CN114405035A - Reaction equipment and reaction process for preparing high-purity sulfur tetrafluoride - Google Patents
Reaction equipment and reaction process for preparing high-purity sulfur tetrafluoride Download PDFInfo
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Abstract
The invention provides reaction equipment for preparing high-purity sulfur tetrafluoride and a reaction process thereof, wherein the reaction equipment comprises a fluorination reactor, a reaction cold trap, a rectifying tower and a sulfur tetrafluoride storage tank; the fluorination reactor is provided with a first connecting pipeline and a sulfur liquid inlet pipeline which are communicated with the interior of the fluorination reactor, and the upper end of the fluorination reactor is communicated with the reaction cold trap through a second connecting pipeline; the reaction cold trap is provided with a vacuum pipeline and a process gas outlet pipeline, the other end of the process gas outlet pipeline is communicated with the middle part of the rectifying tower, the top of the rectifying tower is connected with a high-purity sulfur tetrafluoride gas outlet pipeline, and the other end of the rectifying tower is communicated with a sulfur tetrafluoride storage tank. The method for preparing the sulfur tetrafluoride takes the nitrogen trifluoride as the fluorinating agent, so that the safety risk of the raw material is reduced, the process method is safer and is suitable for industrialization, and the method for preparing the sulfur tetrafluoride takes the nitrogen trifluoride as the fluorinating agent, so that the problem of blockage of a pipeline valve caused by the sublimation and condensation processes of solids in a product is solved.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to reaction equipment for preparing high-purity sulfur tetrafluoride and a reaction process thereof.
Background
Sulfur tetrafluoride is a colorless gas with a unique sulfur gas, and has attracted more and more attention as a fluorinating agent, a surfactant, plasma etching, and the like. Meanwhile, sulfur tetrafluoride is the most effective high-selectivity fluorinating agent at present, and has an irreplaceable position in high-end pharmaceutical industrial production such as national defense, fine chemical engineering, liquid crystal materials, fluorine-containing pesticides, medicines and intermediates thereof. Meanwhile, with the rapid development of the electronic industry, the demand of liquid crystal for the application of the liquid crystal display device is rapidly increased, and the market of sulfur tetrafluoride products is not in demand at present.
At present, two main processes for industrially producing sulfur tetrafluoride exist, wherein the first process is to directly fluorinate liquid elemental sulfur by fluorine gas to generate sulfur tetrafluoride and sulfur hexafluoride;
S+2F2＝SF4
S+3F2＝SF6
the sulfur is easy to condense and block pipelines in the production process of the method, the selectivity of sulfur tetrafluoride is low, and the method is mainly used for producing and preparing sulfur hexafluoride in industry. Meanwhile, the fluorine gas is extremely toxic, and is strongly corroded and oxidized, so that the production process has high risk; fluorine gas has a limited purity, and it is difficult to prepare high-purity sulfur tetrafluoride.
The second method for producing sulfur tetrafluoride is to react iodine pentafluoride with liquid elemental sulfur to generate sulfur tetrafluoride and elemental iodine;
5S+4IF5＝5SF4+2I2
in the method, the sublimation and condensation of the raw material sulfur and the byproduct iodine simple substance are easy to cause the blockage of pipelines, valves and the like, and are not beneficial to the industrialized continuous production. The purity of the raw material iodine pentafluoride is usually 99%, and the purity is limited, so that the high-purity sulfur tetrafluoride cannot be prepared by the method.
In conclusion, the existing preparation method for industrially producing sulfur tetrafluoride mainly has the problems of low selectivity, easy blockage of pipelines and valves by reactants or products, discontinuous production process and the like, high safety risk of the production process, limited purity of sulfur tetrafluoride products and the like.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a reaction process for preparing high-purity sulfur tetrafluoride, which solves the problems mentioned in the background art.
