WO2024027149A1 - Phosphorus pentafluoride gas generator and phosphorus pentafluoride gas generation method - Google Patents

Phosphorus pentafluoride gas generator and phosphorus pentafluoride gas generation method Download PDF

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Publication number
WO2024027149A1
WO2024027149A1 PCT/CN2023/079338 CN2023079338W WO2024027149A1 WO 2024027149 A1 WO2024027149 A1 WO 2024027149A1 CN 2023079338 W CN2023079338 W CN 2023079338W WO 2024027149 A1 WO2024027149 A1 WO 2024027149A1
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Prior art keywords
hydrogen fluoride
liquid hydrogen
generator
phosphorus pentafluoride
pentafluoride gas
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PCT/CN2023/079338
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French (fr)
Chinese (zh)
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李振星
许晟
陈宏伟
西松江英
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森松（江苏）重工有限公司
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Publication of WO2024027149A1 publication Critical patent/WO2024027149A1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/10—Halides or oxyhalides of phosphorus
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a phosphorus pentafluoride gas generator and a phosphorus pentafluoride gas generating method, in particular to a phosphorus pentafluoride gas generator for producing phosphorus pentafluoride gas required when using a hydrogen fluoride solvent method to synthesize lithium hexafluorophosphate. and a phosphorus pentafluoride gas generating method using a phosphorus pentafluoride gas generator to generate phosphorus pentafluoride gas.
  • lithium hexafluorophosphate As the key material of lithium ion batteries, lithium hexafluorophosphate is used in lithium ion electrolyte in two main forms. One is crystalline lithium hexafluorophosphate, and the other is liquid lithium salt prepared with organic solvents. Currently, crystalline lithium hexafluorophosphate is sold in foreign markets. The main reason is that it is easier to transport and preserve products, has fewer safety hazards, and is more consistent with the process system of electrolyte manufacturers. With the healthy and steady development of the domestic new energy industry, the demand for crystalline lithium hexafluorophosphate is also increasing day by day. Breaking through and improving the production process of crystalline lithium hexafluorophosphate and improving the quality of crystalline lithium hexafluorophosphate products are the focus of current domestic research.
  • the preparation methods of lithium hexafluorophosphate mainly include the following: gas-solid direct reaction method, solvent method and ion exchange method.
  • the most researched, most mature technology and most widely used industrial method is the hydrogen fluoride solvent method.
  • the existing hydrogen fluoride solvent method is to dissolve lithium salt in anhydrous hydrofluoric acid to form a LiFHF solution, and then introduce phosphorus pentafluoride (PF 5 ) gas to react to produce lithium hexafluorophosphate. That is, the process of preparing lithium hexafluorophosphate by hydrogen fluoride solvent method is currently a relatively mature process and is also the easiest production method to achieve industrialization.
  • the hydrogen fluoride solvent method uses hydrogen fluoride as the reaction medium, dissolves the raw material lithium halide in the hydrogen fluoride, and then vaporizes the high-purity phosphorus pentafluoride, then passes the gas into the solvent to react to generate lithium hexafluorophosphate crystals, and the reaction is completed Afterwards, the lithium hexafluorophosphate product is finally obtained through crystallization, separation, drying, etc.
  • phosphorus pentafluoride gas generators that produce phosphorus pentafluoride gas used when synthesizing lithium hexafluorophosphate using the hydrogen fluoride solvent method
  • phosphorus pentafluoride gas generators there are two types of phosphorus pentafluoride gas generators: a horizontal phosphorus pentafluoride gas generator and a vertical phosphorus pentafluoride gas generator.
  • the infusion tubes should be inserted more and more evenly into the generator; on the other hand, , by setting a stirring device in the generator to stir and reverse the phosphorus pentachloride solid. That is to say, the solid material of phosphorus pentachloride is allowed to contact and react with liquid hydrogen fluoride while stirring, which can make the reaction more complete and increase the amount of phosphorus pentafluoride gas produced per unit time.
  • the number and distribution of the inserted infusion tubes will affect and limit the sufficient mixing of the materials by the stirrer installed in the generator. That is to say, the existing technology of the generator has sacrifices to prevent the infusion tubes from fighting with the stirrer. The opportunity for liquid hydrogen fluoride to come into contact with solid phosphorus pentachloride will affect the gas generation efficiency of the generator.
  • the invention provides a phosphorus pentafluoride gas generator, which includes: a generator cylinder composed of an upper cylinder and a lower cylinder, a stirring device arranged in the generator cylinder, a liquid hydrogen fluoride supply device and a gas generator connected to the generator cylinder.
  • the gas delivery pipeline for transporting phosphorus pentafluoride gas to the next process device is connected to the device cylinder.
  • the upper cylinder is provided with a liquid material adder for adding liquid hydrogen fluoride into the generator cylinder.
  • the liquid material adder is connected to the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline;
  • the lower cylinder has a liquid hydrogen fluoride permeability jacket arranged along the inner wall of the lower cylinder, and the liquid hydrogen fluoride permeability jacket has a load-bearing and an isolation filter plate that contacts the phosphorus pentachloride solid material in the generator barrel.
  • the liquid hydrogen fluoride permeability jacket is connected to the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline; it is supplied to the liquid hydrogen fluoride supply device through the liquid hydrogen fluoride supply device.
  • the liquid hydrogen fluoride in the liquid hydrogen fluoride penetration jacket penetrates into the generator barrel through the isolation filter plate, and reacts with the phosphorus pentachloride solid material in the generator barrel.
  • At least the isolation filter plate of the liquid hydrogen fluoride permeation jacket is formed into a cone shape.
  • the isolation filter plate adopts a multi-layer sintered filter mesh.
  • a cooling jacket is provided on the outer wall of at least one of the upper cylinder and the lower cylinder, and the cooling jacket is connected to the cooling circulation device through a cooling medium delivery pipeline.
  • the stirring device has a hollow spiral belt, and the spiral belt is connected to the cooling circulation device.
  • a powder filter is provided on the gas delivery pipeline.
  • a temperature transmitter is provided in the generator barrel, and a regulating valve is provided on the cooling medium delivery pipeline.
  • the present invention also provides a phosphorus pentafluoride gas generation method that utilizes the above-mentioned phosphorus pentafluoride gas generator to generate phosphorus pentafluoride gas, which at least includes the following steps: adding phosphorus pentachloride solid material to the The solid material feeding process in the generator barrel; and the liquid material feeding process of adding liquid hydrogen fluoride into the generator barrel through the liquid material feeder; and penetrating liquid hydrogen fluoride into the generator barrel through the liquid hydrogen fluoride penetration jacket. The liquid material penetration process in the generator barrel.
  • the pressure in the generator barrel is adjusted through the liquid material feeding process.
