken at D in FIG. 1;

FIG. 9 is an enlarged top view at E in FIG. 1;

FIG. 10 is a control cabinet of the present invention;

FIG. 11 is a gas chromatogram of a sample analysis of the circulating reaction fluid in example 1;

FIG. 12 is a gas chromatogram for sampling and analyzing the circulating reaction fluid when the circulating reaction fluid collecting port is in the optimum position in example 1;

FIG. 13 is a gas chromatogram for sampling and analyzing a circulating reaction fluid when a circulating reaction fluid collection port is in an optimal position in example 2;

FIG. 14 is a schematic view showing the heat absorption or release of reactants and products in the reaction system in example 1;

the labels in the figure are: 100. the device comprises a cylindrical section, 101, an upper circular table section, 102, a lower circular table section, 103, a catalyst isolator, 104, a heat insulation layer, 105, a cooling jacket, 106, an upper column jacket connecting pipe, 107, an inner and outer composite transmission rod, 108, a lower column jacket connecting pipe, 109, a cooling jacket water inlet valve, 110, a circulating reaction fluid collecting pipe, 111, a liquid level meter, 112, a cooling jacket water outlet valve, 113, a cooling water pump, 114, a cooling water flow measuring and controlling instrument, 115, a cooling water tank, 116 and a filter screen one-way valve;

201. the device comprises nozzle pipes I and 202, nozzle pipes II and 203, nozzle pipes III and 204, nozzle pipes IV and 2011 and a tangential inlet of a feeding nozzle; 210. acetaldehyde storage tanks I and 211, plunger pumps I and 212, a first inlet switch valve of a heat exchanger I, 213, heat exchangers I and 214, a first outlet switch valve of the heat exchanger I, 215, acetaldehyde flow measuring and controlling instruments I and 216, a first one-way valve, 217 and a second inlet of the heat exchanger I; 220. the acetaldehyde storage tank II, 221, the plunger pump II, 222, the first path of inlet switch valve of the heat exchanger II, 223, the heat exchanger II, 224, the first path of outlet switch valve of the heat exchanger II, 225, the acetaldehyde flow measuring and controlling instrument II, 226, the second one-way valve, 227 and the second path of inlet of the heat exchanger II; 230. acetaldehyde storage tanks III, 231, plunger pumps III, 232, switch valves, 233, acetaldehyde flow measuring and controlling instruments III, 234 and a third one-way valve; 240. the acetaldehyde storage tanks IV and 241, the plunger pumps IV and 242, a first path of inlet switch valve of the heat exchanger IV, 243, the heat exchangers IV and 244, a first path of outlet switch valve of the heat exchanger IV, 245, acetaldehyde flow measuring and controlling instruments IV and 246, a fourth one-way valve, 247 and a second path of inlet of the heat exchanger IV;

310. a water vapor switch valve 311, a pressure measuring and controlling instrument 312, a fifth one-way valve 313, a two-way tank 314, an air cooler 315, a pressure relief valve 316, a view port 317 and a discharge valve; 320. an acetaldehyde reflux pipeline 321, an acetaldehyde steam switch valve 322, a sixth one-way valve 323, an acetaldehyde steam flow measuring and controlling instrument 324, an acetaldehyde steam reflux valve I, an acetaldehyde steam reflux valve 325, an acetaldehyde steam reflux valve II, an acetaldehyde steam sampling valve 326; 330. a gas collecting and separating tube 331, a water vapor collecting port 332 and an acetaldehyde vapor collecting port;

400. the system comprises an ethyl acetate collecting device, 410, an ethyl acetate steam switch valve, 411, a seventh one-way valve, 412, an ethyl acetate content tester, 413, an ethyl acetate steam flow measuring and controlling instrument, 414, a heat exchanger III, 415, a first path outlet switch valve of the heat exchanger III, 416, an ethyl acetate storage tank, 417, a second path inlet of the heat exchanger III, 418 and a second path outlet switch valve of the heat exchanger III;

500. a circulating reaction fluid collecting device 501, circulating reaction fluid inlets I and 502, circulating reaction fluid inlets II and 503, circulating reaction fluid inlets III and 504 and a circulating reaction fluid inlet IV; 510. the system comprises a circulating reaction fluid switch valve, 511, a three-way branch pipe, 512, an eighth one-way valve, 513, a sampling valve, 514, a reaction temperature measuring and controlling instrument, 515, a circulating reaction fluid flow measuring and controlling instrument, 516, a flow dividing head, 517, a first flow dividing pipe, 518, a second flow dividing pipe, 519, a third flow dividing pipe, 520, a fourth flow dividing pipe, 521, a centrifugal fan I, 522, a centrifugal fan II, 523, a centrifugal fan III, 524 and a centrifugal fan IV;

600. a sediment collecting device, 610, a sediment fluid outlet switch valve, 611, a sediment tank inlet switch valve, 612, a sediment tank, 613, a sediment tank tangential inlet, 614, a reaction liquid collecting port, 615, a sediment tank sight glass, 616, a tank body fastener, 617, a reaction liquid collecting pipe fastener, 618, a reaction liquid tangential outlet, 619, a reaction liquid reflux valve, 620, a reaction liquid sampling valve, 621 and a pollution cleaning switch valve;

710. an inner transmission rod 711, an inner transmission rod shaft seal 712, an inner transmission rod positioning pin 713, an outer thread section 714, a first worm gear 715, a rotation stop key 716 and an axial movement driving mechanism; 720. the device comprises an outer transmission rod 721, an outer transmission rod shaft seal 722, a second worm gear 723, a guide rail fastener 724, a radial movement driving mechanism 725 and a vertical guide rail;

800. a circulating reaction fluid collecting port 810, a lower disc 811, a collecting funnel 812, a countersunk head bolt 813, a bell mouth of a circulating reaction fluid collecting pipe 814, a discharge port 820, an upper disc 815, a lower strip-shaped hole 821 and an upper strip-shaped hole;

901. the device comprises a first collecting pipe, a second collecting pipe, a third collecting pipe, a first blocking disc, a second collecting disc, a separation cavity, a second collecting slot, a third collecting slot, a slag-containing fluid tangential outlet, a first collecting slot, a second collecting slot, a third collecting slot, a slag-containing fluid tangential outlet, a first connecting wire port, a second connecting wire port, a;

11. control cabinet 1101, power line 1102, power supply and signal line of each instrument 1103 and main power supply.

Detailed Description

The present invention will be described in further detail with reference to the following drawings and examples, but the invention is not limited thereto.

Referring to the attached drawings, the ethyl acetate production equipment comprises a sub-reaction tank as a reactor, an ethyl acetate collecting device 400 for collecting ethyl acetate products, a gas collecting and separating device for collecting gas in reaction, a sediment collecting device 600 for collecting sediment, a circulating reaction fluid collecting device 500 for collecting reaction fluid in the sub-reaction tank and making the reaction fluid flow back, and a control cabinet 11.

The structure of the sub-tank is shown in figure 1, the tank body of the sub-tank is divided into an upper, middle and lower structure with one column and two platforms, an upper round platform section 101, a cylindrical section 100 and a lower round platform section 102 are respectively arranged from top to bottom, the three sections are fixedly connected through fasteners, and the inner cavity is communicated to form a reaction cavity. The outer wall of the tank body of the sub-tank is provided with a cooling jacket 105 and an insulating layer 104.

