CN217016619U - Preparation facilities of tungsten hexafluoride - Google Patents
Preparation facilities of tungsten hexafluoride Download PDFInfo
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- CN217016619U CN217016619U CN202123428237.4U CN202123428237U CN217016619U CN 217016619 U CN217016619 U CN 217016619U CN 202123428237 U CN202123428237 U CN 202123428237U CN 217016619 U CN217016619 U CN 217016619U
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Abstract
The utility model provides a preparation device of tungsten hexafluoride, and relates to the technical field of electronic special gas production. The preparation device of tungsten hexafluoride provided by the utility model comprises a vertical tungsten fluoride reactor (1), wherein the vertical tungsten fluoride reactor (1) is provided with a reaction cavity tungsten powder feed inlet (1-1), a tungsten hexafluoride gas outlet (1-2) and a fluorinating agent inlet (1-3); the temperature control jacket (2) is arranged on the outer side wall of the vertical fluorine-tungsten reactor (1); and the tungsten powder automatic feeding device (3) is communicated with the tungsten powder feeding hole (1-1) of the reaction cavity. When the preparation device provided by the utility model is used for preparing tungsten hexafluoride, tungsten powder is continuously conveyed into the vertical tungsten fluoride reactor (1) through the automatic tungsten powder feeding device (3) and continuously reacts with fluorine gas conveyed into the vertical tungsten fluoride reactor (1), and impurities such as moisture, air and the like are not easily introduced, so that the continuous production of high-purity tungsten hexafluoride gas is realized.
Description
Technical Field
The utility model relates to the technical field of electronic special gas production, in particular to a preparation device of tungsten hexafluoride.
Background
Tungsten hexafluoride (WF)6) The solid is a white crystal which is easy to deliquesce and smoke in humid air. High purity WF in the preparation of semiconductor materials6Unit operations for Chemical Vapor Deposition (CVD) and Atomic Layer Deposition (ALD) generally to produce tungsten contact plugs and tungsten silicide electrodes, particularly WSi made therewith2Can be used as a wiring material in a large scale integrated circuit (LSI).
Currently, there are two main methods for industrially producing tungsten hexafluoride: (1) preparation of WF by reaction of fluorine gas as fluorinating agent with tungsten6(reaction formula is W + 3F)2→WF6) Firstly, preparing crude fluorine gas through electrolysis, removing a large amount of HF, nitrogen, carbon dioxide, metal particles and other impurities carried in the fluorine gas by the crude fluorine gas through adsorption, deep cooling or rectification processes, and reacting the purified fluorine gas with tungsten metal to synthesize the tungsten hexafluoride. (2) With NF3Used as fluorinating agent to react with tungsten to prepare tungsten hexafluoride gas (the reaction formula is W +2 NF)3→WF6+N2) The method is to make the raw material gas NF3And high purity N2Introducing into a high-temperature cracker according to the same volume ratio, NF3Cracking in a cracker to form F2，F2Enters a reactor to react with metal W to generate WF6Synthesized WF6Liquefying and collecting the gas by adopting a low-temperature collector; refined NF of Mitsui chemical3Introducing into a reactor made of nickel or monel alloy, and directly reacting with metal tungsten at 200-400 ℃ to obtain WF6。
The common tungsten hexafluoride reactor is mainly a fixed bed and has two types of vertical and horizontal structures, tungsten metal is added into the tungsten hexafluoride reactor, the reactor is controlled at 200-450 ℃, and then fluorine gas or nitrogen trifluoride gas is introduced to react with tungsten to generate tungsten hexafluoride gas. However, when the fixed bed reactor is used for preparing tungsten hexafluoride, the tungsten metal feeding mode is intermittent, impurities such as moisture, air and the like are easily introduced due to frequent disassembly and inspection of the fixed bed reactor and addition of tungsten metal, and the obtained tungsten hexafluoride is not high in purity and cannot be continuously produced.
SUMMERY OF THE UTILITY MODEL
In view of this, an object of the present invention is to provide a tungsten hexafluoride production apparatus capable of realizing continuous production of high-purity tungsten hexafluoride.
