A preparation device and preparation method of high-purity phosphorus trifluoride
By designing a high-purity phosphorus trifluoride preparation equipment combining microchannel reactors and condensers, the problems of leakage hazards and insufficient heat exchange performance in the prior art are solved, and the continuous production of phosphorus trifluoride is achieved, and the production efficiency and product quality stability are improved.
Patent Information
- Application Number
- CN202411601881.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-11
- Publication Date
- 2025-03-21
- Estimated Expiration
- 2044-11-11
AI Technical Summary
The existing microchannel reactors have hidden leakage risks and insufficient heat exchange performance during the production process of phosphorus trifluoride, making it difficult to achieve continuous production of phosphorus trifluoride, low production efficiency and difficult to stabilize product quality.
A high-purity phosphorus trifluoride preparation equipment is designed, and a structure combining a microchannel reactor and a condenser is used to set the reaction chamber through integrated molding, and the reaction chamber is connected through the guide hole, and the heat exchange mechanism is combined to improve the control effect of the reaction temperature.
It effectively solves the leakage risks during the reaction process, improves the control effect of reaction temperature, realizes continuous production of phosphorus trifluoride, improves production efficiency and ensures the stability of product quality.
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Figure CN119098126B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of phosphorus trifluoride production, and in particular to a preparation device and a preparation method of high-purity phosphorus trifluoride, which can realize the continuous production of phosphorus trifluoride, can not only improve the production efficiency, but also can ensure the quality stability of the product. 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 methods of phosphorus trifluoride are relatively limited. Among them, phosphorus trifluoride and hydrogen chloride can be produced by replacement reaction using phosphorus trichloride and anhydrous hydrogen fluoride as raw materials. The chemical reaction equation is: PCI3 + 3HF→ 3HCI + PF3. Since the reaction rate of this 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 intermittent reactions. In its production process, phosphorus trichloride is first transferred to the reactor, and then anhydrous hydrogen fluoride is slowly and intermittently passed into the bottom of the reactor for reaction. Not only is the production efficiency low, but the quality of the product is also difficult to maintain stably.
[0004] Through the intervention of the 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 hidden danger of leakage. Once a leak occurs during the reaction process, a serious production accident will occur; 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 phosphorus trifluoride reaction processing for the time being, resulting in the inability to implement the continuous production of phosphorus trifluoride.
[0005] Therefore, the purpose of the present invention is to design a preparation device and a preparation method for high-purity phosphorus trifluoride that can effectively ensure production safety and effectively and significantly improve the control effect of reaction temperature, thereby realizing continuous production of phosphorus trifluoride, effectively and significantly improving production efficiency and ensuring product quality stability. Summary of the invention
[0006] In view of the technical problems existing in the above-mentioned prior art, the present invention provides a preparation device for high-purity phosphorus trifluoride and a preparation method thereof, which can effectively solve the technical problems existing in the above-mentioned prior art.
[0007] The technical solution of the present invention is:
[0008] A preparation device for high-purity phosphorus trifluoride, comprising:
[0009] A microchannel reactor comprises a fixed support and a plurality of reaction modules fixedly mounted on the fixed support in parallel, wherein the reaction modules comprise a plurality of rows of first reaction chambers integrally formed and convexly arranged on the side surfaces of corresponding fixed substrates, the first reaction chambers in the same row are arranged at intervals respectively, and the first reaction chambers in two adjacent rows are arranged in a staggered manner respectively; a plurality of second reaction chambers are integrally formed and convexly arranged on the other side surface of the fixed substrate, the second reaction chambers are obliquely arranged between the two sides of two adjacent first reaction chambers in the same row, and between the last first reaction chamber and the first first reaction chamber in two adjacent rows of first reaction chambers, the fixed substrate is provided with a material guide hole for conducting the first reaction chamber and the second reaction chamber; the fixed substrate is provided with a material feed hole connected to the first first reaction chamber in the first row, the material feed hole is externally connected to a corresponding three-way material feed pipe; the fixed substrate is provided with a material discharge hole connected to the last first reaction chamber in the last row, the material discharge hole is externally connected to a corresponding material discharge pipe;
[0010] The condenser comprises a condensing cylinder with sealing plates fixedly connected at both ends, and corresponding refrigerant circulation containers are respectively sealed and fixedly connected at both ends of the condensing cylinder, wherein the end of one refrigerant circulation container is externally connected to a refrigerant inlet pipe, and the other refrigerant circulation container is externally connected to a refrigerant discharge pipe, and a plurality of corresponding condensing tubes are evenly distributed and installed through the sealing plates, and external refrigerant enters through the refrigerant inlet pipe, and is discharged along the refrigerant discharge pipe after passing through the condensing tubes; the top of the condensing cylinder is upwardly connected to a precooling cylinder with a closed top, and a corresponding condensing coil is arranged in the precooling cylinder, the feed end of the condensing coil is connected to the external refrigerant, and the discharge end of the condensing coil is connected to one of the condensing tubes through a corresponding siphon tee; the discharge pipe is connected in parallel to the top of the precooling cylinder, and a corresponding material discharge pipe is externally arranged at the bottom of the condensing cylinder.