With continued reference to fig. 1, the cooling jacket 105 includes a plurality of cooling jacket units distributed on the side walls of the upper circular truncated cone section 101, the cylindrical section 100 and the lower circular truncated cone section 102, the cooling jacket unit located in the upper circular truncated cone section 101 is communicated with the cooling jacket unit located in the cylindrical section 100 through an upper circular truncated cone jacket connecting pipe 106, and the cooling jacket unit located in the lower circular truncated cone section 102 is communicated with the cooling jacket unit located in the cylindrical section 100 through a lower circular truncated cone jacket connecting pipe 108; the top of the cooling jacket 105 is provided with a drain pipe and a cooling jacket outlet valve 112 is arranged, and the opening of the drain pipe is positioned above the water surface of the cooling water tank 114; the bottom of the cooling jacket 105 is provided with a water inlet pipe and a water inlet valve 112 of the cooling jacket, the water inlet pipe is also provided with a cooling water flow measuring and controlling instrument 116, the water inlet end of a cooling water pump 115 for pumping cooling water is positioned below the water surface of the cooling water tank 115, a filter screen one-way valve 116 is arranged, and the water outlet end of the cooling water pump 113 is connected with the cooling water flow measuring and controlling instrument 114.

The insulating layer 104 is disposed on the cooling jacket unit and the outer wall of the tank body not covered by the cooling jacket 105, and preferably, the insulating layer 104 is also wrapped on the upper column jacket connecting pipe 106 and the lower column jacket connecting pipe 108.

And a liquid level meter 111 is further installed on the outer side of the cylindrical section 100 so as to realize real-time monitoring of the liquid level height in the tank body. And a catalyst isolator 107 is arranged in the reaction cavity of the sub-reaction tank and is used for intercepting the catalyst in the sub-reaction tank so as to prevent the catalyst from flowing to the lower round platform section 102 and being collected by other collecting devices. The catalyst isolator 107 is arranged at the joint of the cylindrical section 100 and the lower round platform section 102, and comprises an annular baffle plate and a cylindrical barrel with openings at two ends, the outer edge of the annular baffle plate is fixed at the upper part of the lower round platform section 102, and the inner edge of the annular baffle plate is fixedly connected with the opening at the bottom of the cylindrical barrel, so that an annular space between the outer cylindrical surface of the cylindrical barrel and the inner wall of the cylindrical section 100 can be used as an isolation space of the catalyst, and the concentration of a catalyst solution in the space is higher.

Referring to fig. 1 and 2, four nozzle pipes feeding tangentially to the partial reaction tank are uniformly distributed on the side wall of the cylindrical section 100 along the circumferential direction, the reaction raw material provided by the nozzle pipes is acetaldehyde, a circulating reaction fluid inlet is also arranged above each nozzle pipe, the circulating reaction fluid inlet is also feeding tangentially, the circulating reaction fluid collecting device 500 feeds the collected circulating reaction fluid into the partial reaction tank again through the circulating reaction fluid inlet to participate in the reaction, and the circulating reaction fluid enters the tank body along the tangential direction and can supplement the kinetic energy of the reaction fluid in the tank body. The nozzle pipes and the circulating reaction fluid inlet are both disposed within the height of the catalytic separator 107.

With reference to fig. 1 and 4, a gas collecting and separating device at the top of the upper round table section 101 is illustrated. In the process of producing ethyl acetate by using acetaldehyde, the generated gas mainly comprises water vapor and acetaldehyde vapor, and the densities of the water vapor and the acetaldehyde vapor are different, so that the two gases can be respectively collected by arranging collection ports at different radial positions. The gas collecting and separating device is provided with a gas collecting and separating pipe 330 inserted into the sub-reverse tank from the top of the upper round platform section 101, the gas collecting and separating pipe 330 comprises an inner pipe and an outer pipe which are mutually nested and extend into the upper round platform section 101 of the sub-reverse tank, the top of the outer pipe is fixedly connected with a connecting ring on the inner pipe, the lower part of the outer pipe is provided with a ring, and the ring is connected with an opening at the top of the upper round platform section 101 of the sub-reverse tank; the mouth of pipe of inner tube bottom stretches into last round section 101, for steam gathers mouth 331, inner tube upper portion stretches out the outer tube, and is equipped with at the extension the steam export to connect steam collection device. An annular gap is reserved between the part of the inner pipe extending into the outer pipe and is used as an acetaldehyde steam annular channel; the bottom pipe opening of the outer pipe also extends into the upper round platform section, the extending length of the bottom pipe opening of the outer pipe is smaller than that of the inner pipe, the pipe opening of the outer pipe and the pipe opening of the inner pipe form an annular acetaldehyde steam collecting opening 332, and an acetaldehyde steam outlet communicated with the acetaldehyde steam annular channel is formed in the side surface of the outer pipe. The water vapor outlet and the acetaldehyde vapor outlet are tangential outlets, and the pipe orifice at the bottom of the inner pipe and the pipe orifice at the bottom of the outer pipe are necking.

The water vapor collecting device comprises a collecting pipeline arranged at a water vapor outlet, a water vapor switch valve 310, a pressure measuring and controlling instrument 311, a fifth one-way valve 312 and a two-way tank 313 are sequentially arranged on the collecting pipeline along the water vapor flow direction, an air cooler 314 is arranged at the top of the two-way tank 313, the top of the air cooler 314 is a pressure release valve 315, and a discharge valve 317 is arranged at the bottom of the two-way tank 313. The pressure value measured by the pressure measuring and controlling instrument 311 is equal to the pressure value in the sub-reverse tank, the pressure measuring and controlling instrument sends the measured pressure value to the control cabinet of the equipment, and the controller of the control cabinet can adjust the work of the plunger pump II 221 and the plunger pump IV according to the pressure value. The plunger pump is adjusted through a pressure value, belongs to the conventional automatic control technology in the industrial field, and the principle and the implementation mode of the plunger pump can be realized through the selection of the conventional technology.

The acetaldehyde vapor outlet is connected with the inlet of the acetaldehyde return pipeline 320, the outlet of the acetaldehyde return pipeline 320 is connected with the circulating reaction fluid collecting device 500, the acetaldehyde return pipeline 320 is sequentially provided with an acetaldehyde vapor switch valve 321, a sixth one-way valve 322, an acetaldehyde vapor flow measuring and controlling instrument 323 and an acetaldehyde vapor return valve I324, and the acetaldehyde vapor enters the circulating reaction fluid collecting device 500 through the acetaldehyde return pipeline 320 and returns to the sub-reaction tank along with the circulating reaction fluid to participate in the reaction.

Referring to fig. 1 and 8, a collecting pipe formed by sequentially connecting three pipe bodies with different diameters is arranged at the bottom of the lower circular platform section 102, and tangential outlets are arranged on the different pipe bodies to respectively collect separated fluids. The collecting pipes comprise a first collecting pipe 901, a second collecting pipe 902 and a third collecting pipe 903, the pipe diameters of which are sequentially increased; the upper end of the third collecting pipe 903 is fixedly connected with the lower end of the lower round platform section 102, the second collecting pipe 902 is sleeved in the third collecting pipe 903, the distance from the upper edge of the second collecting pipe 902 to the bottom surface of the third collecting pipe 903 is larger than the size of a tangential opening at a corresponding position on the third collecting pipe 903, and the length of the second collecting pipe 902 exposed from the bottom surface of the third collecting pipe 903 is larger than the size of a tangential opening at a corresponding position on the second collecting pipe 902; the pipe orifice of the first collecting pipe 901 is butted with the pipe orifice of the bottom surface of the second collecting pipe 902, the bottom surface of the first collecting pipe 901 is closed, and a tangential opening is arranged on the side surface of the first collecting pipe 901; the sediment collecting device 600 is connected with a tangential opening of the third collecting pipe 903; the ethyl acetate collecting device 400 is connected with a tangential opening of a second collecting pipe 902; the inlet end of the circulating reaction fluid collection apparatus 500 is connected to the tangential opening of the first collection pipe 901.

