CN112573575A - Tungsten hexafluoride preparation device and method for improving raw material utilization rate - Google Patents
Tungsten hexafluoride preparation device and method for improving raw material utilization rate Download PDFInfo
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- CN112573575A CN112573575A CN202011536403.XA CN202011536403A CN112573575A CN 112573575 A CN112573575 A CN 112573575A CN 202011536403 A CN202011536403 A CN 202011536403A CN 112573575 A CN112573575 A CN 112573575A
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- NXHILIPIEUBEPD-UHFFFAOYSA-H tungsten hexafluoride Chemical compound F[W](F)(F)(F)(F)F NXHILIPIEUBEPD-UHFFFAOYSA-H 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000002994 raw material Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000010926 purge Methods 0.000 claims abstract description 41
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 32
- 239000011737 fluorine Substances 0.000 claims abstract description 32
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims abstract description 14
- 239000007789 gas Substances 0.000 claims description 89
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- 229910052751 metal Inorganic materials 0.000 claims description 38
- 239000002184 metal Substances 0.000 claims description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 238000003860 storage Methods 0.000 claims description 13
- 238000007664 blowing Methods 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- 229910000792 Monel Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 7
- 238000000151 deposition Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000010408 sweeping Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/04—Halides
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention relates to a tungsten hexafluoride preparation device and method for improving the utilization rate of raw materials, and belongs to the technical field of tungsten hexafluoride preparation. The device comprises a recovery tank, a fluidized bed reactor, a purge gas pipe, a condenser, a collecting tank, a compressor, a buffer tank, a fluorine-containing mixed gas tank and a feeding mechanism. Before tungsten hexafluoride preparation reaction, under the even gas tray effect in fluidized bed reactor, the purge gas is evenly divided and blown out, the purge gas sweeps and evacuates the inside of fluidized bed reactor, during tungsten hexafluoride preparation, the take-up (stock) pan can avoid tungsten powder deposit can't participate in the reaction in fluidized bed reactor bottom, guarantee tungsten powder fully react, and utilize the filter disc to filter tungsten powder, avoid tungsten powder to get into inside the first pipeline along with gas, the utilization ratio of raw materials has been improved, also make the tungsten hexafluoride purity that generates high, after tungsten hexafluoride preparation, utilize the purge gas of purge gas pipe to carry out the pulsed blowback, make the tungsten powder attached on the filter disc blown down, the recovery tank is retrieved, it is extravagant to reduce the material.
Description
Technical Field
The invention relates to a tungsten hexafluoride preparation device and method for improving the utilization rate of raw materials, and belongs to the technical field of tungsten hexafluoride preparation.
Background
Tungsten hexafluoride, molecular formula WF6, molecular weight 297.830. Colorless gas or pale yellow liquid, and the solid is white crystal easy to deliquesce and smoke in humid air.
Tungsten hexafluoride is mainly used in the electronic industry, has very wide application in the field of semiconductors, is a raw material of a chemical vapor deposition process of metal tungsten, and can avoid soft errors of radioactive impurity alpha particles in a memory circuit to a great extent.
In the prior art, a fixed bed reactor is commonly used in industry for preparing tungsten hexafluoride, but the following problems exist:
1. in the preparation reaction process, the generated gas is easy to carry tungsten powder into the condenser, so that the preparation quality is reduced, and the material waste is also caused;
2. before the preparation reaction, the fluidized bed reactor cannot be fully purged, so that the preparation effect is influenced;
3. in the preparation reaction process, the metal tungsten powder is easy to deposit at the bottom of the fluidized bed reactor and cannot participate in the reaction, so that the utilization rate of the metal tungsten powder is low.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a tungsten hexafluoride preparation device and a method for improving the utilization rate of raw materials.
In order to achieve the purpose of the invention, the following technical scheme is provided.
The utility model provides an improve tungsten hexafluoride preparation facilities of utilization ratio of raw materials, the device is including retrieving jar, fluidized bed reactor, purge gas pipe, condenser, holding vessel, compressor, buffer tank, fluorine-containing gas mixture jar and feed mechanism.