[0011] The material discharge pipe is connected to the feed end of the corresponding primary distillation tower, the discharge end of the primary distillation tower is connected to the feed end of the corresponding secondary distillation tower, and the discharge end of the secondary distillation tower is connected to the feed end of the corresponding material filling equipment.
[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; corresponding sealing gaskets are respectively clamped at the connection between the isolation cover and the fixed base plate.
[0018] The feed ends of the three-way feed pipes are respectively connected in parallel to corresponding reactant feed pipes.
[0019] A method for preparing high-purity phosphorus trifluoride, based on the above-mentioned high-purity phosphorus trifluoride preparation equipment, comprises the following steps:
[0020] S1, adding the reactants phosphorus trichloride and anhydrous hydrogen fluoride into the reaction module through the three-way feed pipe, respectively, and the mixed phosphorus trichloride and anhydrous hydrogen fluoride are alternately passed through the first reaction chamber and the second reaction chamber in sequence to perform a replacement reaction, the reaction temperature is maintained at 40 to 50° C., and the reaction product is discharged along the discharge pipe;
[0021] S2, the product enters through the top of the precooling cylinder, is precooled in the precooling cylinder, and then enters the condensing cylinder for condensation treatment;
[0022] S3, the condensed liquid material enters a primary distillation tower, the primary distillation condensation temperature is between -80°C and -100°C, and the by-product hydrogen chloride produced by the reaction is initially separated and recovered;
[0023] S4, the crude phosphorus trifluoride is transferred to a secondary distillation tower for secondary distillation and purification, and the condensation temperature of the secondary distillation is maintained between -80°C and -100°C;
[0024] S5, the electronic grade phosphorus trifluoride after secondary distillation is filled into a steel cylinder through the corresponding material filling equipment.
[0025] Advantages of the present invention:
[0026] 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. It 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.
[0027] 2) Since the continuous reaction processing of phosphorus trifluoride can significantly improve production efficiency, the subsequent condensation efficiency also needs to be improved accordingly. If a precooling condenser is added, not only will the production cost increase, but some of the liquid materials formed by precooling are likely to carry some gaseous materials when they are extracted, thereby causing adverse effects on subsequent distillation and purification, which is very troublesome. To this end, the present invention further connects a precooling cylinder to the top of the condensing cylinder of the existing condenser, and the feed end of the condensing coil in the precooling cylinder is connected to the external refrigerant, and the discharge end is connected to one of the condensing tubes through a corresponding siphon tee. In this way, during the circulation of the refrigerant in the condenser tube, the refrigerant in the condenser coil can be siphoned synchronously, so that the refrigerant flows through the condenser coil at a smaller flow rate, so that the material in the precooling cylinder can be effectively precooled, and the small amount of liquid material formed by the precooling can be directly discharged into the condenser cylinder to facilitate the extraction of the liquid material, thereby effectively improving the condensation efficiency of the product of the present invention without excessively increasing the cost and energy consumption, so as to help ensure that the continuous reaction processing of phosphorus trifluoride can proceed smoothly.
[0028] 3) 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.