The second collecting pipe 902 is composed of an upper section and a lower section, the top of the upper section is provided with an outward-expanded bell mouth, the outer pipe wall of the bottom of the upper section is provided with a first connecting screw port 912 which is in screw connection with the pipe orifice at the bottom of the third collecting pipe 903, the top of the lower section is detachably connected with the bottom surface of the third collecting pipe 903, and the pipe orifice at the bottom of the lower section is provided with a second connecting screw port 913 so as to be connected with the circulating reaction fluid collecting pipe 110 of the circulating reaction fluid collecting device; the upper part of the third collecting pipe 903 is provided with a bell mouth which is in butt joint with the bottom end of the lower circular table section 102.

The circulating reaction fluid collecting pipe 110 is sleeved with a first blocking disc 904 and a second blocking disc 905, a first collecting slit 907 is reserved between the edge of the first blocking disc 904 and the pipe wall of the bell mouth of the third collecting pipe 903, a second collecting slit 909 is reserved between the edge of the second blocking disc 905 and the inner wall of the bell mouth of the upper section of the second collecting pipe 902, a third collecting slit 910 is reserved between the upper edge of the bell mouth of the upper section of the second collecting pipe 902 and the pipe wall of the third collecting pipe 903, a plurality of return ports 906 are respectively arranged between the first blocking disc 904 and the circulating reaction fluid collecting pipe 110 and between the second blocking disc 905 and the circulating reaction fluid collecting pipe 110, and a separation cavity 908 is arranged between the two blocking discs.

In the process of rotating the reaction fluid in the separating and reaction tank, due to the action of centrifugal force, the ethyl acetate steam, the slag-containing fluid and a part of low-density fluid enter the separation cavity 908 through the first collecting slit 907, and because the separation cavity 908 is located at the diameter-variable position of the third collecting pipe 903, the rotating radius of the fluid becomes smaller and the centrifugal force becomes larger, so that the fluid in the separation cavity 908 is further separated into slag-containing fluid with the maximum density, ethyl acetate steam with the medium density and a small amount of low-density fluid; a small amount of separated low-density fluid can flow back upwards through the return port 906 to participate in the reaction again, so that excessive accumulation is avoided and the low-density fluid is prevented from being mixed into ethyl acetate to be collected; the separated ethyl acetate vapor enters the second collecting pipe 902 through the second collecting slit 909, is collected by the ethyl acetate collecting device 400, has the highest density of the slag-containing fluid containing solid particles, enters the third collecting pipe 903 through the third collecting slit 910, and is collected by the sediment collecting device 600.

The structure of the ethyl acetate collecting device 400 can be seen from fig. 1, an inlet of a collecting pipeline of the ethyl acetate collecting device 400 is connected with a tangential opening of a second collecting pipe 902, the tail end of the collecting pipeline is connected with a first inlet of a heat exchanger iii 414, an ethyl acetate steam switch valve 410, a seventh one-way valve 411, an ethyl acetate content measuring instrument 412 and an ethyl acetate steam flow measuring and controlling instrument 413 are sequentially arranged on the collecting pipeline according to the ethyl acetate flow direction, and a first outlet of the heat exchanger iii 414 is connected with an ethyl acetate storage tank 416. The second inlet 417 of the heat exchanger III is connected with the acetaldehyde storage tank III 230 through a plunger pump III 231, and the second outlet is connected with a nozzle pipe on the distribution tank. The acetaldehyde needing to enter the separate reaction tank can be preheated by ethyl acetate steam and then enters the separate reaction tank for reaction after preheating.

The structure of the collection device 500 for the circulating reaction fluid is shown in fig. 1 and 8, one end of a collection pipeline is connected with a tangential outlet 914 for the circulating reaction fluid on a first collection pipe, the other end of the collection pipeline is connected with a flow dividing head 516, a circulating reaction fluid switch valve 510, a three-way branch pipe 511, an eighth one-way valve 512, a sampling valve 513, a reaction temperature measuring and controlling instrument 514 and a circulating reaction fluid flow measuring and controlling instrument 515 are sequentially arranged on the collection pipeline, four flow dividing pipes are respectively arranged on the flow dividing head 516, namely a first flow dividing pipe 517, a second flow dividing pipe 518, a third flow dividing pipe 519 and a fourth flow dividing pipe 520, and a flow dividing valve is arranged. Each shunt pipe is correspondingly connected with one circulating reaction fluid inlet on the distribution and reaction tank.

A section of branch is further arranged between the eighth one-way valve 512 and the sampling valve 513, the branch is connected with an acetaldehyde return pipeline 320 for acetaldehyde vapor return through a tee joint, and an acetaldehyde vapor return valve II 325 and an acetaldehyde vapor sampling valve 326 are arranged on the branch.

Sampling valve 513 is used to analyze the composition of the reaction fluid after sampling to help determine the optimal spatial location and pore size of the circulating reaction fluid collection port in the circulating reaction fluid collection apparatus.

The reaction temperature measurement and control instrument 514 can send the measured temperature of the circulating reaction fluid to the control cabinet, and the controller of the control cabinet adjusts the cooling water flow of the cooling water pump according to the temperature so as to avoid overhigh or overlow temperature in the sub-tank. The control and regulation of the part belong to the conventional control and regulation method in the industrial field.

The collection of the circulating reaction fluid is realized by a circulating reaction fluid collecting device arranged in the reaction separating tank. The structure of the circulating reaction fluid collecting device is described with reference to FIGS. 4 to 8.

The circulating reaction fluid collecting device comprises a circulating reaction fluid collecting pipe 110 downwards passing through a third collecting pipe 903, and the bottom of the circulating reaction fluid collecting pipe 110 is connected with a pipe orifice at the bottom surface of a second collecting pipe 902 so as to be communicated with the first collecting pipe 901; the upper opening of the circulating reaction fluid collection pipe 110 is sleeved on a funnel neck of a collection funnel 811, the upper edge of the collection funnel 811 is fixedly connected with a lower disc 810 through a countersunk head 812, the lower end of the collection funnel 811 is inserted into the circulating reaction fluid collection pipe 110, and the collection funnel 811 is positioned at the joint of the upper truncated cone section 101 and the cylindrical section 100. The lower disk 810 is provided with an upper disk 820 which is coaxial with the lower disk 810 in a fitting manner and has the same diameter as the lower disk, the upper disk 820 is provided with two upper strip-shaped holes 821 which take the axis as a symmetric center, the lower disk 810 is provided with two lower strip-shaped holes 815 which take the axis as the symmetric center, the radius of each strip-shaped hole is gradually increased along the radial direction of the disk where the hole is located, and the shape of the upper strip-shaped hole 821 on the upper disk 820 and the shape of the lower strip-shaped hole 815 on the lower disk 810 are mirror images of each other by using the axial surface (namely, the vertical surface where the axis is located.

As shown in fig. 7, fig. 7(a) is a top view of the lower disk 810, fig. 7(b) is a top view of the upper disk 820, the state diagram of fig. 7(c, 0 °) is obtained by superposing fig. 7(a) and fig. 7(b), at this time, the overlapped part of the upper strip-shaped hole 821 and the lower strip-shaped hole 815 forms the cyclic reaction fluid collecting port 800, when the upper disk 820 rotates 76 ° relative to the lower disk 810, the overlapped state of the strip-shaped holes of the two disks is shown in fig. 7(d, 76 °), it can be seen that the radial position and size of the cyclic reaction fluid collecting port 800 are changed, when the upper disk 820 rotates to 152 ° relative to the lower disk 810, the overlapped state of the strip-shaped holes of the two disks is shown in fig. 7(e, 152 °), it can be seen that the radial position and size of the cyclic reaction fluid collecting port 800 are further changed, so that the overlapped state of the two strip-shaped holes of the two disks is adjusted by, the radial position of the circulating reaction fluid collection port 800 can be adjusted to meet the collection requirements of reaction products of different reactions, and the change of the radial position of the circulating reaction fluid collection port 800 can bring about the change of the size of the circulating reaction fluid collection port 800. The rotation of the upper disc 820 needs to be controlled by a circulating reaction fluid collecting and adjusting device at the top of the sub-reaction tank. Note that fig. 7(c, 0 °) schematically shows an initial radial position of the upper disc 820 with respect to the lower disc 810.