The recovery tank is communicated with the fluidized bed reactor through a connecting pipeline, the top of the fluidized bed reactor is provided with an air outlet which is communicated with a condenser through a first pipeline, the condenser is communicated with a collecting tank, the condenser is communicated with a compressor through a second pipeline, the compressor is communicated with a buffer tank through a pipeline, the buffer tank is communicated with the fluidized bed reactor through a third pipeline, and a fluorine-containing mixed air tank is communicated with the third pipeline through a fourth pipeline; the left side of the fluidized bed reactor is provided with a feeding mechanism, and the feeding mechanism is communicated with the fluidized bed reactor through a material conveying port. The lateral wall of first pipeline is provided with the purge gas pipe, and the purge gas pipe is connected with the gas pitcher that sweeps, the sweep gas is nitrogen gas or inert gas.
The purge air pipe, the first pipeline, the second pipeline, the third pipeline and the fourth pipeline are all provided with electromagnetic valves.
The fluidized bed reactor comprises a lower fluidized bed reactor shell, a middle fluidized bed reactor shell and an upper fluidized bed reactor shell which are sequentially connected from bottom to top; an air homogenizing disc is arranged in the lower shell of the fluidized bed reactor, an air inlet is arranged on the side wall of one side below the air homogenizing disc in an upstream mode, and the side wall of the other side is communicated with a third pipeline; the inside of the middle shell of the fluidized bed reactor is provided with a receiving disc, the inside of the upper shell of the fluidized bed reactor is provided with a filter disc, and the material conveying opening is positioned on the side wall above the receiving disc of the middle shell of the fluidized bed reactor and below the filter disc.
The optimized feeding mechanism comprises a nitrogen tank, a quantitative hopper and a storage tank, the discharge end of the storage tank is communicated with the quantitative hopper, the discharge end of the quantitative hopper is communicated with the upper part of a receiving disc of a middle shell of the fluidized bed reactor through a conveying pipe, and the output end of the nitrogen tank is communicated with the conveying pipe.
Preferably, the recovery tank, the fluidized bed reactor, the purge gas pipe, the first pipeline, the collecting tank, the buffer tank, the third pipeline, the fourth pipeline and the fluorine-containing mixed gas tank are respectively and independently prepared from stainless steel, nickel or Monel alloy materials.
The invention discloses a tungsten hexafluoride preparation method for improving the utilization rate of raw materials, which is carried out by adopting a tungsten hexafluoride preparation device for improving the utilization rate of raw materials, and comprises the following steps:
1) cleaning by blowing: before reaction, the purging gas enters the interior of the fluidized bed reactor through the purging gas pipe, and meanwhile, under the action of the gas homogenizing disc, the purging gas can be uniformly blown out, so that the purging gas purges the interior of the fluidized bed reactor and is vacuumized and cleaned.
2) Adding materials: feeding the metal tungsten powder into the fluidized bed reactor from a feeding mechanism through an air inlet under the action of nitrogen, wherein the feeding rate is 0.07 kg/min-0.12 kg/min; preferably, the metal tungsten powder is discharged through a storage tank, and is quantitatively discharged through a quantitative hopper, and nitrogen is blown into a nitrogen tank to feed under the action of the nitrogen.
3) The preparation reaction comprises the following steps: when the temperature of the fluidized bed reactor is 230-260 ℃ and the reaction pressure is 0.1-0.15 MPa, the electromagnetic valve on the fourth pipeline is opened, so that the fluorine-containing mixed gas in the fluorine-containing mixed gas tank enters the fluidized bed reactor, the metal tungsten powder is blown up by the entering fluorine-containing mixed gas in the fluidized bed reactor to be in a fluidized state and can fully contact with fluorine gas for reaction, and meanwhile, the receiving disc can prevent the metal tungsten powder from depositing at the bottom of the fluidized bed reactor and not participating in the reaction, so that the full reaction of the metal tungsten powder is ensured.
4) Condensing and collecting: when gaseous tungsten hexafluoride who generates and fluorine-containing gas mixture enter into the inside of first pipeline through the gas outlet, open the solenoid valve of first pipeline, make gas get into the inside of condenser, can filter metal tungsten powder through the filter disc simultaneously, avoid metal tungsten powder along with gaseous inside that gets into the condenser, the utilization ratio of raw materials has been improved, accomplish the condensation in the gaseous entering condenser, gaseous tungsten hexafluoride liquefaction is collected through the collection tank, unreacted fluorine-containing gas mixture passes through the second pipeline, and under the effect of compressor, store after the compression and wait to continue to let in the participation reaction in the buffer tank, recycle's effect has been reached, fluorine-containing gas mixture's utilization ratio has been improved.
