阅读说明：本技术 一种皂脚酸化脱磷设备及工艺 (Soapstock acidification dephosphorization equipment and technology ) 是由 江建 种裕瀚 李道强 桑莹莹 李伍 张鑫伟 黄晗名 于 2021-08-23 设计创作，主要内容包括：本发明涉及油脂废弃物的开发利用技术领域,尤其涉及一种皂脚酸化脱磷设备及工艺。该工艺包括以下步骤：S1.将皂脚与小分子有机酸混合,中和反应后,除去水相,得到油相；S2.将所述油相和超临界二氧化碳混合反应后,除去二氧化碳,得到低磷酸化油。本申请中对皂脚先通过小分子有机酸中和除去皂脚中的碱、然后再通过二氧化碳酸化,避免了传统工艺中硫酸的使用,极大地提高了皂脚的脱磷率,降低了制得的酸化油中磷的含量。(The invention relates to the technical field of development and utilization of grease waste, in particular to soapstock acidification dephosphorization equipment and a soapstock acidification dephosphorization process. The process comprises the following steps: s1, mixing soapstock and small molecular organic acid, and removing a water phase to obtain an oil phase after a neutralization reaction; and S2, mixing the oil phase with supercritical carbon dioxide for reaction, and removing the carbon dioxide to obtain the low-phosphate oil. In the application, the soapstock is neutralized by the small-molecular organic acid to remove alkali in the soapstock and then is acidified by the carbon dioxide, so that the use of sulfuric acid in the traditional process is avoided, the dephosphorization rate of the soapstock is greatly improved, and the content of phosphorus in the prepared acidified oil is reduced.)

1. A soapstock acidification dephosphorization process is characterized by comprising the following steps: the method comprises the following steps:

s1, mixing soapstock and small molecular organic acid, and removing a water phase to obtain an oil phase after a neutralization reaction;

and S2, mixing the oil phase with supercritical carbon dioxide for reaction, and removing the carbon dioxide to obtain the low-phosphate oil.

2. The process for acidification and dephosphorization of soapstock according to claim 1, wherein: in step S1, the neutralization reaction is carried out for 1-2h at the temperature of 160-210 ℃.

3. The process for acidification and dephosphorization of soapstock according to claim 1, wherein: in step S2, the oil phase and the supercritical carbon dioxide are mixed and reacted for 2-4 h.

4. The process for acidification and dephosphorization of soapstock according to claim 1, wherein: the acid value of the low-phosphorylated oil is 110-140mgKOH/g, and the phosphorus content is less than 15 mg/kg.

5. An apparatus for conducting the acidulated dephosphorization process of soapstock according to any one of claims 1-4, characterized in that: comprises an outer shell (1), an inner shell (2) arranged in the outer shell (1) and a temperature control element arranged in the outer shell (1); the inner shell (2) comprises an inner shell (21) with an opening at the top and an inner shell cover (22) for covering the opening, the inner shell (21) and the inner shell cover (22) both comprise cylindrical inner shell side parts, the inner shell side part of the inner shell (21) is provided with an external thread, and the inner shell side part of the inner shell cover (22) is provided with an internal thread in threaded connection with the external thread; the side part of the inner shell (21) sequentially comprises a closed upper part, a middle part provided with a plurality of communicating holes (211) and a lower part provided with a plurality of centrifugal holes (212) from the opening to the bottom of the inner shell (21), and the centrifugal holes (212) are covered with oil-water separation membranes; the side part of the inner shell cover (22) comprises a closed part which can be connected with the lower part and a communication part which can be connected with the middle part, and the communication part is provided with a through hole (221) which can be communicated with the communication hole (211); the shell (1) comprises a shell body (11) and a shell cover (12), the shell cover (12) is connected with the inner shell cover (22), the shell body (11) and the shell cover (12) respectively comprise shell side parts, and the shell side parts of the shell body (11) are provided with vertical insertion grooves (111) into which the shell side parts of the shell cover (12) can be inserted; the bottom of the inner shell (21) is connected with an output shaft of the motor (3), and the inner shell cover (22) is in sliding connection with a vertical limiting groove (112) arranged on the inner wall of the outer shell (11) through a connecting rod (4); the carbon dioxide feeding device is characterized in that a carbon dioxide inlet (121) is formed in the outer shell cover (12), and a feeding hole (122) used for feeding materials into the inner shell (2) is formed in the connection position of the outer shell cover (12) and the inner shell cover (22).

