A microchannel reactor for producing phosphorus trifluoride

By designing a 3D printing technology for microchannel reactors in the production of phosphorus trifluoride, the problems of leakage hazards and insufficient heat exchange performance are solved, and the continuous reaction processing and reaction temperature stability of phosphorus trifluoride are achieved. control.

CN119140029BActive Publication Date: 2025-02-18FUJIAN DEER TECH CORP
View PDF 1 Cites 0 Cited by

Patent Information

Application Number
CN202411601375.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-11
Publication Date
2025-02-18
Estimated Expiration
2044-11-11

AI Technical Summary

Technical Problem

The existing microchannel reactors have hidden dangers of leakage and insufficient heat exchange performance in the production of phosphorus trifluoride, which makes it difficult to effectively maintain the reaction temperature and cannot achieve continuous reaction processing of phosphorus trifluoride.

Method used

A microchannel reactor for phosphorus trifluoride production was designed. The outer convexity of the reaction chamber was placed on the fixed substrate through integrated processing method (3D printing), and the reaction chamber was connected through the guide hole, and the three-way was used to enter the reaction chamber. The material pipe and the discharge pipe are processed by treating reactants and products, while enhancing the sealing property of the heat exchange mechanism and the circulation effect of the heat exchange medium.

Benefits of technology

It effectively solves the leakage risks during the reaction process, improves heat exchange performance, ensures stable maintenance of reaction temperature, realizes continuous reaction processing of phosphorus trifluoride, and ensures production safety and efficiency.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119140029B_ABST
    Figure CN119140029B_ABST
Patent Text Reader

Abstract

The present invention discloses a microchannel reactor for phosphorus trifluoride production, comprising a plurality of reaction modules fixedly mounted side by side on a fixed bracket, wherein the reaction modules include: a plurality of rows of first reaction chambers, which are integrally formed and convexly arranged on the side of the corresponding fixed substrate; a plurality of second reaction chambers, which are integrally formed and convexly arranged on the other side of the fixed substrate, and the fixed substrate is provided with a guide hole for conducting the first reaction chamber and the second reaction chamber; a feed mechanism, comprising a feed hole arranged on the fixed substrate; a discharge mechanism, comprising a discharge hole arranged on the fixed substrate; reactants enter through the feed hole, and the mixed materials alternately pass through the first reaction chamber and the second reaction chamber in sequence to perform a replacement reaction, and the products after the reaction are discharged along the discharge hole. The present invention can effectively and practically solve the leakage risk in the reaction process, and can ensure that the present invention has sufficient heat exchange effect.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to reaction equipment for producing phosphorus trifluoride, in particular to a microchannel reactor for producing phosphorus trifluoride, which can realize continuous reaction processing of phosphorus trifluoride. Background Art

[0002] Phosphorus trifluoride can be used as a fluorinating agent, which can perform ion transfer and is used in the fields of electronics industry, battery manufacturing, polymer materials and catalysts. In semiconductor manufacturing, literature reports that phosphorus trifluoride can be converted into plasma gas under the action of microwaves for doping, which can significantly improve semiconductor performance. In the field of polymer materials, literature reports that phosphorus trifluoride can be used as a reactant to synthesize fluorinated organic dithiophosphates, terephthalate esters and other polymer materials with excellent anti-corrosion properties, which have good economic benefits.

