A microchannel production device for phosphates

Abstract

The present invention belongs to the technical field of chemical production, and specifically relates to a production device for microchannel phosphate esters; it includes a microchannel reactor, a plug flow reactor, and a microporous purification reactor; the microchannel reactor includes a reactor cylinder body; a vertical microchannel heat exchange tube is arranged inside the cylinder body; a number of microchannel reaction grooves are arranged on the outer wall of the microchannel heat exchange tube; the microchannel reaction grooves are communicated with the inner cavity of the reactor cylinder body; the hydrogen chloride gas entrained with butanol generated by the present invention is introduced into the microporous purification reactor to realize the separation of hydrogen chloride gas and butanol; the products and heat energy in the production process are recycled, so that the synthesis conversion rate of phosphorus oxychloride reaches 99%; at the same time, the generation of reaction by-products is reduced, and the purity of the main product is improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of chemical production, and particularly relates to a microchannel device for producing phosphate esters. Background Art

[0002] The raw materials for manufacturing phosphate esters mainly include phosphoric acid, alcohol compounds and catalysts. Phosphoric acid is the main acidic raw material, alcohol compounds are the nucleophilic reagents for the esterification reaction, 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 products.

[0003] The manufacture of phosphate esters is mainly obtained by the esterification reaction of phosphoric acid with alcohol compounds. The esterification reaction is a reversible reaction catalyzed by acid and base, and the reaction conditions need to be controlled to promote the forward reaction. In the manufacturing process of phosphate esters, phosphoric acid reacts with alcohol compounds under the action of a catalyst to generate phosphate esters and water.

[0004] The phosphorus oxychloride (POCl3) method is an important method for industrial synthesis of phosphate esters. The products obtained by this method are also mixtures of monoester, diester and triester, but the content of monoester is relatively large.

[0005] For the phosphorus oxychloride method, in the preparation process of tributyl phosphate, due to the characteristics of tributyl phosphate itself and the constraints of production equipment, it is difficult to obtain high-purity tributyl phosphate products. Industrially, tributyl phosphate is generally directly esterified and synthesized from phosphorus oxychloride and n-butanol. In order to inhibit the continuous reaction of hydrogen chloride generated in the reaction with n-butanol and tributyl phosphate to form chlorobutane, it is usually necessary to control a very low reaction temperature. It is difficult for traditional batch 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 production process for stably producing high-purity tributyl phosphate and its series products (including triisobutyl phosphate, trioctyl phosphate, etc.).

[0006] A microreactor is a device for carrying out chemical reactions at the microscale, usually composed of microchannels, mixers, separators and control units. With the continuous progress of microfabrication technology and microfluidics technology, microreactors have gradually become a research hotspot in the fields of chemical synthesis, biomedicine, materials science, etc. Their characteristics include miniaturization, efficient mixing, rapid heat and mass transfer, and precise control. The advantages are reducing the usage amount of reaction materials, increasing the reaction rate and product purity, and achieving precise control of reaction conditions.

[0007] The existing microchannel reactor is provided with microchannels having a channel width of 10 μm to 1000 μm. In the microchannel reactor, at least two fluids diverge through the microchannels and then converge with each other. In the microchannel reactor, the fluid will be split, thereby reducing the distance of fluid diffusion and increasing the fluid mixing speed, and 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 that some reactions are not suitable to be carried out in the microchannel reactor; especially for the reaction of phosphoryl chloride method which is exothermic and gas-evolving, since HCl gas is released during the reaction of phosphoryl chloride method, when the released HCl gas cannot be discharged from the microchannel in time, it will cause an increase in the local pressure in the channel, change the pressure of the reaction system, and lead to a decrease in the reaction rate; especially when the generated gas will undergo a secondary reaction with the substances in the reaction system, it will inhibit the main reaction in the microchannel and increase the by-products. Summary of the Invention

[0008] The present invention overcomes the deficiencies of the prior art and provides a microchannel phosphoric ester production device; it is applicable to reaction systems such as the phosphoryl chloride method of phosphoric esters which are exothermic, gas-evolving and have side reactions, and solves the problems that in the existing microchannel reactor for such reaction systems, due to the inability of gas to be discharged from the reaction system in time or the discharge rate being low, the pressure of the reaction system increases or the by-products increase.

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

[0010] A microchannel phosphoric ester production device includes a microchannel reactor, a plug flow reactor and a microporous purification reactor;

[0011] 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;

[0012] 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;

[0013] 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.

[0014] Further, two material guiding plates are arranged inside the reactor cylinder body, namely a material A guiding plate and a material B guiding plate; the material A guiding plate and the material B guiding plate are arranged in parallel up and down. All the drainage grooves on the material A guiding plate are connected to the material A feed pipe, and all the drainage grooves on the material B guiding plate are connected to the material B feed pipe. The two raw materials are respectively introduced into the drainage grooves of the material A guiding plate and the material B guiding plate through the material A feed pipe and the material B feed pipe. The drainage grooves introduce the raw materials into the distribution groove, and then the distribution groove respectively flows the two raw materials into each micro-channel reaction groove of the micro-channel heat exchange pipe through a circle of micro-channel diversion holes.