[0029] 4) 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 phosphorus trifluoride reaction processing.
[0030] 5) 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.
[0031] 6) 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 chamber of the present invention are regularly convex, 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
[0032] Figure 1 It is a schematic diagram of the structure of the present invention.
[0033] Figure 2 Schematic diagram of the structure of the microchannel reactor.
[0034] Figure 3 Schematic diagram of the condenser structure.
[0035] Figure 4 Schematic diagram of the structure of the microchannel reactor after removing the fixed bracket.
[0036] Figure 5 Schematic diagram of the reaction module.
[0037] Figure 6 This is a schematic diagram of the structure of the other side of the reaction module.
[0038] Figure 7 It is a schematic diagram of the connection between the first reaction chamber and the second reaction chamber of the reaction module.
[0039] Figure 8 is a cross-sectional view of the first reaction chamber.
[0040] Fig. 9 is a cross-sectional view of the second reaction chamber.
[0041] In the figure: fixed support 1, reaction module 2, first reaction chamber 201, fixed substrate 202, second reaction chamber 203, connecting hole 2031, feed hole 2041, three-way feed pipe 2042, discharge hole 2051, discharge pipe 2052, guide hole 3, block 4, heat exchange mechanism 5, isolation cover 501, heat exchange medium discharge pipe 502, heat exchange medium output pipe 503, heat exchange medium inlet main pipe 504, heat exchange Medium extraction pump 505, heat exchange medium output main pipe 506, locking bolts 6, reactant feed pipe 7, product output pipe 8, condenser 9, sealing plate 901, condensation cylinder 902, refrigerant circulation container 903, condensation pipe 904, pre-cooling cylinder 905, condensation coil 906, refrigerant inlet pipe 10, refrigerant discharge pipe 11, siphon tee 12, material discharge pipe 13, primary distillation tower 14, secondary distillation tower 15. DETAILED DESCRIPTION
[0042] 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:
[0043] Embodiment 1
[0044] refer to Figure 1-9 , a preparation device for high-purity phosphorus trifluoride, comprising:
[0045] The microchannel reactor comprises 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 comprise a plurality of rows of first reaction chambers 201 integrally formed and convexly arranged on the side of a corresponding fixed substrate 202, wherein 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 alternately; a plurality of second reaction chambers 203 are integrally formed and convexly arranged on the other side of the fixed substrate 202, wherein the second reaction chambers 203 are obliquely arranged between the two sides of the adjacent first reaction chambers 201 in the same row, and between the last first reaction chamber 201 and the first first reaction chamber 201 of 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; the fixed substrate 202 is provided with a feed hole 2041 connected to the first first reaction chamber 201 of the first row, and the feed hole 2041 is externally connected to a corresponding three-way feed pipe 2042; the fixed substrate 202 is provided with a discharge hole 2051 connected to the last first reaction chamber 201 of the last row, and the discharge hole 2051 is externally connected to a corresponding discharge pipe 2052;
[0046] The condenser 9 comprises a condensing cylinder 902 with sealing plates 901 fixedly connected at both ends, and corresponding refrigerant circulation containers 903 are respectively sealed and fixedly connected at both ends of the condensing cylinder 902, wherein the end of one refrigerant circulation container 903 is externally connected to a refrigerant inlet pipe 10, and the other refrigerant circulation container 903 is externally connected to a refrigerant outlet pipe 11, and a plurality of corresponding condensing tubes 904 are evenly distributed and installed through the sealing plates 901, and the external refrigerant enters through the refrigerant inlet pipe 10, and the refrigerant flows through the condensing tube 904 and then flows along the refrigerant outlet pipe 11 for discharge; the top of the condensing cylinder 902 is upwardly connected to a precooling cylinder 905 with a closed top, and a corresponding condensing coil 906 is arranged in the precooling cylinder 905, and the feed end of the condensing coil 906 is connected to the external refrigerant, and the discharge end of the condensing coil 906 is connected to one of the condensing pipes 904 through a corresponding siphon tee pipe 12; the discharge pipe 2052 is connected in parallel to the top of the precooling cylinder 905, and the bottom of the condensing cylinder 902 is provided with a corresponding material discharge pipe 13 outwardly.
