Micro-channel phosphate ester production device

Abstract

The invention belongs to the technical field of chemical production, and particularly relates to a micro-channel phosphate ester production device. Comprising a micro-channel reactor, a horizontal pushing reactor and a microporous purification reactor, the micro-channel reactor comprises a reactor cylinder; a vertical micro-channel heat exchange tube is arranged in the barrel; a plurality of micro-channel reaction grooves are formed in the outer wall of the micro-channel heat exchange tube; the micro-channel reaction tank is communicated with the inner cavity of the reactor cylinder; the hydrogen chloride gas entrained with butanol generated by the invention is introduced into the microporous purification reactor to realize the separation of the hydrogen chloride gas and butanol; products and heat energy in the production process are recycled, so that the synthesis conversion rate of phosphorus oxychloride reaches 99%; meanwhile, the generation of reaction byproducts is reduced, and the purity of a main product is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical production, and in particular relates to a microchannel phosphate production device. Background Art

[0002] The raw materials for the manufacture of phosphate esters mainly include phosphoric acid, alcohol compounds and catalysts. Phosphoric acid is the main acidic raw material, alcohol compounds are nucleophilic reagents for esterification reactions, and catalysts are used to accelerate the reaction process. When selecting raw materials, factors such as purity, activity, and cost need to be considered to ensure the quality and economy of the product.

[0003] Phosphate esters are mainly produced by esterification of phosphoric acid and alcohol compounds. Esterification is a reversible reaction catalyzed by acid and base, and the reaction conditions need to be controlled to promote the forward reaction. In the process of producing phosphate esters, phosphoric acid and alcohol compounds react under the action of a catalyst to produce phosphate esters and water.

[0004] The phosphorus oxychloride (POCl3) method is an important method for the industrial synthesis of phosphate esters. The product obtained by this method is also a mixture of monoesters, diesters and triesters, but the content of monoesters is relatively large.

[0005] For the phosphorus oxychloride method, such as the preparation process of tributyl phosphate, it is difficult to obtain high-purity tributyl phosphate products due to the characteristics of tributyl phosphate itself and the constraints of production equipment. In industry, tributyl phosphate is generally synthesized by direct esterification of phosphorus oxychloride and n-butanol. In order to inhibit the hydrogen chloride generated in the reaction from continuing to react with n-butanol and tributyl phosphate to form chlorobutane, it is usually necessary to control the reaction temperature very low. It is difficult for traditional kettle reactors to control the temperature below 10°C, and the yield of tributyl phosphate is difficult to exceed 85%. Therefore, it is imperative and crucial to seek a stable production process for high-purity tributyl phosphate and its series products (including triisobutyl phosphate, trioctyl phosphate, etc.).

[0006] A microreactor is a device that conducts chemical reactions at a microscopic scale, usually consisting of a microchannel, a mixer, a separator, and a control unit. With the continuous advancement of micromachining technology and microfluidics technology, microreactors have gradually become a research hotspot in the fields of chemical synthesis, biomedicine, and materials science. Its characteristics include miniaturization, efficient mixing, rapid heat and mass transfer, and precise control. Its advantages are reducing the amount of reaction materials used, increasing the reaction rate and product purity, and achieving precise control of reaction conditions.

[0007] The existing microchannel reactor is provided with a microchannel with a channel width of 10 μm to 1000 μm. In the microchannel reactor, at least two fluids diverge through the microchannel and then meet each other. In the microchannel reactor, the fluid will be split, thereby reducing the distance of fluid diffusion and increasing the speed of fluid mixing, so that the fluid can be effectively mixed in a shorter time. However, the existing microchannel reactor has high requirements for the purity and stability of the reaction materials, resulting in some reactions being unsuitable for being carried out in the microchannel reactor; especially for the exothermic and gas-releasing reaction of the phosphorus oxychloride method, since the phosphorus oxychloride method releases HCl gas during the reaction process, when the released HCl gas cannot be discharged from the microchannel in time, it will cause the local pressure in the channel to increase, change the pressure of the reaction system, and cause the reaction rate to decrease; especially when the generated gas will react with the substances in the reaction system for a secondary reaction, it will inhibit the main reaction in the microchannel and increase the by-products. Summary of the invention

[0008] The present invention overcomes the shortcomings of the prior art and provides a microchannel phosphate production device; the device is suitable for a reaction system such as the phosphorus oxychloride method of phosphate esters that releases heat and gas and has side reactions, and solves the problem that in the existing microchannel reactor, the gas cannot be discharged from the reaction system in time or the discharge rate is low, resulting in an increase in the pressure of the reaction system or an increase in by-products.

[0009] In order to achieve the above object, the present invention is implemented through the following technical solutions.

[0010] A microchannel phosphate production device, comprising a microchannel reactor, a push reactor and a microporous purification reactor; The microfluidic reactor comprises a vertically arranged reactor cylinder, in which a plurality of vertical microchannel heat exchange tubes are arranged, and a circle of microchannel reaction grooves are arranged on the outer wall of the microchannel heat exchange tubes, and the microchannel reaction grooves are used for exothermic and gas-releasing reactions, and heat exchange fins are carved on the inner wall of the microchannel heat exchange tubes; the same material guide plate is connected to the tops of the plurality of microchannel heat exchange tubes, and a plurality of plug holes are arranged on the material guide plate, and the upper ends of the microchannel heat exchange tubes are plugged into the corresponding plug holes, and the material guide plate is provided with a distribution groove on the outer side of each plug hole, and the distribution groove is connected to the microchannel heat exchange tubes. A circle of microchannel guide holes is arranged on the side wall between the plug holes; a plurality of drainage grooves are arranged on the material guide plate, and the plurality of drainage grooves are connected with the plurality of distribution grooves in a one-to-one correspondence, and the reaction raw materials are introduced into each distribution groove through the drainage groove, and the distribution groove introduces the reaction raw materials into each microchannel reaction groove of the microchannel heat exchange tube through a circle of microchannel guide holes; the reactor cylinder is provided with an exhaust port, and the gas generated by the exothermic and gas-releasing reaction is directly discharged from the reactor cylinder through the exhaust port; a reaction solution discharge port is arranged on the lower side wall of the reactor cylinder; the microchannel heat exchange tube is used to pass the heat exchange medium; The push reactor comprises a horizontal kettle body arranged horizontally, a first microchannel heat exchanger is arranged above the interior of the horizontal kettle body, a second microchannel heat exchanger is arranged below the interior of the horizontal kettle body, a cooling medium circulation pipe is arranged inside the first microchannel heat exchanger, a heating medium circulation pipe is arranged inside the second microchannel heat exchanger, a reaction liquid inlet is arranged at the bottom of one end of the horizontal kettle body, a liquid discharge port is arranged at the bottom of the other end of the horizontal kettle body, and the reaction liquid inlet is connected to the micron dispersion mill through a feeding pipeline; a liquid level controller is also arranged at the bottom surface of the interior of the horizontal kettle body, the liquid level controller is arranged adjacent to the liquid discharge port, a plurality of microchannel holes are arranged on the liquid level controller, the top of the liquid level controller is located between the first microchannel heat exchanger and the second microchannel heat exchanger, and a liquid flow tank is arranged at the bottom of the liquid level controller; a third exhaust port is arranged at the top of the horizontal kettle body; The exhaust port arranged on the reactor cylinder and the third exhaust port arranged on the top of the horizontal kettle body are both connected to the microporous purification reactor; the reaction solution discharge port arranged on the reactor cylinder is connected to the micron dispersion mill.