[0015] Further, the upper end of the micro-channel heat exchange pipe is kept closed and the lower end is kept open. A first coolant inlet pipe is inserted into each micro-channel heat exchange pipe. The first coolant inlet pipe extends vertically upward from the bottom into the inner side of the micro-channel heat exchange pipe. A first coolant storage cavity and a first coolant inlet cavity are sequentially fixed at the bottom of the reactor cylinder body. The coolant inlet at the bottom of the first coolant inlet pipe is communicated with the inside of the first coolant inlet cavity; the lower end opening of the micro-channel heat exchange pipe is communicated with the inside of the first coolant storage cavity.

[0016] Further, one end of the first micro-channel heat exchanger and the second micro-channel heat exchanger is kept closed and the other end is kept open. The closed ends of the first micro-channel heat exchanger and the second micro-channel heat exchanger both face the side of the liquid discharge port, and the open ends both face the side of the reaction liquid inlet port; a medium return liquid cavity and a medium inlet cavity are sequentially fixed at the end of the horizontal kettle body where the reaction liquid inlet port is arranged. The inside of the medium return liquid cavity is divided into an upper cooling medium return liquid cavity and a lower heating medium return liquid cavity, and the inside of the medium inlet cavity is divided into an upper cooling medium inlet cavity and a lower heating medium inlet cavity; the open end of the first micro-channel heat exchanger is communicated with the cooling medium return liquid cavity. The outlet end of the cooling medium circulation pipe is inserted into the open end of the first micro-channel heat exchanger, and the inlet end of the cooling medium circulation pipe extends into the inside of the cooling medium inlet cavity; the open end of the second micro-channel heat exchanger is communicated with the heating medium return liquid cavity. The outlet end of the heating medium circulation pipe is inserted into the open end of the second micro-channel heat exchanger, and the inlet end of the heating medium circulation pipe extends into the inside of the heating medium inlet cavity.

[0017] Further, the microporous purification reactor includes a vertically arranged purification tank body. A plurality of shear gas inlet pipes are arranged inside the purification tank body. The top of the shear gas inlet pipe is connected to a blower, and a micron ceramic bubbler is arranged at the bottom of the shear gas inlet pipe; a plurality of micro-channel gas heat exchangers are arranged inside the purification tank body, and a purified gas outlet is arranged on the purification tank body.

[0018] Furthermore, the upper end of the microchannel gas heat exchanger is kept closed and the lower end is kept open. A second coolant inlet pipe is inserted into each microchannel gas heat exchanger. The second coolant inlet pipe extends vertically upward from the bottom into the inside of the microchannel gas heat exchanger. A second coolant storage cavity and a second coolant inlet cavity are sequentially fixed at the lower end of the purification tank body. The coolant inlet at the bottom of the second coolant inlet pipe is communicated with the inside of the second coolant inlet cavity; the lower end opening of the microchannel gas heat exchanger is communicated with the inside of the second coolant storage cavity.

[0019] Furthermore, the raw material A feed pipe is connected to a phosphorus oxychloride high-level metering tank; the raw material B feed pipe is connected to a butanol high-level metering tank; the purified gas outlet is connected to the butanol high-level metering tank; the purification tank body is provided with a washing liquid inlet, and the washing liquid inlet is connected to the phosphorus oxychloride high-level metering tank.

[0020] Furthermore, it also includes a variable-pressure self-circulation tank and an atomizing purging device; the reaction solution drain port is connected to the variable-pressure self-circulation tank; the discharge port of the variable-pressure self-circulation tank is connected to the atomizing purging device through a multiphase flow shear atomizing pump; a nitrogen tank is connected to the pipeline where the discharge port of the variable-pressure self-circulation tank is connected to the multiphase flow shear atomizing pump; the atomizing purging device is connected to a micron dispersing mill; the micron dispersing mill is connected to a regenerated raw material tank and a fresh raw material tank.

[0021] Furthermore, it also includes a Venturi jet vacuum pump and a circulation pump; the third exhaust port provided on the horizontal kettle body is connected to the Venturi jet vacuum pump through a gas pipeline, and a circulation path is formed among the Venturi jet vacuum pump, the circulation pump and the variable-pressure self-circulation tank; the exhaust port provided on the reactor cylinder body is connected to the variable-pressure self-circulation tank; the variable-pressure 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.

[0022] Even further, it also includes a submerged 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; the variable-pressure self-circulation tank is connected to the first coolant inlet on the first coolant inlet cavity through the submerged pump; the first coolant drain port is connected to the variable-pressure self-circulation tank.