6. The apparatus for acidification and dephosphorization of soapstock according to claim 5, wherein: be equipped with stirring roller (213) in interior casing (21), stirring roller (213) one end with interior casing (21) inner wall connection, the other end is unsettled.

7. The apparatus for acidification and dephosphorization of soapstock according to claim 5, wherein: the outer shell (11) comprises a fixed outer shell (11 a) and a movable outer shell (11 b) arranged in the fixed outer shell (11 a), and the inner shell (21) is arranged in the movable outer shell (11 b); the fixed outer shell (11 a) is provided with the vertical slot (111), and the movable outer shell (11 b) is provided with the vertical limiting groove (112); the filter block is filled between the movable outer shell (11 b) and the fixed outer shell (11 a), the movable outer shell (11 b) is provided with a guide hole, and the fixed outer shell (11 a) is provided with a collection hole.

8. The apparatus for acidification and dephosphorization of soapstock according to claim 7, wherein: the movable outer shell (11 b) is provided with a mechanical cavity, a first rotating shaft and a second rotating shaft which are driven by a gear tooth chain structure are arranged in the mechanical cavity, and the first rotating shaft is close to the bottom of the movable outer shell (11 b) relative to the second rotating shaft; the first rotating shaft is provided with a transmission gear (11 b 1), one end of a rack (5) is inserted into the mechanical cavity and meshed with the transmission gear (11 b 1), and the other end of the rack can be inserted into a slot (214) formed in the inner shell (21); the second rotating shaft is provided with a control block (11 b 2), one end of the control block (11 b 2) is connected with the second rotating shaft, and the other end of the control block is inserted into the vertical limiting groove (112).

9. The apparatus for acidification and dephosphorization of soapstock according to claim 8, wherein: connecting rod (4) include hollow fixed cover (41) and insert movable rod (42) in fixed cover (41), the one end of movable rod (42) inserts vertical spacing groove (112), the other end pass through the spring with the bottom is connected in fixed cover (41), the bottom is equipped with the electro-magnet in fixed cover (41), movable rod (42) are the iron pole.

10. The apparatus for acidification and dephosphorization of soapstock according to claim 8, wherein: the inner shell cover (22) is connected with the outer shell cover (12) through a connecting column, one end of the connecting column is fixedly connected with the inner shell cover (22), the other end of the connecting column is connected with the outer shell cover (12) through a rotating bearing, and the connecting column is hollow inside to form the feeding hole (122).

Technical Field

The invention relates to the technical field of development and utilization of grease waste, in particular to soapstock acidification dephosphorization equipment and a soapstock acidification dephosphorization process.

Background

With the development of economic globalization, petrochemical energy is continuously reduced, and environmental problems are more and more prominent. The biodiesel has excellent physical and chemical properties and is an optimal product for replacing petroleum diesel. A large amount of leftovers are generated in the process of producing grease in China every year, wherein the leftovers contain saponin and oil residue, and acidified oil can be obtained through acidification treatment and converted into raw materials for preparing biodiesel, so that the cost is greatly reduced by using cheap leftovers as raw materials for preparing the biodiesel.

The soapstock is the leftovers of the alkali refining process of crude oil of edible vegetable oil processing enterprises, and the phospholipid content in the soapstock is also high due to the phospholipid contained in the oil seeds. Most of the conventional acidified oil processes use a sulfuric acid acidification method to reduce the phospholipid content, such as the method disclosed in patent document CN109554230A, which is characterized in that the preparation method comprises heating the soapstock to 88-92 ℃ and adding acid and acid water to perform a primary acidification reaction, and separating to obtain a primary acidified oil; heating the primary acidified oil to 88-92 ℃, adding concentrated sulfuric acid for secondary acidification reaction, and separating to obtain acidified oil; wherein the acid water is acidified water obtained by separation after secondary acidification reaction. In the primary acidification reaction, the acid is sulfuric acid with the mass fraction not less than 70%; in the secondary acidification reaction, the concentrated sulfuric acid is sulfuric acid with the mass fraction not less than 90%. The acidified oil produced by the method has the problem of high phospholipid content, and the subsequent treatment and utilization stages of the acidified oil are easy to emulsify. The acidified oil obtained by the method has low yield, poor product quality, large acid and alkali dosage, high energy consumption, serious wastewater pollution and difficult treatment. With the rapid development of the biodiesel industry, low-phosphate oil is more and more favored by the market. In order to improve the quality of the acidified oil, it is urgently needed to improve the existing equipment and process, so that acid wastewater is generated as little as possible in the production process of the acidified oil, and the phosphorus content in the acidified oil can be reduced.