[0011] Furthermore, two material guide trays are arranged inside the reactor cylinder, namely, the raw material A material guide tray and the raw material B material guide tray; the raw material A material guide tray and the raw material B material guide tray are arranged in parallel up and down, all the drainage grooves on the raw material A material guide tray are connected to the raw material A feed pipe, and all the drainage grooves on the raw material B material guide tray are connected to the raw material B feed pipe, and the two raw materials are respectively introduced into the drainage grooves of the raw material A material guide tray and the raw material B material guide tray through the raw material A feed pipe and the raw material B feed pipe, the drainage groove introduces the raw materials into the distribution groove, and then the distribution groove respectively flows the two raw materials into each microchannel reaction groove of the microchannel heat exchange tube through a circle of microchannel guide holes.

[0012] Furthermore, the upper end of the microchannel heat exchange tube remains closed and the lower end remains open, and a first coolant inlet pipe is inserted into each microchannel heat exchange tube, and the first coolant inlet pipe extends vertically upward from the bottom to the inside of the microchannel heat exchange tube, and the bottom of the reactor cylinder is fixedly provided with a first coolant storage cavity and a first coolant inlet cavity in sequence, and the coolant inlet at the bottom of the first coolant inlet pipe is connected to the interior of the first coolant inlet cavity; the lower end opening of the microchannel heat exchange tube is connected to the interior of the first coolant storage cavity.

[0013] Furthermore, one end of the first microchannel heat exchanger and the second microchannel heat exchanger are both kept closed and the other end are both kept open, the closed end of the first microchannel heat exchanger and the second microchannel heat exchanger are both facing the side of the discharge port, and the open end is both facing the side of the reaction liquid inlet; a medium return liquid cavity and a medium inlet liquid cavity are fixedly arranged in sequence at one end of the horizontal kettle body where the reaction liquid inlet is arranged, the inner part of the medium return liquid cavity is a cooling medium return liquid cavity on the upper side and a heating medium return liquid cavity on the lower side, and the inner part of the medium inlet liquid cavity is an upper side The cooling medium liquid inlet cavity is connected to the heating medium liquid inlet cavity on the lower side; the open end of the first microchannel heat exchanger is connected to the cooling medium liquid return cavity, the outlet end of the cooling medium circulation pipe is inserted from the open end of the first microchannel heat exchanger, and the inlet end of the cooling medium circulation pipe extends to the interior of the cooling medium liquid inlet cavity; the open end of the second microchannel heat exchanger is connected to the heating medium liquid return cavity, the outlet end of the heating medium circulation pipe is inserted from the open end of the second microchannel heat exchanger, and the inlet end of the heating medium circulation pipe extends to the interior of the heating medium liquid inlet cavity.

[0014] Furthermore, the microporous purification reactor includes a vertically arranged purification tank body, a plurality of shear gas inlet pipes are arranged in the purification tank body, the top of the shear gas inlet pipe is connected to the induced draft fan, and a micron ceramic bubbler is arranged at the bottom of the shear gas inlet pipe; a plurality of microchannel gas heat exchangers are arranged in the purification tank body, and the purification tank body is provided with a purified gas outlet.

[0015] Furthermore, the upper end of the microchannel gas heat exchanger remains closed and the lower end remains open, and a second coolant inlet pipe is inserted into each microchannel gas heat exchanger, and the second coolant inlet pipe extends vertically upward from the bottom to the inside of the microchannel gas heat exchanger, and a second coolant storage cavity and a second coolant inlet cavity are fixedly arranged at the lower end of the purification tank body in sequence, and the coolant inlet at the bottom of the second coolant inlet pipe is connected to the interior of the second coolant inlet cavity; the lower end opening of the microchannel gas heat exchanger is connected to the interior of the second coolant storage cavity.

[0016] Furthermore, the feed pipe of raw material A is connected to a high-level metering tank of phosphorus oxychloride; the feed pipe of raw material B is connected to a high-level metering tank of butanol; the purified gas outlet is connected to the high-level metering tank of butanol; the purification tank body is provided with a scrubbing liquid inlet, and the scrubbing liquid inlet is connected to the high-level metering tank of phosphorus oxychloride.

[0017] Furthermore, it also includes a pressure-changing self-circulating tank and an atomizing purge device; the reaction solution discharge port is connected to the pressure-changing self-circulating tank; the discharge port of the pressure-changing self-circulating tank is connected to the atomizing purge device through a multiphase flow shear atomizing pump; a nitrogen tank is connected to the pipeline connecting the discharge port of the pressure-changing self-circulating tank and the multiphase flow shear atomizing pump; the atomizing purge device is connected to a micron dispersion mill; and the micron dispersion mill is connected to a regenerated raw material tank and a fresh raw material tank.

[0018] Furthermore, it also includes a Venturi jet pressure reducing pump and a circulation pump; the third exhaust port arranged on the horizontal kettle body is connected to the Venturi jet pressure reducing pump through a gas pipeline, and a circulation passage is formed between the Venturi jet pressure reducing pump, the circulation pump and the pressure transformer self-circulation tank; the exhaust port arranged on the reactor cylinder is connected to the pressure transformer self-circulation tank; the pressure transformer self-circulation tank is connected to an induced draft fan, and the induced draft fan is connected to the microporous purification reactor through a pipeline.

[0019] Furthermore, it also includes a submersible pump, the first coolant storage cavity is provided with a first coolant drain port; the first coolant inlet cavity is provided with a first coolant inlet port; the transformer self-circulation tank is connected to the first coolant inlet port on the first coolant inlet cavity through the submersible pump; the first coolant drain port is connected to the transformer self-circulation tank.