[0003] At present, the production method of phosphorus trifluoride is relatively limited, in which phosphorus trichloride and anhydrous hydrogen fluoride are used as raw materials for replacement reaction, and phosphorus trifluoride and hydrogen chloride can be produced. The chemical reaction equation is: PCI3 + 3HF→ 3HCI + PF3. Since the reaction rate of the replacement is very fast and the reaction heat is extremely strong, it is difficult to effectively maintain the reaction temperature at 40-60 ° C, resulting in only intermittent reactions. In its production process, phosphorus trichloride is first transferred to the reactor, and then anhydrous hydrogen fluoride is slowly and intermittently introduced into the bottom of the reactor for reaction. The overall reaction process is not only inefficient, but also the quality of the obtained product is difficult to maintain stably. Through the intervention of a microchannel reactor, the above-mentioned replacement reaction can be carried out continuously, thereby improving production efficiency and maintaining stable product quality. However, the reaction channels of the existing microchannel reactors are mostly directly arranged on the surface of the reactor substrate, and then sealed and closed by other fixed plates. To ensure the sealing effect, a corresponding sealing gasket is often sandwiched between the reactor substrate and the corresponding fixed plate. Although the setting of the sealing gasket can improve the sealing of the reactor to a certain extent, the joint seam always exists, so there is still a risk of leakage. Once a leak occurs during the reaction, it will lead to a serious production accident; in addition, the heat exchange performance of the existing microchannel reactor is relatively difficult to break through, resulting in the reaction temperature of the continuous reaction being difficult to effectively maintain within a reasonable range. Therefore, the existing microchannel reactor cannot be used for the continuous reaction processing of phosphorus trifluoride for the time being.

[0004] Therefore, the research purpose of the present invention is to design a microchannel reactor for phosphorus trifluoride production that can effectively and practically solve the leakage risk in the reaction process and ensure the heat exchange effect so as to effectively maintain the reaction temperature of the continuous reaction within a reasonable range. Summary of the invention

[0005] In view of the technical problems existing in the above-mentioned prior art, the present invention provides a microchannel reactor for producing phosphorus trifluoride, which can effectively solve the technical problems existing in the above-mentioned prior art.

[0006] The technical solution of the present invention is:

[0007] A microchannel reactor for phosphorus trifluoride production, comprising a fixed support and a plurality of reaction modules fixedly mounted side by side on the fixed support, wherein the reaction modules include:

[0008] Several rows of first reaction chambers are integrally formed and convexly disposed on the side of the corresponding fixed substrate, the first reaction chambers in the same row are arranged at intervals, and the first reaction chambers in two adjacent rows are arranged in a staggered manner;

[0009] A plurality of second reaction chambers are integrally formed and convexly disposed on the other side of the fixed substrate, the second reaction chambers are obliquely disposed between the two sides of two adjacent first reaction chambers in the same row of first reaction chambers, and between the last first reaction chamber and the first first reaction chamber in two adjacent rows of first reaction chambers, and the fixed substrate is provided with a material guide hole for conducting the first reaction chamber and the second reaction chamber;

[0010] A feeding mechanism, comprising a feeding hole disposed on the fixed substrate, wherein a feeding end of the feeding hole is externally connected to a corresponding three-way feeding pipe, and a discharge end of the feeding hole is connected to an end of the first reaction chamber of the first row that is not connected to the second reaction chamber;

[0011] The discharge mechanism comprises a discharge hole arranged on the fixed base plate, the discharge end of the discharge hole is connected to a corresponding discharge pipe outwardly, and the feed end of the discharge hole is connected to an end of the last first reaction chamber in the last row that is not connected to the second reaction chamber; the reactants enter through the three-way feed pipe, and the mixed materials pass through the first reaction chamber and the second reaction chamber alternately in sequence to perform replacement reaction, and the reaction products are discharged along the discharge pipe.

[0012] The first reaction chamber is arranged in parallel with the fixed substrate, and the second reaction chamber is arranged in a vertical position with the fixed substrate.

[0013] The first reaction chamber is arranged in an elliptical shape, and a stopper with a triangular cross-section is integrally formed on one side of the feeding end of the first reaction chamber.

[0014] The top of the second reaction chamber is arranged in an arc shape, and connecting holes connected to the material guiding hole are respectively arranged on both sides of the second reaction chamber.

[0015] The first reaction chamber and the second reaction chamber are respectively formed in an integrated manner by 3D printing and arranged on the fixed substrate.