[0047] 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.
[0048] The present invention further connects a precooling cylinder 905 to the top of the condensing cylinder 902 of the existing condenser 9, and the feed end of the condensing coil 906 in the precooling cylinder 905 is connected to the external refrigerant, and the discharge end is connected to one of the condensing tubes 904 through the corresponding siphon tee 12. In this way, during the circulation of the refrigerant in the condensing tube 904, the refrigerant in the condensing coil 906 can be siphoned synchronously, so that the refrigerant flows through the condensing coil 906 at a relatively small flow rate, so that the material in the precooling cylinder 905 can be effectively precooled, and a small amount of liquid material formed by precooling can be directly discharged into the condensing cylinder 902, so as to facilitate the extraction of liquid materials, thereby effectively improving the condensation efficiency of the product of the present invention without excessively increasing costs and energy consumption, so as to help ensure that the continuous reaction processing of phosphorus trifluoride can proceed smoothly.
[0049] The material discharge pipe 13 is connected to the feed end of the corresponding primary distillation tower 14, the discharge end of the primary distillation tower 14 is connected to the feed end of the corresponding secondary distillation tower 15, and the discharge end of the secondary distillation tower 15 is connected to the feed end of the corresponding material filling equipment.
[0050] 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.
[0051] 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.
[0052] 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.
[0053] The first reaction chamber 201 and the second reaction chamber 203 are integrally formed on the fixed substrate 202 by 3D printing.
[0054] 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 second reaction chamber 202 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, and thus the present invention can be further smoothly applied to the reaction processing of phosphorus trifluoride to realize the continuous reaction processing of phosphorus trifluoride.
[0055] The isolation cover 501 and the fixed base plate 202 are respectively locked and installed by a plurality of corresponding locking bolts 6; corresponding sealing gaskets are respectively clamped at the connection between the isolation cover 501 and the fixed base plate 202.
[0056] The feed ends of the three-way feed pipe 2042 are respectively connected in parallel to the corresponding reactant feed pipes 7 .
[0057] Embodiment 2
[0058] A method for preparing high-purity phosphorus trifluoride, based on the high-purity phosphorus trifluoride preparation equipment described in the above embodiment 1, comprises the following steps:
[0059] S1, adding the reactants phosphorus trichloride and anhydrous hydrogen fluoride into the reaction module 2 through the three-way feed pipe 2042, and the mixed phosphorus trichloride and anhydrous hydrogen fluoride are alternately passed through the first reaction chamber 201 and the second reaction chamber 203 in sequence to perform a replacement reaction, and the reaction temperature is maintained at 40 to 50° C. The product after the reaction is discharged along the discharge pipe 2052;
[0060] S2, the product enters through the top of the precooling cylinder 905, is precooled in the precooling cylinder 905, and then enters the condensing cylinder 902 for condensation treatment;
[0061] S3, the condensed liquid material enters the primary distillation tower 14, the primary distillation condensation temperature is between -80°C and -100°C, and the by-product hydrogen chloride produced by the reaction is initially separated and recovered;
[0062] S4, the crude phosphorus trifluoride is taken out and transferred to the secondary distillation tower 15 for secondary distillation and purification, and the secondary distillation condensation temperature is maintained between -80°C and -100°C;
[0063] S5, the electronic grade phosphorus trifluoride after secondary distillation is filled into a steel cylinder through the corresponding material filling equipment.
[0064] The present invention adopts a continuous reaction, which can not only improve the production efficiency, but also keep the reaction conditions under relatively constant conditions, thereby ensuring the quality stability of the product.