[0020] The beneficial effects of the present invention compared with the prior art are as follows: 1. The present invention uses several microchannels on the outer wall of the microchannel heat exchange tube as reaction tanks for solution chemical reactions, and the interior of the microchannel heat exchange tube as a heat exchange channel, which increases the contact area of ​​the solution, improves the heat exchange capacity, and achieves the dual effects of reaction heat exchange and exhaust. Since the microchannel reaction tank is an open structure, the hydrogen chloride gas generated by the reaction substances in the microchannel reaction tank will be directly discharged from the exhaust port of the reactor cylinder without causing pressure buildup; at the same time, the hydrogen chloride gas generated by the reaction can be separated from the reaction system in time, further promoting the positive reaction of the reaction system, greatly improving the chemical reaction rate, while reducing the generation of reaction by-products and improving the purity of the main product.

[0021] 2. Through the chemical reaction of the microchannel reactor, a mixed product of halogenated ester, hydrogen chloride and butanol is generated. At the same time, a small amount of hydrogen chloride gas with butanol generated by the microchannel reactor can be led to the pressure-changing self-circulating tank and, together with the hydrogen chloride gas with butanol generated by the push reactor, it is converted into normal pressure through the induced draft fan and sent to the microporous purification reactor, so that the hydrogen chloride gas can be 100% purified and the raw material recycling can be realized.

[0022] 3. The present invention uses a microchannel reactor, a push reactor and a microporous purification reactor to complete the production of the final product phosphate compounds. The generated hydrogen chloride gas with butanol is introduced into the microporous purification reactor to separate the hydrogen chloride gas from butanol. The separated butanol is returned to the butanol high-level metering tank to achieve the recycling of raw materials. The separated hydrogen chloride gas is purer and can be used to make other products. Compared with the traditional system, the present invention is more environmentally friendly and energy-saving, and can achieve a 99% phosphorus oxychloride synthesis conversion rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The present invention will be further described in detail below in conjunction with the accompanying drawings: Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a schematic structural diagram of the microfluidic channel reactor of the present invention; Figure 3 Schematic diagram of the external structure of the microchannel heat exchange tube of the present invention; Figure 4 It is a schematic diagram of the flow direction of the heat exchange fluid in the microchannel heat exchange tube of the present invention; Figure 5 It is a schematic structural diagram of a microchannel reaction tank on the wall of a microchannel heat exchange tube according to the present invention; Figure 6 for Figure 5 A magnified cross-sectional view along the AA axis; Figure 7 This is a schematic diagram of the position structure of the guide plate for raw material A of the present invention; Figure 8 This is a schematic diagram of the structure of the material guide plate of raw material A of the present invention; Fig. 9 It is a schematic structural diagram of the push reactor of the present invention; Fig.10 It is a structural schematic diagram of the liquid level controller of the present invention; Fig.11 It is a structural schematic diagram of the microporous purification reactor of the present invention; Fig.12 This is a schematic diagram of the structure of the shear gas inlet pipe of the present invention; Among them, 1 is a feed pipe for raw material A, 2 is a feed pipe for raw material B, 3 is a guide plate for raw material A, 4 is a guide plate for raw material B, 5 is a first exhaust port, 6 is a second exhaust port, 7 is a microchannel heat exchange tube, 8 is a reactor barrel, 9 is a reaction solution discharge port, 10 is a first coolant inlet pipe, 11 is a first coolant discharge port, 12 is a first coolant storage cavity, 13 is a first coolant inlet, 14 is a first coolant inlet cavity, 15 is a microchannel 1 is a reaction tank, 16 is a distribution tank, 17 is a drainage tank, 18 is a heat exchange fin, 19 is a horizontal kettle, 20 is a first microchannel heat exchanger, 21 is a second microchannel heat exchanger, 22 is a reaction liquid inlet, 23 is a discharge port, 24 is a liquid level controller, 25 is a microchannel hole, 26 is a third exhaust port, 27 is a micron dispersion mill, 28 is a variable pressure self-circulation tank, 29 is a multiphase flow shear atomization pump, 30 is an atomization purge device, 31 is a regeneration source material tank, 32 is a fresh raw material tank, 33 is a venturi jet pressure reducing pump, 34 is a circulation pump, 35 is a submersible pump, 36 is an induced draft fan, 37 is a nitrogen tank, 38 is a purification tank, 39 is a shear gas inlet pipe, 40 is a micron ceramic bubbler, 41 is a microchannel gas heat exchanger, 42 is a liquid level detection sensor, 43 is a flow tank, 44 is a high-level metering tank for phosphorus oxychloride, 45 is a high-level metering tank for butanol, 46 is a purified gas outlet, and 47 is a gas washing liquid Inlet, 48 is the medium return cavity, 49 is the medium inlet cavity, 50 is the cooling medium return cavity, 51 is the heating medium return cavity, 52 is the cooling medium inlet cavity, 53 is the heating medium inlet cavity, 54 is the cooling medium circulation pipe, 55 is the heating medium circulation pipe, 56 is the second coolant inlet pipe, 57 is the second coolant storage cavity, 58 is the second coolant inlet cavity, 59 is the second coolant discharge port, and 60 is the second coolant inlet port. DETAILED DESCRIPTION

[0024] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer, the present invention is further described in detail in conjunction with the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. The technical solutions of the present invention are described in detail below in conjunction with the embodiments and the accompanying drawings, but the scope of protection is not limited thereto.

[0025] See also Figures 1 to 12 This embodiment proposes a microchannel tributyl phosphate production device, including a microchannel reactor, a push reactor, a microporous purification reactor, a variable pressure self-circulation tank 28 and an atomization purge device 30.

[0026] The microfluidic channel reactor comprises a reactor barrel 8, and the reactor barrel 8 is a vertically arranged hollow cylindrical structure.

[0027] A plurality of microchannel heat exchange tubes 7 are arranged in the reactor barrel 8. The microchannel heat exchange tubes 7 are hollow circular tubular structures arranged vertically. The upper end of the microchannel heat exchange tubes 7 remains closed, and the lower end of the microchannel heat exchange tubes 7 remains open. The inside of the microchannel heat exchange tubes 7 is used to pass heat exchange medium. A circle of microfluidic reaction tanks 15 arranged in a circular array are arranged on the outer wall of the microchannel heat exchange tubes 7. The microfluidic reaction tanks 15 are extended along the axial direction of the microchannel heat exchange tubes 7; the microfluidic reaction tanks 15 are carved on the outer wall of the microchannel heat exchange tubes 7, and the cross-section of the microfluidic reaction tanks 15 can have various forms such as triangles and rectangles. This structure makes the microfluidic reaction tanks 15 an open structure as a whole, and the microfluidic reaction tanks 15 are directly connected to the inner cavity of the reactor barrel 8.

[0028] The reactor cylinder 8 is provided with an exhaust port; the exhaust port includes a first exhaust port 5 and a second exhaust port 6; the first exhaust port 5 and the second exhaust port 6 are symmetrically arranged on both sides of the upper end of the side wall of the reactor cylinder 8, and the gas inside the reactor cylinder 8 is discharged to the outside of the reactor cylinder 8 through the first exhaust port 5 and the second exhaust port 6.