Disclosure of Invention

The invention aims to solve the problems and provides soapstock acidification dephosphorization equipment and a soapstock acidification dephosphorization process capable of effectively reducing the phosphorus content in acidified oil.

The technical scheme for solving the problems is to firstly provide a soapstock acidification dephosphorization process, which comprises the following steps:

s1, mixing soapstock and small molecular organic acid, and removing a water phase to obtain an oil phase after a neutralization reaction;

and S2, mixing the oil phase with supercritical carbon dioxide for reaction, and removing the carbon dioxide to obtain the low-phosphate oil.

As a preference of the present invention, in step S1, the neutralization reaction is carried out at 160-210 ℃ for 1-2 h.

Preferably, in step S2, the oil phase is mixed with supercritical carbon dioxide and reacted for 2-4 h.

Preferably, the acid value of the low-phosphorylated oil is 110-140mgKOH/g, and the phosphorus content is less than 15 mg/kg.

Preferably, the small-molecule organic acid comprises one or more of formic acid, acetic acid and oxalic acid. Further preferably, the small molecule organic acid is formic acid.

Preferably, step S2 further includes the steps of: before removing carbon dioxide, introducing hydrogen into the system, raising the temperature to 160-210 ℃ again, reacting for 1-2h to obtain an oil body and a water body, then separating the water body, and heating and deacidifying the remaining oil body to obtain the low-phosphate oil.

Wherein, hydrogen can carry out hydrogenation hardening to the low-phosphate oil on the one hand to obtain stearic acid with wider application. On the other hand, the catalyst can also react with carbon dioxide to generate formic acid, so that the acidification dephosphorization effect of the catalyst is further improved.

The invention also aims to provide equipment for the soapstock acidification dephosphorization process, which comprises an outer shell, an inner shell arranged in the outer shell and a temperature control element arranged in the outer shell; the inner shell comprises an inner shell with an opening at the top and an inner shell cover for covering the opening, the inner shell and the inner shell cover both comprise cylindrical inner shell side parts, the inner shell side parts of the inner shell are provided with external threads, and the inner shell side parts of the inner shell cover are provided with internal threads in threaded connection with the external threads; the side part of the inner shell sequentially comprises a closed upper part, a middle part provided with a plurality of communicating holes and a lower part provided with a plurality of centrifugal holes from the opening to the bottom of the inner shell, and the centrifugal holes are covered with oil-water separation membranes; the side part of the inner shell cover comprises a closed part which can be connected with the lower part and a communication part which can be connected with the middle part, and the communication part is provided with a through hole which can be communicated with the communication hole; the outer shell comprises an outer shell body and an outer shell cover, the outer shell cover is connected with the inner shell cover, the outer shell body and the outer shell cover respectively comprise outer shell side parts, and the outer shell side parts of the outer shell body are provided with vertical slots into which the outer shell side parts of the outer shell cover can be inserted; the bottom of the inner shell is connected with an output shaft of the motor, and the inner shell cover is in sliding connection with a vertical limiting groove arranged on the inner wall of the outer shell through a connecting rod; the shell cover is provided with a carbon dioxide inlet, and a feed inlet for feeding materials into the inner shell is formed in the joint of the shell cover and the inner shell cover.

Preferably, the inner wall of the vertical slot is provided with a rubber sealing layer.

Preferably, a stirring roller is arranged in the inner shell, one end of the stirring roller is connected with the inner wall of the inner shell, and the other end of the stirring roller is suspended.

Preferably, the outer shell comprises a fixed outer shell and a movable outer shell arranged in the fixed outer shell, and the inner shell is arranged in the movable outer shell; the fixed outer shell is provided with the vertical slot, and the movable outer shell is provided with the vertical limiting slot; the filter block is filled between the movable outer shell and the fixed outer shell, the movable outer shell is provided with a guide hole, and the fixed outer shell is provided with a collection hole.

