阅读说明：本技术 一种强化液-液反应的装置和方法 (Device and method for enhancing liquid-liquid reaction ) 是由 杨强 李裕东 卢浩 刘懿谦 武世汉 代品一 于 2021-01-05 设计创作，主要内容包括：本发明提供了一种强化液液反应的装置,所述装置包括混合部分和反应器,所述混合部分包括进料三通和用于强化反应物混合的混合器,所述进料三通包括第一端口、第二端口和第三端口,其中第一端和第二端口分别用于反应物的进料,所述第二端口设置一喷射器,用于将其中一种反应物压缩剪切产生湍动能,通过喷射器喷射进入,所述第三端口与所述混合器通过法兰连接；所述反应器内部设有盘管式换热结构,用于液液反应时的热量交换。本发明还提供了利用所述装置的强化液液反应的方法,所述装置和方法具有结构紧凑、可连续反应、反应效率高的特点,通过强化反应物的混合而强化液液反应,适用于化工、制药、生物等液液反应领域。(The invention provides a device for enhancing liquid-liquid reaction, which comprises a mixing part and a reactor, wherein the mixing part comprises a feeding tee joint and a mixer for enhancing the mixing of reactants, the feeding tee joint comprises a first port, a second port and a third port, the first port and the second port are respectively used for feeding the reactants, the second port is provided with an ejector for compressing and shearing one of the reactants to generate turbulent kinetic energy, the turbulent kinetic energy is injected into the second port through the ejector, and the third port is connected with the mixer through a flange; and a coil pipe type heat exchange structure is arranged in the reactor and is used for heat exchange during liquid-liquid reaction. The invention also provides a method for strengthening liquid-liquid reaction by using the device, the device and the method have the characteristics of compact structure, continuous reaction and high reaction efficiency, the liquid-liquid reaction is strengthened by mixing the strengthened reactants, and the device and the method are suitable for the liquid-liquid reaction fields of chemical industry, pharmacy, biology and the like.)

1. An apparatus for enhancing liquid-liquid reaction, comprising a mixing section and a reactor, the mixing section comprising a feed tee for feeding reactants and a mixer for enhancing mixing of the reactants, wherein,

the feeding tee joint comprises a first port, a second port and a third port, wherein the first port and the second port are respectively used for feeding reactants, the second port is provided with an ejector and is used for compressing and shearing one of the reactants to generate turbulent kinetic energy, the turbulent kinetic energy is injected through the ejector and enters the mixer, and the third port is connected with the mixer through a flange;

the mixer comprises a cylindrical mixer shell, and a mixer inlet section, a mixer spiral section with a spiral structure with opposite rotation directions and a mixer outlet section are sequentially arranged in the mixer shell;

the reactor is internally provided with a coil tube type heat exchange structure for heat exchange during liquid-liquid reaction, and comprises a shell side inlet, a shell side outlet, a tube side inlet and a tube side outlet.

2. The apparatus of claim 1, wherein the injector comprises a cylindrical housing with an opening at one side and a hemispherical structure at the other side, the opening side of the housing is an inlet section of the injector, the injector is internally provided with a supporting structure, a flow guiding structure and a thimble structure which are connected with each other in sequence along the inlet section, and a jet orifice is arranged at one side of the hemispherical structure of the housing.

3. The apparatus for enhancing liquid-liquid reaction of claim 2 wherein said inlet section has a diameter d 1; the supporting structure comprises a cylindrical supporting rod and a hollow-out supporting frame which is connected with the supporting rod and the inner wall of the shell along the radial direction of the supporting rod outwards, and the diameter of the supporting rod is 1/4-1/2 of the diameter d1 of the inlet section; the flow guide structure comprises a cylindrical flow guide section and a truncated cone-shaped flow guide section with gradually reduced diameter, the diameter of the cylindrical flow guide section is 1/2-3/4 of the diameter d1 of the inlet section, the length of the cylindrical flow guide section is 1/4-3/4 of the diameter d1 of the inlet section, and the bottom angle alpha of the truncated cone-shaped flow guide section is 30-60 degrees; the thimble structure is a cylindrical structure, and the diameter of the thimble structure is 0.4-2 mm; the diameter of the jet orifice is 0.1-4.4mm, and the distance between the jet orifice inlet and the thimble structure is 1-10 mm.