[0029] The microfluidic reaction tank 15 is used for the exothermic and degassing reaction. The gas generated by the exothermic and degassing reaction escapes from the microfluidic reaction tank 15 to the inside of the reactor cylinder 8, and can finally be directly discharged to the outside of the reactor cylinder 8 through the first exhaust port 5 and the second exhaust port 6. In this embodiment, the first exhaust port 5 and the second exhaust port 6 are connected to the exhaust device. Since the gas generated by the reaction can be discharged in a timely and large amount, the reactor cylinder 8 is in a negative pressure environment, which is more conducive to the exothermic and degassing reaction in the microfluidic reaction tank 15. In addition, the gas product is separated from the reaction system in time, avoiding the generation of secondary side reactions.

[0030] In order to improve the accuracy of feeding, the same material guide plate is connected to the top of several microchannel heat exchange tubes 7. The material guide plate is a horizontally arranged circular plate-like structure, and a plurality of circular plug holes that penetrate up and down are arranged on the material guide plate. The number of the plug holes is equal to the number of microchannel heat exchange tubes 7 and corresponds one to one. The upper end of the microchannel heat exchange tube 7 is plugged into the corresponding plug hole, and the outer wall of the microchannel heat exchange tube 7 is in contact with the inner wall of the plug hole. The material guide plate is provided with a coaxial annular distribution groove 16 on the outside of each plug hole, and a circle of microchannel guide holes arranged in a circular array is arranged on the side wall between the distribution groove 16 and the plug hole. The number of microchannel guide holes is equal to the number of microfluidic reaction grooves 15 on the microchannel heat exchange tube 7 and corresponds one to one. A plurality of drainage grooves 17 are arranged on the material guide plate, and the number of drainage grooves 17 is equal to the number of distribution grooves 16 and is connected one to one. The reaction raw materials are introduced into each distribution groove 16 through the drainage groove 17 , and the distribution groove 16 introduces the reaction raw materials into each microchannel reaction groove 15 of the microchannel heat exchange tube 7 through a circle of microchannel guide holes.

[0031] Multiple guide plates can be set according to the number of reaction raw materials. Different reaction raw materials enter the distribution groove 16 from the drainage grooves 17 on different guide plates respectively. The reaction raw materials inside the distribution groove 16 are introduced into each microfluidic reaction groove 15 from the microchannel guide holes to achieve rapid reaction.

[0032] In this embodiment, two guide plates are provided, namely, the raw material A guide plate 3 and the raw material B guide plate 4; the raw material A guide plate 3 and the raw material B guide plate 4 are arranged in parallel up and down, and are used to introduce the reaction raw materials A and the reaction raw materials B into the microchannel reaction tank 15 of all microchannel heat exchange tubes 7 respectively. All the drainage grooves 17 on the raw material A guide plate 3 are connected to the raw material A feed pipe 1, and all the drainage grooves 17 on the raw material B guide plate 4 are connected to the raw material B feed pipe 2. The raw material A feed pipe 1 is connected to a phosphorus oxychloride high-level metering tank 44; the raw material B feed pipe 2 is connected to a butanol high-level metering tank 45. Phosphorus oxychloride and butanol are introduced into the drainage groove 17 of the raw material A guide plate 3 and the raw material B guide plate 4 respectively through the raw material A feed pipe 1 and the raw material B feed pipe 2, and the drainage groove 17 introduces the raw materials into the distribution groove 16, and then the distribution groove 16 respectively flows the phosphorus oxychloride and butanol into each microchannel reaction groove 15 of the microchannel heat exchange tube 7 through a circle of microchannel guide holes.

[0033] Since the reaction between phosphorus oxychloride and butanol is an exothermic reaction, it is important to maintain an appropriate reaction temperature of the reaction system. In this embodiment, by reacting on the outer wall of the microchannel heat exchange tube 7, the inner wall of the microchannel heat exchange tube 7 is directly introduced with coolant, which can greatly improve the heat exchange efficiency. Specifically, a plurality of first coolant inlet pipes 10 are provided on the reactor barrel 8; the first coolant inlet pipes 10 correspond to the microchannel heat exchange tube 7 one by one, and the first coolant inlet pipes 10 extend vertically upward from the bottom into the microchannel heat exchange tube 7 and extend to the inner top of the microchannel heat exchange tube 7. The bottom of the first coolant inlet pipe 10 is the coolant inlet, and the coolant enters from the bottom of the first coolant inlet pipe 10 and flows out from the top of the first coolant inlet pipe 10 to the inner top of the microchannel heat exchange tube 7 under the action of the pressure pump, and then flows down along the top of the inner wall of the microchannel heat exchange tube 7, thereby realizing heat exchange for the chemical reaction carried out on the outer wall of the microchannel heat exchange tube 7. In order to further improve the heat exchange efficiency, a number of heat exchange fins 18 are carved on the inner wall of the microchannel heat exchange tube 7 .

[0034] The bottom of the reactor cylinder 8 is fixedly provided with a first cooling liquid storage cavity 12, and the bottom of the first cooling liquid storage cavity 12 is fixedly provided with a first cooling liquid inlet cavity 14. The cooling liquid inlet at the bottom of the first cooling liquid inlet pipe 10 is connected to the inside of the first cooling liquid inlet cavity 14; the lower end opening of the microchannel heat exchange tube 7 is connected to the inside of the first cooling liquid storage cavity 12, and a circle of microfluidic reaction grooves 15 outside the microchannel heat exchange tube 7 does not extend to the inside of the first cooling liquid storage cavity 12. The first cooling liquid storage cavity 12 is provided with a first cooling liquid discharge port 11; the first cooling liquid inlet cavity 14 is provided with a first cooling liquid inlet port 13. A cooling liquid circulation cooling channel is formed by the first cooling liquid storage cavity 12, the first cooling liquid inlet cavity 14, the first cooling liquid inlet pipe 10 and the internal channel of the microchannel heat exchange tube 7.

[0035] A reaction solution discharge port 9 is provided on the lower side wall of the reactor barrel 8 ; the reactants in the microfluidic reaction tank 15 flow down along the microfluidic reaction tank 15 and flow into the cavity of the reactor barrel 8 , and are finally discharged from the reaction solution discharge port 9 .

[0036] The push reactor comprises a horizontal kettle body 19, which is a horizontally arranged hollow cylindrical structure. A reaction liquid inlet 22 is arranged at the bottom of one end of the horizontal kettle body 19, and a liquid discharge port 23 is arranged at the bottom of the other end of the horizontal kettle body 19.