In order to solve the technical problems, the invention adopts the technical scheme that: a reaction device for preparing high-purity sulfur tetrafluoride comprises a fluorination reactor, a reaction cold trap, a rectifying tower and a sulfur tetrafluoride storage tank;
the fluorination reactor is provided with a first connecting pipeline and a sulfur liquid inlet pipeline which are communicated with the interior of the fluorination reactor, and the upper end of the fluorination reactor is communicated with the reaction cold trap through a second connecting pipeline;
the reaction cold trap is provided with a vacuum pipeline and a process gas outlet pipeline, the other end of the process gas outlet pipeline is communicated with the middle part of the rectifying tower, the top of the rectifying tower is connected with a high-purity sulfur tetrafluoride gas outlet pipeline, and the other end of the high-purity sulfur tetrafluoride gas outlet pipeline is communicated with a sulfur tetrafluoride storage tank.
Furthermore, the other end of the first connecting pipeline is communicated with a preheater, and the preheater is communicated with a nitrogen trifluoride pipeline.
Furthermore, a heat exchanger is arranged at the top end of the fluorination reactor, and the second connecting pipeline is communicated with the outlet end of the heat exchanger.
Furthermore, a vacuum pump is installed at the outlet end of the vacuum pipeline.
Further, the fluorination reactor is a tank reactor.
Further, the preheater and the fluorination reactor are made of Monel alloy, and the reaction cold trap, the rectifying tower and the sulfur tetrafluoride storage tank are made of stainless steel.
Furthermore, the first connecting pipeline, the second connecting pipeline, the process gas outlet pipeline and the high-purity sulfur tetrafluoride gas outlet pipeline are all made of stainless steel or hastelloy.
A reaction process of reaction equipment for preparing high-purity sulfur tetrafluoride comprises the following steps:
s1, firstly, conveying nitrogen trifluoride to a preheater through a nitrogen trifluoride pipeline, preheating to 150-350 ℃, and introducing into a fluorination reactor;
s2, synchronously introducing molten sulfur into the fluorination reactor through a sulfur liquid inlet pipeline for reaction to obtain a first product;
s3, conveying the first product to a reaction cold trap through a second connecting pipeline for treatment to obtain a second product;
and S4, conveying the second product to a rectifying tower through a process gas outlet pipeline for separation, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower through a high-purity sulfur tetrafluoride gas outlet pipeline, and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank.
Further, in S1, the purity of nitrogen trifluoride is not less than 99.99%, the reaction temperature of nitrogen trifluoride and molten sulfur in the fluorination reactor is 300-400 ℃, and the reaction pressure is 0-0.5 MPa.
Furthermore, the rectification parameters of the rectification tower are-38 to-5 ℃ at a pressure of 0.01 to 0.3 MPa.
Compared with the prior art, the invention has the following advantages:
1. the method for preparing sulfur tetrafluoride takes nitrogen trifluoride as a fluorinating agent, so that the safety risk of raw materials is reduced, and the process method is safer and more suitable for industrialization.
2. The method for preparing sulfur tetrafluoride takes nitrogen trifluoride as a fluorinating agent, and avoids the problem of blockage of pipelines and valves caused by the processes of sublimation and condensation of solids in products.
3. According to the method for preparing the sulfur tetrafluoride, the raw material nitrogen trifluoride is a high-purity product, is low in price and easy to obtain, and the high-purity sulfur tetrafluoride can be obtained after the sulfur tetrafluoride prepared by reacting with sulfur is simply rectified.
