CN106976913A - A kind of synthetic method of tungsten hexafluoride - Google Patents
A kind of synthetic method of tungsten hexafluoride Download PDFInfo
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- CN106976913A CN106976913A CN201710358430.4A CN201710358430A CN106976913A CN 106976913 A CN106976913 A CN 106976913A CN 201710358430 A CN201710358430 A CN 201710358430A CN 106976913 A CN106976913 A CN 106976913A
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- C01—INORGANIC CHEMISTRY
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- C01G41/00—Compounds of tungsten
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Abstract
A kind of synthetic method of tungsten hexafluoride.It is to be fitted into tungsten powder in reactor with metal fluoride to be sufficiently mixed, and fluorine gas is passed through at reaction conditions and carries out reaction synthesis tungsten hexafluoride, the complete raw material fluorine gas of unreacted after condensation gas-liquid separation, returns again to reactor cycles reaction with product tungsten hexafluoride.Synthetic method of the present invention is reacted using the fluorine gas and tungsten powder of circulation in the presence of metal fluoride, effectively increases the efficiency of the reaction, reduces the waste of raw material fluorine gas, and effectively reduces volume needed for reactor.
Description
Technical field
The present invention relates to a kind of new method for synthesizing tungsten hexafluoride, this method is that in cobalt, system urges using tungsten powder as preparing raw material
In the presence of agent, reacted synthesis tungsten hexafluoride with fluorine gas
Background technology
Tungsten hexafluoride, chemical formula is WF6, is a kind of colourless gas, during condensation, is weak yellow liquid, and molal weight is
297.83g/mol, is one of maximum gas of density.Tungsten hexafluoride is mainly used in chemical vapor deposition tungsten, is also used for preparing low
Resistance, dystectic interconnection line and large-scale integrated circuit electronic component, anti-X-ray or gamma-ray protective cover, high-efficiency solar
Absorber.
On the synthesis of tungsten hexafluoride, current topmost synthetic route still makees the technique of fluorization agent with fluorine gas, a small number of
Producer can synthesize tungsten hexafluoride using NF3 as fluorization agent.Tungsten hexafluoride is wherein synthesized with NF3, cost is too high, and reaction efficiency has
Limit, is not suitable for industrialized production.The technique that fluorization agent is made with fluorine gas be by make fluorine gas flow through tungsten (graininess or
It is powdered) fluid bed or fixed bed synthesize, but the technique falls within gas-solid reaction, and gas only in the reaction of tungsten surface, connects
Limited area is touched, it is low to there is reaction efficiency, the problems such as unreacting material gas is wasted.
The content of the invention
In order to overcome the above-mentioned deficiency of prior art, the present invention provides a kind of synthetic method of tungsten hexafluoride, can significantly carried
High reaction efficiency, can reduce influence of the concentration of fluorine to reaction, it is to avoid wastage of material, mitigate follow-up noxious gas emission processing
Difficulty, saves cost, can also reduce the volume of reactor, reaction temperature is relatively low, reduces energy consumption, and course of reaction is simple, operation side
Just, it is easy to accomplish industrialization.
The present invention solve its technical problem use technical scheme be：It is that tungsten powder and metal fluoride are fitted into reactor
It is sufficiently mixed, fluorine gas is passed through at reaction conditions and carries out reaction synthesis tungsten hexafluoride, the complete raw material fluorine gas of unreacted and product six
Tungsten fluoride returns again to reactor cycles reaction after condensation gas-liquid separation.
Compared with prior art, what a kind of synthetic method of tungsten hexafluoride of the invention was brought has the beneficial effect that：
1. this method is reacted using the raw material fluorine gas and tungsten powder of circulation in the presence of metal fluoride, effectively improve
The efficiency of the reaction, reduces the waste of raw material fluorine gas, and effectively reduce volume needed for reactor；
2. the metal fluoride that this method is introduced, itself has high fluorination property, can participate in reaction, it is reduced into tungsten powder reaction
After keen price fluoride, the fluoride of high price can be regenerated with fluorine gas again, this effectively increases reaction efficiency, also reduces fluorine gas
Influence of the concentration to reaction；
3. this method course of reaction is simple, easy to operate, reaction temperature is relatively low, reduces energy consumption.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the one of the present invention
Section Example, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under the premise of creative work, belong to protection scope of the present invention.