  • liquid hydrogen fluoride is added to the liquid hydrogen fluoride penetration jacket. inside the generator barrel.
  • the liquid hydrogen fluoride participating in the reaction can fully contact and react with the phosphorus pentachloride solid material of the reaction object, thereby improving the efficiency of the phosphorus pentafluoride gas. efficiency occurs.
  • Figure 1 shows a schematic structural diagram of the phosphorus pentafluoride gas generator of the present invention.
  • the phosphorus pentafluoride gas generator 10 of the present invention has a generator cylinder 11 and a stirring device 12 provided in the generator cylinder 11 .
  • the generator cylinder 11 is composed of an upper cylinder 11a and a lower cylinder 11b.
  • a solid material feeding device 13 is provided on the upper cylinder 11a.
  • the solid material feeding device 13 includes a hard-sealed ball valve 13a and a sealed funnel 13b.
  • the upper cylinder 11a is provided with two sprayers 11c as liquid material adders for adding liquid hydrogen fluoride into the generator cylinder 11. Each of the sprayers 11c passes through a liquid hydrogen fluoride supply pipe. The path 11d is connected to the liquid hydrogen fluoride supply device 20.
  • the liquid material feeder is provided with a flow meter 11e and a regulating valve 11f.
  • the upper cylinder 11a is connected to the next process device 30 through a gas delivery pipeline 11g, and a powder filter 40 is provided on the gas delivery pipeline 11g.
  • the next process device 30 is, for example, a synthesis system for lithium hexafluorophosphate.
  • the lower cylinder 11b has a liquid hydrogen fluoride permeation jacket 14 provided along the inner wall of the lower cylinder 11b.
  • the hydrogen fluoride permeation jacket 14 has an isolation filter plate 14a for carrying and contacting the phosphorus pentachloride solid material in the generator barrel 11.
  • the liquid hydrogen fluoride permeation jacket 14 is connected to the liquid hydrogen fluoride supply pipeline 14b through the liquid hydrogen fluoride supply pipeline 14b.
  • the liquid hydrogen fluoride supply device 20 is connected.
  • the liquid hydrogen fluoride supply pipeline 14b is connected with the other liquid hydrogen fluoride supply pipeline 11d.
  • the lower cylinder 11b is formed into a cone, and the diameter of the cone bottom circumference is basically the same as the diameter of the cylindrical upper cylinder 11a, and they are connected together.
  • the liquid hydrogen fluoride permeation jacket 14 is formed along the conical surface of the lower cylinder 11b, and the isolation filter plate 14a is formed in a cone shape.
  • the isolation filter plate 14a adopts a multi-layer sintered filter mesh.
  • the liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket 14 through the liquid hydrogen fluoride supply device 20 penetrates into the generator cylinder 11 through the isolation filter plate 14a, and interacts with the liquid hydrogen fluoride in the generator cylinder 11.
  • the solid material of phosphorus pentachloride in contact with the isolation filter plate 14a reacts.
  • the isolation filter plate 14a has a structure and characteristics that allow liquid hydrogen fluoride to permeate but prevent the solid material of phosphorus pentachloride from passing through.
  • cooling jackets 15a and 15b are respectively provided on the outer walls of the upper cylinder 11a and the lower cylinder 11b.
  • the cooling jackets 15a and 15b communicate with the cooling circulation device through the cooling medium delivery pipelines 15c and 15d. 50 connected.
  • the cooling cycle device 50 includes a cooling medium supply device 50b and a cooling medium recovery device 50a.
  • the cooling medium is transported from the cooling medium supply device 50b through the cooling medium delivery pipe 15d into the cooling jackets 15a and 15b respectively, and then passes through the cooling medium delivery pipes from the cooling jackets 15a and 15b respectively.
  • the path 15c is conveyed back to the cooling medium recovery device 50a.
  • the cooling medium delivery pipeline 15c is provided with a regulating valve 15e.
  • a hard-sealed ball valve 16 for discharging unreacted phosphorus pentachloride solid material is provided at the bottom of the lower cylinder 11b.
  • the stirring device 12 includes a spiral blade 12a that stirs and rotates in the generator cylinder 11 and a drive motor 12b that drives the blade 12a.
  • the blades 12a are hollow and connected to a cooling circulation device (not shown). During the stirring process, the temperature of the reaction between the stirred phosphorus pentachloride solid material and the liquid hydrogen fluoride can be adjusted by passing a temperature adjustment medium into the hollow blade 12a.
  • a temperature transmitter 60 is also provided in the generator barrel 11.
  • the temperature transmitter 60 is used to monitor the temperature changes in the generator barrel 11, thereby adjusting and controlling it in coordination with the regulating valve 15e.
  • the phosphorus pentafluoride gas generator of the present invention and the method for generating phosphorus pentafluoride gas using the phosphorus pentafluoride gas generator will be described with reference to FIG. 1 .
  • the drive motor 12b is turned on to drive the paddle 12a to rotate, and then the solid material of phosphorus pentachloride is added to the generator barrel 11 through the hard-sealed ball valve 13a and the closed funnel 13b.
  • the upper cover of the hard-sealed ball valve 13a and the sealed funnel 13b is opened, the solid material of phosphorus pentachloride is added from the sealed funnel 13b into the generator barrel 11, and closed after the addition is completed.
  • the hard-sealed ball valve 13a and the upper cover plate of the airtight funnel 13b At this point, the solid material feeding process of adding phosphorus pentachloride solid material into the generator barrel 11 is completed.
  • liquid hydrogen fluoride is transported from the liquid hydrogen fluoride supply device 20 to the sprinkler 11c through the flow meter 11e and the regulating valve 11f through the liquid hydrogen fluoride supply pipeline 11d, and then is sprayed to all locations through the sprinkler 11c. inside the generator barrel 11.
  • the pressure in the generator barrel 11 is monitored through a pressure monitoring device (not shown).
  • the liquid hydrogen fluoride permeability jacket 14 is used to monitor the pressure inside the generator barrel 11 .
  • Liquid hydrogen fluoride is permeated into the generator barrel 11 . That is, the liquid material feeding process of adding liquid hydrogen fluoride into the generator barrel 11 through the liquid material feeder 11c and penetrating liquid hydrogen fluoride into the generator barrel through the liquid hydrogen fluoride penetration jacket 14 are performed. Liquid material penetration process within 11.
  • the cooling circulation device 50 supplies cooling medium to the cooling jackets 15a, 15b and circulates the cooling medium, thereby controlling the temperature of the generator barrel 11.
  • the transmitter 60 is used to monitor the temperature change in the generator barrel 11, and coordinates with the regulating valve 15e to adjust and control the temperature in the generator barrel 11.
  • the temperature of the reaction between the stirred phosphorus pentachloride solid material and the liquid hydrogen fluoride is adjusted by passing the temperature adjustment medium into the hollow blade 12a.