4. The apparatus for enhancing liquid-liquid reaction of claim 1 wherein the mixer inlet section and mixer outlet section have the same diameter; a cylindrical supporting structure is arranged at the axis in the mixer; the mixer spiral section comprises a plurality of spiral sections, the spiral sections are sequentially and repeatedly arranged, and the repeated number n of the spiral sections is the mixing series; each stage of helical section comprises a first helical structure and a second helical structure, the rotation directions of the first helical structure and the second helical structure are opposite, and helical blades of the first helical structure and the second helical structure are connected with the inner wall of the mixer shell and the supporting structure; and a middle section is arranged between the adjacent spiral structures.

5. The apparatus for enhancing liquid-liquid reaction of claim 4, wherein the overall length of the mixer is L, the lengths of the first helical structure and the second helical structure are 1/8 n-1/2 n of the length L of the mixer, and the length of the middle section is 1/8 n-1/2 n of the length L of the mixer.

6. A method for enhancing liquid-liquid reactions using the apparatus of any of claims 1 to 5, characterized in that the method comprises the steps of:

(1) reactants enter the feed tee joint from the first port and the second port respectively, wherein one reactant enters the feed tee joint from the injector of the second port after being subjected to compression shearing, and the reactants are preliminarily mixed in the feed tee joint;

(2) the reactants which are preliminarily mixed enter a mixer and pass through a spiral section of the mixer with a spiral structure with opposite rotation directions, so that the dispersion degree of the two phases is improved, and the mixing is strengthened;

(3) the mixed reactants enter a reactor for reaction and exchange heat with the heat exchange water in a countercurrent way, wherein the reactants flow from bottom to top, and the heat exchange water flows from top to bottom.

7. The method for enhancing liquid-liquid reaction according to claim 6, wherein the mixing part is arranged outside or inside the reactor, when the mixing part is arranged outside the reactor, reactants enter the reactor from a shell side inlet, flow from bottom to top along the shell side, are discharged from a shell side outlet after reaction, and heat exchange water enters the reactor from a tube side inlet, flows from top to bottom along the tube side, and flows from the tube side outlet; when the mixing part is arranged in the reactor, reactants enter the reactor when entering the first port and the second port of the feeding tee joint, flow from bottom to top along the tube pass after flowing out of the mixer, are discharged from the tube pass outlet after reaction, and heat exchange water enters the reactor from the shell pass inlet, flows from top to bottom along the shell pass and flows from the shell pass outlet.

8. The method for enhancing liquid-liquid reaction according to claim 6, wherein the reactants involved in the reaction enter the feed tee in a contact manner of convection, forward flow or counter flow.

9. The method for enhancing liquid-liquid reaction of claim 6, wherein the mixing part is connected in parallel by a single ejector or a plurality of ejectors, and is used for adjusting the ratio of the flow rates of the reactants or adjusting the treatment capacity of the reactor according to the actual requirement.

Technical Field

The invention belongs to the field of liquid-liquid reaction of chemical industry, pharmacy, biology and the like, and particularly relates to a device and a method for strengthening liquid-liquid reaction.

Background

The liquid-liquid reaction refers to a reaction of generating another substance in the process of mixing and contacting two liquids, and has wide application in the fields of chemical industry, pharmacy, biology and the like. For some reactions with slower reaction rate, the mixing degree of liquid-liquid two phases directly affects the reaction rate, and the reactors commonly used in industry at present, such as batch type reaction kettle, add one reactant into the reaction kettle, start the stirring paddle and then add the second reactant until the reaction is finished, but the reaction time of the liquid-liquid mixing reaction is long, the yield is low, the continuous production cannot be realized, and the energy consumption is high.

CN206027667U proposes a liquid-liquid reaction apparatus, in which two reactants are mixed and reacted by a mixing pump, and the apparatus for liquid-liquid mixing by the continuous operation of the mixing pump has the disadvantage of high energy consumption, especially for high viscosity fluid; CN106423002A proposes an impinging stream reaction and separation integrated device and method for a liquid-liquid reaction system, in which two liquids are mixed and reacted in a fluid convection manner, and this method has a poor mixing effect, needs to enhance the mixing effect of two phases by multiple times of impingement, and has a long reaction time.