Furthermore, the upper opening of the circulating reaction fluid collection tube 110 is an outward-expanding bell-mouth to reduce the positioning requirement when the collection funnel 811 is inserted, and a drainage opening 814 is formed at one side of the bell-mouth, so that the redundant liquid in the circulating reaction fluid collection tube 110 can flow back to the reaction cavity of the distribution tank through the drainage opening 814.

Further, in consideration of the difference in the composition of the reaction fluid at different height positions in the separate reaction tank, it is necessary to axially adjust the position of the circulating reaction fluid collection port 800 in order to collect the most suitable reaction fluid. The magnitude of the axial adjustment should not exceed the length of the socket between the funnel neck of collection funnel 811 and collection tube 110 of the circulating reaction fluid to prevent disengagement of collection tube 110 and collection funnel 811. Axial adjustment of the position of the circulating reaction fluid collection port 800 also needs to be accomplished by a circulating reaction fluid collection adjustment device.

The structure of the circulating reaction fluid collecting and adjusting device is shown in fig. 4-6, the circulating reaction fluid collecting and adjusting device is arranged above the gas collecting and separating pipe 330 through a bracket, and the circulating reaction fluid collecting and adjusting device further comprises an inner composite transmission rod 107, an outer composite transmission rod 107, an axial movement driving mechanism 716 and a rotation driving mechanism 724; the inner and outer composite transmission rod 107 is composed of an inner transmission rod 710 and an outer transmission rod 720 which can synchronously move axially and rotate relatively; the inner driving rod 710 is sleeved in the rod cavity of the outer driving rod 720, the lower end of the inner driving rod 710 extends out and penetrates through the central hole of the upper disc 820 to be fixed at the center of the lower disc 810, and the lower end of the outer driving rod 720 is fixed on the upper surface of the upper disc 820. The inner and outer composite transmission rods 107 are arranged through the gas collecting and separating pipe 330. The gap between the outer transmission rod 720 and the central hole of the bottom plate of the bracket is dynamically sealed by an outer transmission rod shaft sealing part 721 sleeved on the outer transmission rod 720, and the outer transmission rod shaft sealing part 721 is fixed on the bottom plate of the bracket through screws.

The upper end of the inner driving rod 710 is provided with an external thread section 713 extending out of the outer driving rod 720, the external thread section 713 is provided with a key slot so as to be connected with the bracket through a rotation stop key 715, the rotation of the inner driving rod 710 can be limited in the process that the inner driving rod 710 axially moves, and the upper part of the inner driving rod 710 is guided to axially move through the matching of the key and the key slot. The external thread section 713 is further in threaded connection with a central hole of a first worm wheel 714 to form a screw-nut structure, the first worm wheel 714 is rotatably arranged at the top of the bracket, a first worm in matching connection with the first worm wheel 714 is horizontally arranged at the top of the bracket, and the first worm is connected with an axial movement driving mechanism 716; a second worm gear 722 is sleeved outside the outer transmission rod 720, the second worm gear 722 is in rotational connection with a guide rail fastener 723, a second worm in matching connection with the second worm gear 722 is horizontally arranged on the guide rail fastener 723, the second worm is driven by the rotary driving mechanism 724, and the guide rail fastener 723 is slidably mounted on a vertical guide rail 725 of the bracket; a positioning pin 712 is further arranged below the external thread section 713 of the inner driving rod 710, the positioning pin 712 abuts against the upper surface of an inner driving rod shaft seal 711 on the guide rail fastener 723, the inner driving rod shaft seal 711 is sleeved on the inner driving rod 710 and fixed on the guide rail fastener 723 through a screw, and dynamic sealing is performed between the inner driving rod 710 and the guide rail fastener 723.

The rotary driving mechanism 724 and the axial movement driving mechanism 716 can both adopt servo motors, when the servo motor drives the second worm to rotate, the second worm drives the second worm wheel 722 to rotate, and further drives the outer transmission rod 720 to rotate, so that the upper disc 820 rotates relative to the lower disc 810, and the adjustment of the radial position of the circulating reaction fluid acquisition port 800 is realized; when another servo motor drives the first worm to rotate, the first worm drives the first worm wheel 714 to rotate, the first worm wheel 714 drives the inner transmission rod 710 to move up and down axially through the matching of the outer thread section 713, when the first worm wheel 714 moves up, the lower disc 810 pushes the upper disc 820 and the outer transmission rod 820 to synchronously move up, and when the first worm wheel moves down, the positioning pin 712 pushes the guide rail fastener 723 to drive the outer transmission rod 720 to move down, so that the adjustment of the axial position of the circulating reaction fluid collection port 800 in the reverse separating tank is realized. After the radial position and the axial position are respectively adjusted, the adjustment of the spatial position of the circulating reaction fluid collecting port 800 can be realized.

The structure of the slag-containing fluid collecting device 600 will be described with reference to fig. 1, 3 and 8. As shown in fig. 1, 3 and 8, the sediment trap 600 comprises a connecting pipeline connected with the third collecting pipe 903, one end of the connecting pipeline is connected with a sediment-containing fluid tangential outlet 911 on the side surface of the third collecting pipe 903, the other end of the connecting pipeline is connected with a sediment tank tangential inlet 613 on the tank body of the sediment tank 612, a sediment-containing fluid outlet switch valve 610 is installed on one end of the connecting pipeline close to the distribution tank, and a sediment tank inlet switch valve 611 is installed on one end close to the sediment tank 612. The top and middle cylindrical tanks of the sediment tank 612 are connected through a tank body fastener 616, a reaction liquid collecting pipe is inserted into a center hole in the top of the tank body, a connecting ring is arranged on the outer side of the reaction liquid collecting pipe, the connecting ring is fixedly connected with a flange on the top of the tank body, one end of the reaction liquid collecting pipe, which extends into the sediment tank 612, is provided with a bell mouth with a convergent opening, which is used as a reaction liquid collecting port 614, one end of the reaction liquid collecting pipe, which is positioned outside the sediment tank 612, is connected and sealed with an end cover through a reaction liquid collecting pipe fastener 617, a reaction liquid tangential outlet 618 is arranged on the side surface of the reaction liquid collecting pipe, an outlet pipe is arranged on the reaction liquid tangential outlet 618, the outlet pipe is respectively connected with a reaction liquid sampling valve 620 and a return pipe through a tee joint, the return pipe is connected with a tee joint branch pipe 511 of. In order to observe the precipitation condition in the slag settling tank 604, a slag settling tank sight glass 615 is arranged at the upper part of the tank body, and a cleaning switch valve 621 is arranged at the bottom of the tank body so as to discharge the precipitation in the tank.

The slag-containing fluid containing solid particles enters the slag settling tank 612 through the third collecting pipe 903, and the supernatant after settling can enter the return pipe along the reaction liquid collecting pipe, and is converged into the circulating reaction fluid of the circulating reaction fluid collecting device 500, and is sent to the sub-reaction tank together to participate in the reaction again.

The feeding of the partial reaction tank and the circulation of the reaction liquid according to the present invention will be described with reference to FIGS. 1 and 2.

FIG. 2 shows the distribution and connection of the individual nozzle pipes and the individual inlets for the circulating reaction fluid in the cylindrical section of the partial reverse tank in a top view. In fig. 2, there are 4 nozzle pipes, which are respectively a nozzle pipe i 201, a nozzle pipe ii 202, a nozzle pipe iii 203 and a nozzle pipe iv 204, and there are 4 circulating reaction fluid inlets above each nozzle pipe, which are respectively a circulating reaction fluid inlet i 501, a circulating reaction fluid inlet ii 502, a circulating reaction fluid inlet iii 503 and a circulating reaction fluid inlet iv 504.