  • the phosphorus pentafluoride gas reacted in the generator cylinder 11 is filtered by the powder filter 40 and then transported to the next process device 30 through the gas transport pipeline 11g.
  • the unreacted phosphorus pentachloride solid material is discharged from the generator barrel 11 through the hard-sealed ball valve 16 for recycling.
  • the use of the phosphorus pentafluoride gas generator and the phosphorus pentafluoride gas generation method of the present invention has the following advantages.
  • the present invention provides a liquid hydrogen fluoride permeation jacket 14 with an isolation filter plate 14a for carrying and contacting the phosphorus pentachloride solid material in the generator barrel 11, and allows the liquid hydrogen fluoride to pass through the liquid hydrogen fluoride supply device 20
  • the liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket 14 penetrates into the generator barrel 11 through the isolation filter plate 14a, and reacts with the phosphorus pentachloride solid material in the generator barrel 11. Therefore, the liquid hydrogen fluoride participating in the reaction can fully contact and react with the solid material of phosphorus pentachloride as the reaction object, thereby improving the generation efficiency of phosphorus pentafluoride gas.
  • the liquid hydrogen fluoride permeation jacket 14 has a cone-shaped isolation filter plate 14a, which can increase the contact area between the liquid hydrogen fluoride and the phosphorus pentachloride solid material.
  • Cooling jackets 15a and 15b are provided on the generator cylinder 11, and the blades 12a of the stirring device 12 are also Formed into a hollow shape, the temperature and reaction temperature of the phosphorus pentafluoride gas generator 10 during the generation of phosphorus pentafluoride gas can be controlled through a circulating cooling medium, thereby improving the generation efficiency of phosphorus pentafluoride gas.
  • a flow meter and a regulating valve may be provided on the liquid hydrogen fluoride supply line 14b to control the liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket 14.
  • the number of sprinklers 11c serving as liquid material feeders may be one or three or more.
  • liquid hydrogen fluoride permeation jacket 14 and its isolation filter plate 14a may also be made into shapes other than conical shapes.

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  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention provides a phosphorus pentafluoride gas generator and a phosphorus pentafluoride gas generation method. Two liquid material feeders used for feeding liquid hydrogen fluoride into a generator cylinder are arranged on an upper cylinder of the generator cylinder. A lower cylinder of the generator cylinder is provided with a liquid hydrogen fluoride permeation jacket arranged along the inner wall of the lower cylinder. The liquid hydrogen fluoride permeation jacket is provided with an isolation filter plate used for bearing and contacting a phosphorus pentachloride solid material in the generator cylinder. The liquid hydrogen fluoride supplied by a liquid hydrogen fluoride supply device permeates into the generator cylinder through the isolation filter plate and reacts with the phosphorus pentachloride solid material. By using the phosphorus pentafluoride gas generator and the phosphorus pentafluoride gas generation method, liquid hydrogen fluoride participating in reaction can fully contact and react with a phosphorus pentachloride solid material of a reaction object, so that the generation efficiency of a phosphorus pentafluoride gas is improved.

Description

一种五氟化磷气体发生器和五氟化磷气体发生方法A phosphorus pentafluoride gas generator and a phosphorus pentafluoride gas generating method
本申请要求申请号为202210916053.2、申请日为2022年08月01日、发明名称为“一种五氟化磷气体发生器和五氟化磷气体发生方法”的中国发明专利申请的优先权，在此通过引用并入本文。This application requires the priority of the Chinese invention patent application with the application number 202210916053.2, the filing date being August 1, 2022, and the invention title being "a phosphorus pentafluoride gas generator and a phosphorus pentafluoride gas generating method", in This is incorporated herein by reference.
技术领域Technical field
本发明涉及一种五氟化磷气体发生器和五氟化磷气体发生方法，特别是一种为了生产采用氟化氢溶剂法合成六氟磷酸锂时所需的五氟化磷气体的五氟化磷气体发生器和利用五氟化磷气体发生器来产生五氟化磷气体的五氟化磷气体发生方法。The present invention relates to a phosphorus pentafluoride gas generator and a phosphorus pentafluoride gas generating method, in particular to a phosphorus pentafluoride gas generator for producing phosphorus pentafluoride gas required when using a hydrogen fluoride solvent method to synthesize lithium hexafluorophosphate. and a phosphorus pentafluoride gas generating method using a phosphorus pentafluoride gas generator to generate phosphorus pentafluoride gas.
背景技术Background technique
作为锂离子电池关键材料锂盐的六氟磷酸锂应用于锂离子电解液主要有两种形态，一是晶体六氟磷酸锂，二是与有机溶剂配制的液态锂盐。目前国外市场销售的均为晶体六氟磷酸锂，其原因主要是有利于产品运输与保存、安全隐患较小，与电解液生产厂家工艺体系更为匹配。随着国内新能源产业的健康持续稳步发展，晶体六氟磷酸锂的需求也与日俱增，突破和完善晶体六氟磷酸锂生产工艺，提高晶体六氟磷酸锂产品品质是当前国内研究的重点。As the key material of lithium ion batteries, lithium hexafluorophosphate is used in lithium ion electrolyte in two main forms. One is crystalline lithium hexafluorophosphate, and the other is liquid lithium salt prepared with organic solvents. Currently, crystalline lithium hexafluorophosphate is sold in foreign markets. The main reason is that it is easier to transport and preserve products, has fewer safety hazards, and is more consistent with the process system of electrolyte manufacturers. With the healthy and steady development of the domestic new energy industry, the demand for crystalline lithium hexafluorophosphate is also increasing day by day. Breaking through and improving the production process of crystalline lithium hexafluorophosphate and improving the quality of crystalline lithium hexafluorophosphate products are the focus of current domestic research.
目前，六氟磷酸锂的制备方法主要有以下几种：气固直接反应法、溶剂法以及离子交换法，其中研究最多、技术最为成熟、产业化应用最广泛的工艺是氟化氢溶剂法。现有氟化氢溶剂法是将锂盐溶于无水氢氟酸中形成LiFHF溶液，然后通入五氟化磷(PF5)气体进行反应而生产出六氟磷酸锂。即，氟化氢溶剂法制备六氟磷酸锂的工艺是目前较为成熟的工艺，也是最易于实现工业化的生产方法。At present, the preparation methods of lithium hexafluorophosphate mainly include the following: gas-solid direct reaction method, solvent method and ion exchange method. Among them, the most researched, most mature technology and most widely used industrial method is the hydrogen fluoride solvent method. The existing hydrogen fluoride solvent method is to dissolve lithium salt in anhydrous hydrofluoric acid to form a LiFHF solution, and then introduce phosphorus pentafluoride (PF 5 ) gas to react to produce lithium hexafluorophosphate. That is, the process of preparing lithium hexafluorophosphate by hydrogen fluoride solvent method is currently a relatively mature process and is also the easiest production method to achieve industrialization.