Disclosure of Invention

In order to solve the defects of the prior art, the invention provides a device and a method for strengthening liquid-liquid reaction, which have compact structure, continuous reaction and high liquid-liquid reaction efficiency.

In order to achieve the purpose, the invention adopts the following technical scheme:

an apparatus for enhancing liquid-liquid reactions, the apparatus comprising a mixing section and a reactor, the mixing section comprising a feed tee for reactant feed and a mixer for enhancing reactant mixing, wherein,

the feeding tee joint comprises a first port, a second port and a third port, wherein the first port and the second port are respectively used for feeding reactants, the second port is provided with an ejector and is used for compressing and shearing one of the reactants to generate turbulent kinetic energy, the turbulent kinetic energy is injected through the ejector and enters the mixer, and the third port is connected with the mixer through a flange;

the mixer comprises a cylindrical mixer shell, and a mixer inlet section, a mixer spiral section with a spiral structure with opposite rotation directions and a mixer outlet section are sequentially arranged in the mixer shell;

the reactor is internally provided with a coil tube type heat exchange structure for heat exchange during liquid-liquid reaction, and comprises a shell side inlet, a shell side outlet, a tube side inlet and a tube side outlet.

According to a preferred embodiment of the present invention, the injector includes a cylindrical housing having an opening on one side and a hemispherical structure on the other side, the opening side of the housing is an inlet section of the injector, a support structure, a flow guiding structure and a thimble structure are sequentially disposed inside the injector along the inlet section, the support structure, the flow guiding structure and the thimble structure are connected to each other, and an injection port is disposed on one side of the hemispherical structure of the housing.

According to a preferred embodiment of the invention, the diameter of the inducer is d 1; the supporting structure comprises a cylindrical supporting rod and a hollow-out supporting frame which is connected with the supporting rod and the inner wall of the shell along the radial direction of the supporting rod outwards, and the diameter of the supporting rod is 1/4-1/2 of the diameter d1 of the inlet section; the flow guide structure comprises a cylindrical flow guide section and a truncated cone-shaped flow guide section with gradually reduced diameter, the diameter of the cylindrical flow guide section is 1/2-3/4 of the diameter d1 of the inlet section, the length of the cylindrical flow guide section is 1/4-3/4 of the diameter d1 of the inlet section, and the bottom angle alpha of the truncated cone-shaped flow guide section is 30-60 degrees; the thimble structure is a cylindrical structure, and the diameter of the thimble structure is 0.4-2 mm; the diameter of the jet orifice is 0.1-4.4mm, and the distance between the jet orifice inlet and the thimble structure is 1-10 mm.

According to a preferred embodiment of the invention, the mixer inlet section and the mixer outlet section have the same diameter; a cylindrical supporting structure is arranged at the axis in the mixer; the mixer spiral section comprises a plurality of spiral sections, the spiral sections are sequentially and repeatedly arranged, and the repeated number n of the spiral sections is the mixing series; each stage of helical section comprises a first helical structure and a second helical structure, the rotation directions of the first helical structure and the second helical structure are opposite, and helical blades of the first helical structure and the second helical structure are connected with the inner wall of the mixer shell and the supporting structure; and a middle section is arranged between the adjacent spiral structures.

According to the preferred embodiment of the present invention, the overall length of the mixer is L, the lengths of the first and second helical structures are 1/8 n-1/2 n of the length L of the mixer, and the length of the intermediate section is 1/8 n-1/2 n of the length L of the mixer.

The invention also provides a method for strengthening liquid-liquid reaction by using the device, which comprises the following steps:

(1) reactants enter the feed tee joint from the first port and the second port respectively, wherein one reactant enters the feed tee joint from the injector of the second port after being subjected to compression shearing, and the reactants are preliminarily mixed in the feed tee joint;

(2) the reactants which are preliminarily mixed enter a mixer and pass through a spiral section of the mixer with a spiral structure with opposite rotation directions, so that the dispersion degree of the two phases is improved, and the mixing is strengthened;

(3) the mixed reactants enter a reactor for reaction and exchange heat with the heat exchange water in a countercurrent way, wherein the reactants flow from bottom to top, and the heat exchange water flows from top to bottom.