[0016] The microchannel reactor also includes a heat exchange mechanism, which includes an isolation cover with a sealing cover arranged on both sides of the fixed substrate, one end of the isolation cover is respectively connected to a plurality of corresponding heat exchange medium discharge pipes, and the other end of the isolation cover is respectively connected to a plurality of corresponding heat exchange medium output pipes; the heat exchange medium discharge pipe is connected to an external heat exchange medium source through a corresponding heat exchange medium inlet main pipe and a heat exchange medium extraction pump, and the heat exchange medium output pipe is discharged through a corresponding heat exchange medium output main pipe.

[0017] The isolation cover and the fixed base plate are respectively locked and installed by a plurality of corresponding locking bolts.

[0018] Corresponding sealing gaskets are respectively disposed at the joints between the isolation cover and the fixed base plate.

[0019] The feeding ends of the three-way feeding pipes of the feeding mechanism are respectively connected in parallel to the corresponding reactant feeding pipes.

[0020] The discharge pipe of the discharge mechanism is connected in parallel to the corresponding product output pipe.

[0021] Advantages of the present invention:

[0022] 1) The present invention uses an integrated processing method (3D printing) to integrate several rows of first reaction chambers and several second reaction chambers into an integrated shape and convexly set on the side of the fixed substrate, and the first reaction chamber and the second reaction chamber are connected one by one through the intervention of the guide hole. During the reaction process, the reactants (phosphorus trichloride and anhydrous hydrogen fluoride) enter respectively through the three-way feed pipe, and the mixed materials pass through the first reaction chamber and the second reaction chamber alternately in sequence for replacement reaction, and the reaction product is discharged along the discharge pipe. The present invention not only has sufficient reaction and mixing area, but also there is no connection seam between the first reaction chamber, the second reaction chamber and the fixed substrate. Therefore, it can effectively and practically solve the leakage risk in the reaction process, so that the present invention can be smoothly applied to the reaction processing of phosphorus trifluoride, so as to realize the continuous reaction processing of phosphorus trifluoride under the premise of ensuring safety.

[0023] 2) The first reaction chamber of the present invention is arranged in parallel with the fixed substrate, and the second reaction chamber is arranged in a vertical state with the fixed substrate, so that the materials can be mixed in the longitudinal plane when entering the first reaction chamber, and in the inclined transverse plane when entering the second reaction chamber, and the longitudinal plane mixing and the inclined transverse plane mixing are performed alternately, thereby effectively ensuring the mixing effect of the materials and ensuring the smooth progress of the phosphorus trifluoride reaction processing.

[0024] 3) The first reaction chamber of the present invention is arranged in an elliptical shape, and a baffle with a triangular cross-section is integrally formed on one side of the feed end of the first reaction chamber, so that the material flowing through the first reaction chamber can form a reasonable turbulence and eddy current, so as to further effectively ensure the mixing effect of the material, thereby further ensuring the smooth progress of the continuous reaction processing of phosphorus trifluoride.

[0025] 4) The top of the second reaction chamber of the present invention is arranged in an arc shape, and connecting holes connected to the material guide holes are respectively arranged on both sides of the second reaction chamber, which can ensure the smooth flow of the material, and under the guidance of the arc top, the material can form a certain turbulence and eddy current, so as to further effectively ensure the mixing effect of the material, thereby further ensuring the smooth progress of the phosphorus trifluoride reaction processing.

[0026] 5) The heat exchange mechanism of the present invention comprises an isolation cover with a sealing cover disposed on both sides of the fixed substrate, one end of the isolation cover is respectively connected to a number of corresponding heat exchange medium discharge pipes, and the other end of the isolation cover is respectively connected to a number of corresponding heat exchange medium output pipes. Since the first reaction chamber and the second reaction chambers of the present invention are regularly convexly arranged, the heat exchange medium can be circulated by multi-point lateral input and discharge, which can effectively make the heat exchange medium contact with the reaction area more quickly and fully, thereby achieving a better heat exchange effect, so as to effectively maintain the reaction temperature of the continuous reaction within a reasonable range, so that the present invention can be further smoothly applied to the reaction processing of phosphorus trifluoride to achieve the continuous reaction processing of phosphorus trifluoride. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a structural schematic diagram of the present invention.