具体地说，氟化氢溶剂法是利用氟化氢作为反应介质，将原料卤化锂溶解在氟化氢中，再将高纯五氟化磷气化后，将气体通入溶剂中进行反应来生成六氟磷酸锂晶体，反应结束后，再经过结晶分离、干燥等最终得到六氟磷酸锂产品。Specifically, the hydrogen fluoride solvent method uses hydrogen fluoride as the reaction medium, dissolves the raw material lithium halide in the hydrogen fluoride, and then vaporizes the high-purity phosphorus pentafluoride, then passes the gas into the solvent to react to generate lithium hexafluorophosphate crystals, and the reaction is completed Afterwards, the lithium hexafluorophosphate product is finally obtained through crystallization, separation, drying, etc.
作为现有的生产采用氟化氢溶剂法来合成六氟磷酸锂时使用的五氟化磷气体的五氟化磷气体发生器，具有卧式五氟化磷气体发生器和立式五氟化磷气体发生器两大类，但无论是哪种五氟化磷气体发生器，其结构和工艺流程都是在发生器的容器中插入有用于输入液态氟化氢的输液管，通过该输液管输入的液态氟化氢跟装入到发生器中的物料(五氯化磷固体)反应后，便产生所需的五氟化磷气体。 As existing phosphorus pentafluoride gas generators that produce phosphorus pentafluoride gas used when synthesizing lithium hexafluorophosphate using the hydrogen fluoride solvent method, there are two types of phosphorus pentafluoride gas generators: a horizontal phosphorus pentafluoride gas generator and a vertical phosphorus pentafluoride gas generator. Large categories, but no matter what kind of phosphorus pentafluoride gas generator, its structure and process flow are that an infusion tube for inputting liquid hydrogen fluoride is inserted into the container of the generator, and the liquid hydrogen fluoride input through the infusion tube is followed by the After the material in the generator (phosphorus pentachloride solid) reacts, the required phosphorus pentafluoride gas is produced.
为了提高液态氟化氢与五氯化磷固体的接触机会，以此提高五氟化磷气体的发生效率，一方面是让所述输液管插入较多且较均匀地插入到发生器中，另一方面，通过在发生器中设置搅拌装置，来对五氯化磷固体进行搅拌反转。就是说，让五氯化磷固体物料一边搅拌一边与液态氟化氢接触反应，这样可以让反应更加充分，使得单位时间里所产生的五氟化磷气体的量变大。但插入的输液管的数量以及分布情况，会影响和限制到发生器内设置的搅拌器对物料的充分搅拌，也就是说现有技术的发生器，存在为防止输液管与搅拌器打架而牺牲让液态氟化氢与五氯化磷固体接触的机会，从而影响到发生器的气体发生效率的问题。In order to increase the contact opportunities between liquid hydrogen fluoride and solid phosphorus pentachloride, thereby improving the generation efficiency of phosphorus pentafluoride gas, on the one hand, the infusion tubes should be inserted more and more evenly into the generator; on the other hand, , by setting a stirring device in the generator to stir and reverse the phosphorus pentachloride solid. That is to say, the solid material of phosphorus pentachloride is allowed to contact and react with liquid hydrogen fluoride while stirring, which can make the reaction more complete and increase the amount of phosphorus pentafluoride gas produced per unit time. However, the number and distribution of the inserted infusion tubes will affect and limit the sufficient mixing of the materials by the stirrer installed in the generator. That is to say, the existing technology of the generator has sacrifices to prevent the infusion tubes from fighting with the stirrer. The opportunity for liquid hydrogen fluoride to come into contact with solid phosphorus pentachloride will affect the gas generation efficiency of the generator.
因此，本技术领域急需一种让参与反应的液态氟化氢能充分与反应对象的五氯化磷固体物料接触反应，从而提高气体发生效率的五氟化磷气体发生器。Therefore, there is an urgent need in this technical field for a phosphorus pentafluoride gas generator that allows the liquid hydrogen fluoride participating in the reaction to fully contact and react with the phosphorus pentachloride solid material of the reaction object, thereby improving the gas generation efficiency.
发明内容Contents of the invention
本发明提供的一种五氟化磷气体发生器，包括：由上筒体和下筒体构成的发生器筒体、设置在该发生器筒体内的搅拌装置、液态氟化氢供给装置以及与该发生器筒体连通的将五氟化磷气体输送至下一工序装置的气体输送管路，所述上筒体上设置有用于将液态氟化氢加入至发生器筒体内的液体物料加入器，各所述液体物料加入器通过液态氟化氢供给管路与所述液态氟化氢供给装置相连；所述下筒体，具有沿下筒体内壁设置的液态氟化氢渗透夹套，该液态氟化氢渗透夹套，具有用于承载和接触所述发生器筒体内的五氯化磷固体物料的隔离滤板，该液态氟化氢渗透夹套通过液态氟化氢供给管路与所述液态氟化氢供给装置相连；通过所述液态氟化氢供给装置供给到所述液态氟化氢渗透夹套的液态氟化氢，通过隔离滤板渗透到所述发生器筒体内，与所述发生器筒体内的五氯化磷固体物料进行反应。The invention provides a phosphorus pentafluoride gas generator, which includes: a generator cylinder composed of an upper cylinder and a lower cylinder, a stirring device arranged in the generator cylinder, a liquid hydrogen fluoride supply device and a gas generator connected to the generator cylinder. The gas delivery pipeline for transporting phosphorus pentafluoride gas to the next process device is connected to the device cylinder. The upper cylinder is provided with a liquid material adder for adding liquid hydrogen fluoride into the generator cylinder. Each of the above mentioned The liquid material adder is connected to the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline; the lower cylinder has a liquid hydrogen fluoride permeability jacket arranged along the inner wall of the lower cylinder, and the liquid hydrogen fluoride permeability jacket has a load-bearing and an isolation filter plate that contacts the phosphorus pentachloride solid material in the generator barrel. The liquid hydrogen fluoride permeability jacket is connected to the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline; it is supplied to the liquid hydrogen fluoride supply device through the liquid hydrogen fluoride supply device. The liquid hydrogen fluoride in the liquid hydrogen fluoride penetration jacket penetrates into the generator barrel through the isolation filter plate, and reacts with the phosphorus pentachloride solid material in the generator barrel.
优选地，所述液态氟化氢渗透夹套，至少其所述隔离滤板形成为锥体状。Preferably, at least the isolation filter plate of the liquid hydrogen fluoride permeation jacket is formed into a cone shape.
优选地，所述隔离滤板，采用多层烧结滤网。Preferably, the isolation filter plate adopts a multi-layer sintered filter mesh.