According to the preferred embodiment of the invention, the mixing part is arranged outside the reactor or inside the reactor, when the mixing part is arranged outside the reactor, reactants enter the reactor from a shell side inlet and flow from bottom to top along the shell side, the reactants are discharged from a shell side outlet after reaction, heat exchange water enters the reactor from a tube side inlet, flows from top to bottom along the tube side, and flows out from a tube side outlet; when the mixing part is arranged in the reactor, reactants enter the reactor when entering the first port and the second port of the feeding tee joint, flow from bottom to top along the tube pass after flowing out of the mixer, are discharged from the tube pass outlet after reaction, and heat exchange water enters the reactor from the shell pass inlet, flows from top to bottom along the shell pass and flows from the shell pass outlet.

According to a preferred embodiment of the present invention, the reactants involved in the reaction enter the feed tee in a contact manner of convection, cocurrent or countercurrent.

According to a preferred embodiment of the invention, the mixing section is connected in parallel with a single ejector or several ejectors for adjusting the ratio of the flow rates of the reactants or adjusting the throughput of the reactor according to the actual demand.

The invention has the beneficial effects that:

the invention provides a device and a method for strengthening liquid-liquid reaction by strengthening mixing of reactants, wherein the mixing part of the device for strengthening liquid-liquid reaction comprises an injector and a mixer, the injector sprays one reactant by compression shearing to be in contact with the other reactant for mixing, so as to play a role of premixing, and the mixer comprises a spiral structure with opposite rotation directions, so as to play a role of improving dispersion degree of two phases and strengthening mixing. Compared with the traditional batch type reaction kettle, the device and the method have the characteristics of compact structure, continuous reaction and high reaction efficiency, strengthen the liquid-liquid reaction by strengthening the mixing of reactants, and are particularly suitable for the liquid-liquid reaction fields of chemical industry, pharmacy, biology and the like.

Drawings

FIG. 1 is a diagram of an apparatus for enhancing liquid-liquid reaction according to the present invention;

FIG. 2 is a schematic view of the structure of a mixing section according to the present invention;

FIG. 3 is a schematic diagram of an injector according to the present invention;

FIG. 4 is a cross-sectional view of a support structure for an injector in accordance with the present invention;

FIG. 5 is a schematic view of a flow directing structure and a thimble structure of an injector according to the present invention;

FIG. 6 is a diagram of an apparatus in which a mixing section according to the present invention is disposed inside a reactor;

FIG. 7 is a schematic view of a structure in which the contact of reactants according to the present invention is a forward flow type;

FIG. 8 is a schematic view of a structure in which the contact mode of reactants according to the present invention is a counter-flow type;

FIG. 9 is a process flow diagram for producing isopropanolamine using the apparatus and method of the present invention.

Detailed Description

The present invention will be described in further detail with reference to examples. It is to be understood that the following examples are for illustrative purposes only and are not to be construed as limiting the scope of the present invention, and that certain insubstantial modifications and adaptations of the invention may be made by those skilled in the art based on the teachings herein.

Example 1

FIG. 1 is a device for enhancing liquid-liquid reaction of the present invention, which comprises a mixing part and a reactor 4, wherein the mixing part comprises a feed tee 1 for feeding reactants and a mixer 2 for enhancing mixing of the reactants, as shown in FIG. 2, the feed tee 1 comprises a first port 11, a second port 12 and a third port 13, wherein the first port 11 is used for feeding a first reactant participating in liquid-liquid reaction, the second port 12 is used for feeding a second reactant participating in liquid-liquid reaction, the second port 12 is provided with an ejector 3 for compressing and shearing the second reactant to generate turbulent energy, the turbulent energy is injected into the second reactant through the ejector 3 at an angle, and the third port 13 is connected with the mixer 2 through a flange; the reactor 4 is internally provided with a coil tube type heat exchange structure for heat exchange during liquid-liquid reaction, and the reactor 4 comprises a shell-side inlet 41, a shell-side outlet 42, a tube-side inlet 43 and a tube-side outlet 44.