[0023] The beneficial effects of the present invention compared with the prior art are as follows:

[0024] 1. In the present invention, several microchannels on the outer wall of the microchannel heat exchange tube are used as reaction tanks for solution chemical reactions, and the inside of the microchannel heat exchange tube is used as a heat exchange channel, which increases the solution contact area, improves the heat transfer amount, and achieves the dual effects of reaction heat transfer and exhaust. Since the microchannel reaction tank is an open structure, the hydrogen chloride gas generated by the reactants in the microchannel reaction tank will directly discharge from the exhaust port of the reactor cylinder body, without causing pressure buildup; at the same time, the generated hydrogen chloride gas can be separated from the reaction system in a timely manner, further promoting the forward reaction of the reaction system, greatly improving the chemical reaction rate, reducing the generation of reaction by-products, and improving the purity of the main product.

[0025] 2. Through the chemical reaction in the microchannel reactor, a mixed product of haloester, hydrogen chloride, and butanol is generated. At the same time, a small part of the hydrogen chloride gas entrained with butanol generated by the microchannel reactor can be led to a pressure swing self-circulation tank and, together with the hydrogen chloride gas entrained with butanol generated by the plug flow reactor, pass through a draft fan and be sent to a microporous purification reactor at atmospheric pressure, enabling 100% purification treatment of the hydrogen chloride gas and realizing the recycling of raw materials.

[0026] 3. By the combined use of the microchannel reactor, the plug flow reactor, and the microporous purification reactor in the present invention, the production of the final product phosphate ester compounds is completed. The generated hydrogen chloride gas entrained with butanol is introduced into the microporous purification reactor to separate the hydrogen chloride gas from butanol. The separated butanol returns to the butanol high-level metering tank to realize the recycling of raw materials. The separated hydrogen chloride gas is purer and can be used for the production of other products. The present invention is more environmentally friendly and energy-saving compared with traditional systems and can achieve a 99% conversion rate of phosphorus oxychloride synthesis. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The present invention will be further described in detail below with reference to the drawings:

[0028] Figure 1 is a schematic structural diagram of the whole of the present invention;

[0029] Figure 2 is a schematic structural diagram of the microchannel reactor of the present invention;

[0030] Figure 3 is a schematic external structural diagram of the microchannel heat exchange tube of the present invention;

[0031] Figure 4 is a schematic diagram of the flow direction of the heat exchange fluid inside the microchannel heat exchange tube of the present invention;

[0032] Figure 5 is a schematic structural diagram of the microchannel reaction tank on the wall of the microchannel heat exchange tube described in the present invention;

[0033] Figure 6 isFigure 5 The enlarged sectional view in the A-A direction;

[0034] Figure 7 Schematic diagram of the position structure of the feed tray for raw material A according to the present invention;

[0035] Figure 8 Schematic diagram of the structure of the feed tray for raw material A of the present invention;

[0036] Figure 9 Schematic diagram of the structure of the flat-push reactor according to the present invention;

[0037] Figure 10 Schematic diagram of the structure of the liquid level controller according to the present invention;

[0038] Figure 11 Schematic diagram of the structure of the microporous purification reactor according to the present invention;

[0039] Figure 12 Schematic diagram of the structure of the shear gas inlet pipe according to the present invention;

[0040] Among them, 1 is the feed pipe for raw material A, 2 is the feed pipe for raw material B, 3 is the feed tray for raw material A, 4 is the feed tray for raw material B, 5 is the first exhaust port, 6 is the second exhaust port, 7 is the microchannel heat exchange tube, 8 is the reactor cylinder, 9 is the reaction solution drain port, 10 is the first coolant inlet pipe, 11 is the first coolant drain port, 12 is the first coolant storage cavity, 13 is the first coolant inlet, 14 is the first coolant inlet cavity, 15 is the microchannel reaction tank, 16 is the distribution tank, 17 is the drainage tank, 18 is the heat exchange fin, 19 is the horizontal kettle body, 20 is the first microchannel heat exchanger, 21 is the second microchannel heat exchanger, 22 is the reaction liquid inlet, 23 is the drain port, 24 is the liquid level controller, 25 is the microchannel hole, 26 is the third exhaust port, 27 is the micron dispersion mill, 28 is the variable pressure self-circulation tank, 29 is the multiphase flow shear atomization pump, 30 is the atomization purge device, 31 is the regenerated raw material tank, 32 is the fresh raw material tank, 33 is the Venturi jet vacuum pump, 34 is the circulation pump, 35 is the submersible pump, 36 is the induced draft fan, 37 is the nitrogen tank, 38 is the purification tank body, 39 is the shear gas inlet pipe, 40 is the micron ceramic bubbler, 41 is the microchannel gas heat exchanger, 42 is the liquid level detection sensor, 43 is the liquid flow tank, 44 is the phosphorus oxychloride high-level metering tank, 45 is the butanol high-level metering tank, 46 is the purified gas outlet, 47 is the washing liquid inlet, 48 is the medium return liquid cavity, 49 is the medium inlet cavity, 50 is the cooling medium return liquid cavity, 51 is the heating medium return liquid 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 drain port, 60 is the second coolant inlet. Detailed implementation mode

[0041] In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer and more understandable, the present invention will be further described in detail in combination with embodiments and drawings. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. The technical solutions of the present invention will be described in detail below in combination with embodiments and drawings, but the protection scope is not limited by this.