In order to realize the purpose of the utility model, the utility model provides the following technical scheme:
the utility model provides a tungsten hexafluoride preparation device which comprises a vertical tungsten fluoride reactor 1, wherein the vertical tungsten fluoride reactor 1 is provided with a reaction cavity tungsten powder feed inlet 1-1, a tungsten hexafluoride gas outlet 1-2 and a fluorinating agent inlet 1-3;
the temperature control jacket 2 is arranged on the outer side wall of the vertical fluorine-tungsten reactor 1;
and the tungsten powder automatic feeding device 3 is communicated with the tungsten powder feeding hole 1-1 of the reaction cavity.
Preferably, the tungsten powder automatic feeding device 3 comprises a tungsten powder feeding bin 3-1, a feeding machine 3-2 communicated with an outlet of the tungsten powder feeding bin 3-1, a driving motor 3-3 electrically connected with the feeding machine 3-2, and a tungsten powder feeding pipe 3-5 communicated with the feeding machine 3-2, wherein the tungsten powder feeding pipe 3-5 extends into the vertical fluorine tungsten reactor 1 through a tungsten powder feeding port 1-1 of the reaction cavity;
the tungsten powder feeding bin 3-1 is respectively communicated with a pressure display instrument 3-4, a nitrogen blowing device 3-6 and a vacuumizing device 3-7.
Preferably, a fluorinating agent redistribution device 1-4 is further arranged in the vertical type tungsten fluoride reactor 1, the fluorinating agent redistribution device 1-4 comprises a fluorinating agent gas outlet pipeline, a gas outlet hole is formed in the fluorinating agent gas outlet pipeline, and a first dust baffle 1-4-1 is connected with the edge of the gas outlet hole.
Preferably, a second dust baffle 1-5 is further arranged in the vertical tungsten fluoride reactor 1, the second dust baffle 1-5 is arranged between the tungsten hexafluoride gas outlet 1-2 and the tungsten powder feeding pipe 3-5, and the horizontal height of the lowest end of the second dust baffle 1-5 is lower than the horizontal height of the lowest end of the tungsten powder feeding pipe 3-5.
Preferably, the vertical tungsten fluoro-material reactor 1 is further provided with a plurality of temperature monitoring ports 1-6, and the temperature monitoring ports 1-6 penetrate through the wall of the vertical tungsten fluoro-material reactor 1 and the temperature control jacket 2.
Preferably, the device also comprises a fixed bed reactor 5 connected with the vertical fluorine-tungsten reactor in series; the fixed bed reactor 5 is provided with a fixed bed reactor inlet 5-1 and a fixed bed reactor outlet 5-2;
and a heating unit 5-3 disposed on an outer sidewall of the fixed bed reactor 5.
Preferably, the device further comprises a tungsten hexafluoride storage device 4, and an inlet of the tungsten hexafluoride storage device 4 is communicated with the tungsten hexafluoride gas outlet 1-2 or the fixed bed reactor outlet 5-2.
The utility model provides a preparation device of tungsten hexafluoride, which comprises a vertical tungsten fluoride reactor 1, wherein the vertical tungsten fluoride reactor 1 is provided with a reaction cavity tungsten powder feed inlet 1-1, a tungsten hexafluoride gas outlet 1-2 and a fluorinating agent inlet 1-3; the temperature control jacket 2 is arranged on the outer side wall of the vertical fluorine-tungsten reactor 1; and a tungsten powder automatic feeding device 3 communicated with a tungsten powder feeding port 1-1 of a reaction cavity of the vertical tungsten-fluorine reactor. When the preparation device provided by the utility model is used for preparing tungsten hexafluoride, tungsten powder is continuously conveyed into the vertical tungsten fluoride reactor 1 through the automatic tungsten powder feeding device 3 and continuously reacts with a fluorinating agent conveyed into the vertical tungsten fluoride reactor 1, so that the continuous production of tungsten hexafluoride gas is realized, and the generated tungsten hexafluoride is continuously output through the tungsten hexafluoride gas outlet 1-2, so that the continuous mass production of the tungsten hexafluoride gas is realized; moreover, the preparation device provided by the utility model has the advantages of simple structure, high safety and low environmental pollution, does not need to frequently disassemble and inspect the reactor and supplement tungsten powder, is not easy to introduce impurities such as moisture, air and the like, and the prepared tungsten hexafluoride has high purity.