The acetaldehyde as a reaction raw material is divided into four paths, enters the partial reaction tank through 4 nozzle pipes along the tangential direction, and is preheated by a heat exchanger before the acetaldehyde enters the partial reaction tank to participate in the reaction, so that four heat exchangers are also needed, namely a heat exchanger I213, a heat exchanger II 214, a heat exchanger III 414 and a heat exchanger IV 243.

In the first way of acetaldehyde feeding, exit linkage is gone all the way to I201 nozzle pipes and I heat exchanger I, and I import of the first way of heat exchanger is connected with I210 acetaldehyde storage tanks through plunger pump I211, is equipped with I first import ooff valve 212 of heat exchanger all the way in I first import position of heat exchanger, sets up I first export ooff valve 214 of heat exchanger all the way in I first export position of heat exchanger, sets gradually I215 of acetaldehyde flow measurement and control appearance and first check valve 216 between I201 nozzle pipes and I214 of I first export ooff valve 214 of heat exchanger all the way. The first shunt pipe 517 of the circulating reaction fluid collecting device 500 is connected with the second inlet 217 of the heat exchanger I, and the second outlet of the heat exchanger I is connected with the circulating reaction fluid inlet I501 through a centrifugal fan I521.

In the second path of acetaldehyde feeding, a nozzle pipe II 202 is connected with a first path outlet of a heat exchanger II, a first path inlet of the heat exchanger II is connected with an acetaldehyde storage tank II 220 through a plunger pump II 221, a first path inlet switch valve 222 of the heat exchanger II is arranged at the position of the first path inlet of the heat exchanger II, a first path outlet switch valve 224 of the heat exchanger II is arranged at the position of the first path outlet of the heat exchanger II, and an acetaldehyde flow measuring and controlling instrument II 225 and a second one-way valve 226 are sequentially arranged between the first path outlet switch valve 224 of the heat exchanger II and the nozzle pipe II 202. And a second shunt pipe 518 of the circulating reaction fluid collecting device 500 is connected with a second inlet 227 of the heat exchanger II, and a second outlet of the heat exchanger II is connected with a circulating reaction fluid inlet II 502 through a centrifugal fan II 522.

In the fourth path of acetaldehyde feeding, a nozzle pipe IV 204 is connected with a first path outlet of a heat exchanger IV, a first path inlet of the heat exchanger IV is connected with an acetaldehyde storage tank IV 240 through a plunger pump IV 241, a first path inlet switching valve 242 of the heat exchanger IV is arranged at the position of the first path inlet of the heat exchanger IV, a first path outlet switching valve 244 of the heat exchanger IV is arranged at the position of the first path outlet of the heat exchanger IV, and an acetaldehyde flow measuring and controlling instrument IV 245 and a fourth one-way valve 246 are sequentially arranged between the first path outlet switching valve 244 of the heat exchanger IV and the nozzle pipe IV 204. The fourth flow-dividing pipe 520 of the circulating reaction fluid collecting device 500 is connected with the second inlet 247 of the heat exchanger IV, and the second outlet of the heat exchanger IV is connected with the circulating reaction fluid inlet IV 504 through a centrifugal fan IV 524.

In the three paths, the reaction liquid flowing out of the sub-tank preheats acetaldehyde in the corresponding heat exchanger, so that the temperature of a reaction system can be prevented from being greatly fluctuated due to low acetaldehyde temperature, the reaction liquid is cooled, and the reaction system can be prevented from being too high after entering the sub-tank again, so that certain cold energy is saved.

For the third path of acetaldehyde feeding, a nozzle pipe III 203 is connected with a second path outlet of a heat exchanger III, a second path inlet 417 of the heat exchanger III is connected with an acetaldehyde storage tank III 230 through a plunger pump III 231, a second path outlet switching valve 418 of the heat exchanger III is arranged at the position of the second path outlet of the heat exchanger III, and a switching valve 232, an acetaldehyde flow rate measuring and controlling instrument III 233 and a third one-way valve 234 are sequentially arranged between the second path outlet switching valve 418 of the heat exchanger III and the nozzle pipe III 203. The pipeline of the ethyl acetate collecting device is connected with the inlet of the first path of the heat exchanger III, the outlet of the first path of the heat exchanger III is connected with an ethyl acetate storage tank 416, and the collected ethyl acetate preheats acetaldehyde in the heat exchanger III 414. The third shunt tube 519 of the circulating reaction fluid collecting device 500 is connected with the circulating reaction fluid inlet III 503 through the centrifugal fan III 523.

The circulating reaction fluid entering the sub-reaction tank enters tangentially under the action of the centrifugal fan, so that kinetic energy can be supplemented to the reaction fluid in the sub-reaction tank and the reaction fluid can participate in the reaction again.

The invention also controls various devices in the reaction equipment through the control cabinet 11, and obtains relevant information, such as an ethyl acetate content tester, a flow rate tester, a pressure tester, a reaction temperature tester, a centrifugal fan, a cooling water pump and the like, which belong to the conventional technology in the field, so too much description is not provided.

The method of operation of the apparatus of the present invention is further described below with reference to the accompanying drawings.

1. As shown in fig. 1, 2 and 3, a discharge valve 317 at the bottom of the bisection tank 313, an ethyl acetate vapor switch valve 410 connected with the second collecting pipe 903, a reflux switch valve 619, a reaction liquid sampling valve 620 and an acetaldehyde vapor sampling valve 326 are closed; all other valves are in an open state;

2. as shown in fig. 10, a main power supply 1103 of the control cabinet 11 is turned on, a setting button for setting the pressure measurement and control instrument 311 on the control cabinet 11 is pressed, the operating pressure of the partial-reaction tank is set, the partial-reaction tank is sprung up by pressing the button once again, that is, the pressure measurement state is entered, the measurement and control temperature of the reaction temperature measurement and control instrument 514 is set to (79 ± 0.5) ° c by the same method, four channels are equally divided according to the total acetaldehyde flow, the flow of four acetaldehyde flow measurement and control instruments (215, 225, 233, 245) are set by the same method, the flow of the circulating reaction fluid flow measurement and control instrument 515, the flow of the acetaldehyde steam flow measurement and control instrument 323, the flow of the ethyl acetate steam flow measurement and control instrument 413, the flow of the cooling water flow measurement and control instrument 114 is set by the same method, and finally the position reading of the circulating reaction fluid collection port 800 in the circulating loop is set to be "10 cm, and the inlets of four plunger pumps (211, 221, 231, 241) are connected with a 'triethanolate aluminum-ethyl ester' solution (namely a catalyst);

3. connecting a sampling valve 513 with a nitrogen container, opening the nitrogen container to fill nitrogen into the sub-reaction tank, simultaneously opening four centrifugal fans (521-524), discharging air (mainly for discharging oxygen) in the sub-reaction tank through a pipeline of the slag-containing fluid collecting device 600 and a cleaning switch valve 621 of the slag settling tank 612, detecting at an outlet of the cleaning switch valve 621 at the bottom of the slag settling tank 612 by using an oxygen detector, and closing the cleaning switch valve 621 when the oxygen cannot be detected; then opening a reflux switch valve 619 and a discharge valve 317 of the two-part tank 313, detecting 'water vapor' by using blue silica gel at the outlet of the discharge valve 317 of the two-part tank 313, and closing the discharge valve 317 of the two-part tank 313 until the blue silica gel does not change color within 2 min; an ethyl acetate steam switch valve 410 connected with the second collecting pipe 903 is opened, oxygen detector detects oxygen at a first outlet switch valve 415 of the heat exchanger III, until the oxygen is not detected, a sampling valve 513 is closed, and the connection between the sampling valve 513 and a nitrogen container is disconnected;