优选地，所述上筒体和所述下筒体的至少一者的外壁上设置有冷却夹套，所述冷却夹套通过冷却媒介输送管路与冷却循环装置相连。Preferably, a cooling jacket is provided on the outer wall of at least one of the upper cylinder and the lower cylinder, and the cooling jacket is connected to the cooling circulation device through a cooling medium delivery pipeline.
进一步优选地，所述搅拌装置，具有中空构造的螺带，且该螺带与冷却循环装置相连。Further preferably, the stirring device has a hollow spiral belt, and the spiral belt is connected to the cooling circulation device.
进一步优选地，所述气体输送管路上设置有粉体过滤器。Further preferably, a powder filter is provided on the gas delivery pipeline.
进一步优选地，所述发生器筒体内设有温度变送器，所述冷却媒介输送管路上设有调节阀。 Further preferably, a temperature transmitter is provided in the generator barrel, and a regulating valve is provided on the cooling medium delivery pipeline.
本发明还提供一种利用上述的五氟化磷气体发生器来产生五氟化磷气体的五氟化磷气体发生方法，其中，至少包括以下工序：将五氯化磷固体物料加入到所述发生器筒体内的固体物料加料工序；和通过所述液体物料加入器将液态氟化氢加入到所述发生器筒体内的液体物料加料工序；和通过所述液态氟化氢渗透夹套将液态氟化氢渗透加入到所述发生器筒体内的液体物料渗透工序。The present invention also provides a phosphorus pentafluoride gas generation method that utilizes the above-mentioned phosphorus pentafluoride gas generator to generate phosphorus pentafluoride gas, which at least includes the following steps: adding phosphorus pentachloride solid material to the The solid material feeding process in the generator barrel; and the liquid material feeding process of adding liquid hydrogen fluoride into the generator barrel through the liquid material feeder; and penetrating liquid hydrogen fluoride into the generator barrel through the liquid hydrogen fluoride penetration jacket. The liquid material penetration process in the generator barrel.
优选地，通过所述液体物料加料工序来调整所述发生器筒体内的压力，当所述发生器筒体内的压力达到规定压力后，再通过所述液态氟化氢渗透夹套将液态氟化氢渗透加入到所述发生器筒体内。Preferably, the pressure in the generator barrel is adjusted through the liquid material feeding process. When the pressure in the generator barrel reaches a prescribed pressure, liquid hydrogen fluoride is added to the liquid hydrogen fluoride penetration jacket. inside the generator barrel.
根据本发明的五氟化磷气体发生器及五氟化磷气体发生方法，可以让参与反应的液态氟化氢能充分与反应对象的五氯化磷固体物料接触反应，从而提高五氟化磷气体的发生效率。According to the phosphorus pentafluoride gas generator and the phosphorus pentafluoride gas generating method of the present invention, the liquid hydrogen fluoride participating in the reaction can fully contact and react with the phosphorus pentachloride solid material of the reaction object, thereby improving the efficiency of the phosphorus pentafluoride gas. efficiency occurs.
附图说明Description of the drawings
图1示出本发明的五氟化磷气体发生器的结构示意图。Figure 1 shows a schematic structural diagram of the phosphorus pentafluoride gas generator of the present invention.
图中：10-五氟化磷气体发生器；11-发生器筒体；12-搅拌装置；13-固体物料加料装置；14-液态氟化氢渗透夹套；11c-液体物料加入器；14a-隔离滤板；20-液态氟化氢供给装置；50-冷却循环装置。In the picture: 10-phosphorus pentafluoride gas generator; 11-generator cylinder; 12-stirring device; 13-solid material feeding device; 14-liquid hydrogen fluoride penetration jacket; 11c-liquid material feeder; 14a-isolation Filter plate; 20-liquid hydrogen fluoride supply device; 50-cooling circulation device.
具体实施方式Detailed ways
以下通过具体实施方式对本发明的技术方案及其效果进行详细说明。以下实施方式仅用于说明本发明的内容，发明并不仅限于下述实施方式或实施例。应用本发明的构思对本发明进行的简单改变都在本发明要求保护的范围内。The technical solutions and effects of the present invention will be described in detail below through specific embodiments. The following embodiments are only used to illustrate the content of the present invention, and the invention is not limited to the following embodiments or examples. Simple changes made to the present invention by applying the concept of the present invention are within the scope of protection claimed by the present invention.
本发明的五氟化磷气体发生器10，如图1所示，具有发生器筒体11和该发生器筒体11内设置的搅拌装置12。The phosphorus pentafluoride gas generator 10 of the present invention, as shown in FIG. 1 , has a generator cylinder 11 and a stirring device 12 provided in the generator cylinder 11 .
所述发生器筒体11，由上筒体11a和下筒体11b构成。在上筒体11a上设置有固体物料加料装置13，该固体物料加料装置13包含硬密封球阀13a及密闭漏斗13b。The generator cylinder 11 is composed of an upper cylinder 11a and a lower cylinder 11b. A solid material feeding device 13 is provided on the upper cylinder 11a. The solid material feeding device 13 includes a hard-sealed ball valve 13a and a sealed funnel 13b.
所述上筒体11a上设置有2个用于将液态氟化氢加入到所述发生器筒体11内的作为液体物料加入器的喷淋器11c，各所述喷淋器11c通过液态氟化氢供给管路11d与液态氟化氢供给装置20相连。该液体物料加入器上设置有流量计11e和调节阀11f。The upper cylinder 11a is provided with two sprayers 11c as liquid material adders for adding liquid hydrogen fluoride into the generator cylinder 11. Each of the sprayers 11c passes through a liquid hydrogen fluoride supply pipe. The path 11d is connected to the liquid hydrogen fluoride supply device 20. The liquid material feeder is provided with a flow meter 11e and a regulating valve 11f.
另外，所述上筒体11a，通过气体输送管路11g与下一工序装置30相连，该气体输送管路11g上设有粉体过滤器40。该下一工序装置30，比如是六氟磷酸锂的合成系统。In addition, the upper cylinder 11a is connected to the next process device 30 through a gas delivery pipeline 11g, and a powder filter 40 is provided on the gas delivery pipeline 11g. The next process device 30 is, for example, a synthesis system for lithium hexafluorophosphate.
所述下筒体11b，具有沿该下筒体11b内壁设置的液态氟化氢渗透夹套14，该液态 氟化氢渗透夹套14，具有用于承载和接触所述发生器筒体11内的五氯化磷固体物料的隔离滤板14a，该液态氟化氢渗透夹套14通过液态氟化氢供给管路14b与所述液态氟化氢供给装置20相连。本实施例中，所述液态氟化氢供给管路14b，与另一所述液态氟化氢供给管路11d相连通的。The lower cylinder 11b has a liquid hydrogen fluoride permeation jacket 14 provided along the inner wall of the lower cylinder 11b. The hydrogen fluoride permeation jacket 14 has an isolation filter plate 14a for carrying and contacting the phosphorus pentachloride solid material in the generator barrel 11. The liquid hydrogen fluoride permeation jacket 14 is connected to the liquid hydrogen fluoride supply pipeline 14b through the liquid hydrogen fluoride supply pipeline 14b. The liquid hydrogen fluoride supply device 20 is connected. In this embodiment, the liquid hydrogen fluoride supply pipeline 14b is connected with the other liquid hydrogen fluoride supply pipeline 11d.