Further, the preparation device of tungsten hexafluoride provided by the utility model further comprises a fixed bed reactor 5 connected with the vertical tungsten fluoride reactor in series. The utility model adopts the fixed bed reactor 5 as supplement, and can reduce the loss of the fluorinating agent.
Drawings
FIG. 1 is a schematic structural diagram of a tungsten hexafluoride production apparatus;
FIG. 2 is a schematic structural view of an automatic feeding device for tungsten powder;
FIG. 3 is a schematic view of a fluorinating agent distributor structure, wherein a is a front view and b is a top view;
FIG. 4 is a schematic view of a fixed bed reactor configuration;
FIG. 5 is a schematic view of a tungsten hexafluoride production apparatus;
in the drawings 1-5, 1 is a vertical fluorine-tungsten reactor, 1-1 is a reaction chamber tungsten powder feed inlet, 1-2 is a tungsten hexafluoride gas outlet, 1-3 is a fluorinating agent inlet, 1-4 is a fluorinating agent redistributor, 1-4-1 is a first dust baffle, 1-5 is a second dust baffle, 1-6 is a first temperature monitoring port, 1-7 is a flange, 2 is a temperature control jacket, 2-1 is a temperature control medium inlet, 2-2 is a temperature control medium outlet, 3 is an automatic tungsten powder feeding device, 3-1 is a tungsten powder feeding bin, 3-2 is a feeding machine, 3-3 is a driving motor, 3-4 is a pressure display instrument, 3-5 is a tungsten powder feeding pipe, 3-6 is a nitrogen blowing device, 3-7 is a vacuumizing device, 4 is a tungsten hexafluoride storage device, 5 is a fixed bed reactor, 5-1 is an inlet of the fixed bed reactor, 5-2 is an outlet of the fixed bed reactor, 5-3 is a heating component, and 5-4 is a second temperature monitoring device.
Detailed Description
The utility model provides a tungsten hexafluoride preparation device which comprises a vertical tungsten fluoride reactor 1, wherein the vertical tungsten fluoride reactor 1 is provided with a reaction cavity tungsten powder feed inlet 1-1, a tungsten hexafluoride gas outlet 1-2 and a fluorinating agent inlet 1-3;
the temperature control jacket 2 is arranged on the outer side wall of the vertical fluorine-tungsten reactor 1;
and a tungsten powder automatic feeding device 3 communicated with the tungsten powder feeding port 1-1 of the reaction cavity.
The structural schematic diagrams of the preparation device of tungsten hexafluoride provided by the utility model are shown in fig. 1-5, wherein fig. 1 is the structural schematic diagram of the preparation device of tungsten hexafluoride; FIG. 2 is a schematic structural view of an automatic feeding device for tungsten powder; FIG. 3 is a schematic view of a fluorinating agent distributor structure, wherein a is a front view and b is a top view; FIG. 4 is a schematic view of a fixed bed reactor configuration; FIG. 5 is a schematic structural diagram of a device for preparing tungsten hexafluoride. The following is a detailed description with reference to fig. 1 to 5.
The preparation device of tungsten hexafluoride provided by the utility model comprises a vertical tungsten fluoride reactor 1, the material of the vertical tungsten fluoride reactor 1 is not particularly limited, and the vertical tungsten fluoride reactor is not corroded by a fluorinating agent, such as nickel, Monel alloy, Hastelloy, stainless steel, copper or low-carbon steel. In the present invention, the material of the vertical fluorotungsten reactor 1 is preferably nickel or monel, and more preferably monel.