[0042] See Figures 1 to 12 , this embodiment proposes a microchannel tributyl phosphate production device, which includes a microchannel reactor, a plug-flow reactor, a microporous purification reactor, a variable-pressure self-circulation tank 28 and an atomizing purge device 30.

[0043] The microchannel reactor includes a reactor cylinder 8, and the reactor cylinder 8 is a vertically arranged hollow cylindrical structure.

[0044] A plurality of microchannel heat exchange tubes 7 are arranged in the reactor cylinder 8. The microchannel heat exchange tubes 7 are vertically arranged hollow circular tube structures. The upper ends of the microchannel heat exchange tubes 7 are kept closed, and the lower ends of the microchannel heat exchange tubes 7 are kept open. The inside of the microchannel heat exchange tubes 7 is used to pass a heat exchange medium. A circular array of microchannel reaction grooves 15 is arranged on the outer wall of the microchannel heat exchange tubes 7. The microchannel reaction grooves 15 extend along the axial direction of the microchannel heat exchange tubes 7. The microchannel reaction grooves 15 are formed by engraving on the outer wall of the microchannel heat exchange tubes 7. The cross-section of the microchannel reaction grooves 15 can have various forms such as triangular and rectangular. This structure makes the microchannel reaction grooves 15 as an open structure as a whole, and the microchannel reaction grooves 15 are directly communicated with the inner cavity of the reactor cylinder 8.

[0045] The reactor cylinder 8 is provided with exhaust ports. The exhaust ports include 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. 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.

[0046] The microchannel reaction grooves 15 are used for the exothermic and gas-evolving reaction to proceed. The gas generated by the exothermic and gas-evolving reaction escapes from the microchannel reaction grooves 15 into the inside of the reactor cylinder 8, and finally can 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, an exhaust device is connected to the first exhaust port 5 and the second exhaust port 6. Since the gas generated by the reaction can be discharged in time and in large quantities, a negative pressure environment is created inside the reactor cylinder 8, which is more conducive to the exothermic and gas-evolving reaction in the microchannel reaction grooves 15. Moreover, the gas product is separated from the reaction system in time, avoiding the generation of secondary side reactions.

[0047] To improve the accuracy of the feed, the same material guiding plate is connected to the tops of a number of microchannel heat exchange tubes 7. The material guiding plate is a horizontally arranged circular plate structure, and a plurality of vertically penetrating circular insertion holes are arranged on the material guiding plate. The number of insertion holes is equal to and corresponds one by one to the number of microchannel heat exchange tubes 7. The upper ends of the microchannel heat exchange tubes 7 are inserted into the corresponding insertion holes, and the outer walls of the microchannel heat exchange tubes 7 are in contact with the inner walls of the insertion holes. The material guiding plate is provided with a coaxial circular distribution groove 16 on the outside of each insertion hole. A circle of microchannel diversion holes arranged in a circular array is provided on the side wall between the distribution groove 16 and the insertion hole. The number of microchannel diversion holes is equal to and corresponds one by one to the number of microchannel reaction grooves 15 on the microchannel heat exchange tubes 7. A plurality of drainage grooves 17 are arranged on the material guiding plate. The number of drainage grooves 17 is equal to and corresponds one by one to the number of distribution grooves 16 and is connected. The reaction raw materials are introduced into each distribution groove 16 through the drainage grooves 17, and the distribution groove 16 introduces the reaction raw materials into each microchannel reaction groove 15 of the microchannel heat exchange tubes 7 through a circle of microchannel diversion holes.

[0048] According to the quantity of the reaction raw materials, a plurality of material guiding plates can be set. Different reaction raw materials enter the distribution grooves 16 from the drainage grooves 17 on different material guiding plates respectively. The reaction raw materials inside the distribution grooves 16 are introduced into each microchannel reaction groove 15 through the microchannel diversion holes, realizing a rapid reaction.