[0028] Figure 2 This is a schematic diagram of the structure of the present invention after removing the fixing bracket.

[0029] Figure 3 Schematic diagram of the reaction module.

[0030] Figure 4 This is a schematic diagram of the structure of the other side of the reaction module.

[0031] Figure 5 It is a schematic diagram of the connection between the first reaction chamber and the second reaction chamber of the reaction module.

[0032] Figure 6 is a cross-sectional view of the first reaction chamber.

[0033] Figure 7 is a cross-sectional view of the second reaction chamber.

[0034] In the accompanying drawings: a fixed bracket 1, a reaction module 2, a first reaction chamber 201, a fixed substrate 202, a second reaction chamber 203, a connecting hole 2031, a feeding mechanism 204, a feeding hole 2041, a three-way feeding pipe 2042, a discharging mechanism 205, a discharging hole 2051, a discharge pipe 2052, a guide hole 3, a stopper 4, a heat exchange mechanism 5, an isolation cover 501, a heat exchange medium discharge pipe 502, a heat exchange medium output pipe 503, a heat exchange medium inlet main pipe 504, a heat exchange medium extraction pump 505, a heat exchange medium output main pipe 506, locking bolts 6, a reactant feed pipe 7, and a product output pipe 8. DETAILED DESCRIPTION

[0035] In order to facilitate understanding by those skilled in the art, the structure of the present invention is further described in detail with reference to the embodiments in conjunction with the accompanying drawings:

[0036] refer to Figure 1-7 A microchannel reactor for phosphorus trifluoride production includes a fixed support 1 and a plurality of reaction modules 2 fixedly mounted side by side on the fixed support 1, wherein the reaction modules 2 include:

[0037] Several rows of first reaction chambers 201 are integrally formed and convexly disposed on the side of the corresponding fixed substrate 202. The first reaction chambers 201 in the same row are arranged at intervals, and the first reaction chambers 201 in two adjacent rows are arranged in a staggered manner.

[0038] A plurality of second reaction chambers 203 are integrally formed and convexly disposed on the other side of the fixed substrate 202. The second reaction chambers 203 are obliquely disposed between the two sides of two adjacent first reaction chambers 201 in the same row of first reaction chambers 201, and between the last first reaction chamber 201 and the first first reaction chamber 201 in two adjacent rows of first reaction chambers 201. The fixed substrate 202 is provided with a material guide hole 3 for conducting the first reaction chamber 201 and the second reaction chamber 203.

[0039] The feeding mechanism 204 comprises a feeding hole 2041 disposed on the fixed substrate 202, the feeding end of the feeding hole 2041 is connected to a corresponding three-way feeding pipe 2042, and the discharge end of the feeding hole 2041 is connected to an end of the first reaction chamber 201 of the first row that is not connected to the second reaction chamber 203;

[0040] The discharge mechanism 205 comprises a discharge hole 2051 arranged on the fixed base plate 202, the discharge end of the discharge hole 2051 is connected to the outside with a corresponding discharge pipe 2052, and the feed end of the discharge hole 2051 is connected to the end of the last first reaction chamber 201 in the last row that is not connected to the second reaction chamber 203; the reactants enter through the three-way feed pipe 2042, and the mixed materials pass through the first reaction chamber 201 and the second reaction chamber 203 alternately in sequence for replacement reaction, and the reaction products are discharged along the discharge pipe 2052.

[0041] The present invention uses an integrated processing method to integrate several rows of first reaction chambers 201 and several second reaction chambers 203 to form an integrated shape and convexly set on the side of the fixed substrate 202, and the first reaction chamber 201 and the second reaction chamber 203 are connected one by one through the intervention of the material guide hole 3. During the reaction process, the reactants (phosphorus trichloride and anhydrous hydrogen fluoride) enter through the three-way feed pipe 2042 respectively, and the mixed materials pass through the first reaction chamber 201 and the second reaction chamber 203 alternately in sequence to perform a replacement reaction, and the reaction product is discharged along the discharge pipe 2052. Not only does it have a sufficient reaction and mixing area, but there is no connection seam between the first reaction chamber 201, the second reaction chamber 203 and the fixed substrate 202. Therefore, it can effectively and practically solve the leakage risk in the reaction process, so that the present invention can be smoothly applied to the reaction processing of phosphorus trifluoride, so as to achieve the continuous reaction processing of phosphorus trifluoride under the premise of ensuring safety.