4. The process device adopts a special tank reactor to replace the traditional tubular reactor, the sublimed sulfur in the reactor is condensed at the lower part of an upper heat exchanger of the reactor, and the heat exchanger is heated to melt the condensed sulfur and return the melted sulfur to the reactor; after the reaction, no solid matter exists in the gas outlet pipeline, so that the problem of blockage of subsequent pipelines and valves is avoided, and the process for producing the sulfur tetrafluoride is more stable.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
1-nitrogen trifluoride pipeline, 2-preheater, 3-first connecting pipeline, 4-fluorination reactor, 5-sulfur liquid inlet pipeline, 6-heat exchanger, 7-second connecting pipeline, 8-reaction cold trap, 9-vacuum pipeline, 10-vacuum pump, 11-process gas outlet pipeline, 12-rectifying tower, 13-high-purity sulfur tetrafluoride gas outlet pipeline and 14-sulfur tetrafluoride storage tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Embodiment 1, as shown in fig. 1, the present invention provides a technical solution: a reaction device for preparing high-purity sulfur tetrafluoride comprises a fluorination reactor 4, a reaction cold trap 8, a rectifying tower 12 and a sulfur tetrafluoride storage tank 14;
be provided with on the fluorination reactor 4 with the inside first connecting tube 3 and the sulphur inlet conduit 5 of intercommunication of fluorination reactor 4, the 3 other ends of first connecting tube intercommunication have preheater 2, preheater 2 and nitrogen trifluoride pipeline 1 intercommunication.
The top end of the fluorination reactor 4 is also provided with a heat exchanger 6, and the second connecting pipeline 7 is communicated with the outlet end of the heat exchanger 6 and is communicated with a reaction cold trap 8 through the second connecting pipeline 7;
the reaction cold trap 8 is provided with a vacuum pipeline 9 and a process gas outlet pipeline 11, the outlet end of the vacuum pipeline 9 is provided with a vacuum pump 10, the other end of the process gas outlet pipeline 11 is communicated with the middle of a rectifying tower 12, the top of the rectifying tower 12 is connected with a high-purity sulfur tetrafluoride gas outlet pipeline 13, and the other end of the high-purity sulfur tetrafluoride gas outlet pipeline 13 is communicated with a sulfur tetrafluoride storage tank 14.
The fluorination reactor 4 is a tank reactor, the preheater 2 and the fluorination reactor 4 are made of Monel alloy, the reaction cold trap 8, the rectifying tower 12 and the sulfur tetrafluoride storage tank 14 are made of stainless steel, and the first connecting pipeline 3, the second connecting pipeline 7, the process gas outlet pipeline 11 and the high-purity sulfur tetrafluoride gas outlet pipeline 13 are made of stainless steel or Hastelloy alloy.
When in use, the vacuum pump 10 is firstly used for carrying out vacuum-pumping pretreatment on the components; then purging and replacing residual air and moisture in the system by using high-purity nitrogen trifluoride gas; then liquid sulfur is input into the fluorination reactor 4 through a sulfur liquid inlet pipeline 5; introducing high-purity nitrogen trifluoride into a preheater 2, introducing the preheated nitrogen trifluoride into a fluorination reactor 4 through a first connecting pipeline 3 for reaction, controlling the temperature of the fluorination reactor at 300-400 ℃, and controlling the reaction pressure at 0-0.5 MPa; the reacted gas enters a reaction cold trap 8, low-temperature liquid/solidified sulfur tetrafluoride, and light gas discharged in vacuum is sent to a tail gas treatment system, and is discharged after harmless treatment; after the vacuum light emission, the sulfur tetrafluoride is vaporized and transferred into a rectifying tower 12 for rectification to obtain high-purity sulfur tetrafluoride, and the high-purity sulfur tetrafluoride is sent to a sulfur tetrafluoride storage tank 14.