本实施方式中，所述下筒体11b形成为圆锥体，其锥体底部圆周的直径与成圆筒状的所述上筒体11a的直径基本相同，且连接成一体。所述液态氟化氢渗透夹套14，沿着所述下筒体11b的圆锥面形成，所述隔离滤板14a形成为锥体状。所述隔离滤板14a，采用多层烧结滤网。通过所述液态氟化氢供给装置20供给到所述液态氟化氢渗透夹套14的液态氟化氢，通过所述隔离滤板14a渗透到所述发生器筒体11内，与所述发生器筒体11内的与所述隔离滤板14a接触的五氯化磷固体物料进行反应。所述隔离滤板14a，具有能让液态氟化氢渗透又不让五氯化磷固体物料通过的结构和特性。In this embodiment, the lower cylinder 11b is formed into a cone, and the diameter of the cone bottom circumference is basically the same as the diameter of the cylindrical upper cylinder 11a, and they are connected together. The liquid hydrogen fluoride permeation jacket 14 is formed along the conical surface of the lower cylinder 11b, and the isolation filter plate 14a is formed in a cone shape. The isolation filter plate 14a adopts a multi-layer sintered filter mesh. The liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket 14 through the liquid hydrogen fluoride supply device 20 penetrates into the generator cylinder 11 through the isolation filter plate 14a, and interacts with the liquid hydrogen fluoride in the generator cylinder 11. The solid material of phosphorus pentachloride in contact with the isolation filter plate 14a reacts. The isolation filter plate 14a has a structure and characteristics that allow liquid hydrogen fluoride to permeate but prevent the solid material of phosphorus pentachloride from passing through.
另外，所述上筒体11a和所述下筒体11b的外壁上，分别设置有冷却夹套15a、15b，所述冷却夹套15a、15b通过冷却媒介输送管路15c、15d与冷却循环装置50相连。冷却循环装置50，包括冷却媒介供给装置50b和冷却媒介回收装置50a。冷却媒介从所述冷却媒介供给装置50b经过所述冷却媒介输送管路15d被分别输送进所述冷却夹套15a、15b，然后又分别从所述冷却夹套15a、15b经过述冷却媒介输送管路15c被输送回冷却媒介回收装置50a。所述冷却媒介输送管路15c上，设有调节阀15e。In addition, cooling jackets 15a and 15b are respectively provided on the outer walls of the upper cylinder 11a and the lower cylinder 11b. The cooling jackets 15a and 15b communicate with the cooling circulation device through the cooling medium delivery pipelines 15c and 15d. 50 connected. The cooling cycle device 50 includes a cooling medium supply device 50b and a cooling medium recovery device 50a. The cooling medium is transported from the cooling medium supply device 50b through the cooling medium delivery pipe 15d into the cooling jackets 15a and 15b respectively, and then passes through the cooling medium delivery pipes from the cooling jackets 15a and 15b respectively. The path 15c is conveyed back to the cooling medium recovery device 50a. The cooling medium delivery pipeline 15c is provided with a regulating valve 15e.
另外，所述下筒体11b的底部，设置有用于将未反应的五氯化磷固体物料排出的硬密封球阀16。In addition, a hard-sealed ball valve 16 for discharging unreacted phosphorus pentachloride solid material is provided at the bottom of the lower cylinder 11b.
所述搅拌装置12，包括在所述发生器筒体11内搅拌旋转的呈螺旋状的桨叶12a和驱动该桨叶12a的驱动电机12b。所述桨叶12a，为中空状，其与冷却循环装置(未图示)相连。在搅拌过程中，可通过在中空的所述桨叶12a中通入温度调节媒介，来调节被搅拌的五氯化磷固体物料与液态氟化氢反应的温度。The stirring device 12 includes a spiral blade 12a that stirs and rotates in the generator cylinder 11 and a drive motor 12b that drives the blade 12a. The blades 12a are hollow and connected to a cooling circulation device (not shown). During the stirring process, the temperature of the reaction between the stirred phosphorus pentachloride solid material and the liquid hydrogen fluoride can be adjusted by passing a temperature adjustment medium into the hollow blade 12a.
另外，所述发生器筒体11内还设有温度变送器60，通过该温度变送器60来监测所述发生器筒体11内的温度变化，从而与所述调节阀15e协同调节控制所述发生器筒体11内的温度。In addition, a temperature transmitter 60 is also provided in the generator barrel 11. The temperature transmitter 60 is used to monitor the temperature changes in the generator barrel 11, thereby adjusting and controlling it in coordination with the regulating valve 15e. The temperature inside the generator barrel 11.
以下，参照图1，对本发明的五氟化磷气体发生器和利用该五氟化磷气体发生器发生五氟化磷气体的方法进行说明。Hereinafter, the phosphorus pentafluoride gas generator of the present invention and the method for generating phosphorus pentafluoride gas using the phosphorus pentafluoride gas generator will be described with reference to FIG. 1 .
如图1所示，首先开启所述驱动电机12b驱动桨叶12a旋转，然后通过将五氯化磷固体物料通过所述硬密封球阀13a和所述密闭漏斗13b加入到所述发生器筒体11内。具 体地说，是打开所述硬密封球阀13a及密闭漏斗13b的上盖板，将五氯化磷固体物料从所述密闭漏斗13b中加入到所述发生器筒体11内，加料完成后关闭所述硬密封球阀13a及所述密闭漏斗13b的上盖板，至此，将五氯化磷固体物料加入到所述发生器筒体11内的固体物料加料工序便结束。As shown in Figure 1, first the drive motor 12b is turned on to drive the paddle 12a to rotate, and then the solid material of phosphorus pentachloride is added to the generator barrel 11 through the hard-sealed ball valve 13a and the closed funnel 13b. Inside. Tool Specifically, the upper cover of the hard-sealed ball valve 13a and the sealed funnel 13b is opened, the solid material of phosphorus pentachloride is added from the sealed funnel 13b into the generator barrel 11, and closed after the addition is completed. The hard-sealed ball valve 13a and the upper cover plate of the airtight funnel 13b. At this point, the solid material feeding process of adding phosphorus pentachloride solid material into the generator barrel 11 is completed.