Preferably, purging again: the electromagnetic valve of the purge gas pipe is opened, other electromagnetic valves are closed, the metal tungsten powder adhered to the filter disc is purged by using the purge gas, the metal tungsten powder is prevented from being adhered to the surface of the filter disc, and the tungsten hexafluoride is conveniently prepared again.
Advantageous effects
The invention provides a tungsten hexafluoride preparation device and a method for improving the utilization rate of raw materials, before tungsten hexafluoride preparation reaction, under the action of an even gas disk, sweeping gas can be uniformly and separately blown out, so that the interior of a fluidized bed reactor is swept by the sweeping gas and is vacuumized and cleaned, in the tungsten hexafluoride preparation reaction process, a receiving disk can be used for preventing metal tungsten powder from depositing at the bottom of the fluidized bed reactor and failing to participate in the reaction, the sufficient reaction of the metal tungsten powder is ensured, and under the action of a filter disk, the metal tungsten powder can be filtered, the metal tungsten powder is prevented from entering the interior of a first pipeline along with the gas, the utilization rate of the raw materials is improved, the purity of the generated tungsten hexafluoride is high, after the tungsten hexafluoride preparation reaction, a blowing pipe can be used for pulse type back blowing by using nitrogen, so that the metal tungsten powder attached to the filter disk is blown down and can be recovered by using a recovery tank, the waste of materials is reduced.
Drawings
Fig. 1 is a schematic structural diagram of a tungsten hexafluoride preparation apparatus for improving a raw material utilization rate in example 1.
Wherein, 1-recovery tank, 2-connecting pipeline, 3-air inlet, 4-lower shell of fluidized bed reactor, 5-middle shell of fluidized bed reactor, 6-upper shell of fluidized bed reactor, 7-air homogenizing disc, 8-receiving disc, 9-material conveying opening, 10-filter disc, 11-air outlet, 12-material conveying pipe, 13-nitrogen tank, 14-quantitative hopper, 15-material storage tank, 16-purge air pipe, 17-first pipeline, 18-condenser, 19-second pipeline, 20-collecting tank, 21-compressor, 22-buffer tank, 23-third pipeline, 24-fourth pipeline, 25-fluorine-containing mixed gas tank
Detailed Description
The invention is described in detail below with reference to the drawings and specific examples, but the invention is not limited thereto.
A tungsten hexafluoride preparation device for improving the utilization rate of raw materials is shown in figure 1 and comprises a recovery tank 1, a fluidized bed reactor, a purge gas pipe 16, a condenser 18, a collection tank 20, a compressor 21, a buffer tank 22, a fluorine-containing mixed gas tank 25 and a feeding mechanism.
The recovery tank 1 is communicated with the fluidized bed reactor through a connecting pipeline 2, the top of the fluidized bed reactor is provided with an air outlet 11 which is communicated with a condenser 18 through a first pipeline 17, the condenser 18 is communicated with a collecting tank 20, the condenser 18 is communicated with a compressor 21 through a second pipeline 19, the compressor 21 is communicated with a buffer tank 22 through a pipeline, the buffer tank 22 is communicated with the fluidized bed reactor through a third pipeline 23, and a fluorine-containing mixed air tank 25 is communicated with the third pipeline 23 through a fourth pipeline 24.
The fluidized bed reactor comprises a lower fluidized bed reactor shell 4, a middle fluidized bed reactor shell 5 and an upper fluidized bed reactor shell 6 which are sequentially connected from bottom to top; a gas homogenizing disc 7 is arranged in the lower shell 4 of the fluidized bed reactor, a gas inlet 3 is arranged on the side wall of one side below the gas homogenizing disc 7 in an up-flow mode, the side wall of the other side is communicated with a third pipeline 23, the gas homogenizing disc 7 can enable sweeping gas nitrogen to be uniformly blown out, and the interior of the fluidized bed reactor is swept by the nitrogen and is vacuumized and cleaned; a receiving tray 8 is arranged in the shell 5 of the fluidized bed reactor, and the receiving tray 8 can prevent the metal tungsten powder from depositing at the bottom of the fluidized bed reactor and failing to participate in the reaction, so that the sufficient reaction of the metal tungsten powder is ensured; the filter disc 10 is arranged in the upper shell 6 of the fluidized bed reactor, the material conveying opening 9 is located in the side wall above the material receiving disc 8 of the middle shell 5 of the fluidized bed reactor and located below the filter disc 10, the metal tungsten powder can be filtered by the filter disc 10, the metal tungsten powder is prevented from entering the condenser 18 along with gas, and the utilization rate of raw materials is improved.