[0042] The first reaction chamber 201 is arranged in parallel with the fixed substrate 202, and the second reaction chamber 203 is arranged in a perpendicular state with the fixed substrate 202. The materials can be mixed in the longitudinal plane when entering the first reaction chamber 201, and mixed in the inclined transverse plane when entering the second reaction chamber 203, and the longitudinal plane mixing and the inclined transverse plane mixing are performed alternately, thereby effectively ensuring the mixing effect of the materials and ensuring the smooth progress of the phosphorus trifluoride reaction process.

[0043] The first reaction chamber 201 is arranged in an elliptical shape, and a stopper 4 having a triangular cross section is formed integrally on one side of the feed end of the first reaction chamber 201. Under the action of the stopper 4, the material flowing through the first reaction chamber 201 can form a reasonable turbulence and eddy current, so as to further effectively ensure the mixing effect of the material, thereby further ensuring the smooth progress of the phosphorus trifluoride reaction process.

[0044] The top of the second reaction chamber 203 is arranged in an arc shape, and connecting holes 2031 connected to the material guide hole 3 are respectively arranged on both sides of the second reaction chamber 203. Thus, the smooth flow of the material can be ensured, and under the guidance of the arc-shaped top, the material can form a certain turbulence and eddy current, so as to further effectively ensure the mixing effect of the material, thereby further ensuring the smooth progress of the phosphorus trifluoride reaction process.

[0045] The first reaction chamber 201 and the second reaction chamber 203 are integrally formed on the fixed substrate 202 by 3D printing.

[0046] The microchannel reactor also includes a heat exchange mechanism 5, which includes an isolation cover 501 with sealing covers arranged on both sides of the fixed substrate 202, one end of the isolation cover 501 is respectively connected to a number of corresponding heat exchange medium discharge pipes 502, and the other end of the isolation cover 501 is respectively connected to a number of corresponding heat exchange medium output pipes 503; the heat exchange medium discharge pipe 502 is connected to an external heat exchange medium source through a corresponding heat exchange medium inlet main pipe 504 and a heat exchange medium extraction pump 505, and the heat exchange medium output pipe 503 is discharged through a corresponding heat exchange medium output main pipe 506. Since the first reaction chamber 201 and the plurality of second reaction chambers 202 of the present invention are regularly convexly arranged, the heat exchange medium can be circulated by means of multi-point lateral input and discharge, so that the heat exchange medium can be effectively brought into contact with the reaction area more quickly and fully, thereby achieving a better heat exchange effect, so as to effectively maintain the reaction temperature of the continuous reaction within a reasonable range, thereby enabling the present invention to be further smoothly applied to the reaction processing of phosphorus trifluoride to realize the continuous reaction processing of phosphorus trifluoride.

[0047] The isolation cover 501 and the fixed base plate 202 are respectively locked and installed by a plurality of corresponding locking bolts 6. The connection between the isolation cover 501 and the fixed base plate 202 is respectively provided with corresponding sealing gaskets.

[0048] The feeding ends of the three-way feeding pipe 2042 of the feeding mechanism 204 are respectively connected in parallel to the corresponding reactant feeding pipe 7. The discharge pipe 2052 of the discharging mechanism 205 is connected in parallel to the corresponding product output pipe 8.