4. starting a power supply of the cooling water pump 113, starting four plunger pumps (211, 221, 231 and 241), pumping the 'aluminum triethoxide-ethyl ester' solution into the secondary reaction tank, observing the liquid level of the liquid level meter 111, immediately closing the plunger pumps after the liquid level reaches a set liquid level height, connecting inlet pipes of the plunger pumps with corresponding acetaldehyde storage tanks, and restarting the plunger pumps;

5. as the main reaction proceeds, two side reactions occur, namely, acetaldehyde acetal monoethanol (acetal for short) and water are further generated, because the boiling points of the substances are all higher than the temperature set value (79 +/-0.5) DEG C of the reaction temperature measuring and controlling instrument 514, most of them will remain in the "aluminum-ethyl-triethoxide" solution, increasing its volume, drifting the liquid level of the level gauge 111 upward, therefore, the temperature setting of the reaction temperature monitor 514 should be gradually increased to 85, 90, 95 deg.C … … to (101 + -0.5) deg.C, meanwhile, the flow set value of the ethyl acetate steam flow measuring and controlling instrument 413 is properly increased (about 1% of the original flow is increased every time), the specific increment is determined according to the liquid level of the liquid level meter 111, the liquid level is adjusted more and less when the liquid level is lower, and the purpose is to keep the liquid level of the liquid level meter 111 in an observable range;

6. when the temperature set value of the reaction temperature measuring and controlling instrument 514 is stabilized at (101 +/-0.5) DEG C, the flow of the ethyl acetate steam flow measuring and controlling instrument 413 is recovered to the initial set value, and the cooling water pump 113 is intermittently started and stopped, the reaction system can be considered to be in an 'equilibrium reaction' state, and at the moment, the flow of the cooling water flow measuring and controlling instrument 114 is adjusted, so that the starting time of the cooling water pump 113 is longer than the stopping time of the cooling water pump 113;

7. when the reaction state is stable, if the reading of the ethyl acetate content tester 412 is lower than 99%, indicating that the impurity is "hemiacetal" or "acetal", adjusting the flow of the ethyl acetate steam flow rate tester 413 to force the hemiacetal "or" acetal "to enter the sediment tank 612 through the third collecting pipe 903, and after separating from the sediment, the hemiacetal" or "acetal" enters the reaction separation tank again through the reaction liquid tangential outlet 618 and the reaction liquid reflux valve 619 to participate in the reaction; when the reading of the ethyl acetate content tester 412 is higher than 99%, the product ethyl acetate is collected;

8. if the liquid level of the liquid level meter 111 continuously rises, part of the product should be discharged from the reaction liquid sampling valve 620 so as to maintain the liquid level of the liquid level meter 111 always in an observable range, and in fact, if the liquid level of the liquid level meter 111 is too high, even too high to be observed, the result is that the reading of the ethyl acetate content meter is necessarily reduced obviously;

9. when the liquid level of the water reaches the middle part of the view port 316, the discharge valve 317 at the bottom of the two-part tank 313 is opened to discharge the water;

10. the raw materials often bring a small amount of inert solid particles, a small amount of insoluble substances can be generated in the reaction, and as the reaction liquid in the reaction separating tank rotates ceaselessly, the density of the solid particles is the highest, so the solid particles can only be finally concentrated at the bottom of the sediment tank 612, when the solid is observed through the sediment tank sight glass 615, under the condition of non-stop production, the inlet switch valve 611 and the reaction liquid reflux valve 619 of the sediment tank are closed, the tank body fastener 616 of the sediment tank 612 or the reaction liquid collecting pipe fastener 617 are opened, and the equipment is recovered after the sediment in the solid is removed;

11. sampling is carried out from a sampling valve 513, and gas chromatography analysis is carried out, wherein the gas chromatography determination conditions are as follows: capillary column (30m × 0.25mm × 0.33 μm), column temperature 120 deg.C, stationary liquid 5% diphenyl (95%) dimethyl polysiloxane, mobile phase hydrogen, air as internal standard, and detector as thermal conductivity detector. Adjusting the position of the circulating reaction fluid collecting port 800 according to the result to make the circulating reaction fluid only contain a large amount of acetaldehyde and a very small amount of ethanol as the best;

12. in the above operation, if the relief valve 315 is opened due to misoperation or abnormal response in any step, the main power supply 1103 of the control cabinet 11 should be immediately closed, the reason should be carefully checked, the overflowed liquid or gas should be recovered, and the machine should be tested after correction;

13. when the production is suspended, the power supply of each plunger pump is turned off, then the cooling jacket inlet switch valve 109, the water vapor switch valve 310, the acetaldehyde vapor switch valve 321, the ethyl acetate vapor switch valve 410, the first outlet switch valve 415 of the heat exchanger III, the slag-containing fluid outlet switch valve 610 and the circulating reaction fluid switch valve 510 of the sub-tank are turned off, and then the main power supply 1103 is turned off.

14. And (3) emptying the sub-tank and closing all valves in principle after long-term shutdown, and repeating the steps 1-12 when restarting.

The above apparatus structure and the operation method thereof will be described below with reference to an embodiment.

Example 1: the position of the collection port for the recycled reaction fluid in this example is represented by readings on the axial displacement drive mechanism and the rotary drive mechanism, respectively: axial 10cm and radial 120 deg. The data are based on corresponding starting positions, which are explained in the following steps.

Firstly, equipment type selection

1. Distribution tank key data: the diameter of the cylindrical section 100 is 3m, the height is 0.75m, the height of the upper round platform section 101 is 0.9m, the height of the lower round platform section 102 is 0.6m, and the volume of the return tank is 8.84m 3. The diameter of the water vapor collection port 331 is 9.84cm, the diameter of the acetaldehyde vapor collection port 332 is 15.21cm, the diameter of the first barrier disc 904 is 49.05cm, the width of the first collection slit 907 is 3.24cm, the diameter of the second barrier disc 905 is 30.23cm, the width of the second collection slit 909 is 5.40cm, and the width of the third collection slit 910 is 0.5 cm.

2. Plunger pump power and pipe diameter: the total number of plunger pumps (7.65L/min, power 500w) for feeding acetaldehyde was 4, the inner diameters of the plunger pump pipes were 8mm, and the inner diameters of the nozzle outlets were 2.5 mm.

3. Heat balance, cooling water circulation power and pipeline

In this example, 5.82kg of ethyl acetate was produced per minute. The reactants and products have a heat capacity from 25 ℃ to 105 ℃ and the heat absorbed or released by their heat capacities is negligible small relative to their heat of reaction, heat of vaporization (or heat of condensation). The cooling load can be calculated from this. The change in the heat of the reactants and products in the reaction system is shown in FIG. 14.

In FIG. 14,. DELTA.H₁＝-13686＝ΔH₂+ΔH₃+ΔH₄＝3434+ΔH₃2239, the cooling amount is Δ H₃＝-13686-3434+2236＝-8013(kJ/min)；

1kg of water, heat Q can be taken away at 101 → 25 ℃: when Q is 4.18J/(g. degree) × 1000/1000 × (101-25) × 317.68(kJ/kg), the flow rate of the cooling water is:

ΔH₃8013/317.68-46.84 (kg/min) -2.81 ton/h-2.81 m 3/h.

Considering that the cooling water flow of the invention is controlled by the reaction temperature measuring and controlling instrument, in order to prevent unexpected rapid temperature rise, the cooling water pump selects 10.0m³H, power of 1.10kw, and water pipe internal diameter: the suction pipe is 65mm, and the calandria is 50 mm.