Further, as shown in fig. 3, the injector 3 includes a cylindrical housing 31 having one side opened and the other side formed in a hemispherical structure, an inlet section 32 of the injector 3 is formed at one side of the opening of the housing 31, and the diameter of the inlet section 32 is d 1; inside the injector 3, inward along the inlet section 32, a supporting structure 33, a flow guiding structure 34 and a thimble structure 35 are sequentially arranged, as shown in fig. 4, the supporting structure 33 includes a cylindrical supporting rod 331 and a hollowed-out supporting frame 332 radially outward along the supporting rod 331 and connected with the supporting rod 331 and the inner wall of the housing 31, and a diameter d3 of the supporting rod 331 is 1/4-1/2 of a diameter d1 of the inlet section 32; the flow guiding structure 34 comprises a cylindrical flow guiding section 341 and a truncated cone-shaped flow guiding section 342 with a gradually reduced diameter, the diameter d4 of the cylindrical flow guiding section 341 is 1/2-3/4 of the diameter d1 of the inlet section 32, the length L1 is 1/4-3/4 of the diameter d1 of the inlet section 32, and as shown in FIG. 5, the bottom angle alpha of the truncated cone-shaped flow guiding section 342 is 30-60 degrees; the thimble structure 35 is a cylindrical structure with the diameter of 0.4-2 mm; an injection port 36 is arranged on one side of the hemispherical structure of the shell 31, the diameter d5 of the injection port 36 is 0.1-4.4mm, and the distance between the inlet of the injection port 36 and the thimble structure 35 is 1-10 mm.

Further, returning to fig. 2, the mixer 2 includes a cylindrical mixer housing 21, and a mixer inlet section 22, a mixer spiral section 23 and a mixer outlet section 24 are sequentially arranged in the mixer housing 21; the mixer inlet section 22 and the mixer outlet section 24 have the same diameter; a cylindrical supporting structure 25 is arranged at the axis in the mixer 2; the mixer spiral section 23 comprises a plurality of spiral sections, the spiral sections are sequentially and repeatedly arranged, and the number n of repeated spiral sections is the number of mixing stages; each of the spiral sections includes a first spiral structure 231 and a second spiral structure 232, the spiral directions of the first spiral structure 231 and the second spiral structure 232 are opposite, and the spiral blades of the first spiral structure 231 and the second spiral structure 232 are connected with the inner wall of the mixer housing 21 and the support structure 25; between the adjacent helical structures is a middle section 233.

Further, the overall length of the mixer is L, the lengths L2 and L4 of the first helical structure 231 and the second helical structure 232 are 1/8n to 1/2n of the length L of the mixer, and the length L3 of the intermediate section 233 is 1/8n to 1/2n of the length L of the mixer.

The method for strengthening liquid-liquid reaction by using the device comprises the following steps:

(1) a first reactant participating in liquid-liquid reaction enters the feed tee joint 1 from the first port 11, a second reactant enters the inlet section 32 of the ejector 3 of the second port 12, and after the flow is guided along the flow guide structure 34, the first reactant is ejected from the ejection port 36 through shearing and crushing between the ejector pin structure 35 and the ejector shell 31 and is in contact with the first reactant to be primarily mixed;

(2) the reactants which are preliminarily mixed enter a mixer 2 and sequentially pass through spiral structures with opposite rotation directions, so that the dispersion degree of the two phases is improved, and the mixing is strengthened;

(3) the mixed reactants enter the reactor 4 for reaction and exchange heat with the heat exchange water in a counter-flow manner, wherein the reactants flow from bottom to top, and the heat exchange water flows from top to bottom.

Further, as shown in fig. 1 and 6, respectively, the mixing part is disposed outside the reactor or inside the reactor according to actual requirements, when the mixing part is disposed outside the reactor (fig. 1), the reactant enters the reactor 4 from the shell side inlet 41, flows from bottom to top along the shell side, is discharged from the shell side outlet 42 after reaction, and the heat exchange water enters the reactor 4 from the tube side inlet 43, flows from top to bottom along the tube side, and flows out from the tube side outlet 44; when the mixing part is arranged in the reactor (figure 6), reactants enter the reactor 4 when entering the first port 11 and the second port 12 of the feeding tee joint 1, flow from bottom to top along the tube pass after flowing out of the mixer 2, are discharged from the tube pass outlet 44 after reaction, and heat exchange water enters the reactor 4 from the shell pass inlet 41, flows from top to bottom along the shell pass and flows out of the shell pass outlet 42.