[0037] A first microchannel heat exchanger 20 is arranged above the interior of the horizontal kettle 19, and a second microchannel heat exchanger 21 is arranged below the interior of the horizontal kettle 19. The first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are both horizontally arranged hollow tubular structures. The axes of the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are parallel to the axis of the horizontal kettle 19, and one end of the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are both closed, and the other end is open. The closed ends of the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are both facing the side of the drain port 23, and the open ends are both facing the side of the reaction liquid inlet 22.

[0038] The structures of the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are similar to those of the microchannel heat exchange tube 7. The difference from the microchannel heat exchange tube 7 is that the outer walls of the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are not engraved with microfluidic reaction grooves 15 for reaction, but are engraved with spiral heat exchange grooves for increasing the heat exchange area.

[0039] A medium return cavity 48 and a medium inlet cavity 49 are fixedly arranged in sequence at one end of the horizontal kettle body 19 where the reaction liquid inlet 22 is arranged. The medium return cavity 48 and the medium inlet cavity 49 are both horizontally arranged hollow cylindrical structures. A horizontal first partition plate is fixedly arranged in the middle of the inner side of the medium return cavity 48, and the inside of the medium return cavity 48 is divided into a cooling medium return cavity 50 on the upper side and a heating medium return cavity 51 on the lower side by the first partition plate. A horizontal second partition plate is fixedly arranged in the middle of the inner side of the medium inlet cavity 49, and the inside of the medium inlet cavity 49 is divided into a cooling medium inlet cavity 52 on the upper side and a heating medium inlet cavity 53 on the lower side by the second partition plate. A cooling medium outlet is arranged at the lower end of the front side wall of the cooling medium return cavity 50, and a cooling medium inlet is arranged on the top wall of the cooling medium inlet cavity 52. A heating medium outlet is provided at the bottom end of the heating medium return chamber 51 , and a heating medium inlet is provided at the upper end of the front side wall of the heating medium inlet chamber 53 .

[0040] The open end of the first microchannel heat exchanger 20 is connected to the cooling medium liquid return chamber 50. A cooling medium circulation pipe 54 is inserted into the interior of the first microchannel heat exchanger 20. The outlet end of the cooling medium circulation pipe 54 is inserted from the open end of the first microchannel heat exchanger 20 and extends to the closed end of the first microchannel heat exchanger 20. The inlet end of the cooling medium circulation pipe 54 extends to the interior of the cooling medium liquid inlet chamber 52. The cooling medium in the cooling medium liquid inlet chamber 52 enters from the inlet end of the cooling medium circulation pipe 54, and then flows out from the interior of the first microchannel heat exchanger 20 to the interior of the cooling medium liquid return chamber 50. The cooling medium liquid inlet chamber 52, the cooling medium circulation pipe 54, the interior of the first microchannel heat exchanger 20, and the cooling medium liquid return chamber 50 constitute a cooling medium circulation cooling channel.

[0041] The open end of the second microchannel heat exchanger 21 is connected to the heating medium liquid return chamber 51. A heating medium circulation pipe 55 is inserted into the interior of the second microchannel heat exchanger 21. The outlet end of the heating medium circulation pipe 55 is inserted from the open end of the second microchannel heat exchanger 21 and extends to the closed end of the second microchannel heat exchanger 21. The inlet end of the heating medium circulation pipe 55 extends to the interior of the heating medium liquid inlet chamber 53. The heating medium in the heating medium liquid inlet chamber 53 enters from the inlet end of the heating medium circulation pipe 55, and then flows out from the interior of the second microchannel heat exchanger 21 to the interior of the heating medium liquid return chamber 51. The heating medium liquid inlet chamber 53, the heating medium circulation pipe 55, the interior of the second microchannel heat exchanger 21, and the heating medium liquid return chamber 51 constitute a heating medium circulation heating channel.

[0042] The reaction liquid inlet 22 of the horizontal kettle 19 is connected to the micron dispersing mill 27 through a feeding pipeline; the reaction solution discharge port 9 of the reactor barrel 8 is connected to the variable pressure self-circulating tank 28; the discharge port of the variable pressure self-circulating tank 28 is connected to the atomizing purge device 30 through a multiphase flow shearing atomizing pump 29; the atomizing purge device 30 is connected to the micron dispersing mill 27. The product after the esterification reaction in the microchannel reaction tank 15 enters the variable pressure self-circulating tank 28 through the reaction solution discharge port 9, and then enters the horizontal kettle 19 through the multiphase flow shearing atomizing pump 29, the atomizing purge device 30, and the micron dispersing mill 27 in sequence for deep esterification reaction. The second microchannel heat exchanger 21 is passed with a high temperature heat exchange medium to provide the necessary temperature conditions for the deep esterification reaction. In this process, a part of hydrogen chloride gas entrained with butanol will also be generated. This part of gas is refluxed to the horizontal kettle 19 through the condensation of the first microchannel heat exchanger 20 for further reaction. The micron dispersing mill 27 is used to further grind the esterification reaction product to reduce the particle size of the esterification reaction product, so as to promote the subsequent deep esterification reaction. The micron dispersing mill 27 is connected to a regeneration raw material tank 31 (containing recovered butanol) and a fresh raw material tank 32 (containing butanol). A nitrogen tank 37 is connected to the pipeline connecting the discharge port of the variable pressure self-circulating tank 28 and the multiphase flow shear atomizing pump 29.

[0043] A liquid level controller 24 is also provided at the bottom of the horizontal kettle 19. The liquid level controller 24 is provided near the drain port 23 and is located on the side of the drain port 23 close to the reaction liquid inlet 22; the top of the liquid level controller 24 is located between the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21. The liquid level controller 24 is provided with a plurality of microchannel holes 25 that are through on both sides, and the extension direction of the microchannel holes 25 is parallel to the axial direction of the horizontal kettle 19; the bottom of the liquid level controller 24 is provided with a plurality of flow grooves 43 that are through on both sides, and the extension direction of the flow grooves 43 is parallel to the extension direction of the microchannel holes 25. A liquid level detection sensor 42 is provided in the horizontal kettle 19, and the liquid level detection sensor 42 is located on the side of the liquid level controller 24 close to the reaction liquid inlet 22. After the deep esterification reaction product in the horizontal kettle 19 reaches a certain liquid level, it overflows from the top of the liquid level controller 24 and flows to the drain port 23 to be discharged to obtain the final product tributyl phosphate. When the horizontal kettle body 19 needs to be emptied, the residual liquid in the horizontal kettle body 19 will be drained through a plurality of microchannel holes 25 provided on the liquid level controller 24 and a liquid flow trough 43 provided at the bottom.