Preferably, the movable outer shell is provided with a mechanical cavity, a first rotating shaft and a second rotating shaft which are driven by a gear and gear chain structure are arranged in the mechanical cavity, and the first rotating shaft is close to the bottom of the movable outer shell relative to the second rotating shaft; the first rotating shaft is provided with a transmission gear, one end of a rack is inserted into the mechanical cavity and meshed with the transmission gear, and the other end of the rack can be inserted into a slot formed in the inner shell; the second rotating shaft is provided with a control block, one end of the control block is connected with the second rotating shaft, and the other end of the control block is inserted into the vertical limiting groove.

Preferably, the connecting rod comprises a hollow fixed sleeve and a movable rod inserted into the fixed sleeve, one end of the movable rod is inserted into the vertical limiting groove, the other end of the movable rod is connected with the inner bottom of the fixed sleeve through a spring, an electromagnet is arranged at the inner bottom of the fixed sleeve, and the movable rod is an iron rod.

Preferably, the inner shell cover and the outer shell cover are connected through a connecting column, one end of the connecting column is fixedly connected with the inner shell cover, the other end of the connecting column is connected with the outer shell cover through a rotating bearing, and the connecting column is hollow inside to form the feed port.

The invention has the beneficial effects that:

1. in the application, the soapstock is neutralized by the small-molecular organic acid to remove alkali in the soapstock, and then is acidified by the carbon dioxide, so that the use of sulfuric acid in the traditional process is avoided, the dephosphorization rate of the soapstock is greatly improved, and the content of phosphorus in the prepared acidified oil is reduced.

2. In this application, mix soapstock and supercritical carbon dioxide, regard as the soapstock solvent through supercritical carbon dioxide, improved the dispersity of soapstock in equipment, in order to improve dephosphorization efficiency.

3. In this application, set up the motor and drive pivoted inner casing, it both had been regarded as reaction vessel, as centrifugal device again, has improved the dephosphorization efficiency.

Drawings

FIG. 1 is a schematic diagram of an embodiment of a soapstock acidification dephosphorization apparatus;

FIG. 2 is a schematic diagram of another embodiment of a soapstock acidification dephosphorization apparatus;

FIG. 3 is a schematic diagram of the operation of another embodiment of the soapstock acidification dephosphorization apparatus;

in the figure: a housing 1; an outer shell 11, a fixed outer shell 11a, a movable outer shell 11b, a transmission gear 11b1 and a control block 11b 2; housing cover 12, carbon dioxide inlet 121, feed inlet 122; an inner casing 2; the inner shell 21, a communication hole 211, a centrifugal hole 212, a containing roller 213 and a slot 214; the inner shell cover 22, the through hole 221; a motor 3; connecting rod 4, fixed cover 41, movable rod 42.

Detailed Description

The following are specific embodiments of the present invention and are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.

Example 1

A soapstock acidification dephosphorization process comprises the following steps:

s1, mixing the soapstock with a small molecular organic acid, carrying out neutralization reaction at the temperature of 160-210 ℃ for 1-2h to obtain an oil phase and a water phase, and removing the water phase to obtain the oil phase;

and S2, mixing the oil phase and supercritical carbon dioxide, reacting for 2-4h, and removing carbon dioxide to obtain the low-phosphate oil.

In order to carry out the process, the application also discloses soapstock acidification and dephosphorization equipment, which comprises an outer shell 1, an inner shell 2 arranged in the outer shell 1 and a temperature control part arranged in the outer shell 1, as shown in fig. 1.

The inner housing 2 includes an inner housing 21 and an inner housing cover 22, and the inner housing 21 and the inner housing cover 22 are both hollow cylinders with an open bottom and a closed bottom, so that the inner housing 21 and the inner housing cover 22 both include cylindrical inner housing sides. The radius of the bottom surface of the inner housing cover 22 is slightly larger than that of the bottom surface of the inner housing 21, and the opening of the inner housing 21 faces upward and the opening of the inner housing cover 22 faces downward in the direction of fig. 1. In this application, the inner shell lateral part of interior casing 21 and the inner shell lateral part of interior casing lid 22 are more or less high, and the inner shell lateral part of interior casing 21 is equipped with the external screw thread, and the inner shell lateral part of interior casing lid 22 is equipped with the internal thread with external screw thread connection, consequently interior casing lid 22 and interior casing 21 threaded connection.