The left end of the fluidized bed reactor is provided with a feeding mechanism, and the feeding mechanism is communicated with the fluidized bed reactor through a material conveying port 9. The feeding mechanism comprises a nitrogen tank 13, a quantitative hopper 14 and a storage tank 15, the discharge end of the storage tank 15 is communicated with the quantitative hopper 14, the quantitative hopper 14 is communicated with the upper part of a receiving disc 8 of the middle shell 5 of the fluidized bed reactor through a conveying pipe 12, and the output end of the nitrogen tank 13 is communicated with the conveying pipe 12.
The side wall of the first pipeline 17 is provided with a purge gas pipe 16, pulse type back blowing can be carried out by using nitrogen, so that metal tungsten powder attached to the filter disc 10 is blown down and can be recovered by using the recovery tank 1, and the purge gas pipe 16, the first pipeline 17, the second pipeline 19, the third pipeline 23 and the fourth pipeline 24 are all provided with electromagnetic valves.
The recovery tank 1, the fluidized bed reactor, the purge gas pipe 16, the first pipeline 17, the collection tank 20, the buffer tank 22, the third pipeline 23, the fourth pipeline 24 and the fluorine-containing mixed gas tank 25 are all made of stainless steel, nickel or monel alloy materials, have good corrosion resistance and are convenient for preparation and use of tungsten hexafluoride.
A tungsten hexafluoride preparation method for improving the utilization rate of raw materials is carried out by adopting the tungsten hexafluoride preparation device for improving the utilization rate of raw materials, and comprises the following steps:
1) cleaning by blowing: before reaction, the nitrogen gas as the purging gas enters the interior of the fluidized bed reactor through the purging gas pipe 16, and meanwhile, under the action of the gas homogenizing disc 7, the nitrogen gas can be uniformly blown out, so that the interior of the fluidized bed reactor is purged by the nitrogen gas and is vacuumized and cleaned.
2) Adding materials: the metal tungsten powder is discharged through a material storage tank 15, quantitatively discharged through a quantitative hopper 14, simultaneously blown by nitrogen gas through a nitrogen gas tank 13, and fed to the fluidized bed reactor through an air inlet 3 under the action of the nitrogen gas, wherein the feeding rate is 0.07 kg/min-0.12 kg/min.
3) The preparation reaction comprises the following steps: when the temperature of the fluidized bed reactor is 230-260 ℃ and the reaction pressure is 0.1-0.15 Mpa, the electromagnetic valve on the fourth pipeline 24 is opened, so that the fluorine-containing mixed gas in the fluorine-containing mixed gas tank 25 enters the fluidized bed reactor, the metal tungsten powder is blown up by the entering fluorine-containing mixed gas in the fluidized bed reactor to be in a fluidized state and can fully contact with fluorine gas for reaction, and meanwhile, the receiving disc 8 can prevent the metal tungsten powder from depositing at the bottom of the fluidized bed reactor and failing to participate in the reaction, so that the sufficient reaction of the metal tungsten powder is ensured.