s1, firstly, sending nitrogen trifluoride to a preheater 2 through a nitrogen trifluoride pipeline 1, preheating to 150 ℃, and then introducing into a fluorination reactor 4;
s2, synchronously introducing molten sulfur into a fluorination reactor 4 through a sulfur liquid inlet pipeline 5 for reaction, setting the operation temperature of the fluorination reactor at 300 ℃ and the operation pressure at 0, and introducing nitrogen trifluoride gas for reaction to obtain a first product;
s3, conveying the first product to a reaction cold trap 8 through a second connecting pipeline 7 for treatment, setting the operation temperature of the cold trap at-150 ℃ and the operation pressure at-0.09 MPa, cooling and solidifying the first product, conveying the unliquefied gas impurities to a tail gas treatment system through a vacuum pipeline 9, and emptying after harmless treatment; the liquid/solidified product is vaporized at-20 ℃ and-0.01 MPa to obtain a product, and a second product is obtained after the product is processed;
and S4, sending the second product to a rectifying tower 12 through a process gas outlet pipeline 11 for separation, setting the operating temperature of the rectifying tower at-38 ℃ and the operating pressure at 0.01MPa, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower 12 through a high-purity sulfur tetrafluoride outlet pipeline 13, and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank 14.
The purity of the sulfur tetrafluoride collected in the storage tank is 99.91 percent through analysis, and the purity of the electronic-grade sulfur tetrafluoride is achieved, wherein the content of sulfur hexafluoride is 500ppm, and the content of nitrogen is 70 ppm.
s1, firstly, sending nitrogen trifluoride to a preheater 2 through a nitrogen trifluoride pipeline 1, preheating to 200 ℃, and then introducing into a fluorination reactor 4;
s2, synchronously introducing molten sulfur into a fluorination reactor 4 through a sulfur liquid inlet pipeline 5 for reaction, setting the operation temperature of the fluorination reactor 4 at 325 ℃ and the operation pressure at 0.1MPa, and introducing nitrogen trifluoride gas for reaction to obtain a first product;
s3, conveying the first product to a reaction cold trap 8 through a second connecting pipeline 7 for treatment, setting the operation temperature of the cold trap at-130 ℃ and the operation pressure at-0.01 MPa, cooling, liquid/solidifying the first product, conveying the unliquefied gas impurities to a tail gas treatment system through a vacuum pipeline 9, and emptying after harmless treatment; vaporizing the liquid/cured product at-5 ℃ and 0MPa to obtain a product, and processing the product to obtain a second product;
and S4, sending the second product to a rectifying tower 12 through a process gas outlet pipeline 11 for separation, setting the temperature of the rectifying tower at-30 ℃, the operating pressure at 0.05MPa, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower 12 through a high-purity sulfur tetrafluoride outlet pipeline 13, and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank 14.
The purity of the sulfur tetrafluoride collected in the storage tank is 99.93 percent through analysis, and the purity of the electronic-grade sulfur tetrafluoride is achieved, wherein the content of sulfur hexafluoride is 415ppm, and the content of nitrogen is 66 ppm.
s1, firstly, sending nitrogen trifluoride to a preheater 2 through a nitrogen trifluoride pipeline 1, preheating to 250 ℃, and then introducing into a fluorination reactor 4;
s2, synchronously introducing molten sulfur into a fluorination reactor 4 through a sulfur liquid inlet pipeline 5 for reaction, setting the operating temperature of the fluorination reactor 4 at 350 ℃ and the operating pressure at 0.2MPa, and introducing nitrogen trifluoride gas for reaction to obtain a first product;
s3, conveying the first product to a reaction cold trap 8 through a second connecting pipeline 7 for treatment, setting the operation temperature of the cold trap at-110 ℃ and the operation pressure at 0, cooling and solidifying the first product, conveying the unliquefied gas impurities to a tail gas treatment system through a vacuum pipeline 9, and emptying after harmless treatment; vaporizing the liquid/solidified product at 10 ℃ and 0.1MPa to obtain a product, and processing the product to obtain a second product;
and S4, sending the second product to a rectifying tower 12 through a process gas outlet pipeline 11 for separation, setting the operating temperature of the rectifying tower at-20 ℃ and the operating pressure at 0.1MPa, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower 12 through a high-purity sulfur tetrafluoride outlet pipeline 13, and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank 14.
The purity of the sulfur tetrafluoride collected in the storage tank is 99.96 percent by analysis, and the purity of the electronic-grade sulfur tetrafluoride is achieved, wherein the content of sulfur hexafluoride is 260ppm, and the content of nitrogen is 25 ppm.