[0049] In this embodiment, two material guiding plates are provided, namely a material A guiding plate 3 and a material B guiding plate 4. The material A guiding plate 3 and the material B guiding plate 4 are arranged parallel to each other up and down, and are used to introduce reaction raw material A and reaction raw material B into the microchannel reaction grooves 15 of all the microchannel heat exchange tubes 7 respectively. All the drainage grooves 17 on the material A guiding plate 3 are connected to the material A feed pipe 1, and all the drainage grooves 17 on the material B guiding plate 4 are connected to the material B feed pipe 2. The material A feed pipe 1 is connected to a phosphorus oxychloride high-level metering tank 44; the material B feed pipe 2 is connected to a butanol high-level metering tank 45. The two raw materials, phosphorus oxychloride and butanol, are introduced into the drainage grooves 17 of the material A guiding plate 3 and the material B guiding plate 4 respectively through the material A feed pipe 1 and the material B feed pipe 2. The drainage grooves 17 introduce the raw materials into the distribution grooves 16, and then the distribution grooves 16 flow the two raw materials, phosphorus oxychloride and butanol, into the respective microchannel reaction grooves 15 of the microchannel heat exchange tubes 7 through a circle of microchannel diversion holes.

[0050] Since the reaction between phosphorus oxychloride and butanol is an exothermic reaction, it is very important to maintain an appropriate reaction temperature in the reaction system. In this embodiment, the reaction is carried out on the outer wall of the microchannel heat exchange tube 7, and directly introducing a coolant into the inner wall of the microchannel heat exchange tube 7 can greatly improve the heat exchange efficiency. Specifically, a number of first coolant inlet tubes 10 are provided on the reactor cylinder 8; the first coolant inlet tubes 10 correspond to the microchannel heat exchange tubes 7 one by one. The first coolant inlet tubes 10 extend vertically upward from the bottom into the microchannel heat exchange tubes 7 and extend to the inner top of the microchannel heat exchange tubes 7. The bottom of the first coolant inlet tube 10 is the coolant inlet. The coolant enters from the bottom of the first coolant inlet tube 10 and flows out from the top of the first coolant inlet tube 10 to the inner top of the microchannel heat exchange tube 7 under the action of a pressure pump, and then flows down along the inner wall top 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. To further improve the heat exchange efficiency, a number of heat exchange fins 18 are engraved on the inner wall of the microchannel heat exchange tube 7.

[0051] A first coolant storage cavity 12 is fixedly provided at the bottom of the reactor cylinder 8, and a first coolant inlet cavity 14 is fixedly provided at the bottom of the first coolant storage cavity 12. The coolant inlet at the bottom of the first coolant inlet tube 10 is communicated with the inside of the first coolant inlet cavity 14; the lower end opening of the microchannel heat exchange tube 7 is communicated with the inside of the first coolant storage cavity 12, and the microchannel reaction grooves 15 on the outer side of the microchannel heat exchange tube 7 do not extend into the inside of the first coolant storage cavity 12. The first coolant storage cavity 12 is provided with a first coolant drain port 11; the first coolant inlet cavity 14 is provided with a first coolant inlet 13. A coolant circulation cooling channel is formed through the first coolant storage cavity 12, the first coolant inlet cavity 14, the first coolant inlet tubes 10 and the internal channels of the microchannel heat exchange tubes 7.

[0052] A reaction solution drain port 9 is provided on the lower side wall of the reactor cylinder 8; the reactants in the microchannel reaction grooves 15 flow down along the microchannel reaction grooves 15 and flow into the cavity of the reactor cylinder 8, and finally are discharged from the reaction solution drain port 9.

[0053] The plug flow reactor includes a horizontal kettle body 19, and the horizontal kettle body 19 is a horizontally arranged hollow cylindrical structure. A reaction liquid inlet 22 is provided at the bottom of one end of the horizontal kettle body 19, and a drain port 23 is provided at the bottom of the other end of the horizontal kettle body 19.

[0054] Above the interior of the horizontal kettle body 19, a first microchannel heat exchanger 20 is provided. Below the interior of the horizontal kettle body 19, a second microchannel heat exchanger 21 is provided. Both the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are horizontally arranged hollow circular tubular structures. The axes of both the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 are parallel to the axis of the horizontal kettle body 19. One end of both the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 is closed, and the other end is open. The closed ends of both the first microchannel heat exchanger 20 and the second microchannel heat exchanger 21 face the side of the liquid discharge port 23, and the open ends face the side of the reaction liquid inlet 22.

[0055] The structures of both 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 between them and 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 engraved with spiral heat exchange grooves for increasing the heat exchange area instead of the microchannel reaction grooves 15 for reaction.