4) Condensing and collecting: when the generated gaseous tungsten hexafluoride and fluorine-containing mixed gas enters the interior of the first pipeline 17 through the gas outlet 11, the electromagnetic valve of the first pipeline 17 is opened, so that the gas enters the interior of the condenser 18, meanwhile, the metal tungsten powder can be filtered through the filter disc 10, the metal tungsten powder is prevented from entering the interior of the condenser 18 along with the gas, the utilization rate of raw materials is improved, the gas enters the condenser 18 to be condensed, the liquefied gaseous tungsten hexafluoride can be collected through the collection tank 20, the unreacted fluorine-containing mixed gas passes through the second pipeline 19 and is compressed and stored in the buffer tank 22 under the action of the compressor 21 to be continuously introduced and participate in the reaction, the recycling effect is achieved, and the utilization rate of the fluorine-containing mixed gas is improved;
and (3) secondary blowing and cleaning: and opening the electromagnetic valve of the purge gas pipe 16, closing other electromagnetic valves, and purging the metal tungsten powder adhered to the filter disc 10 by using nitrogen, so that the metal tungsten powder is prevented from being adhered to the surface of the filter disc 10, and the tungsten hexafluoride is conveniently prepared again.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The utility model provides an improve tungsten hexafluoride preparation facilities of utilization ratio of raw materials which characterized in that: the device comprises a recovery tank (1), a fluidized bed reactor, a purge gas pipe (16), a condenser (18), a collecting tank (20), a compressor (21), a buffer tank (22), a fluorine-containing mixed gas tank (25) and a feeding mechanism;
the recovery tank (1) is communicated with the fluidized bed reactor through a connecting pipeline (2), the top of the fluidized bed reactor is provided with a gas outlet (11) which is communicated with a condenser (18) through a first pipeline (17), the condenser (18) is communicated with a collection tank (20), the condenser (18) is communicated with a compressor (21) through a second pipeline (19), the compressor (21) is communicated with a buffer tank (22) through a pipeline, the buffer tank (22) is communicated with the fluidized bed reactor through a third pipeline (23), and a fluorine-containing gas mixture tank (25) is communicated with the third pipeline (23) through a fourth pipeline (24); a feeding mechanism is arranged on the left side of the fluidized bed reactor and is communicated with the fluidized bed reactor through a material conveying port (9); a purge gas pipe (16) is arranged on the side wall of the first pipeline (17), the purge gas pipe (16) is connected with a purge gas tank, and the purge gas is nitrogen or inert gas;
electromagnetic valves are arranged on the purge air pipe (16), the first pipeline (17), the second pipeline (19), the third pipeline (23) and the fourth pipeline (24);
the fluidized bed reactor comprises a lower fluidized bed reactor shell (4), a middle fluidized bed reactor shell (5) and an upper fluidized bed reactor shell (6) which are sequentially connected from bottom to top; an air homogenizing disc (7) is arranged in the lower shell (4) of the fluidized bed reactor, an air inlet (3) is arranged on the side wall of one side below the air homogenizing disc (7) in an up-flow mode, and the side wall of the other side is communicated with a third pipeline (23); a receiving disc (8) is arranged inside a shell (5) in the fluidized bed reactor, a filter disc (10) is arranged inside an upper shell (6) of the fluidized bed reactor, and a material conveying opening (9) is located in the side wall above the receiving disc (8) of the shell (5) in the fluidized bed reactor and below the filter disc (10).
2. The apparatus for preparing tungsten hexafluoride according to claim 1, wherein: the feeding mechanism comprises a nitrogen tank (13), a quantitative hopper (14) and a storage tank (15), the discharge end of the storage tank (15) is communicated with the quantitative hopper (14), the discharge end of the quantitative hopper (14) is communicated with the upper part of a receiving disc (8) of a shell (5) in the fluidized bed reactor through a conveying pipe (12), and the output end of the nitrogen tank (13) is communicated with the conveying pipe (12).
3. The apparatus for preparing tungsten hexafluoride according to claim 1, wherein: the recovery tank (1), the fluidized bed reactor, the purge gas pipe (16), the first pipeline (17), the collection tank (20), the buffer tank (22), the third pipeline (23), the fourth pipeline (24) and the fluorine-containing mixed gas tank (25) are respectively and independently prepared from stainless steel, nickel or Monel alloy materials.
4. The apparatus for preparing tungsten hexafluoride according to claim 1, wherein: the feeding mechanism comprises a nitrogen tank (13), a quantitative hopper (14) and a storage tank (15), the discharge end of the storage tank (15) is communicated with the quantitative hopper (14), the discharge end of the quantitative hopper (14) is communicated with the upper part of a receiving disc (8) of a shell (5) in the fluidized bed reactor through a conveying pipe (12), and the output end of the nitrogen tank (13) is communicated with the conveying pipe (12);
the recovery tank (1), the fluidized bed reactor, the purge gas pipe (16), the first pipeline (17), the collection tank (20), the buffer tank (22), the third pipeline (23), the fourth pipeline (24) and the fluorine-containing mixed gas tank (25) are respectively and independently prepared from stainless steel, nickel or Monel alloy materials.