Embodiment 5, a reaction process of a reaction apparatus for preparing high-purity sulfur tetrafluoride, comprising the steps of:
s1, firstly, sending nitrogen trifluoride to a preheater 2 through a nitrogen trifluoride pipeline 1, preheating to 300 ℃, and then introducing into a fluorination reactor 4;
s2, synchronously introducing molten sulfur into a fluorination reactor 4 through a sulfur liquid inlet pipeline 5 for reaction, setting the operation temperature of the fluorination reactor 4 at 375 ℃ and the operation pressure at 0.3MPa, and introducing nitrogen trifluoride gas for reaction to obtain a first product;
s3, conveying the first product to a reaction cold trap 8 through a second connecting pipeline 7 for treatment, setting the operation temperature of the cold trap at-10 ℃ and the operation pressure at 0.2MPa, cooling and solidifying the first product, conveying the non-liquefied gas impurities to a tail gas treatment system through a vacuum pipeline 9, and emptying after harmless treatment; vaporizing the liquid/solidified product at 25 ℃ and 0.2MPa to obtain a product, and processing the product to obtain a second product;
and S4, sending the second product to a rectifying tower 12 through a process gas outlet pipeline 11 for separation, setting the operating temperature of the rectifying tower at-10 ℃ and the operating pressure at 0.2MPa, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower 12 through a high-purity sulfur tetrafluoride outlet pipeline 13, and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank 14.
The purity of the sulfur tetrafluoride collected in the storage tank is 99.94 percent by analysis, and the purity of the electronic-grade sulfur tetrafluoride is achieved, wherein the content of sulfur hexafluoride is 402ppm, and the content of nitrogen is 30 ppm.
Example 6, a reaction process of a reaction apparatus for preparing high-purity sulfur tetrafluoride, comprising the steps of:
s1, firstly, sending nitrogen trifluoride to a preheater 2 through a nitrogen trifluoride pipeline 1, preheating to 350 ℃, and then introducing into a fluorination reactor 4;
s2, synchronously introducing molten sulfur into a fluorination reactor 4 through a sulfur liquid inlet pipeline 5 for reaction, setting the operating temperature of the fluorination reactor 4 at 400 ℃ and the operating pressure at 0.5MPa, and introducing nitrogen trifluoride gas for reaction to obtain a first product;
s3, conveying the first product to a reaction cold trap 8 through a second connecting pipeline 7 for treatment, setting the operation temperature of the cold trap at-70 ℃ and the operation pressure at 0.2MPa, cooling and solidifying the first product, conveying the non-liquefied gas impurities to a tail gas treatment system through a vacuum pipeline 9, and emptying after harmless treatment; the liquid/solidified product is vaporized at 40 ℃ and 0.3MPa to obtain a product, and a second product is obtained after the product is processed;
and S4, sending the second product to a rectifying tower 12 through a process gas outlet pipeline 11 for separation, setting the operating temperature of the rectifying tower at-5 ℃ and the operating pressure at 0.3MPa, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower 12 through a high-purity sulfur tetrafluoride outlet pipeline 13, and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank 14.
The purity of the sulfur tetrafluoride collected in the storage tank is 99.92 percent through analysis, and the purity of the electronic-grade sulfur tetrafluoride is achieved, wherein the content of sulfur hexafluoride is 610ppm, and the content of nitrogen is 60 ppm.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The reaction equipment for preparing the high-purity sulfur tetrafluoride is characterized by comprising a fluorination reactor (4), a reaction cold trap (8), a rectifying tower (12) and a sulfur tetrafluoride storage tank (14);
the fluorination reactor (4) is provided with a first connecting pipeline (3) and a sulfur liquid inlet pipeline (5) which are communicated with the interior of the fluorination reactor (4), and the upper end of the fluorination reactor (4) is communicated with a reaction cold trap (8) through a second connecting pipeline (7);
the reaction cold trap (8) is provided with a vacuum pipeline (9) and a process gas outlet pipeline (11), the other end of the process gas outlet pipeline (11) is communicated with the middle of a rectifying tower (12), the top of the rectifying tower (12) is connected with a high-purity sulfur tetrafluoride gas outlet pipeline (13), and the other end of the high-purity sulfur tetrafluoride gas outlet pipeline (13) is communicated with a sulfur tetrafluoride storage tank (14).