The inner shell side of the inner shell 21 includes a closed upper portion, a middle portion provided with a plurality of communicating holes 211, and a lower portion provided with a plurality of centrifugal holes 212 in sequence from the opening to the bottom of the inner shell 21, and the centrifugal holes 212 are covered with an oil-water separation membrane, which only allows water to pass through but not oil to pass through. When the inner case cover 22 is completely provided to the inner case 21, the inner case side portion of the inner case cover 22 includes a closed portion connected to the lower portion, a communicating portion connected to the middle portion, and another closed portion connected to the upper portion. The communication portion is provided with a through hole 221 communicable with the communication hole 211, and the through hole 221 communicates with the communication hole 211 only when the inner housing cover 22 is screwed to the bottom with the inner housing 21.

In addition, in order to further improve the mixing uniformity, a stirring roller 213 is provided in the inner housing 21, and one end of the stirring roller 213 is connected to the inner wall of the inner housing 21 and the other end is suspended.

The outer casing 1 includes an outer casing 11 and an outer casing cover 12, and similar to the inner casing 2, the outer casing 11 and the outer casing cover 12 are both hollow cylinders with an open bottom and a closed bottom, but the bottom of the outer casing 1 may be any shape, such as direction, circular shape, etc., and in this embodiment, the bottom of the outer casing 1 is also circular. The outer shell 11 and the outer shell cover 12 both include outer shell side portions, and different from the inner shell 2 in connection manner, the outer shell side portions of the outer shell 11 are provided with vertical insertion grooves into which the outer shell side portions of the outer shell cover 12 can be inserted. In order to guarantee the sealing effect, the inner wall of the vertical slot is provided with a rubber sealing layer.

The inner housing 21 may be directly disposed in the outer housing 11, or the bottom of the inner housing 21 may be connected to the bottom of the outer housing 11 through a rotation bearing. The outer housing cover 12 is connected to the inner housing cover 22. Then make motor 3 output shaft pass behind the bottom of shell body 11 and be connected with the bottom of interior casing 21, pass through the vertical spacing groove 110 sliding connection that connecting rod 221 and shell body 11 inner wall set up with interior casing 22 simultaneously, just can be when motor 3 drives interior casing 21 and rotates for interior casing 22 moves in vertical direction, drives outer cover 12 simultaneously and removes to change the volume size in the shell 1.

In addition, to assist the feeding, the outer housing cover 12 is provided with a carbon dioxide inlet 121, and a feed opening 122 for feeding into the inner housing 21 is provided at a junction of the outer housing cover 12 and the inner housing cover 22.

When in use, the method comprises the following steps:

s1, mixing the nigre with small molecular organic acid, carrying out neutralization reaction at the temperature of 160-210 ℃ for 1-2h to obtain an oil phase and a water phase, and removing the water phase to obtain an oil phase; the small molecular organic acid in this example is formic acid.

I.e. first to remove the air inside the apparatus: the communication between the communication hole 211 and the through hole 221 is maintained, the carbon dioxide inlet 121 and the feed inlet 122 are opened, carbon dioxide is introduced into the apparatus through the carbon dioxide inlet 121, at this time, the feed inlet 122 serves as an air exhaust port until air in the casing 1 is exhausted, and then the carbon dioxide inlet 121 is closed.

Then the control motor 3 drives the inner housing 21 to rotate a small circle, so that the inner housing cover 22 moves upward a small distance, the communication hole 211 and the through hole 221 are not communicated, and the closing part covers the centrifugal hole 212. Then soapstock and formic acid are introduced into the inner shell 2 through the feed inlet 122, the feed inlet 122 is closed, and the temperature in the equipment is controlled to rise to 160-210 ℃ through the temperature control part for reaction for 1-2h to obtain an oil phase and a water phase.

Then, the control motor 3 drives the inner housing 21 to rotate, so that the inner housing cover 22 continues to move upwards and drives the outer housing cover 12 to move upwards, so that the centrifugal hole 212 is no longer covered by the closed portion, meanwhile, during the rotation of the inner housing 21, the water phase in the inner housing enters between the outer housing 11 and the inner housing 21 through the oil-water separation membrane on the centrifugal hole 212, and the oil phase is remained in the inner housing 2.

And S2, mixing the oil phase with supercritical carbon dioxide, reacting for 2-4h, and removing the carbon dioxide to obtain the low-phosphate oil.