In the utility model, the vertical tungsten fluoride reactor 1 is provided with a reaction cavity tungsten powder feed inlet 1-1, a tungsten hexafluoride gas outlet 1-2 and a fluorinating agent inlet 1-3, the tungsten hexafluoride gas outlet 1-2 is preferably arranged at the top of the side wall, and the fluorinating agent inlet 1-3 is preferably arranged at the bottom of the side wall. In the utility model, a fluorinating agent redistributor 1-4 is preferably further arranged in the vertical fluorotungsten reactor 1, and the structural schematic diagram of the fluorinating agent redistributor 1-4 is shown in fig. 3, wherein a is a front view, and b is a top view; the fluorinating agent redistributor 1-4 comprises a fluorinating agent outlet pipeline, wherein an outlet hole is formed in the fluorinating agent outlet pipeline, and a first dust baffle plate 1-4-1 connected with the edge of the outlet hole is arranged on the fluorinating agent outlet pipeline, the fluorinating agent redistributor 1-4 is preferably of a plate structure, the material of the fluorinating agent redistributor 1-4 is not specially limited, and the fluorinating agent redistributor is not corroded by the fluorinating agent, specifically nickel, Monel alloy, Hastelloy or stainless steel; the shape of the first dust baffle 1-4-1 is not specially limited, so that a fluorinating agent can smoothly enter the vertical tungsten-fluoride reactor 1 through the fluorinating agent redistributor 1-4, and tungsten powder is prevented from falling into fluorinating agent air outlet holes of the fluorinating agent redistributor 1-4 to block the fluorinating agent air outlet holes; in the embodiment of the utility model, the fluorinating agent outlet pipeline, the outlet holes and the first dust baffle 1-4-1 of the fluorinating agent redistributor 1-4 are preferably mushroom head-shaped outlet pipes integrally, the mushroom head top of the mushroom head-shaped outlet pipe receives the tungsten powder falling, and the fluorinating agent is conveyed out from the lower part of the mushroom head top. In the utility model, the fluorinating agent redistributor 1-4 is used for uniformly dispersing the fluorinating agent in the vertical type tungsten fluoride reactor 1.
In the utility model, a second dust baffle 1-5 is preferably further arranged in the vertical tungsten fluoride reactor 1, the second dust baffle 1-5 is preferably arranged between the tungsten hexafluoride gas outlet 1-2 and the tungsten powder feeding pipe 3-5, and the horizontal height of the lowest end of the second dust baffle 1-5 is preferably lower than the horizontal height of the lowest end of the tungsten powder feeding pipe 3-5, so as to prevent tungsten powder from being output along with tungsten hexafluoride gas.
In the utility model, the preparation device of tungsten hexafluoride further comprises a temperature control jacket 2 arranged on the outer side wall of the vertical tungsten fluoride reactor 1; the material of the temperature control jacket 2 preferably comprises low-carbon steel or stainless steel, and more preferably stainless steel; the temperature control jacket 2 is preferably internally provided with a temperature control medium, and the temperature control jacket 2 is preferably provided with a temperature control medium inlet 2-1 and a temperature control medium outlet 2-2; the type of the temperature control medium is not particularly limited, and the temperature can be controlled to be 0-400 ℃, specifically air, water or heat conduction oil, and more preferably alkyl biphenyl type heat conduction oil or biphenyl-biphenyl ether heat conduction oil. In the utility model, the temperature control medium plays a role in heating the vertical fluorine-tungsten reactor in the initial stage of the reaction, and plays a role in guiding out reaction heat for cooling in the reaction process.
In the utility model, the preparation device of tungsten hexafluoride further comprises an automatic tungsten powder feeding device 3 communicated with the tungsten powder feeding port 1-1 of the reaction cavity, and the structural schematic diagram of the automatic tungsten powder feeding device 3 is shown in fig. 2. In the utility model, the tungsten powder automatic feeding device 3 preferably comprises a tungsten powder feeding bin 3-1, a feeding machine 3-2 communicated with an outlet of the tungsten powder feeding bin 3-1, a driving motor 3-3 electrically connected with the feeding machine 3-2, and a tungsten powder feeding pipe 3-5 communicated with the feeding machine 3-2, wherein the tungsten powder feeding pipe 3-5 extends into the vertical fluorine-tungsten reactor 1 through a tungsten powder feeding hole 1-1 of a reaction cavity; the feeding machine 3-2 is preferably a spiral feeding machine; the tungsten powder feeding bin 3-1 is respectively communicated with a pressure display instrument 3-4, a nitrogen blowing device 3-6 and a vacuumizing device 3-7, and the nitrogen blowing device 3-6 is used for replacing air in the tungsten powder feeding bin 3-1 and the feeding machine 3-2 with nitrogen; the evacuation device 3-7 is preferably a vacuum pump. The tungsten powder feeding bin 3-1 is not specially limited in material, does not react with tungsten powder, and is not corroded by a fluorinating agent and tungsten hexafluoride, such as stainless steel or low-carbon steel. In the utility model, the tungsten powder feeding bin 3-1 is provided with a tungsten powder feeding bin cover for sealing the tungsten powder feeding bin 3-1. In the utility model, the driving motor 3-3 is preferably a speed regulating motor, and the driving motor 3-3 is used for controlling the feeding speed of the feeding machine 3-2.