接下来，液态氟化氢从液态氟化氢供给装置20通过所述流量计11e及调节阀11f经过液态氟化氢供给管路11d被输送到所述喷淋器11c，再通过所述喷淋器11c喷淋到所述发生器筒体11内。通过未图示的压力监测装置，对所述发生器筒体11内的压力进行监测，当所述发生器筒体11内的压力达到规定压力后，再通过所述液态氟化氢渗透夹套14将液态氟化氢渗透加入到所述发生器筒体11内。即进行通过所述液体物料加入器11c将液态氟化氢加入到所述发生器筒体11内的液体物料加料工序和通过所述液态氟化氢渗透夹套14将液态氟化氢渗透加入到所述发生器筒体11内的液体物料渗透工序。Next, liquid hydrogen fluoride is transported from the liquid hydrogen fluoride supply device 20 to the sprinkler 11c through the flow meter 11e and the regulating valve 11f through the liquid hydrogen fluoride supply pipeline 11d, and then is sprayed to all locations through the sprinkler 11c. inside the generator barrel 11. The pressure in the generator barrel 11 is monitored through a pressure monitoring device (not shown). When the pressure in the generator barrel 11 reaches a prescribed pressure, the liquid hydrogen fluoride permeability jacket 14 is used to monitor the pressure inside the generator barrel 11 . Liquid hydrogen fluoride is permeated into the generator barrel 11 . That is, the liquid material feeding process of adding liquid hydrogen fluoride into the generator barrel 11 through the liquid material feeder 11c and penetrating liquid hydrogen fluoride into the generator barrel through the liquid hydrogen fluoride penetration jacket 14 are performed. Liquid material penetration process within 11.
在进行以上工序过程中，通过冷却循环装置50向所述冷却夹套15a、15b供给冷却媒介并使冷却媒介循环，从而控制所述发生器筒体11的温度，此时，通过所述温度变送器60来监测所述发生器筒体11内的温度变化，并与所述调节阀15e协同调节控制所述发生器筒体11内的温度。另一方面，在搅拌过程中，通过在中空的所述桨叶12a中通入温度调节媒介，来调节被搅拌的五氯化磷固体物料与液态氟化氢反应的温度。During the above process, the cooling circulation device 50 supplies cooling medium to the cooling jackets 15a, 15b and circulates the cooling medium, thereby controlling the temperature of the generator barrel 11. At this time, through the temperature change, The transmitter 60 is used to monitor the temperature change in the generator barrel 11, and coordinates with the regulating valve 15e to adjust and control the temperature in the generator barrel 11. On the other hand, during the stirring process, the temperature of the reaction between the stirred phosphorus pentachloride solid material and the liquid hydrogen fluoride is adjusted by passing the temperature adjustment medium into the hollow blade 12a.
在所述发生器筒体11内反应发生的五氟化磷气体，经所述粉体过滤器40过滤后，通过所述气体输送管路11g被输送至下一工序装置30。The phosphorus pentafluoride gas reacted in the generator cylinder 11 is filtered by the powder filter 40 and then transported to the next process device 30 through the gas transport pipeline 11g.
而未反应的五氯化磷固体物料则通过所述硬密封球阀16排出所述发生器筒体11之外回收使用。The unreacted phosphorus pentachloride solid material is discharged from the generator barrel 11 through the hard-sealed ball valve 16 for recycling.
采用本发明的五氟化磷气体发生器和五氟化磷气体发生方法，具有以下优点。The use of the phosphorus pentafluoride gas generator and the phosphorus pentafluoride gas generation method of the present invention has the following advantages.
(1)本发明通过设置具有用于承载和接触所述发生器筒体11内的五氯化磷固体物料的隔离滤板14a的液态氟化氢渗透夹套14，并使通过所述液态氟化氢供给装置20供给到所述液态氟化氢渗透夹套14的液态氟化氢，通过隔离滤板14a渗透到所述发生器筒体11内，与所述发生器筒体11内的五氯化磷固体物料进行反应。因此，可以让参与反应的液态氟化氢能充分与反应对象的五氯化磷固体物料接触反应，从而提高五氟化磷气体的发生效率。(1) The present invention provides a liquid hydrogen fluoride permeation jacket 14 with an isolation filter plate 14a for carrying and contacting the phosphorus pentachloride solid material in the generator barrel 11, and allows the liquid hydrogen fluoride to pass through the liquid hydrogen fluoride supply device 20 The liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket 14 penetrates into the generator barrel 11 through the isolation filter plate 14a, and reacts with the phosphorus pentachloride solid material in the generator barrel 11. Therefore, the liquid hydrogen fluoride participating in the reaction can fully contact and react with the solid material of phosphorus pentachloride as the reaction object, thereby improving the generation efficiency of phosphorus pentafluoride gas.
(2)液态氟化氢渗透夹套14具有锥状的隔离滤板14a，可以提高液态氟化氢与五氯化磷固体物料的接触面积。(2) The liquid hydrogen fluoride permeation jacket 14 has a cone-shaped isolation filter plate 14a, which can increase the contact area between the liquid hydrogen fluoride and the phosphorus pentachloride solid material.
(3)在所述发生器筒体11上设置冷却夹套15a、15b，搅拌装置12的桨叶12a也 形成为中空形状，可以通过可循环的冷却媒介来控制五氟化磷气体生成过程中的五氟化磷气体发生器10的温度和反应温度，从而提高五氟化磷气体的发生效率。(3) Cooling jackets 15a and 15b are provided on the generator cylinder 11, and the blades 12a of the stirring device 12 are also Formed into a hollow shape, the temperature and reaction temperature of the phosphorus pentafluoride gas generator 10 during the generation of phosphorus pentafluoride gas can be controlled through a circulating cooling medium, thereby improving the generation efficiency of phosphorus pentafluoride gas.
(4)通过所述液体物料加料工序来调整所述发生器筒体11内的压力，当所述发生器筒体11内的压力达到规定压力后，再通过所述液态氟化氢渗透夹套14将液态氟化氢渗透加入到所述发生器筒体11内。这样可以防止由于所述液态氟化氢渗透夹套14内的压力与所述发生器筒体11内的压力之差过大而使所述隔离滤板14a的寿命缩短或使其被损坏。(4) Adjust the pressure in the generator cylinder 11 through the liquid material feeding process. When the pressure in the generator cylinder 11 reaches the specified pressure, the liquid hydrogen fluoride penetration jacket 14 will Liquid hydrogen fluoride is permeated into the generator barrel 11 . This can prevent the life of the isolation filter plate 14a from being shortened or being damaged due to an excessive difference between the pressure in the liquid hydrogen fluoride permeation jacket 14 and the pressure in the generator barrel 11 .