[0044] The top of the horizontal kettle 19 is provided with a third exhaust port 26; the third exhaust port 26 is connected to the venturi jet pressure reducing pump 33 through a gas pipeline, and a circulation passage is formed between the venturi jet pressure reducing pump 33, the circulation pump 34 and the pressure-changing self-circulating tank 28. The first exhaust port 5 and the second exhaust port 6 provided on the reactor cylinder 8 are both connected to the pressure-changing self-circulating tank 28; the pressure-changing self-circulating tank 28 is connected to an induced draft fan 36, and the induced draft fan 36 is connected to the microporous purification reactor through a pipeline. The hydrogen chloride mixed gas from the horizontal kettle 19 and the reactor cylinder 8 enters the pressure-changing self-circulating tank 28 and is sent to the microporous purification reactor through the induced draft fan 36 for further purification.

[0045] The microporous purification reactor comprises a purification tank 38, which is a hollow circular cylindrical structure arranged vertically. Multiple vertical shear gas inlet pipes 39 are evenly arranged in the purification tank 38, the top of the shear gas inlet pipe 39 is connected to the induced draft fan 36, and a micron ceramic bubbler 40 is arranged at the bottom of the shear gas inlet pipe 39. The hydrogen chloride mixed gas entering the purification tank 38 is released into the purification tank 38 through the multiple shear gas inlet pipes 39 and the micron ceramic bubbler 40. The upper end of the side wall of the purification tank 38 is provided with a scrubbing liquid inlet 47, which is connected to a phosphorus oxychloride high-level metering tank 44, and the phosphorus oxychloride in the phosphorus oxychloride high-level metering tank 44 enters the purification tank 38 to react with the residual butanol in the gas to remove the butanol in the hydrogen chloride gas. The upper end of the side wall of the purification tank 38 is provided with a purified gas outlet 46, which is connected to the butanol high-level metering tank 45. The scrubbing liquid inlet 47 and the purified gas outlet 46 are respectively located on both sides of the purification tank 38.

[0046] A plurality of microchannel gas heat exchangers 41 are evenly distributed in the purification tank body 38. The structure of the microchannel gas heat exchanger 41 in this embodiment is the same as that of the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21. The upper end of the microchannel gas heat exchanger 41 in this embodiment remains closed and the lower end remains open.

[0047] A plurality of second coolant inlet pipes 56 are provided inside the purification tank 38; the second coolant inlet pipes 56 correspond to the microchannel gas heat exchangers 41 one by one, and the second coolant inlet pipes 56 extend vertically upward from the bottom into the microchannel gas heat exchanger 41 and extend to the inner top of the microchannel gas heat exchanger 41. The bottom of the second coolant inlet pipe 56 is a coolant inlet, and the coolant enters from the bottom of the second coolant inlet pipe 56 and flows out from the top of the second coolant inlet pipe 56 to the inner top of the microchannel gas heat exchanger 41, and then flows down along the top of the inner wall of the microchannel gas heat exchanger 41, thereby realizing heat exchange for the reaction carried out outside the microchannel gas heat exchanger 41.

[0048] A second coolant storage cavity 57 and a second coolant inlet cavity 58 are fixedly arranged in sequence at the lower end of the purification tank 38. The coolant inlet at the bottom of the second coolant inlet pipe 56 is connected to the inside of the second coolant inlet cavity 58; the lower end opening of the microchannel gas heat exchanger 41 is connected to the inside of the second coolant storage cavity 57, and a second coolant discharge port 59 is arranged at the lower end of the side wall of the second coolant storage cavity 57; and a second coolant inlet 60 is arranged at the bottom of the second coolant inlet cavity 58. A coolant circulation cooling channel is formed by the second coolant storage cavity 57, the second coolant inlet cavity 58, the second coolant inlet pipe 56 and the internal channel of the microchannel gas heat exchanger 41.

[0049] In order to make full use of the heat carried by the esterification reaction product, the pressure-changing self-circulating tank 28 is connected to the first coolant inlet 13 on the first coolant inlet cavity 14 and the second coolant inlet on the second coolant inlet cavity 58 through the submerged pump 35; the first coolant discharge port 11 and the second coolant discharge port 59 are both connected to the pressure-changing self-circulating tank 28. The submerged pump 35 is used to send the esterification reaction product inside the pressure-changing self-circulating tank 28 to the first coolant inlet cavity 14 and the second coolant inlet cavity 58 for heat exchange, and the esterification reaction product after heat extraction is sent back to the pressure-changing self-circulating tank 28 for the next step of deep esterification reaction.

[0050] In industry, tributyl phosphate is generally synthesized by direct esterification of phosphorus oxychloride and n-butanol. In order to inhibit the hydrogen chloride generated in the reaction from continuing to react with n-butanol and tributyl phosphate to generate chlorobutane, it is usually necessary to control the reaction temperature very low. It is difficult for traditional kettle reactors to control the temperature below 10°C, and the yield of tributyl phosphate is difficult to exceed 85%. The microchannel tributyl phosphate production device described in this embodiment is suitable for reaction systems with gas generation and side reactions, and solves the problem that in existing microchannel reactors, the gas cannot be discharged from the reaction system in time or the discharge rate is low, resulting in an increase in the pressure of the reaction system or an increase in by-products.

[0051] The chemical reaction principle of tributyl phosphate is to mix phosphorus oxychloride and butanol, and then generate tributyl phosphate and hydrogen chloride after a three-stage esterification reaction. The main reaction equation is as follows: POCl3+3C4H9OH→(C4H9O)3PO+3HCl; At the same time, the following side reactions occur: (C4H9O)3PO+HCl→(C4H9O)2POOH+C4H9Cl; C4H9OH+HCl→C4H9Cl+H2O.

[0052] The key technical difficulty is that the organic esterification synthesis reaction is extremely exothermic, and it is difficult to control the reaction temperature in a traditional kettle reactor, which is prone to violent boiling. In addition, hydrogen chloride is difficult to be separated from the reaction system in large quantities and quickly, and the generation rate of by-products is high.

[0053] The above problems can be solved by using a microchannel tributyl phosphate production device proposed in this embodiment. The working principle is as follows: Phosphorus oxychloride and butanol are introduced into the drainage groove 17 of the raw material A guide plate 3 and the raw material B guide plate 4 through the raw material A feed pipe 1 and the raw material B feed pipe 2, respectively. The drainage groove 17 introduces the raw materials into the distribution groove 16, and then the distribution groove 16 flows the phosphorus oxychloride and butanol into each microchannel reaction groove 15 of the microchannel heat exchange tube 7 through a circle of microchannel guide holes. In addition, a coolant flows through the inner wall of the microchannel heat exchange tube 7 to continuously exchange heat with the reaction liquid on the outer wall of the microchannel heat exchange tube 7, and quickly reduce the reaction temperature; at the same time, the first exhaust port 5 and the second exhaust port 6 are connected to the vacuum pump, and the reactor cylinder 8 forms a negative pressure under the action of the vacuum pump. The hydrogen chloride generated by the reaction dissipates from the reaction system in the form of gas into the reactor cylinder 8 under the negative pressure environment, and is discharged from the first exhaust port 5 and the second exhaust port 6 in time, thereby suppressing the occurrence of side reactions involving hydrogen chloride. Phosphorus oxychloride and n-butanol react in the microfluidic reaction tank 15 and flow downward along the microfluidic reaction tank 15 under the action of gravity to generate a mixed product of halogenated ester, hydrogen chloride and butanol. Finally, the mixed product gathers in the cavity of the reactor barrel 8 and is discharged to the pressure-changing self-circulating tank 28 through the reaction solution discharge port 9.