In the utility model, the vertical fluorine tungsten reactor 1 is preferably further provided with a first temperature monitoring port 1-6, and the first temperature monitoring port 1-6 penetrates through the cavity wall of the vertical fluorine tungsten reactor 1 and the temperature control jacket 2; the number of the first temperature monitoring ports 1-6 is preferably 1-6, more preferably 1-3, and the temperatures of different parts in the vertical fluorine-tungsten reactor 1 are monitored through the first temperature monitoring ports 1-6.
In the present invention, the vertical type fluorine-tungsten reactor is preferably further provided with flanges 1 to 7, and the flanges 1 to 7 are used for removing residual tungsten powder which is not reacted or sediments formed in the reaction process.
In the utility model, the preparation device of tungsten hexafluoride preferably further comprises a fixed bed reactor 5 connected in series with the vertical tungsten fluoride reactor, the structural schematic diagram of the fixed bed reactor 5 is shown in fig. 4, the fixed bed reactor 5 is provided with a fixed bed reactor inlet 5-1, a fixed bed reactor outlet 5-2 and a heating component 5-3 arranged on the outer side wall of the fixed bed reactor 5; the heating assembly 5-3 preferably includes electrical heating or thermal oil heating. In the present invention, the fixed bed reactor 5 is preferably a vertical fixed bed reactor or a horizontal fixed bed reactor; the fixed bed reactor 5 is filled with tungsten raw materials, the tungsten raw materials preferably comprise tungsten powder or tungsten blocks, when a vertical fixed bed reactor is adopted, the tungsten raw materials preferably comprise tungsten blocks, and when a horizontal fixed bed reactor is adopted, the tungsten raw materials preferably comprise tungsten powder. In the present invention, the fixed bed reactor 5 is preferably further provided with a second temperature monitoring device 5-4, and the second temperature monitoring device 5-4 penetrates through the wall of the fixed bed reactor 5; the number of the second temperature monitoring devices 5-4 is preferably 1-3, more preferably 1-2, and the temperatures of different parts in the fixed bed reactor 5 are monitored through the second temperature monitoring devices 5-4. In the utility model, the fixed bed reactor 5 is used for generating tungsten hexafluoride gas by reacting a small amount of fluorine gas generated after the unreacted fluorinating agent and/or nitrogen trifluoride in the tungsten hexafluoride crude product generated by the vertical tungsten fluoride reactor 1 are cracked at high temperature with tungsten metal again, thereby improving the conversion rate of the fluorinating agent, reducing the loss amount of the fluorinating agent, and improving the yield and purity of the tungsten hexafluoride.
In the present invention, the apparatus for preparing tungsten hexafluoride preferably further includes a tungsten hexafluoride storage device 4, an inlet of the tungsten hexafluoride storage device 4 is communicated with the tungsten hexafluoride gas outlet 1-2, or the tungsten hexafluoride storage device 4 is communicated with the fixed bed reactor outlet 5-2. In the present invention, the tungsten hexafluoride storage device 4 is preferably a tungsten hexafluoride low-temperature storage device, and the temperature of the tungsten hexafluoride low-temperature storage device is preferably-80 to-15 ℃, and more preferably-70 to-50 ℃; the tungsten hexafluoride storage device 4 preferably comprises nickel, nickel steel, monel, copper, stainless steel, or mild steel, and more preferably monel or nickel.