[0065] 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 preparation device for high-purity phosphorus trifluoride, characterized in that: include: A microchannel reactor comprises 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) comprise a plurality of rows of first reaction chambers (201) 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 an alternating manner; a plurality of second reaction chambers (203) are integrally formed and convexly arranged on the other side surface of the fixed substrate (202), and the second reaction chambers (203) are obliquely arranged between the two sides of the adjacent two first reaction chambers (201) in the same row, and between the adjacent first reaction chambers (201). Between the last first reaction chamber (201) and the first first reaction chamber (201) of the two rows of first reaction chambers (201), a material guide hole (3) for conducting the first reaction chamber (201) and the second reaction chamber (203) is provided on the fixed substrate (202); a material feed hole (2041) connected to the first first reaction chamber (201) of the first row is provided on the fixed substrate (202), and a corresponding three-way material feed pipe (2042) is externally connected to the material feed hole (2041); a material discharge hole (2051) connected to the last first reaction chamber (201) of the last row is provided on the fixed substrate (202), and a corresponding material discharge pipe (2052) is externally connected to the material discharge hole (2051); The condenser (9) comprises a condensing cylinder (902) with sealing plates (901) fixedly connected at both ends, and the two ends of the condensing cylinder (902) are respectively sealed and fixedly connected with corresponding refrigerant circulation containers (903), wherein the end of one refrigerant circulation container (903) is externally connected to a refrigerant inlet pipe (10), and the other refrigerant circulation container (903) is externally connected to a refrigerant outlet pipe (11), and a plurality of corresponding condensing tubes (904) are evenly distributed and installed through the sealing plates (901), and the external refrigerant enters through the refrigerant inlet pipe (10), and the refrigerant flows through the condensing tube (904) and then flows out along the refrigerant outlet pipe (11) for discharge; the top of the condensing cylinder (902) is connected upwardly to a precooling cylinder (905) with a sealed top, a corresponding condensing coil (906) is arranged in the precooling cylinder (905), the feed end of the condensing coil (906) is connected to the external refrigerant, and the discharge end of the condensing coil (906) is connected to one of the condensing tubes (904) through a corresponding siphon tee (12); the discharge pipe (2052) is connected in parallel to the top of the precooling cylinder (905), and a corresponding material discharge pipe (13) is arranged outwardly at the bottom of the condensing cylinder (902); 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).
2. The preparation equipment of high-purity phosphorus trifluoride according to claim 1, characterized in that: The material discharge pipe (13) is connected to the feed end of the corresponding primary distillation tower (14), the discharge end of the primary distillation tower (14) is connected to the feed end of the corresponding secondary distillation tower (15), and the discharge end of the secondary distillation tower (15) is connected to the feed end of the corresponding material filling equipment.
3. The preparation equipment of high-purity phosphorus trifluoride according to claim 2, characterized in that: 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) being 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) being discharged through corresponding heat exchange medium output main pipes (506).
4. The preparation equipment of high-purity phosphorus trifluoride according to claim 3, 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); and corresponding sealing gaskets are respectively provided at the connection points between the isolation cover (501) and the fixed base plate (202).
5. The preparation equipment of high-purity phosphorus trifluoride according to claim 2, characterized in that: The feed ends of the three-way feed pipe (2042) are respectively connected in parallel to the corresponding reactant feed pipes (7).
6. A method for preparing high-purity phosphorus trifluoride, based on the high-purity phosphorus trifluoride preparation equipment according to any one of claims 2 to 5, characterized in that: The following specific steps are included: S1, adding the reactants phosphorus trichloride and anhydrous hydrogen fluoride into the reaction module (2) through the three-way feed pipe (2042), and the mixed phosphorus trichloride and anhydrous hydrogen fluoride are alternately passed through the first reaction chamber (201) and the second reaction chamber (203) in sequence to perform a replacement reaction, the reaction temperature is maintained at 40 to 50° C., and the product after the reaction is discharged along the discharge pipe (2052); S2, the product enters through the top of the precooling cylinder (905), is precooled in the precooling cylinder (905), and then enters the condensing cylinder (902) for condensation treatment; S3, the condensed liquid material enters a primary distillation tower (14), the primary distillation condensation temperature is between -80°C and -100°C, and the by-product hydrogen chloride produced by the reaction is initially separated and recovered; S4, the crude phosphorus trifluoride is taken out and transferred to a secondary distillation tower (15) for secondary distillation and purification, and the secondary distillation condensation temperature is maintained between -80°C and -100°C; S5, the electronic grade phosphorus trifluoride after secondary distillation is filled into a steel cylinder through the corresponding material filling equipment.
Citation Information
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