4. Reaction temperature, pressure and ratio

The reaction temperature is 101 ℃, the reaction pressure is 0.1MPa, and the flow of each substance in the reaction system is as follows:

wherein the catalyst ethyl ester solution is a mixed solution of aluminum triethoxide and ethyl acetate.

5. Through the calculation of material and dynamic energy balance, the specification of the centrifugal fan is obtained: in the reaction system in the sub-reaction tank of the embodiment, when the dynamic energy balance is achieved, the linear speed of the reaction fluid along the inner wall of the sub-reaction tank is 20 m/s. The kinetic energy carried by the reactant acetaldehyde entering the partial reaction tank is calculated to be very small and negligible relative to the kinetic energy carried by the fluid discharged from the water vapor collection port 331, the acetaldehyde vapor collection port 332, the second collection pipe 902, the third collection pipe 903 and the circulating reaction fluid collection port 800. In this example, the mass of water vapor discharged from the water vapor collection port 331 was 0.00041kg/s, the mass of incompletely reacted acetaldehyde vapor discharged from the acetaldehyde vapor collection port 332 was 0.002kg/s, the mass of ethyl acetate produced by the second collection pipe 902 was 0.097kg/s, and the mass of slag-containing fluid (mainly acetal) discharged from the third collection pipe 903 was 0.0026kg/s, and the mass of circulating reaction fluid discharged from the circulating reaction fluid collection port 800 was not set to m kg/s, and the linear velocity was V m/s. According to the formula (4), a

Wherein, i is water vapor (abbreviated as 'steam'), unreacted acetaldehyde (abbreviated as 'residual aldehyde'), ethyl ester, slag-containing fluid (abbreviated as 'slag-containing'), and M_iIs the mass of the substance i in kg/s, r₁Is the maximum radius of the collection opening or the liquid receiving pipe, and the unit is m, r₂Is the minimum radius of the collection opening or the liquid receiving pipe, and has the unit of m, R is the radius of the cylindrical section of the sub-reverse tank, and has the unit of m, v₀At 20m/s, the linear velocity at the inner wall of the cylindrical section of the partial reverse tank, it should be noted that m is the mass of the circulating fluid_{Circulation of}And is a function of the radius of the circulating fluid collection port 800, so (9) is not suitable for circulating a reaction fluid, and thus

Our aim is through E_Into＝E_{Row board}Calculating m_{Circulation of}If it is decided to let V_Into250m/s, in relation to formula (10), then

(11) In the formula, V_{Circulation of}Although it can be calculated by the formula (4), r is considered_{Circulation of}Smaller V_{Circulation of}The larger the diameter, the less reasonable is simply taking the average of the inner and outer radii of the circulating reaction fluid collection ports. To get it for

r_{Circulation of}＝r_{Minimum size}+0.2×(r_{Maximum of}-r_{Minimum size})＝24.66+0.2×(32.83-24.66)＝26.29(cm)

According to the formula (4) above,

thus, the formula (11) can be represented as

Can be solved by the formula (12), m_{Circulation of}The kinetic energy which needs to be supplemented theoretically by substituting the formula (12) left end scorable anti-tank into 1.96kg/s (the reduced gas volume is 2423.07m3/h) is 61.21 kW. Considering the efficiency of the centrifugal fan and the resistance consumption in the sub-reverse tank,therefore, 4 centrifugal fans for supplying motive energy to the distribution tank are needed, the power of each centrifugal fan is 30kw, the flow rate is 605.77m3/h, and the linear speed is 250 m/s.

According to the above parameters and calculation method, the linear speed of the water vapor at 3.24cm from the center of the water vapor collection port 331 is 925.16m/s, and the centrifugal force generated thereby is 269.34 ten thousand times the gravity.

Second, the operation steps

Closing a discharge valve 317 at the bottom of the two-part tank 313, an ethyl acetate steam switch valve 410, a reflux switch valve 619, a reaction liquid sampling valve 620 and an acetaldehyde steam sampling valve 326 which are connected with a second collecting pipe 903; all the other valves are in an opening state;

2. setting the opening pressure of the pressure release valve 315 to be 0.2 Mpa; starting a main power supply 1103 of the control cabinet 11, pressing a setting button on the control cabinet 11 for setting the pressure measurement and control instrument 311, setting the working pressure of the distribution tank to be 0.1-0.12 MPa, pressing the button again to bounce, and entering a pressure measurement state; setting the reaction temperature of the reaction temperature measuring and controlling instrument 514 to be (79 +/-0.5) DEG C by the same method, dividing four paths according to the total acetaldehyde flow, dividing the total acetaldehyde flow into four portions, namely feeding acetaldehyde by four paths, setting the flow of four acetaldehyde flow measuring and controlling instruments (215, 225, 233 and 245) to be 1.50kg/min by the method, and setting the flow of the circulating reaction fluid flow measuring and controlling instrument 515 to be 2423m by the same method³The flow rate of the/h acetaldehyde steam flow rate measuring and controlling instrument 323 is 4.92m³The flow rate of the ethyl acetate steam flow measuring and controlling instrument 413 is 119.41m³The flow of the cooling water flow measuring and controlling instrument 114 is 2.81m³Finally, setting the position reading of a circulating reaction fluid collecting port 800 in a circulating loop as 'axial 15cm, radial 130 degrees', adjusting the position reading according to the reaction condition, and connecting inlets of four plunger pumps (211, 221, 231 and 241) with 'aluminum triethoxide-ethyl ester' solution (namely catalyst);

3. connecting a sampling valve 513 with a nitrogen container, opening the nitrogen container to fill nitrogen into the sub-reaction tank, simultaneously opening four centrifugal fans (521-524), discharging air (mainly for discharging oxygen) in the sub-reaction tank through a pipeline of the slag-containing fluid collecting device 600 and a cleaning switch valve 621 of the slag settling tank 612, detecting at an outlet of the cleaning switch valve 621 at the bottom of the slag settling tank 612 by using an oxygen detector, and closing the cleaning switch valve 621 when the oxygen cannot be detected; then opening a reflux switch valve 619 and a discharge valve 317 of the two-part tank 313, detecting 'water vapor' by using blue silica gel at the outlet of the discharge valve 317 of the two-part tank 313, and closing the discharge valve 317 of the two-part tank 313 until the blue silica gel does not change color within 2 min; an ethyl acetate steam switch valve 410 connected with the second collecting pipe 903 is opened, oxygen detector detects oxygen at a first outlet switch valve 415 of the heat exchanger III, until the oxygen is not detected, a sampling valve 513 is closed, and the connection between the sampling valve 513 and a nitrogen container is disconnected;

4. starting a power supply of the cooling water pump 113, starting four plunger pumps (211, 221, 231 and 241), pumping the 'aluminum triethoxide-ethyl ester' solution into the secondary reaction tank, observing the liquid level of the liquid level meter 111, immediately closing the plunger pumps after the liquid level reaches a set liquid level height, connecting inlet pipes of the plunger pumps with corresponding acetaldehyde storage tanks, and restarting the plunger pumps;

5. as the main reaction proceeds, two side reactions occur, i.e. acetaldehyde acetal-ethanol (abbreviated as hemiacetal) is produced, and acetaldehyde acetal-ethanol (abbreviated as acetal) and water are further produced, because the boiling points of the substances are all higher than the temperature setting value (79 +/-0.5) DEG C of the reaction temperature measuring and controlling instrument 514, most of the substances are left in the solution of the triethanol aluminum-ethyl ester, so that the volume of the solution is increased, meanwhile, the boiling point of the solution of the triethanol aluminum-ethyl ester is also higher than the boiling point of the solution of the pure ethyl ester according to the Henry's law, so the liquid level of the liquid level meter 111 is slowly drifted upwards, therefore, the temperature setting values of the reaction temperature measuring and controlling instrument 514 should be gradually increased to 85, 90 and 95 ℃ … … to (101 +/-0.5) DEG C, and the flow setting value of the ethyl acetate vapor flow measuring and controlling instrument 413 should be appropriately increased (about 1% of the original flow rate, the specific increment is determined according to the liquid level of the liquid level meter 111, and the liquid level is adjusted more and less when the liquid level is low, so as to keep the liquid level of the liquid level meter 111 in an observable range;