The following describes a specific method for preparing tungsten hexafluoride by using the preparation apparatus for tungsten hexafluoride provided by the present invention with reference to fig. 1 to 3, including the following steps:
filling tungsten powder into a tungsten powder feed inlet 1-1 of a reaction cavity, sealing the tungsten powder feed bin cover, vacuumizing the tungsten powder feed bin 3-1 and a feeder 3-2 by using a vacuumizing device 3-7, performing nitrogen gas replacement on the tungsten powder feed bin 3-1 and the feeder 3-2 by using a nitrogen blowing device 3-6, repeating the vacuumizing-nitrogen gas replacement operation until air is completely removed, and filling nitrogen gas by using the nitrogen blowing device 3-6; controlling the temperature in the vertical tungsten fluoride reactor 1 through the temperature control jacket 2, starting the tungsten powder automatic feeding device 3, continuously conveying tungsten powder into the vertical tungsten fluoride reactor 1 through the feeder 3-2 and the reaction cavity tungsten powder feeding port 1-1, and reacting with a fluorinating agent which is continuously input from a fluorinating agent inlet 1-3 and uniformly distributed through a fluorinating agent re-distributor 1-4 to obtain tungsten hexafluoride; the tungsten hexafluoride gas is output to a tungsten hexafluoride storage device 4 from a tungsten hexafluoride gas outlet 1-2, wherein the feeding speed of the feeding machine 3-2 is controlled by a driving motor 3-3; the tungsten powder is prevented from being output along with tungsten hexafluoride gas by the second dust baffle 5-1, and the tungsten powder is prevented from falling into the fluorinating agent re-distributor 1-4 by the first dust baffle 1-4-1.
The following describes a specific method for preparing tungsten hexafluoride by using the preparation apparatus for tungsten hexafluoride provided by the present invention with reference to fig. 1 to 5, including the following steps:
filling tungsten powder into a tungsten powder feed inlet 1-1 of a reaction cavity, sealing the tungsten powder feed bin cover, vacuumizing the tungsten powder feed bin 3-1 and a feeder 3-2 by using a vacuumizing device 3-7, performing nitrogen gas replacement on the tungsten powder feed bin 3-1 and the feeder 3-2 by using a nitrogen blowing device 3-6, repeating the vacuumizing-nitrogen gas replacement operation until air is completely removed, and filling nitrogen gas by using the nitrogen blowing device 3-6; controlling the temperature in a vertical tungsten fluoride reactor 1 through a temperature control jacket 2, starting a tungsten powder automatic feeding device 3, continuously conveying tungsten powder into the vertical tungsten fluoride reactor 1 through a feeder 3-2, a tungsten powder feeding pipe 3-5 and a reaction cavity tungsten powder feeding hole 1-1, continuously inputting a fluorinating agent which is uniformly distributed through a fluorinating agent redistributor 1-4 through a fluorinating agent inlet 1-3 for reaction, outputting an obtained product through a tungsten hexafluoride gas outlet 1-2, entering a fixed bed reactor 5 through a fixed bed reactor inlet 5-1, continuously reacting residual fluorinating agent in the product with a tungsten raw material to obtain tungsten hexafluoride, and conveying the tungsten hexafluoride into a tungsten hexafluoride storage device 4 through a fixed bed reactor outlet 5-2; the temperature of the fixed bed reactor 5 is controlled by a heating assembly 5-3.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the utility model, and not restrictive of the full scope of the utility model. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Tungsten hexafluoride was prepared using the apparatus shown in figure 1.
Filling tungsten powder (20kg) in a tungsten powder feeding bin 3-1, then sealing by a tungsten powder feeding bin cover, vacuumizing the tungsten powder feeding bin 3-1 and a feeder 3-2 by a vacuumizing device 3-7, replacing the tungsten powder feeding bin 3-1 and the feeder 3-2 by nitrogen gas by a nitrogen blowing device 3-6, repeating the vacuumizing-nitrogen gas replacement operation until air is completely removed, filling nitrogen gas by the nitrogen blowing device 3-6 until the pressure is 0.03MPa, controlling the internal pressure of a vertical fluorine-tungsten reactor (with the inner diameter of 150mm and the height of 1200m) to be 0.009MPa, controlling the temperature in the vertical fluorine-tungsten reactor 1 to be 280 ℃ by a temperature control jacket 2, starting a tungsten powder automatic feeding device 3, continuously conveying the tungsten powder into the vertical fluorine-tungsten reactor 1 at the supply of 320g/min through the feeder 3-2, a tungsten powder feeding pipe 3-5 and a reaction cavity tungsten powder feeding port 1-1, continuously reacting with fluorine gas which is continuously input from a fluorinating agent inlet 1-3 at the flow rate of 120L/min and uniformly distributed by a fluorinating agent redistributor 1-4 for 20min to obtain a tungsten hexafluoride crude product; the tungsten hexafluoride gas is output from a tungsten hexafluoride gas outlet 1-2 to a tungsten hexafluoride low-temperature storage device 4 with the temperature of-70 ℃, wherein the feeding speed of the feeding machine 3-2 is controlled by a driving motor 3-3, so that the flow ratio of tungsten powder of the fluoridizing agent is 2.67L: 1g of a compound; the tungsten powder is prevented from being output along with tungsten hexafluoride gas by the second dust baffle 5-1, and the tungsten powder is prevented from falling into the fluorinating agent re-distributor 1-4 by the first dust baffle 1-4-1.