5. A tungsten hexafluoride preparation method for improving raw material utilization rate is characterized by comprising the following steps: the method is carried out by adopting the tungsten hexafluoride preparation device for improving the utilization rate of raw materials as claimed in any one of claims 1 to 4, and the steps comprise:
1) before reaction, the blowing gas enters the interior of the fluidized bed reactor through a blowing gas pipe (16), and meanwhile, under the action of the gas homogenizing disc (7), the blowing gas can be uniformly blown out, so that the blowing gas can blow the interior of the fluidized bed reactor and vacuumize and clean the interior of the fluidized bed reactor;
2) feeding the metal tungsten powder into the fluidized bed reactor from a feeding mechanism through an air inlet (3) under the action of nitrogen, wherein the feeding speed is 0.07 kg/min-0.12 kg/min;
3) when the temperature of the fluidized bed reactor is 230-260 ℃ and the reaction pressure is 0.1-0.15 MPa, opening an electromagnetic valve on a fourth pipeline (24) to ensure that the fluorine-containing mixed gas in the fluorine-containing mixed gas tank (25) enters the fluidized bed reactor, and blowing the metal tungsten powder in the fluidized bed reactor by the entering fluorine-containing mixed gas to be in a fluidized state, so that the metal tungsten powder can be in full contact reaction with fluorine gas;
4) when the generated gaseous tungsten hexafluoride and fluorine-containing mixed gas enter the interior of the first pipeline (17) through the gas outlet (11), the electromagnetic valve of the first pipeline (17) is opened, so that the gas enters the interior of the condenser (18), meanwhile, the metal tungsten powder can be filtered through the filter disc (10), the gas enters the condenser (18) to be condensed, the gaseous tungsten hexafluoride is liquefied and collected through the collection tank (20), the unreacted fluorine-containing mixed gas passes through the second pipeline (19), and under the action of the compressor (21), the compressed gas is stored in the buffer tank (22) to be continuously introduced and participate in the reaction.
6. The method for preparing tungsten hexafluoride according to claim 5, wherein the tungsten hexafluoride is prepared by using a method comprising the following steps: the metal tungsten powder is discharged through a storage tank (15), and is quantitatively discharged through a quantitative hopper (14), and nitrogen is blown into a nitrogen tank (13) and fed under the action of the nitrogen.
7. The method for preparing tungsten hexafluoride according to claim 5, wherein the tungsten hexafluoride is prepared by using a method comprising the following steps: and (4) after the step (4) is finished, opening the electromagnetic valve of the purge gas pipe (16), closing other electromagnetic valves, and purging the metal tungsten powder adhered to the filter disc (10) by using purge gas.
8. The method for preparing tungsten hexafluoride according to claim 5, wherein the tungsten hexafluoride is prepared by using a method comprising the following steps: the metal tungsten powder is discharged through a material storage tank (15), and is quantitatively discharged through a quantitative hopper (14), and nitrogen is blown into a nitrogen tank (13) at the same time, and feeding is carried out under the action of the nitrogen;
and (4) after the step (4) is finished, opening the electromagnetic valve of the purge gas pipe (16), closing other electromagnetic valves, and purging the metal tungsten powder adhered to the filter disc (10) by using purge gas.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| US11504685B1 (en) | 2021-09-27 | 2022-11-22 | Suzhou Yisheng Optical Material Co., Ltd. | Processing equipment and processing technology of gel microsphere material |
| CN116854138A (en) * | 2023-06-13 | 2023-10-10 | 福建德尔科技股份有限公司 | Preparation device, system and method of tungsten hexafluoride |
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| CN101428858A (en) * | 2008-11-07 | 2009-05-13 | 黎明化工研究院 | Method for producing high-purity tungsten hexafluoride with fluidized bed and equipment thereof |
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| CN215626837U (en) * | 2020-12-22 | 2022-01-25 | 中船重工（邯郸）派瑞特种气体有限公司 | Tungsten hexafluoride preparation device capable of improving raw material utilization rate |
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Address after: 057550 No. five Weir Road, chemical industry gathering area, Feixiang District, Handan, Hebei, 1 Applicant after: China shipbuilding (Handan) Perry Special Gas Co.,Ltd. Address before: No.1 Weiwu Road, chemical industry gathering area, Feixiang County, Handan City, Hebei Province Applicant before: PERIC SPECIAL GASES Co.,Ltd. |
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