[0054] A small amount of hydrogen chloride gas containing butanol generated in the microchannel reactor enters the pressure-changing self-circulating tank 28 and, together with the hydrogen chloride gas containing butanol generated in the push reactor, passes through the induced draft fan 36, is converted to normal pressure and sent to the microporous purification reactor for 100% purification treatment to achieve raw material recycling.

[0055] In actual application, the low-temperature halogenated ester in the pressure-changing self-circulating tank 28 is respectively sent to the microchannel reactor and the microporous purification reactor by the submersible pump 35 to take away the heat generated in the two devices. The heated halogenated ester is returned to the pressure-changing self-circulating tank 28 through the pressure difference.

[0056] The mixed product of halogenated ester, hydrogen chloride and butanol in the pressure-changing self-circulating tank 28 passes through the circulation pump 34, enters the venturi jet pressure-reducing pump 33, and then flows back to the pressure-changing self-circulating tank 28 to form a cycle. At the same time, the hydrogen chloride gas with butanol produced by the push reactor is also drawn into the venturi jet pressure-reducing pump 33, flows into the pressure-changing self-circulating tank 28 to participate in the circulation, so that the push reactor forms a negative pressure.

[0057] The halogenated ester, hydrogen chloride and butanol mixed product in the variable pressure self-circulation tank 28 and the external nitrogen provided by the nitrogen tank 37 are sent to the atomization and purge device 30 by the multiphase flow shear atomization pump 29 to separate the hydrogen chloride. The halogenated ester and butanol mixture generated after treatment enters the micron dispersion mill 27, and a certain proportion of butanol and recovered butanol are added at the same time. The three are processed by the micron dispersion mill 27 to form a molecular-level mixture and sent to the push reactor for reaction to generate a mixture of tributyl ester and butanol. The subsequent process separates it to obtain the final product tributyl phosphate, and the separated butanol is stored in the regeneration raw material tank 31 for recycling. According to actual needs, multiple push reactors can be connected in series to form a thorough reaction.

[0058] The raw materials in the phosphorus oxychloride high-level metering tank 44 enter the microporous purification reactor as a scrubbing liquid to react with the incoming hydrogen chloride gas entrained with butanol. The butanol and halogenated ester mixture overflowing during the reaction is returned to the microchannel reactor, realizing the closed-loop use of raw materials in the entire process.

[0059] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations falling within the meaning and scope of the equivalent elements of the claims be included in the invention. Any reference numeral in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A microchannel phosphate production device, characterized in that: Including microfluidic reactor, push reactor and microporous purification reactor; The microfluidic reactor comprises a vertically arranged reactor cylinder (8), a plurality of vertical microchannel heat exchange tubes (7) are arranged in the reactor cylinder (8), a circle of microchannel reaction grooves (15) are arranged on the outer wall of the microchannel heat exchange tube (7), the microchannel reaction grooves (15) are used for exothermic and gas release reactions, and heat exchange fins (18) are carved on the inner wall of the microchannel heat exchange tube (7); the same material guide plate is connected to the top of the plurality of microchannel heat exchange tubes (7), a plurality of plug holes are arranged on the material guide plate, the upper end of the microchannel heat exchange tube (7) is plugged into the corresponding plug holes, and the material guide plate is provided with a distribution groove (16) on the outer side of each plug hole, and the distribution groove (16) and the plug hole are connected. A circle of microchannel guide holes is arranged on the side wall between the two components; a plurality of drainage grooves (17) are arranged on the guide plate, and the plurality of drainage grooves (17) are connected to the plurality of distribution grooves (16) in a one-to-one correspondence, and the reaction raw materials are introduced into each distribution groove (16) through the drainage grooves (17), and the distribution grooves (16) introduce the reaction raw materials into each microchannel reaction groove (15) of the microchannel heat exchange tube (7) through a circle of microchannel guide holes; the reactor cylinder (8) is provided with an exhaust port, and the gas generated by the exothermic and gas-releasing reaction is directly discharged from the reactor cylinder (8) through the exhaust port; the lower side wall of the reactor cylinder (8) is provided with a reaction solution discharge port (9); the microchannel heat exchange tube (7) is used to pass a heat exchange medium; The push reactor comprises a horizontal kettle body (19) arranged horizontally, a first microchannel heat exchanger (20) being arranged above the interior of the horizontal kettle body (19), a second microchannel heat exchanger (21) being arranged below the interior of the horizontal kettle body (19), a cooling medium circulation pipe (54) being arranged inside the first microchannel heat exchanger (20), a heating medium circulation pipe (55) being arranged inside the second microchannel heat exchanger (21), a reaction liquid inlet (22) being arranged at the bottom of one end of the horizontal kettle body (19), and a liquid discharge port (23) being arranged at the bottom of the other end of the horizontal kettle body (19), The reaction liquid inlet (22) is connected to the micron dispersion mill (27) via a feeding pipeline; a liquid level controller (24) is also provided at the bottom surface of the interior of the horizontal kettle body (19); the liquid level controller (24) is provided adjacent to the liquid discharge port (23); a plurality of microchannel holes (25) are provided on the liquid level controller (24); the top of the liquid level controller (24) is located between the first microchannel heat exchanger (20) and the second microchannel heat exchanger (21); a liquid flow trough (43) is provided at the bottom of the liquid level controller (24); and a third exhaust port (26) is provided at the top of the horizontal kettle body (19); The exhaust port provided on the reactor barrel (8) and the third exhaust port (26) provided on the top of the horizontal kettle body (19) are both connected to the microporous purification reactor; and the reaction solution discharge port (9) provided on the reactor barrel (8) is connected to the micron dispersion mill (27).