The control motor 3 drives the inner housing 21 to rotate, so that the inner housing cover 22 moves downwards and the outer housing cover 12 moves downwards, so that the communication hole 211 is communicated with the through hole 221, and the closing part covers the centrifugal hole 212. Then carbon dioxide is introduced into the equipment through the carbon dioxide inlet 121 until the pressure in the equipment reaches the critical pressure of the carbon dioxide, and meanwhile, the temperature in the equipment is controlled through the temperature control part until the temperature reaches the critical temperature of the carbon dioxide, and the temperature is kept for 2-4 hours. Then the carbon dioxide inlet 121 and the feed inlet 122 are opened, the temperature in the equipment is controlled to rise after the equipment is released to normal pressure, the supercritical carbon dioxide is gasified and discharged, and the residual in the inner shell 21 is the low-phosphorylation oil.

The acid value of the obtained low-phosphorylation oil is 110-140mgKOH/g, the phosphorus content is less than 15mg/kg, and the yield of the low-phosphorylation oil is more than 95 percent. The obtained low-phosphorylation oil can be used as raw material for producing hydrocarbon-based biodiesel (HOV).

In step S1, the water phase separated can be reused after being purified, and therefore, in this embodiment, as shown in fig. 2, the outer shell 11 includes a fixed outer shell 11a and a movable outer shell 11b disposed in the fixed outer shell 11a, and the inner shell 21 is disposed in the movable outer shell 11 b. Similarly, the fixed outer casing 11a, the movable outer casing 11b, and the outer casing cover 12 are all hollow cylinders with one open side and the other closed side, the movable outer casing 11b is directly placed in the fixed outer casing 11a, or the bottom surface of the movable outer casing 11b is connected to the bottom surface of the fixed outer casing 11a through a rotation bearing, and the inner casing 21 is directly placed in the movable outer casing 11b, or the bottom surface of the inner casing 21 is connected to the bottom surface of the movable outer casing 11b through a rotation bearing. At this time, the fixed outer housing 11a is provided with a vertical insertion groove 111, and the movable outer housing 11b is provided with a vertical stopper groove 112. The filter block is filled between the movable outer shell 11b and the fixed outer shell 11a, the movable outer shell 11b is provided with a leading-out hole, the fixed outer shell 11a is provided with a collecting hole, and the horizontal plane of the collecting hole is higher than the horizontal plane of the leading-out hole. Still including collecting the box, collect the box and pass through connecting pipe and suction pump intercommunication with the collection hole, the aqueous phase in interior casing 21 is getting into movable outer casing 113 and interior casing 21 between the back, under the effect of suction pump, and reentrant collection box after the filter block edulcoration is collected.

In addition, in this application, the rotation of interior casing 21 can drive interior casing 22 and move up, and after interior casing 22 removed the top, can influence interior casing 21's continuation and rotate, brings the influence for centrifugal operation. Therefore, in this embodiment, the movable outer housing 11b is provided with a mechanical cavity, a first rotating shaft and a second rotating shaft which are driven by the gear and gear chain structure are arranged in the mechanical cavity, and the first rotating shaft is close to the bottom of the movable outer housing 11b relative to the second rotating shaft; the first rotating shaft is provided with a transmission gear 11b1, one end of a rack 5 is inserted into the mechanical cavity and meshed with the transmission gear 11b1, and the other end can be inserted into a slot 214 formed in the inner shell 21; the second rotating shaft is provided with a control block 11b2, one end of the control block 11b2 is connected with the second rotating shaft, the other end of the control block 11b is inserted into the vertical limiting groove 112, and the bottom of the vertical limiting groove 112 is provided with an opening for the control block 11b2 to rotate around the second rotating shaft. The horizontal plane of the second rotating shaft is higher than the horizontal plane of the lower part. The inner shell cover 22 is connected with the outer shell cover 12 through a connecting column, one end of the connecting column is fixedly connected with the inner shell cover 22, the other end of the connecting column is connected with the outer shell cover 12 through a rotating bearing, and the connecting column is hollow to form a feeding hole 122.

As shown in fig. 3, when the inner housing 21 rotates to make the inner housing cover 22 drive the connecting rod 4 to move under the control block 11b2, the connecting rod 4 continues to move upwards, which pushes the end of the control block 11b2 to rotate upwards, thereby driving the second rotating shaft to rotate, driving the first rotating shaft to rotate, further driving the rack 11b1 to move towards the slot 214, so that the rack 11b1 is inserted into the slot 211, so that the movable outer housing 11b is connected with the inner housing 21, so that the inner housing 21 drives the movable outer housing 11b, further driving the inner housing cover 22 to rotate together, and centrifugal efficiency is improved.