The synthetic method of the present invention is to be fitted into reactor tungsten powder with metal fluoride and be sufficiently mixed, such as by tungsten powder
It is fitted into metal fluoride in the reactor with stirring and is sufficiently mixed, fluorine gas is then passed through at reaction conditions and is reacted
Tungsten hexafluoride is synthesized, the complete raw material fluorine gas of unreacted after condensation gas-liquid separation, returns again to reactor with product tungsten hexafluoride
Circular response.
Its specific technical process can be comprised the following steps：
1. described tungsten powder and metal fluoride are fitted into reactor, and it is sufficiently mixed by stirring；
2. described raw material fluorine gas is passed through under the conditions of reaction temperature condition, reaction pressure anti-in described reactor
Should, the gas discharged after reaction is the mixed gas being made up of the tungsten hexafluoride of unreacted raw material fluorine gas and generation；
3. after described mixed gas is removed into solid particle through filter, it is passed through in cryogenic collector tank and carries out tungsten hexafluoride
The collection of crude product, and the uncooled raw material fluorine gas got off re-starts reaction through compressor supercharging Returning reactor again；
4. described in raw material fluorine gas addition, pressure changing can be seen in reaction system to determine；
5. the tungsten hexafluoride crude product of collection is transported into purification system, high-purity hexafluoro is made through drying, absorption, rectifying
Change tungsten product.
In the synthetic method that the present invention is used, it is blended in using the metal fluoride and tungsten powder of high fluorination property with the anti-of stirring
Answer in device, it is therefore an objective to increase reaction contact area, significantly improve reaction efficiency, and the influence to concentration of fluorine is insensitive.Stirring
Effect can make tungsten powder in reactor in fluidisation state, constantly with variable grain collide, have to a certain degree reduce Tungsten Powder Size and
Increase the effect of its total surface area；And metal fluoride itself has high fluorination property, tungsten hexafluoride can be synthesized with tungsten powder, it
In the presence of high reaction efficiency in energy maintenance reaction device, and influence of the concentration of fluorine to reaction can be reduced.
In the synthetic method that the present invention is used, unreacted raw material fluorine gas is circulated reacts again into reactor, it is therefore an objective to
Reduce the discharge of raw material fluorine gas, it is to avoid waste, mitigate the difficulty of follow-up noxious gas emission processing, save cost, in addition raw material
Circulation can also reduce the volume of reactor.
In the synthetic method that the present invention is used, with the progress of reaction, the raw material fluorine gas step-reaction in reaction system is given birth to
Into tungsten hexafluoride, and the tungsten hexafluoride generated is progressively condensed into liquid；That is in reaction system, gas is to gradually reduce
's；Thus, when can set the pressure or flow in reactor less than setting value, supplement raw material fluorine gas enters in reaction cycle.Together
When, with the progress of reaction, the on-condensible gas impurity in addition to raw material fluorine gas in reaction system also can be more poly- more, and this is unfavorable for
Reaction and the progress of subsequent purification, therefore, in reaction at regular intervals or every discharge after several supplement raw material fluorine gas circulations
Tail gas, to reduce the on-condensible gas impurity content in reaction system.
In the synthetic method that the present invention is used, during successive reaction, it is standby that described reactor and cryogenic collector tank can set one
One uses.After tungsten powder runs out of in one reactor, switch to another reactor for completing to dehydrate and reacted, consumption of raw materials is complete
Reactor fed, be dehydrated again, reacted after in case stand-by；Cryogenic collector tank is then to switch to another low temperature after tank is expired to receive
Collect tank to collect, and the cryogenic collector tank filled then is purified into purification system.
It is 5N fluorine gas and 3N tungsten powders that raw material fluorine gas of the present invention and tungsten powder are selected respectively.Tungsten hexafluoride product is mainly used
In semiconductor fabrication process, this purity requirement to it is very high, and as the raw material fluorine gas and tungsten powder of tungsten hexafluoride raw material, its is pure
Degree also should the higher the better, it is to avoid excessive impurity enters in product, increases subsequent purification difficulty.
Metal fluoride of the present invention is one kind in cobalt trifluoride and silver difluoride, preferably cobalt trifluoride, and it is filled
Enter the amount of reactor between the 1/4~1/3 of reactor volume.
Reaction temperature condition of the present invention control in the range of 200 DEG C~400 DEG C, preferably 270 DEG C~350 DEG C it
Between.If temperature is less than 270 DEG C, reaction efficiency is relatively low, whereas if temperature is higher than 350 DEG C, reacts bad control.