6. when the temperature set value of the reaction temperature measuring and controlling instrument 514 is stabilized at 101 +/-0.5 ℃, the flow of the ethyl acetate steam flow measuring and controlling instrument 413 is recovered to the initial set value, and the cooling water pump 113 is intermittently started and stopped, the reaction system can be considered to be in an 'equilibrium reaction' state, and at the moment, the flow of the cooling water flow measuring and controlling instrument 114 is adjusted, so that the starting time of the cooling water pump 113 is longer than the running stopping time of the cooling water pump 113; if the plunger pump II 221 and the plunger pump IV 241 are found to be started and stopped frequently, the pressure of the pressure measuring and controlling instrument needs to be adjusted to be 0.15MPa, and then the plunger pump II 221 and the plunger pump IV 241 can be almost in a continuous operation state;

7. when the reaction state is stable, when the reading of the ethyl acetate content meter 412 is 96.1%, and is less than 99%, it indicates that there is a byproduct of "hemiacetal" or "acetal" mixed in, the flow rate of the ethyl acetate vapor flow rate meter 413 needs to be adjusted to 119.1m³H, after 10min, the reading of the ethyl acetate content measuring and controlling instrument is 97.51%, and when the flow of the ethyl acetate steam flow measuring and controlling instrument 413 is further adjusted to 118.3m³After 10min, if the reading of the ethyl acetate content measuring and controlling instrument 413 is 99.11%, the product ethyl acetate is required to be collected;

8. the byproduct acetal or hemiacetal enters the sediment tank 612 through the third collecting pipe 903, is separated from sediment, and then enters the reaction separation tank again through the reaction liquid tangential outlet 618 and the reaction liquid return pipe switch valve 619 to participate in the reaction; if the liquid level of the liquid level meter 111 continues to rise, part of the products (acetal and hemiacetal) should be discharged from the reaction liquid sampling valve 620 to maintain the liquid level of the liquid level meter 111 always within the observable range;

9. when the liquid level of the water reaches the middle part of the view port 316, the discharge valve 317 at the bottom of the two-part tank 313 is opened to discharge the water;

10. the raw materials often bring a small amount of inert solid particles, a small amount of insoluble substances can be generated in the reaction, and as the reaction liquid in the reaction separating tank rotates ceaselessly, the density of the solid particles is the highest, so the solid particles can only be finally concentrated at the bottom of the sediment tank 612, when the solid is observed through the sediment tank sight glass 615, under the condition of non-stop production, the inlet switch valve 611 and the reaction liquid reflux valve 619 of the sediment tank are closed, the tank body fastener 616 of the sediment tank 612 or the reaction liquid collecting pipe fastener 617 are opened, and the equipment is recovered after the sediment in the solid is removed;

11. sampling is carried out from a sampling valve 513, and gas chromatography analysis is carried out, wherein the gas chromatography determination conditions are as follows: capillary column (30m × 0.25mm × 0.33 μm), column temperature 120 deg.C, stationary liquid 5% diphenyl (95%) dimethyl polysiloxane, mobile phase hydrogen, air as internal standard, and detector as thermal conductivity detector. As shown in fig. 11, when peak 1 is an air peak, peak 2 is an ethyl acetate peak, peak 3 is an acetaldehyde peak, peak 4 is an ethanol peak, peak 5 is a water peak, and (t ═ 0min, h ═ 0mm) is used as a base point, the coordinates of peak 1, peak 2, peak 3, peak 4, and peak 5 are (1.49, 5.2), (14.48, 12.2), (18.49, 59.9), (22.98, 4.1), (28.00, 0.4), respectively. Their peak height ratios are: 1/2.32// 11.45/0.77/0.08. This indicates that, when a trace amount of water vapor enters the circulating reaction fluid, the axial reading of the circulating reaction fluid acquisition port should be reduced or the radial reading of the circulating reaction fluid acquisition port should be increased;

12. setting the axial reading of the position of the circulating reaction fluid collecting port 800 as Z, and taking the lowest point as 'Z is 0' as the starting point of axial movement; the radial reading is J, and "J ═ 0 °" in fig. 7(c) is taken as the starting point of the radial movement (i.e., rotation), then the position of the circulating reaction fluid collection port 800 is the point (Z ═ 15cm, J ═ 130 °), according to the setup of step 2. Starting from a point (Z15 cm, J130 °), the J value is fixed, and one point is measured every "1.0 cm" in Z value. Peak 5 was 0.15mm minimum when Z was 10.0 cm; then fix Z10.0 cm, gradually decrease the radial reading "every 5 ° and then every 2 °, 1 °" to find the point where peak 5 disappears, as shown in fig. 12, when (Z10 cm, J120 °), peak 5 essentially disappears, at which time the peak height ratio of acetaldehyde/ethyl acetate/ethanol is 1/0.218/0.069;

13. when the production is suspended, the power supply of each plunger pump is turned off, then the cooling jacket inlet switch valve 109, the water vapor switch valve 310, the acetaldehyde vapor switch valve 321, the ethyl acetate vapor switch valve 410, the first outlet switch valve 415 of the heat exchanger III, the slag-containing fluid outlet switch valve 610 and the circulating reaction fluid switch valve 510 of the sub-tank are turned off, and then the main power supply 1103 is turned off.

14. The long-term shutdown should in principle empty the knock-out pot and close all valves, and when restarting, the above steps should be repeated.

Example 2: compared with the example 1, the reaction temperature, the reaction pressure, the raw material ratio after the continuous reaction, the operation process, the space position of the circulating reaction fluid collecting port, the calculation method of the material balance and the dynamic energy balance and the gas chromatography analysis method are the same as the best state of the example 1, and the difference is that the total input amount of acetaldehyde is increased from 6.00kg/min to 6.4kg/min, and the catalyst ethyl ester solution does not need to be added. Accordingly, the measuring and controlling instrument for the material flow and the measuring and controlling instrument for the cooling water are reset as follows.

1. Ratio of reactants to product

Anhydrous acetaldehyde (97%) 6.40kg/min

Ethyl acetate (not less than 99%) 6.21kg/min

Acetal (95. + -. 0.2%) 0.166kg/min

2. According to the proportion of the step 1, dividing the total acetaldehyde flow into four paths, setting the four acetaldehyde flow measuring and controlling instruments to have the flow of 1.60kg/min, and setting the flow of the circulating reaction fluid flow measuring and controlling instrument 515 to be 2584m³The flow rate of the acetaldehyde steam flow rate measuring and controlling instrument 323 is 5.25m³The flow rate of the ethyl acetate steam flow measuring and controlling instrument 413 is 127.32m³The flow of the cooling water flow measuring and controlling instrument 114 is 3.04m³/h。

3. The liquid level of the liquid level meter 111 is closely observed, the liquid level is always kept in an observable range by the method of example 1, whether the reading of the ethyl acetate content tester meets the product requirement is closely observed, the running states of the plunger pump II 221, the plunger pump IV 241 and the cooling water pump 113 are closely observed, the water in the two-way tank 313 and the acetal product and the sediment in the sediment tank 612 are timely processed, and after the equipment runs stably, a sample is taken from the sampling valve 513 for gas chromatography analysis, and the result is shown in figure 13.

4. As can be seen from fig. 13, with an increase of 6.62% of the acetaldehyde charge, no chromatographic peak 5 of water vapor was still observed in the recycled reaction stream and the plant was able to operate normally, which indicates that example 2 is feasible.

The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those of ordinary skill in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.