2. A microchannel phosphate production device according to claim 1, characterized in that: Two material guide plates are arranged inside the reactor barrel (8), namely, a material guide plate (3) for raw material A and a material guide plate (4) for raw material B; the material guide plate (3) for raw material A and the material guide plate (4) for raw material B are arranged in parallel up and down; all the drainage grooves (17) on the material guide plate (3) for raw material A are connected to the material feed pipe (1); all the drainage grooves (17) on the material guide plate (4) for raw material B are connected to the material feed pipe (2); the two raw materials are respectively introduced into the drainage grooves (17) of the material guide plate (3) for raw material A and the material guide plate (4) for raw material B through the material feed pipe (1) for raw material A and the material feed pipe (2); the drainage grooves (17) introduce the raw materials into the distribution grooves (16); and then the distribution grooves (16) respectively flow the two raw materials into the respective microchannel reaction grooves (15) of the microchannel heat exchange tube (7) through a circle of microchannel guide holes.

3. A microchannel phosphate production device according to claim 1, characterized in that: The upper end of the microchannel heat exchange tube (7) remains closed and the lower end remains open. A first cooling liquid inlet pipe (10) is inserted into the interior of each microchannel heat exchange tube (7). The first cooling liquid inlet pipe (10) extends vertically upward from the bottom to the inside of the microchannel heat exchange tube (7). The bottom of the reactor cylinder (8) is fixedly provided with a first cooling liquid storage cavity (12) and a first cooling liquid inlet cavity (14) in sequence. The cooling liquid inlet at the bottom of the first cooling liquid inlet pipe (10) is connected to the interior of the first cooling liquid inlet cavity (14); the lower end opening of the microchannel heat exchange tube (7) is connected to the interior of the first cooling liquid storage cavity (12).

4. A microchannel phosphate production device according to claim 1, characterized in that: One end of the first microchannel heat exchanger (20) and the second microchannel heat exchanger (21) are both kept closed and the other end are both kept open; the closed ends of the first microchannel heat exchanger (20) and the second microchannel heat exchanger (21) are both oriented toward the side of the liquid discharge port (23), and the open ends are both oriented toward the side of the reaction liquid inlet (22); a medium liquid return cavity (48) and a medium liquid inlet cavity (49) are fixedly arranged in sequence at one end of the horizontal kettle body (19) provided with the reaction liquid inlet (22); the interior of the medium liquid return cavity (48) is divided into an upper cooling medium liquid return cavity (50) and a lower heating medium liquid return cavity (51); the interior of the medium liquid inlet cavity (49) is divided into an upper cooling medium liquid return cavity (50) and a lower heating medium liquid return cavity (51); The medium liquid inlet cavity (52) is connected to the heating medium liquid inlet cavity (53) at the lower side; the open end of the first microchannel heat exchanger (20) is connected to the cooling medium liquid return cavity (50), the outlet end of the cooling medium circulation pipe (54) is inserted from the open end of the first microchannel heat exchanger (20), and the inlet end of the cooling medium circulation pipe (54) extends to the interior of the cooling medium liquid inlet cavity (52); the open end of the second microchannel heat exchanger (21) is connected to the heating medium liquid return cavity (51), the outlet end of the heating medium circulation pipe (55) is inserted from the open end of the second microchannel heat exchanger (21), and the inlet end of the heating medium circulation pipe (55) extends to the interior of the heating medium liquid inlet cavity (53).

5. A microchannel phosphate production device according to claim 2, characterized in that: The microporous purification reactor comprises a vertically arranged purification tank body (38), wherein a plurality of shear gas inlet pipes (39) are arranged in the purification tank body (38), wherein the top of the shear gas inlet pipe (39) is connected to the induced draft fan (36), and a micron ceramic bubbler (40) is arranged at the bottom of the shear gas inlet pipe (39); a plurality of microchannel gas heat exchangers (41) are arranged in the purification tank body (38), and the purification tank body (38) is provided with a purified gas outlet (46).

6. A microchannel phosphate production device according to claim 5, characterized in that: The upper end of the microchannel gas heat exchanger (41) remains closed and the lower end remains open. A second coolant inlet pipe (56) is inserted into each microchannel gas heat exchanger (41). The second coolant inlet pipe (56) extends vertically upward from the bottom to the inside of the microchannel gas heat exchanger (41). A second coolant storage cavity (57) and a second coolant inlet cavity (58) are fixedly arranged in sequence at the lower end of the purification tank (38). The coolant inlet at the bottom of the second coolant inlet pipe (56) is connected to the inside of the second coolant inlet cavity (58); the lower end opening of the microchannel gas heat exchanger (41) is connected to the inside of the second coolant storage cavity (57).

7. A microchannel phosphate production device according to claim 5, characterized in that: The feed pipe (1) for raw material A is connected to a phosphorus oxychloride high-level metering tank (44); the feed pipe (2) for raw material B is connected to a butanol high-level metering tank (45); the purified gas outlet (46) is connected to the butanol high-level metering tank (45); the purification tank body (38) is provided with a scrubbing liquid inlet (47), and the scrubbing liquid inlet (47) is connected to the phosphorus oxychloride high-level metering tank (44).

8. A microchannel phosphate production device according to claim 3, characterized in that: It also includes a pressure-variable self-circulating tank (28) and an atomizing purge device (30); the reaction solution discharge port (9) is connected to the pressure-variable self-circulating tank (28); the discharge port of the pressure-variable self-circulating tank (28) is connected to the atomizing purge device (30) via a multiphase flow shearing atomizing pump (29); a nitrogen tank (37) is connected to the pipeline connecting the discharge port of the pressure-variable self-circulating tank (28) and the multiphase flow shearing atomizing pump (29); the atomizing purge device (30) is connected to a micron dispersion mill (27); and the micron dispersion mill (27) is connected to a regenerated raw material tank (31) and a fresh raw material tank (32).

9. A microchannel phosphate production device according to claim 8, characterized in that: It also includes a Venturi jet pressure reducing pump (33) and a circulation pump (34); a third exhaust port (26) provided on the horizontal kettle body (19) is connected to the Venturi jet pressure reducing pump (33) through a gas pipeline, and a circulation passage is formed between the Venturi jet pressure reducing pump (33), the circulation pump (34) and the pressure-changing self-circulating tank (28); the exhaust port provided on the reactor cylinder (8) is connected to the pressure-changing self-circulating tank (28); the pressure-changing self-circulating tank (28) is connected to an induced draft fan (36), and the induced draft fan (36) is connected to the microporous purification reactor through a pipeline.

10. The microchannel phosphate production device according to claim 8, characterized in that: It also includes a submersible pump (35); the first coolant storage cavity (12) is provided with a first coolant discharge port (11); the first coolant inlet cavity (14) is provided with a first coolant inlet port (13); the variable pressure self-circulation tank (28) is connected to the first coolant inlet port (13) on the first coolant inlet cavity (14) via the submersible pump (35); and the first coolant discharge port (11) is connected to the variable pressure self-circulation tank (28).

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