[0049] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A microchannel reactor for phosphorus trifluoride production, comprising a fixed support (1), and a plurality of reaction modules (2) fixedly mounted side by side on the fixed support (1), characterized in that: The reaction module (2) comprises: A plurality of rows of first reaction chambers (201) are integrally formed and convexly arranged on the side surfaces of corresponding fixed substrates (202); the first reaction chambers (201) in the same row are arranged at intervals, and the first reaction chambers (201) in two adjacent rows are arranged in a staggered manner; a plurality of second reaction chambers (203) formed in an integrated manner and convexly arranged on the other side surface of the fixed substrate (202); the second reaction chambers (203) are arranged obliquely between the two sides of two adjacent first reaction chambers (201) in the same row of first reaction chambers (201), and between the last first reaction chamber (201) and the first first reaction chamber (201) in two adjacent rows of first reaction chambers (201); and a material guide hole (3) for conducting the first reaction chamber (201) and the second reaction chamber (203) is arranged on the fixed substrate (202); A feeding mechanism (204) comprising a feeding hole (2041) disposed on the fixed substrate (202), wherein a feeding end of the feeding hole (2041) is externally connected to a corresponding three-way feeding pipe (2042), and a discharging end of the feeding hole (2041) is connected to an end of the first first reaction chamber (201) of the first row that is not connected to the second reaction chamber (203); The discharge mechanism (205) comprises a discharge hole (2051) disposed on the fixed substrate (202); the discharge end of the discharge hole (2051) is externally connected to a corresponding discharge pipe (2052); the feed end of the discharge hole (2051) is connected to the end of the last first reaction chamber (201) in the last row that is not connected to the second reaction chamber (203); the reactants enter through the three-way feed pipe (2042), and the mixed materials pass through the first reaction chamber (201) and the second reaction chamber (203) alternately in sequence to perform a replacement reaction, and the products after the reaction are discharged along the discharge pipe (2052); The first reaction chamber (201) and the fixed substrate (202) are arranged in a parallel state, and the second reaction chamber (203) and the fixed substrate (202) are arranged in a vertical state; The first reaction chamber (201) is arranged in an elliptical shape, and a stopper (4) having a triangular cross-section is integrally formed and arranged on one side of the feed end of the first reaction chamber (201); The top of the second reaction chamber (203) is arranged in an arc shape, and connecting holes (2031) connected to the material guide hole (3) are respectively arranged on both sides of the second reaction chamber (203); The first reaction chamber (201) and the second reaction chamber (203) are respectively integrally formed by 3D printing and arranged on the fixed substrate (202); The microchannel reactor further comprises a heat exchange mechanism (5), the heat exchange mechanism (5) comprising an isolation cover (501) with sealing covers arranged on both sides of the fixed substrate (202), one end of the isolation cover (501) being respectively connected to a plurality of corresponding heat exchange medium discharge pipes (502), and the other end of the isolation cover (501) being respectively connected to a plurality of corresponding heat exchange medium output pipes (503); the heat exchange medium discharge pipes (502) are connected to an external heat exchange medium source through corresponding heat exchange medium inlet main pipes (504) and heat exchange medium extraction pumps (505), and the heat exchange medium output pipes (503) are discharged through corresponding heat exchange medium output main pipes (506).

2. A microchannel reactor for producing phosphorus trifluoride according to claim 1, characterized in that: The isolation cover (501) and the fixed base plate (202) are respectively locked and installed via a plurality of corresponding locking bolts (6).

3. A microchannel reactor for phosphorus trifluoride production according to claim 2, characterized in that: Corresponding sealing gaskets are respectively provided at the joints between the isolation cover (501) and the fixed base plate (202).

4. A microchannel reactor for producing phosphorus trifluoride according to claim 1, characterized in that: The feeding ends of the three-way feeding pipe (2042) of the feeding mechanism (204) are respectively connected in parallel to the corresponding reactant feeding pipes (7).

5. A microchannel reactor for producing phosphorus trifluoride according to claim 4, characterized in that: The discharge pipe (2052) of the discharge mechanism (205) is connected in parallel to the corresponding product output pipe (8).

Citation Information

Patent Citations

  • Microreaction channel, reaction substrate and microchannel reactor

    CN111437782A