The TCD chromatography is matched with a preposed potassium chloride fluorine gas conversion column to detect the components of the crude tungsten hexafluoride product after the reactor, the potassium chloride fluorine gas conversion column can convert fluorine gas into chlorine gas, and then the mixed gas enters the chromatography. In the crude tungsten hexafluoride product, the volume fraction of tungsten hexafluoride was 92.7%, the volume fraction of chlorine gas (i.e., fluorine gas) was 7% (by volume), and the volume fraction of nitrogen gas and other impurities was 1.3%. The weight of the tungsten hexafluoride low-temperature storage device 4 is increased by 10.2kg, the mass of the tungsten powder remained in the tungsten powder feeding bin 3-1 is 13.32kg, and the consumption of the tungsten powder is 6.68 kg. The yield of tungsten hexafluoride was 92.55%, calculated as consumption of tungsten powder.
Example 2
Tungsten hexafluoride was prepared using the apparatus shown in fig. 5.
Filling tungsten powder (20kg) in a tungsten powder feeding bin 3-1, sealing by a tungsten powder feeding bin cover, vacuumizing the tungsten powder feeding bin 3-1 and a feeder 3-2 by a vacuumizing device 3-7, performing nitrogen gas replacement on the tungsten powder feeding bin 3-1 and the feeder 3-2 by a nitrogen blowing device 3-6, repeating the vacuumizing-nitrogen gas replacement operation until air is completely removed, filling nitrogen gas by the nitrogen blowing device 3-6 until the pressure is 0.02MPa, controlling the internal pressure of a vertical tungsten fluoride reactor 1 (with the inner diameter of 150mm and the height of 1200m) to be 0.005MPa, controlling the temperature in the vertical tungsten fluoride reactor 1 to be 320 ℃ by a temperature control jacket 2, starting an automatic tungsten powder feeding device 3, continuously conveying the tungsten powder into the vertical tungsten fluoride reactor 1 at the supply of 400g/min through the feeder 3-2, a tungsten powder feeding pipe 3-5 and a tungsten powder feeding hole 1-1 of a reaction cavity, continuously reacting with nitrogen trifluoride which is continuously input from a fluorinating agent inlet 1-3 at the flow rate of 100L/min and uniformly distributed by a fluorinating agent redistributor 1-4 for 20min to obtain a crude tungsten hexafluoride product; the tungsten hexafluoride crude product enters a fixed bed reactor 5 (vertical structure, inner diameter of 108mm, height of 1000m, tungsten metal block filled inside) from a tungsten hexafluoride gas outlet 1-2 to react at 280 ℃, and the obtained tungsten hexafluoride is output to a tungsten hexafluoride low-temperature storage device 4 at-70 ℃ from the fixed bed reactor outlet 5-2.
Wherein, the feeding speed of the feeder 3-2 is controlled by the driving motor 3-3, so that the flow ratio of the tungsten powder fluoride is 4L: 1 g; the tungsten powder is prevented from being output along with tungsten hexafluoride gas by the second dust baffle 5-1, and the tungsten powder is prevented from falling into the fluorinating agent re-distributor 1-4 by the first dust baffle 1-4-1.