作为本发明的实施例的变更形式，例如，可以在液态氟化氢供给管路14b上也设置流量计和调节阀，以此来控制供给所述液态氟化氢渗透夹套14的液态氟化氢。As a modification of the embodiment of the present invention, for example, a flow meter and a regulating valve may be provided on the liquid hydrogen fluoride supply line 14b to control the liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket 14.
另外，作为液体物料加入器的喷淋器11c，也可以设置为1个或3个以上。In addition, the number of sprinklers 11c serving as liquid material feeders may be one or three or more.
另外，所述液态氟化氢渗透夹套14及其隔离滤板14a，也可以做成锥状以外的形状。In addition, the liquid hydrogen fluoride permeation jacket 14 and its isolation filter plate 14a may also be made into shapes other than conical shapes.
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合。 In addition, it should be noted that the specific technical features described in the above-mentioned specific embodiments can be combined in any suitable manner as long as there is no contradiction.

Claims (9)

  1. 一种五氟化磷气体发生器，包括：由上筒体和下筒体构成的发生器筒体、设置在该发生器筒体内的搅拌装置、液态氟化氢供给装置以及与该发生器筒体连通的将五氟化磷气体输送至下一工序装置的气体输送管路，其特征在于，A phosphorus pentafluoride gas generator, including: a generator cylinder composed of an upper cylinder and a lower cylinder, a stirring device arranged in the generator cylinder, a liquid hydrogen fluoride supply device, and a device connected to the generator cylinder A gas transportation pipeline for transporting phosphorus pentafluoride gas to the next process device, characterized in that:
    所述上筒体上设置有用于将液态氟化氢加入至发生器筒体内的液体物料加入器，各所述液体物料加入器通过液态氟化氢供给管路与所述液态氟化氢供给装置相连；The upper cylinder is provided with a liquid material adder for adding liquid hydrogen fluoride into the generator barrel, and each of the liquid material adders is connected to the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline;
    所述下筒体，具有沿下筒体内壁设置的液态氟化氢渗透夹套，该液态氟化氢渗透夹套，具有用于承载和接触所述发生器筒体内的五氯化磷固体物料的隔离滤板，该液态氟化氢渗透夹套通过液态氟化氢供给管路与所述液态氟化氢供给装置相连；The lower cylinder has a liquid hydrogen fluoride permeation jacket arranged along the inner wall of the lower cylinder. The liquid hydrogen fluoride permeation jacket has an isolation filter plate for carrying and contacting the phosphorus pentachloride solid material in the generator cylinder. , the liquid hydrogen fluoride permeability jacket is connected to the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline;
    通过所述液态氟化氢供给装置供给到所述液态氟化氢渗透夹套的液态氟化氢，通过隔离滤板渗透到所述发生器筒体内，与所述发生器筒体内的五氯化磷固体物料进行反应。The liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket through the liquid hydrogen fluoride supply device penetrates into the generator barrel through the isolation filter plate, and reacts with the phosphorus pentachloride solid material in the generator barrel.
  2. 如权利要求1所述的五氟化磷气体发生器，其特征在于，The phosphorus pentafluoride gas generator according to claim 1, characterized in that:
    所述液态氟化氢渗透夹套，至少其所述隔离滤板形成为锥体状。In the liquid hydrogen fluoride permeability jacket, at least the isolation filter plate is formed into a cone shape.
  3. 如权利要求1或2所述的五氟化磷气体发生器，其特征在于，The phosphorus pentafluoride gas generator according to claim 1 or 2, characterized in that,
    所述隔离滤板，采用多层烧结滤网。The isolation filter plate adopts multi-layer sintered filter mesh.
  4. 如权利要求1或2所述的五氟化磷气体发生器，其特征在于，The phosphorus pentafluoride gas generator according to claim 1 or 2, characterized in that,
    所述上筒体和所述下筒体的至少一者的外壁上设置有冷却夹套，所述冷却夹套通过冷却媒介输送管路与冷却循环装置相连。A cooling jacket is provided on the outer wall of at least one of the upper cylinder and the lower cylinder, and the cooling jacket is connected to the cooling circulation device through a cooling medium delivery pipeline.
  5. 如权利要求1或2所述的五氟化磷气体发生器，其特征在于，The phosphorus pentafluoride gas generator according to claim 1 or 2, characterized in that,
    所述搅拌装置，具有中空构造的螺带，且该螺带与冷却循环装置相连。The stirring device has a hollow spiral belt, and the spiral belt is connected to the cooling circulation device.
  6. 如权利要求1或2所述的五氟化磷气体发生器，其特征在于，The phosphorus pentafluoride gas generator according to claim 1 or 2, characterized in that,
    所述气体输送管路上设置有粉体过滤器。A powder filter is provided on the gas delivery pipeline.
  7. 如权利要求4所述的五氟化磷气体发生器，其特征在于，The phosphorus pentafluoride gas generator according to claim 4, characterized in that:
    所述发生器筒体内设有温度变送器，所述冷却媒介输送管路上设有调节阀。A temperature transmitter is provided in the generator barrel, and a regulating valve is provided on the cooling medium delivery pipeline.
  8. 一种利用如权利要求1至7中任一项所述的五氟化磷气体发生器来产生五氟化磷气体的五氟化磷气体发生方法，其中，至少包括以下工序：A phosphorus pentafluoride gas generation method using the phosphorus pentafluoride gas generator according to any one of claims 1 to 7 to generate phosphorus pentafluoride gas, which at least includes the following steps:
    将五氯化磷固体物料加入到所述发生器筒体内的固体物料加料工序；和The solid material feeding process of adding phosphorus pentachloride solid material into the generator barrel; and
    通过所述液体物料加入器将液态氟化氢加入到所述发生器筒体内的液体物料加料工序；和The liquid material feeding process of adding liquid hydrogen fluoride into the generator barrel through the liquid material adding device; and
    通过所述液态氟化氢渗透夹套将液态氟化氢渗透加入到所述发生器筒体内的液体 物料渗透工序。Liquid hydrogen fluoride is added to the liquid in the generator barrel through the liquid hydrogen fluoride penetration jacket. Material penetration process.
  9. 如权利要求8所述的五氟化磷气体发生方法，其特征在于，The phosphorus pentafluoride gas generation method according to claim 8, characterized in that:
    通过所述液体物料加料工序来调整所述发生器筒体内的压力，当所述发生器筒体内的压力达到规定压力后，再通过所述液态氟化氢渗透夹套将液态氟化氢渗透加入到所述发生器筒体内。 The pressure in the generator barrel is adjusted through the liquid material feeding process. When the pressure in the generator barrel reaches the specified pressure, liquid hydrogen fluoride is added to the generator through the liquid hydrogen fluoride penetration jacket. inside the barrel.
PCT/CN2023/079338 2022-08-01 2023-03-02 Phosphorus pentafluoride gas generator and phosphorus pentafluoride gas generation method WO2024027149A1 (en)

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