[0056] At one end of the horizontal kettle body 19 where the reaction liquid inlet 22 is provided, a medium return liquid cavity 48 and a medium inlet cavity 49 are fixedly arranged in sequence. Both the medium return liquid cavity 48 and the medium inlet cavity 49 are horizontally arranged hollow cylindrical structures. In the middle of the inner side of the medium return liquid cavity 48, a horizontal first partition plate is fixedly arranged. By means of the first partition plate, the inner part of the medium return liquid cavity 48 is divided into an upper cooling medium return cavity 50 and a lower temperature-rising medium return cavity 51. In the middle of the inner side of the medium inlet cavity 49, a horizontal second partition plate is fixedly arranged. By means of the second partition plate, the inner part of the medium inlet cavity 49 is divided into an upper cooling medium inlet cavity 52 and a lower temperature-rising medium inlet cavity 53. At the lower end of the front side wall of the cooling medium return cavity 50, a cooling medium outlet is provided. On the top wall of the cooling medium inlet cavity 52, a cooling medium inlet is provided. At the bottom end of the temperature-rising medium return cavity 51, a temperature-rising medium outlet is provided. At the upper end of the front side wall of the temperature-rising medium inlet cavity 53, a temperature-rising medium inlet is provided.

[0057] The open end of the first microchannel heat exchanger 20 is in communication with the cooling medium return chamber 50. A cooling medium circulation pipe 54 is inserted inside 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, and the inlet end of the cooling medium circulation pipe 54 extends into the cooling medium inlet chamber 52. The cooling medium in the cooling medium inlet chamber 52 enters from the inlet end of the cooling medium circulation pipe 54, and then flows out from the inside of the first microchannel heat exchanger 20 into the cooling medium return chamber 50. The cooling medium inlet chamber 52, the cooling medium circulation pipe 54, the inside of the first microchannel heat exchanger 20, and the cooling medium return chamber 50 form a cooling medium circulation cooling channel.

[0058] The open end of the second microchannel heat exchanger 21 is in communication with the heating medium return chamber 51. A heating medium circulation pipe 55 is inserted inside 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, and the inlet end of the heating medium circulation pipe 55 extends into the heating medium inlet chamber 53. The heating medium in the heating medium inlet chamber 53 enters from the inlet end of the heating medium circulation pipe 55, and then flows out from the inside of the second microchannel heat exchanger 21 into the heating medium return chamber 51. The heating medium inlet chamber 53, the heating medium circulation pipe 55, the inside of the second microchannel heat exchanger 21, and the heating medium return chamber 51 form a heating medium circulation heating channel.

[0059] The reaction liquid inlet 22 of the horizontal kettle body 19 is connected to the micron dispersion mill 27 through a feeding pipeline; the reaction solution drain port 9 of the reactor cylinder body 8 is connected to the variable pressure self-circulation tank 28; the discharge port of the variable pressure self-circulation tank 28 is connected to the atomization purging device 30 through the multiphase flow shear atomization pump 29; the atomization purging device 30 is connected to the micron dispersion mill 27. The product after the esterification reaction in the microchannel reaction tank 15 enters the variable pressure self-circulation tank 28 through the reaction solution drain port 9, and then sequentially enters the horizontal kettle body 19 through the multiphase flow shear atomization pump 29, the atomization purging device 30, and the micron dispersion mill 27 for deep esterification reaction. A heat exchange medium with a relatively high temperature is passed through the second microchannel heat exchanger 21 to provide the necessary temperature conditions for the deep esterification reaction. During this process, a part of the hydrogen chloride gas entrained with butanol is also generated, and this part of the gas is refluxed into the horizontal kettle body 19 through the condensation of the first microchannel heat exchanger 20 for further reaction. The micron dispersion mill 27 is used to further finely grind the esterification reaction product, reduce the particle size of the esterification reaction product, and promote the subsequent deep esterification reaction. The micron dispersion mill 27 is connected to a recycled raw material tank 31 (containing recycled butanol) and a fresh raw material tank 32 (containing butanol). A nitrogen gas tank 37 is connected to the pipeline where the discharge port of the variable pressure self-circulation tank 28 is connected to the multiphase flow shear atomization pump 29.

[0060] A liquid level controller 24 is further provided at the inner bottom surface of the horizontal kettle body 19. The liquid level controller 24 is arranged adjacent to 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. A number of microchannel holes 25 that penetrate through both sides are provided on the liquid level controller 24, and the extending direction of the microchannel holes 25 is parallel to the axis direction of the horizontal kettle body 19; a number of liquid flow grooves 43 that penetrate through both sides are provided at the bottom of the liquid level controller 24, and the extending direction of the liquid flow grooves 43 is parallel to the extending direction of the microchannel holes 25. A liquid level detection sensor 42 is arranged in the horizontal kettle body 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 body 19 reaches a certain liquid level height, it overflows from the top of the liquid level controller 24 and flows to the drain port 23 to discharge the final product tributyl phosphate. When it is necessary to empty the horizontal kettle body 19, the residual liquid in the horizontal kettle body 19 will be drained through a number of microchannel holes 25 provided on the liquid level controller 24 and the liquid flow grooves 43 provided at the bottom.