The TCD chromatogram is matched with a preposed potassium chloride fluorine gas conversion column to detect the components of the crude tungsten hexafluoride product output through a tungsten hexafluoride gas outlet 1-2 and the tungsten hexafluoride output through a fixed bed reactor outlet 5-2, the potassium chloride fluorine gas conversion column can convert fluorine gas into chlorine gas, and then the mixed gas enters the chromatogram for analysis. In the crude tungsten hexafluoride product at the outlet of the vertical reactor, the volume fraction of tungsten hexafluoride was 93.7%, the volume fraction of chlorine gas (i.e., fluorine gas) was 3%, the volume fraction of nitrogen trifluoride was 2.3%, and the volume fractions of nitrogen and other impurities were 1.0%. The weight of the tungsten hexafluoride low-temperature storage device 4 is increased by 11.85kg, the mass of the tungsten powder remained in the tungsten powder feeding bin 3-1 is 11.05kg, and the consumption of the tungsten powder is 8.95 kg. The yield of tungsten hexafluoride was 81.7% based on the consumption of tungsten powder. In the crude tungsten hexafluoride product outputted through the outlet 5-2 of the fixed bed reactor, the volume fraction of tungsten hexafluoride is 98.0%, the volume fraction of chlorine gas (i.e., fluorine gas) is 0.3%, the volume fraction of nitrogen trifluoride is 0.7%, and the volume fraction of nitrogen and other impurities is 1.0%. The data show that the fluorine and nitrogen trifluoride content decreased and the tungsten hexafluoride content increased, indicating that the fixed bed reactor serves better to eliminate excess fluorinating agent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The preparation device of tungsten hexafluoride is characterized by comprising a vertical tungsten fluoride reactor (1), wherein the vertical tungsten fluoride reactor (1) is provided with a reaction cavity tungsten powder feed inlet (1-1), a tungsten hexafluoride gas outlet (1-2) and a fluorinating agent inlet (1-3);
the temperature control jacket (2) is arranged on the outer side wall of the vertical fluorine-tungsten reactor (1);
and a tungsten powder automatic feeding device (3) communicated with the tungsten powder feeding hole (1-1) of the reaction cavity;
the tungsten powder automatic feeding device (3) comprises a tungsten powder feeding bin (3-1), a feeding machine (3-2) communicated with an outlet of the tungsten powder feeding bin (3-1), a driving motor (3-3) electrically connected with the feeding machine (3-2), and a tungsten powder feeding pipe (3-5) communicated with the feeding machine (3-2), wherein the tungsten powder feeding pipe (3-5) extends into the vertical fluorine-tungsten reactor (1) through a tungsten powder feeding hole (1-1) of the reaction cavity;
the tungsten powder feeding bin (3-1) is respectively communicated with a pressure display instrument (3-4), a nitrogen blowing device (3-6) and a vacuumizing device (3-7).
2. The preparation device according to claim 1, wherein a fluorinating agent redistributor (1-4) is further arranged in the vertical type fluorine-tungsten reactor (1), the fluorinating agent redistributor (1-4) comprises a fluorinating agent outlet pipeline, an outlet hole is arranged on the fluorinating agent outlet pipeline, and a first dust baffle (1-4-1) is connected with the edge of the outlet hole.
3. The manufacturing apparatus according to claim 1, wherein a second dust baffle (1-5) is further disposed in the vertical type tungsten fluoride reactor (1), the second dust baffle (1-5) is disposed between the tungsten hexafluoride gas outlet (1-2) and the tungsten powder feeding pipe (3-5), and the level of the lowermost end of the second dust baffle (1-5) is lower than the level of the lowermost end of the tungsten powder feeding pipe (3-5).
4. The preparation device according to claim 1, wherein the vertical fluorotungsten reactor (1) is further provided with a plurality of temperature monitoring ports (1-6), and the temperature monitoring ports (1-6) penetrate through the wall of the vertical fluorotungsten reactor (1) and the temperature control jacket (2).
5. The production apparatus according to any one of claims 1 to 4, further comprising a fixed bed reactor (5) connected in series with the vertical fluorotungsten reactor; the fixed bed reactor (5) is provided with a fixed bed reactor inlet (5-1) and a fixed bed reactor outlet (5-2);
and a heating assembly (5-3) arranged on the outer side wall of the fixed bed reactor (5).
6. A production apparatus according to claim 5, characterized in that the apparatus further comprises a tungsten hexafluoride storage means (4), an inlet of the tungsten hexafluoride storage means (4) being in communication with the tungsten hexafluoride gas outlet (1-2) or with the fixed bed reactor outlet (5-2).
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| CN114534678A (en) * | 2021-12-31 | 2022-05-27 | 天津海嘉斯迪新材料合伙企业(有限合伙) | Preparation device and method of tungsten hexafluoride |
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