2. The reaction apparatus for preparing high-purity sulfur tetrafluoride according to claim 1, wherein the other end of the first connecting line (3) is connected to a preheater (2), and the preheater (2) is connected to a nitrogen trifluoride line (1).
3. The reaction equipment for preparing high-purity sulfur tetrafluoride according to claim 1, wherein a heat exchanger (6) is further arranged at the top end of the fluorination reactor (4), and the second connecting pipeline (7) is communicated with the outlet end of the heat exchanger (6).
4. The reaction apparatus for preparing high purity sulfur tetrafluoride according to claim 1, wherein the vacuum line (9) is provided at its outlet end with a vacuum pump (10).
5. The reaction apparatus for preparing high purity sulfur tetrafluoride according to claim 1, wherein the fluorination reactor (4) is a tank reactor.
6. The reaction equipment for preparing high-purity sulfur tetrafluoride according to claim 2, wherein the material of the preheater (2) and the fluorination reactor (4) is monel, and the material of the reaction cold trap (8), the rectifying tower (12) and the sulfur tetrafluoride storage tank (14) is stainless steel.
7. The reaction equipment for preparing high-purity sulfur tetrafluoride according to claim 1, wherein the first connecting pipeline (3), the second connecting pipeline (7), the process gas outlet pipeline (11) and the high-purity sulfur tetrafluoride outlet pipeline (13) are made of stainless steel or hastelloy.
8. The reaction process of the reaction equipment for preparing high-purity sulfur tetrafluoride according to any one of claims 1 to 7, comprising the steps of:
s1, firstly, sending nitrogen trifluoride to a preheater (2) through a nitrogen trifluoride pipeline (1), preheating to 150-350 ℃, and then introducing into a fluorination reactor (4);
s2, synchronously introducing molten sulfur into a fluorination reactor (4) through a sulfur liquid inlet pipeline (5) for reaction to obtain a first product;
s3, sending the first product to a reaction cold trap (8) through a second connecting pipeline (7) for processing to obtain a second product;
s4, sending the second product to a rectifying tower (12) through a process gas outlet pipeline (11) for separation, liquefying the gas-phase high-purity sulfur tetrafluoride obtained at the top of the rectifying tower (12) through a high-purity sulfur tetrafluoride outlet pipeline (13), and storing the liquefied gas-phase high-purity sulfur tetrafluoride in a sulfur tetrafluoride storage tank (14).
9. The reaction process of the reaction equipment for preparing high-purity sulfur tetrafluoride according to claim 8, wherein in S1, the purity of nitrogen trifluoride is not less than 99.99%, the reaction temperature of nitrogen trifluoride and molten sulfur in the fluorination reactor (4) is 300-400 ℃, and the reaction pressure is 0-0.5 MPa.
10. The reaction process of the reaction equipment for preparing high-purity sulfur tetrafluoride according to claim 8, wherein the distillation parameters of the distillation column (12) are-38 ℃ to-5 ℃ and 0.01MPa to 0.3 MPa.
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| CN117339489A (en) * | 2023-10-08 | 2024-01-05 | 湖北工业大学 | Device and method for preparing molybdenum hexafluoride from sulfur hexafluoride |
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| 拉扎列夫等: "《工业生产中的有害物质手册 第3卷》", 31 May 1986, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117339489A (en) * | 2023-10-08 | 2024-01-05 | 湖北工业大学 | Device and method for preparing molybdenum hexafluoride from sulfur hexafluoride |
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