[0061] A third exhaust port 26 is provided at the top of the horizontal kettle body 19; the third exhaust port 26 is connected to a Venturi jet vacuum pump 33 through a gas pipeline, and a circulation path is formed among the Venturi jet vacuum pump 33, a circulation pump 34, and a variable-pressure self-circulation tank 28. A first exhaust port 5 and a second exhaust port 6 provided on the reactor cylinder body 8 are both connected to the variable-pressure self-circulation tank 28; an induced draft fan 36 is connected to the variable-pressure self-circulation tank 28, and the induced draft fan 36 is connected to a microporous purification reactor through a pipeline. The hydrogen chloride mixed gas from the horizontal kettle body 19 and the reactor cylinder body 8 enters the variable-pressure self-circulation tank 28 and is sent into the microporous purification reactor through the induced draft fan 36 for further purification treatment.

[0062] The microporous purification reactor includes a purification tank body 38, and the purification tank body 38 is a vertically arranged hollow circular cylindrical structure. A plurality of vertical shear gas inlet pipes 39 are uniformly arranged in the purification tank body 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 body 38 passes through a plurality of shear gas inlet pipes 39 and is released into the purification tank body 38 through the micron ceramic bubbler 40. A washing liquid inlet 47 is arranged at the upper end of the side wall of the purification tank body 38. The washing liquid inlet 47 is connected to a phosphorus oxychloride high-level metering tank 44. The phosphorus oxychloride in the phosphorus oxychloride high-level metering tank 44 enters the purification tank body 38 to react with the residual butanol in the gas to remove the butanol in the hydrogen chloride gas. A purified gas outlet 46 is arranged at the upper end of the side wall of the purification tank body 38; the purified gas outlet 46 is connected to a butanol high-level metering tank 45. The washing liquid inlet 47 and the purified gas outlet 46 are respectively located on both sides of the purification tank body 38.

[0063] A plurality of microchannel gas heat exchangers 41 are uniformly arranged 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 is kept closed, and the lower end is kept open.

[0064] A number of second coolant inlet pipes 56 are arranged inside the purification tank body 38; the second coolant inlet pipes 56 correspond to the microchannel gas heat exchangers 41 one by one. The second coolant inlet pipes 56 extend vertically upward from the bottom into the microchannel gas heat exchangers 41 and extend to the inner top of the microchannel gas heat exchangers 41. The bottom of the second coolant inlet pipe 56 is a coolant inlet. 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 inner wall top of the microchannel gas heat exchanger 41, thereby realizing heat exchange for the reaction occurring outside the microchannel gas heat exchanger 41.

[0065] At the lower end of the purification tank body 38, a second coolant storage cavity 57 and a second coolant inlet cavity 58 are fixedly arranged in sequence. The coolant inlet at the bottom of the second coolant inlet pipe 56 is communicated with the inside of the second coolant inlet cavity 58; the lower end opening of the microchannel gas heat exchanger 41 is communicated with the inside of the second coolant storage cavity 57, and a second coolant drain port 59 is arranged at the lower end of the side wall of the second coolant storage cavity 57; a second coolant inlet 60 is arranged at the bottom of the second coolant inlet cavity 58. A coolant circulation cooling channel is formed through the inside channels of the second coolant storage cavity 57, the second coolant inlet cavity 58, the second coolant inlet pipe 56 and the microchannel gas heat exchanger 41.

[0066] In order to make full use of the heat carried by the esterification reaction product, the pressure swing self-circulation tank 28 is respectively connected with 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 drain port 11 and the second coolant drain port 59 are both connected with the pressure swing self-circulation tank 28. The submerged pump 35 is used to send the esterification reaction product inside the pressure swing self-circulation tank 28 into 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 into the pressure swing self-circulation tank 28 for the next step of deep esterification reaction.

[0067] Industrially, tributyl phosphate is generally synthesized by direct esterification of phosphorus oxychloride and n-butanol. In order to inhibit the continuous reaction of hydrogen chloride generated in the reaction with n-butanol and tributyl phosphate to generate chlorobutane, it is usually necessary to control a very low reaction temperature. It is difficult for the traditional kettle reactor 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 applicable to a reaction system with gas generation and side reactions, and solves the problems in the existing microchannel reactor for such a reaction system that due to the gas being unable to be discharged from the reaction system in time or the discharge rate being low, the pressure of the reaction system increases or the by-products increase.

[0068] The chemical reaction principle of tributyl phosphate is to mix phosphorus oxychloride and butanol, and after three-stage esterification reaction, tributyl phosphate and hydrogen chloride are generated. The main reaction equation is as follows:

[0069] POCl 3 +3C 4 H 9 OH→(C 4 H 9 O) 3 PO+3HCl ;

[0070] At the same time, the following side reactions also occur:

[0071] (C 4 H 9 O) 3 PO + HCl → (C 4 H 9 O) 2 POOH + C 4 H 9 Cl;

[0072] C 4 H 9 OH + HCl → C 4 H 9 Cl + H 2 O.