Reaction pressure scope control of the present invention is between 0~0.2MPa (gauge pressure), most preferably 0~0.1MPa.This
Because raw material fluorine gas participates in reacting in invention, then the risk that burning or blast occur in reacting increases with the increase of pressure, instead
Pressure is answered properly to select under low pressure, preferably between 0~0.1MPa.
Reactor used in synthetic method of the present invention with the strong oxidizing property gas such as fluorine gas due to contacting, its material
Material preferably, can use Monel, inconel and acidproof nickel alloy.
Embodiment 1
The tungsten powder of the mesh of 30kg raw materials 100 is added and has been loaded with the reactor of cobalt trifluoride (powder) (size is ￠ 89 × 4.5
× 1000) interior, carry out dehydrating operation (heating is vacuumized, water content≤3ppm) with equipment pipe, then by reactor
It is heated to reaction temperature condition.During reaction, reactor is passed through through absorber after fluorine gas pressure is increased into 2bar through compressor
Interior to be reacted, reaction temperature is at 300 DEG C, and charge flow rate is located at 120L/min or so；The tail gas of reactor discharge is through filter
WF6 is collected into the condensation of cryogenic collector tank, it is -5 DEG C to collect temperature；The effect of filter be mainly removing tail gas in dust,
The solid matters such as grain；The effect of absorber is the HF impurity contained in absorption tail gas；WF6 exists into the tail gas of cryogenic collector tank
Under low temperature (be less than its boiling temperature) be progressively condensed into the gas not being condensed in liquid, tail gas again through compressor supercharging return to
Reacted in reactor.The WF6 being collected into enters purification system and carries out the obtained high-purity WF6 of purifying again.
Embodiment 2
The tungsten powder of the mesh of 30kg raw materials 100 is added and has been loaded with the reactor of silver difluoride (powder) (size is ￠ 89 × 4.5
× 1000) interior, carry out dehydrating operation (heating is vacuumized, water content≤3ppm) with equipment pipe, then by reactor
It is heated to reaction temperature.During reaction, it is passed through after fluorine gas pressure is increased into 1.5bar through compressor through absorber in reactor
Reacted, reaction temperature is at 280 DEG C, and charge flow rate is located at 120L/min or so；The tail gas of reactor discharge enters through filter
Enter the condensation of cryogenic collector tank and collect WF6, it is -5 DEG C to collect temperature；The effect of filter is mainly dust, particle in removing tail gas
Deng solid matter；WF6 is progressively condensed into liquid, tail (less than its boiling temperature) at low temperature into the tail gas of cryogenic collector tank
The gas not being condensed in gas is returned through compressor supercharging again to be reacted to reactor.The WF6 being collected into enters purification system again
System carries out purifying and high-purity WF6 is made.
The tungsten hexafluoride synthesized by the embodiment of the present invention, the utilization rate of raw material fluorine gas is up to 95%, obtained tungsten hexafluoride
Through subsequent purification technique (dry, absorption, rectifying), 5N tungsten hexafluoride can be made again in crude product.
It is described above, be only presently preferred embodiments of the present invention, any formal limitation not done to the present invention, it is every according to
According to the technical spirit of the present invention, any simple modification and equal change are made to above example, the guarantor of the present invention is each fallen within
Within the scope of shield.
Claims (10)
1. a kind of synthetic method of tungsten hexafluoride, is to be fitted into tungsten powder in reactor with metal fluoride to be sufficiently mixed, in reaction
Under the conditions of be passed through fluorine gas and carry out reaction synthesis tungsten hexafluoride, the complete raw material fluorine gas of unreacted and product tungsten hexafluoride pass through condensing gas
After liquid separation, reactor cycles reaction is returned again to.
2. a kind of synthetic method of tungsten hexafluoride according to claim 1, it is characterized in that：Processing step is as follows:
A. tungsten powder and metal fluoride are fitted into reactor, and are sufficiently mixed by stirring；
B. described raw material fluorine gas is passed through after absorber under the conditions of reaction temperature condition and reaction pressure anti-in reactor
Should, the gas discharged after reaction is the mixed gas of the tungsten hexafluoride composition of unreacted raw material fluorine gas and generation；
C. after mixed gas being removed into solid particle through filter, the receipts that tungsten hexafluoride crude product is carried out in cryogenic collector tank are passed through
Collection, and the uncooled raw material fluorine gas got off re-starts reaction through compressor supercharging Returning reactor again；
D. the tungsten hexafluoride crude product of collection is transported to purification system, high-purity tungsten hexafluoride is made through drying, absorption, rectifying
Product.