After the centrifugation is completed, if the inner shell cover 22 needs to move upwards continuously, the connecting rod 4 can comprise a hollow fixing sleeve 41 and a movable rod 42 inserted into the fixing sleeve 41, one end of the movable rod 42 is inserted into the vertical limiting groove 112, the other end of the movable rod is connected with the bottom in the fixing sleeve 41 through a spring, an electromagnet is arranged at the bottom in the fixing sleeve 41, and the movable rod 42 is an iron rod. By the attraction of the electromagnet to the iron rod, the movable rod 2212 is contracted and no longer abuts against the control block 11b2, and the control block 11b2 can be restored to the original state, so that the rack 11b1 is pulled out from the slot 214. The electromagnet needs to be energized, so that the inner shell cover 22 can be hollow inside, so that the electric wire can be arranged conveniently. On the basis, an electric heating wire can be arranged in the inner shell cover 22 to form a temperature control element.

Example 2

A soapstock acidification dephosphorization process comprises the following steps:

s1, mixing the soapstock with a small molecular organic acid, carrying out neutralization reaction at the temperature of 160-210 ℃ for 1-2h to obtain an oil phase and a water phase, and removing the water phase to obtain the oil phase;

s2, mixing and reacting the oil phase and the supercritical carbon dioxide for 2-4h, introducing hydrogen into the system, raising the temperature to 160-plus-210 ℃ again, reacting for 1-2h to obtain an oil body and a water body, separating the water body, and heating the remaining oil body to obtain the low-phosphorylation oil.

The apparatus used in this example is the same as that used in example 1, except thatThe method comprises the following steps: due to the need for carbon dioxide hydrogenation to formic acid and fatty acid hydrohardening operations in the inner shell 21, a catalyst is required, preferably Cu/ZrO₂-Al₂O₃Catalyst and nickel formate catalyst. The catalyst may be directly put into the inner case 21 together with the soapstock, or, as in this embodiment, a groove may be formed in the stirring roller 213, and the catalyst may be placed in the groove.

The operation steps for carrying out step S1 are the same as in example 1; when step S2 is implemented, the operation steps are:

the control motor 3 drives the inner housing 21 to rotate, so that the inner housing cover 22 moves downwards and the outer housing cover 12 moves downwards, so that the communication hole 211 is communicated with the through hole 221, and the closing part covers the centrifugal hole 212. Then carbon dioxide is introduced into the equipment through the carbon dioxide inlet 121 until the pressure in the equipment reaches the critical pressure of the carbon dioxide, and meanwhile, the temperature in the equipment is controlled through the temperature control part until the temperature reaches the critical temperature of the carbon dioxide, and the temperature is kept for 2-4 hours.

The control motor 3 then rotates the inner housing 21 a small amount of time, so that the inner housing cover 22 moves upward a small distance, so that the communication hole 211 and the through hole 221 are not communicated, but the closing portion still covers the centrifugal hole 212. Introducing hydrogen into the inner shell 21 through the feed inlet 122 to realize the synthesis of formic acid by hydrogenation of supercritical carbon dioxide and the hydrogenation hardening of fatty acid, and then controlling the temperature in the equipment to further rise to 160-210 ℃ for reaction for 1-2h to obtain oil bodies and water bodies.

Then, the control motor 3 drives the inner housing 21 to rotate, so that the inner housing cover 22 moves upward and the outer housing cover 12 moves upward, so that the closed portion no longer covers the centrifugal hole 212, and the water inside the closed portion enters between the outer housing 11 and the inner housing 21 through the oil-water separation membrane on the centrifugal hole 212. After the equipment is released to normal pressure, the temperature in the equipment is controlled to rise to remove acid, and the residual oil in the inner shell 21 is the low-phosphating oil.

The water body is treated in the same manner as the water phase in embodiment 1, but the water body is mainly acid water, and can be recycled after being collected, so that the collecting box can be preferably communicated with the inner shell 2 through a flexible hose, for example, an opening is formed at the top of the inner shell cover 22, and is communicated with the collecting box through the opening, so as to realize recycling of the water body.

The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.