Further, as shown in fig. 2, fig. 7 and fig. 8, respectively, the first reactant and the second reactant participating in the reaction enter the feed tee 1 in a contact manner of a convection mode (fig. 2), a forward flow mode (fig. 7) or a counter-flow mode (fig. 8).

Further, the mixing section may employ a single injector 3 or a plurality of injectors 3 connected in parallel according to actual throughput, for adjusting the ratio of the flow rates of the first reactant and the second reactant according to actual demand, or adjusting the throughput of the reactor.

Example 2

The production method comprises the steps of producing isopropanolamine by using epoxy propane and strong ammonia water as raw materials by a chemical enterprise, wherein the annual output is 10kt/a, the original process flow comprises the steps of pressurizing the epoxy propane and the strong ammonia water by a high-pressure ammonia water pump, mixing by a static mixer, heating by a preheater to the reaction starting temperature, and then feeding into a reactor to generate a mixture of isopropanolamine, diisopropanolamine and triisopropanolamine. The mixing effect of propylene oxide and ammonia therefore directly affects the formation of the subsequent reactants. In order to reduce the ratio of ammonia water to propylene oxide, reduce the reaction pressure and temperature, reduce by-products, and the like, the device and the method for enhancing the liquid-liquid reaction in example 1 are used for building a side line device, as shown in fig. 9, the method comprises the following steps:

(1) the epoxy propane is pumped into the first port through a buffer tank and enters the feeding tee joint through a pump, and the ammonia water is pumped into an ejector of the second port through the buffer tank and the pump, is compressed and sheared, is ejected from an ejection port, enters the feeding tee joint and is primarily mixed with the epoxy propane;

(2) the initially mixed epoxypropane and ammonia water enter a mixer and are sequentially subjected to reinforced mixing through spiral structures with opposite rotation directions;

(3) the mixed propylene oxide and ammonia water enter the shell side of the reactor through a shell side inlet and flow from bottom to top to react, and exchange heat with heat exchange water flowing from top to bottom in a countercurrent tube side;

(4) the product after the reaction contains excessive ammonia water, isopropanolamine, diisopropanolamine, triisopropanolamine and the like, is led to an ejector of a feeding tee joint of the next stage through a shell outlet of the reactor and is primarily mixed with the propylene oxide which is freshly fed from a first port of the next stage, and the steps (2) and (3) are repeated to carry out the second stage reaction.

(5) And (4) repeating the step (4) to sequentially carry out third-stage reaction, fourth-stage reaction and fifth-stage reaction on the product after the second-stage reaction, and discharging the reaction product through a shell side outlet of a fifth-stage reactor.

The mixing part is arranged outside the reactor, the contact mode of reactants entering the feeding tee joint is a convection mode, the mixing part adopts a single ejector, the overall length L of the mixer is 1.2m, and the number of mixing stages is 1 stage. Compared with the prior static mixer for producing isopropanolamine, the device and the method in the embodiment 1 maintain the same production index, reduce the proportion of consumed ammonia water and propylene oxide (namely the ammonia ring ratio), reduce the reaction pressure and reduce the reaction temperature, and the comparison data are shown in the following table.

Example 3

Some petrochemical enterprises take alkane and olefin and benzene as raw materials, and carry out alkylation reaction under the action of a catalyst, namely hydrogen fluoride, and an original liquid-liquid reaction mixing device is a combination of a static mixer and a reactor. Wherein the flow rate of the alkane and the olefin participating in the reaction is 100t/h, the flow rate of the benzene is 20t/h, and the flow rate of the catalyst hydrogen fluoride is 200 t/h. In order to ensure the complete reaction of olefin, excessive benzene and hydrogen fluoride are introduced, and with the improvement of production capacity, under the condition of reducing the reaction quantity of benzene and hydrogen fluoride, the original reaction mixing device combining a static mixer and a reactor cannot meet the requirement of mixing reaction, so that aiming at the improvement of the original device, the device for enhancing liquid-liquid reaction described in example 1 is adopted to replace the original reaction mixing device, wherein 20 ejectors are connected in parallel, the diameter of an inlet section of the mixer is 400mm, the overall length of the mixer is 2m, and the mixing stage number is 2.

After modification, under the condition of keeping the original flow of benzene and hydrogen fluoride, the flow of alkane and olefin is increased from 100t/h to 140t/h, and the yield of reactants is greatly improved.