3. a kind of synthetic method of tungsten hexafluoride according to claim 1 or 2, it is characterized in that：Described raw material fluorine gas is
5N fluorine gas, tungsten powder is 3N tungsten powders.
4. a kind of synthetic method of tungsten hexafluoride according to claim 1 or 2, it is characterized in that：Described metal fluoride
For cobalt trifluoride or silver difluoride.
5. a kind of synthetic method of tungsten hexafluoride according to claim 1 or 2, it is characterized in that：The metal fluoride dress
Enter the amount of reactor between the 1/4~1/3 of reactor volume.
6. a kind of synthetic method of tungsten hexafluoride according to claim 1 or 2, it is characterized in that：The reaction temperature condition
Control is in the range of 200 DEG C~400 DEG C.
7. a kind of synthetic method of tungsten hexafluoride according to claim 6, it is characterized in that：The reaction temperature condition is
270 DEG C~350 DEG C.
8. a kind of synthetic method of tungsten hexafluoride according to claim 1 or 2, it is characterized in that：The reaction pressure condition
Control is between 0~0.2MPa.
9. a kind of synthetic method of tungsten hexafluoride according to claim 8, it is characterized in that：The reaction pressure condition is 0
~0.1MPa.
10. a kind of synthetic method of tungsten hexafluoride according to claim 1 or 2, it is characterized in that：The material of the reactor
For any one in Monel, inconel, acidproof nickel alloy.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710358430.4A CN106976913A (en) | 2017-05-19 | 2017-05-19 | A kind of synthetic method of tungsten hexafluoride |
| CN201710996957.XA CN107540020B (en) | 2017-05-19 | 2017-10-20 | A kind of synthetic method of tungsten hexafluoride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710358430.4A CN106976913A (en) | 2017-05-19 | 2017-05-19 | A kind of synthetic method of tungsten hexafluoride |
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| CN201710996957.XA Active CN107540020B (en) | 2017-05-19 | 2017-10-20 | A kind of synthetic method of tungsten hexafluoride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112533873A (en) * | 2018-08-17 | 2021-03-19 | 中央硝子株式会社 | Method for producing tungsten hexafluoride |
| CN113636599A (en) * | 2021-08-17 | 2021-11-12 | 中船重工（邯郸）派瑞特种气体有限公司 | Comprehensive utilization method of tungsten hexafluoride waste liquid |
| CN116618190A (en) * | 2023-07-21 | 2023-08-22 | 福建德尔科技股份有限公司 | Centrifugal control system and control method for preparing tungsten hexafluoride |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109250759B (en) * | 2018-12-10 | 2021-03-02 | 湖南省华京粉体材料有限公司 | Preparation method and device of tungsten pentachloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0333084B1 (en) * | 1988-03-16 | 1994-07-27 | MITSUI TOATSU CHEMICALS, Inc. | Method for preparing gaseous fluorides |
| CN101070189B (en) * | 2007-06-16 | 2010-08-11 | 中国船舶重工集团公司第七一八研究所 | Method for preparing tungsten hexafluoride gas |
| KR20100046708A (en) * | 2008-10-28 | 2010-05-07 | (주)후성 | Production method of tungsten hexafluoride using fluidized bed reactor and fluidized bed reactor of the same |
| CN102951684B (en) * | 2012-11-26 | 2014-08-13 | 厦门钨业股份有限公司 | Preparation method for tungsten hexafluoride gas |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112533873A (en) * | 2018-08-17 | 2021-03-19 | 中央硝子株式会社 | Method for producing tungsten hexafluoride |
| KR20210041079A (en) | 2018-08-17 | 2021-04-14 | 샌트랄 글래스 컴퍼니 리미티드 | Method for producing tungsten hexafluoride |
| CN113636599A (en) * | 2021-08-17 | 2021-11-12 | 中船重工（邯郸）派瑞特种气体有限公司 | Comprehensive utilization method of tungsten hexafluoride waste liquid |
| CN116618190A (en) * | 2023-07-21 | 2023-08-22 | 福建德尔科技股份有限公司 | Centrifugal control system and control method for preparing tungsten hexafluoride |
| CN116618190B (en) * | 2023-07-21 | 2023-10-03 | 福建德尔科技股份有限公司 | Centrifugal control system and control method for preparing tungsten hexafluoride |
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| CN107540020B (en) | 2019-08-13 |
| CN107540020A (en) | 2018-01-05 |
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Application publication date: 20170725 |