[0073] The key technical difficulty lies in that the organic esterification synthesis reaction releases heat violently instantaneously, and it is difficult for traditional batch reactors to control the reaction temperature, and boiling over is very likely to occur. Moreover, it is very difficult to separate a large amount of hydrogen chloride rapidly from the reaction system, and the formation rate of by-products is relatively high.

[0074] The above problems can be solved by using a microchannel tributyl phosphate production device proposed in this embodiment. The working principle is as follows:

[0075] Phosphorus oxychloride and butanol, two raw materials, are respectively introduced into the drainage grooves 17 inside 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. The drainage grooves 17 introduce the raw materials into the distribution groove 16, and then the distribution groove 16 flows phosphorus oxychloride and butanol, two raw materials, into each microchannel reaction tank 15 of the microchannel heat exchange tube 7 through a circle of microchannel diversion holes respectively. Moreover, a coolant flows through the inner wall of the microchannel heat exchange tube 7 to continuously exchange heat with the reaction solution on the outer wall of the microchannel heat exchange tube 7, rapidly reducing the reaction temperature; at the same time, an air pump is connected to the first exhaust port 5 and the second exhaust port 6. Under the action of the air pump, a negative pressure is formed in the reactor cylinder 8, and the hydrogen chloride generated by the reaction escapes from the reaction system in the form of gas into the reactor cylinder 8 and is discharged in time from the first exhaust port 5 and the second exhaust port 6, inhibiting the occurrence of side reactions involving hydrogen chloride. Phosphorus oxychloride and n-butanol react in the microchannel reaction tank 15 and flow downward under the action of gravity along the microchannel reaction tank 15, generating a mixed product of haloester, hydrogen chloride and butanol. Finally, the mixed product converges in the cavity of the reactor cylinder 8 and is discharged to the variable-pressure self-circulation tank 28 through the reaction solution drain port 9.

[0076] A small part of the hydrogen chloride gas entraining butanol generated by the microchannel reactor enters the variable-pressure self-circulation tank 28 and, together with the hydrogen chloride gas entraining butanol generated by the plug-flow reactor, passes through the induced draft fan 36, becomes at atmospheric pressure and is sent into the microporous purification reactor for 100% purification treatment to realize the recycling of raw materials.

[0077] In practical applications, the cryogenic haloester in the variable-pressure self-circulation tank 28 is respectively sent into the microchannel reactor and the microporous purification reactor through the submerged pump 35 to carry away the heat generated in the two devices, and the heated haloester returns to the variable-pressure self-circulation tank 28 through the pressure difference.

[0078] The mixed product of haloester, hydrogen chloride and butanol in the variable-pressure self-circulation tank 28 passes through the circulation pump 34, enters the Venturi jet vacuum pump 33, and then flows back to the variable-pressure self-circulation tank 28 to form a cycle. At the same time, the hydrogen chloride gas entrained with butanol generated by the plug-flow reactor is also drawn into the Venturi jet vacuum pump 33 and flows into the variable-pressure self-circulation tank 28 to participate in the cycle, making the plug-flow reactor form a negative pressure.

[0079] The mixed product of haloester, hydrogen chloride and butanol in the variable-pressure self-circulation tank 28 and the external nitrogen provided by the nitrogen gas tank 37 are sent into the atomization and purging device 30 by the multiphase flow shear atomization pump 29 to separate hydrogen chloride. The generated mixture of haloester and butanol after treatment enters the micron dispersion mill 27. At the same time, a certain proportion of butanol and recycled butanol are added. The three are processed into a molecular-level mixture by the micron dispersion mill 27 and sent into the plug-flow reactor for reaction to generate a mixture of tributyl phosphate and butanol. The subsequent process separates it to obtain the final product tributyl phosphate, and the separated butanol is stored in the regenerated raw material tank 31 for recycling. Multiple plug-flow reactors can be connected in series according to actual needs to form a complete reaction.

[0080] The raw material in the phosphorus oxychloride high-level metering tank 44 enters the microporous purification reactor as a scrubbing liquid and reacts with the incoming hydrogen chloride gas entrained with butanol. The mixture of butanol and haloester overflowing during the reaction process returns to the microchannel reactor, realizing the closed-loop use of raw materials throughout the process.

[0081] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be regarded as limiting the claimed claims.

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 of an open structure, the microchannel reaction grooves (15) are used for exothermic and gas-releasing 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 ends of the microchannel heat exchange tubes (7) are 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 A circle of microchannel guide holes is arranged on the side wall between the reactor body (16) and the plug hole; 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 body (8) is provided with an exhaust port, and the gas generated by the exothermic and gas-releasing reaction is directly discharged from the reactor body (8) through the exhaust port; the lower side wall of the reactor body (8) is provided with a reaction solution discharge port (9); the microchannel heat exchange tube (7) is used to pass the 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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