CN1644490A - Continuous production of sulfur tetrafluoride - Google Patents
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- CN1644490A CN1644490A CN 200410100441 CN200410100441A CN1644490A CN 1644490 A CN1644490 A CN 1644490A CN 200410100441 CN200410100441 CN 200410100441 CN 200410100441 A CN200410100441 A CN 200410100441A CN 1644490 A CN1644490 A CN 1644490A
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- QHMQWEPBXSHHLH-UHFFFAOYSA-N sulfur tetrafluoride Chemical compound FS(F)(F)F QHMQWEPBXSHHLH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000010924 continuous production Methods 0.000 title abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 25
- -1 halogen fluoride Chemical class 0.000 claims abstract description 23
- 150000002367 halogens Chemical class 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000011049 filling Methods 0.000 claims abstract description 4
- 239000011593 sulfur Substances 0.000 claims description 38
- 229910052717 sulfur Inorganic materials 0.000 claims description 37
- 229910052731 fluorine Inorganic materials 0.000 claims description 11
- 239000011737 fluorine Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000005192 partition Methods 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 239000012025 fluorinating agent Substances 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- FQFKTKUFHWNTBN-UHFFFAOYSA-N trifluoro-$l^{3}-bromane Chemical compound FBr(F)F FQFKTKUFHWNTBN-UHFFFAOYSA-N 0.000 claims description 3
- CEBDXRXVGUQZJK-UHFFFAOYSA-N 2-methyl-1-benzofuran-7-carboxylic acid Chemical compound C1=CC(C(O)=O)=C2OC(C)=CC2=C1 CEBDXRXVGUQZJK-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 230000001502 supplementing effect Effects 0.000 claims 1
- 241001313207 Gonepteryx rhamni Species 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 229910018503 SF6 Inorganic materials 0.000 description 7
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 6
- 239000011630 iodine Substances 0.000 description 6
- 229910052740 iodine Inorganic materials 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 5
- 229960000909 sulfur hexafluoride Drugs 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000003682 fluorination reaction Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 3
- 229910014263 BrF3 Inorganic materials 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910018105 SCl2 Inorganic materials 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- TVVNZBSLUREFJN-UHFFFAOYSA-N 2-(4-chlorophenyl)sulfanyl-5-nitrobenzaldehyde Chemical compound O=CC1=CC([N+](=O)[O-])=CC=C1SC1=CC=C(Cl)C=C1 TVVNZBSLUREFJN-UHFFFAOYSA-N 0.000 description 1
- 241001131796 Botaurus stellaris Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- FMSYTQMJOCCCQS-UHFFFAOYSA-L difluoromercury Chemical compound F[Hg]F FMSYTQMJOCCCQS-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- OMRRUNXAWXNVFW-UHFFFAOYSA-N fluoridochlorine Chemical compound ClF OMRRUNXAWXNVFW-UHFFFAOYSA-N 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- XRURPHMPXJDCOO-UHFFFAOYSA-N iodine heptafluoride Chemical compound FI(F)(F)(F)(F)(F)F XRURPHMPXJDCOO-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- FWMUJAIKEJWSSY-UHFFFAOYSA-N sulfur dichloride Chemical compound ClSCl FWMUJAIKEJWSSY-UHFFFAOYSA-N 0.000 description 1
- JMPVZWBJWHQJDD-UHFFFAOYSA-N sulfur tetrachloride Chemical compound ClS(Cl)(Cl)Cl JMPVZWBJWHQJDD-UHFFFAOYSA-N 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 125000005270 trialkylamine group Chemical group 0.000 description 1
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Continuous production of sulfur tetrafluoride is carried out by synthetic reacting, cooling to separate SF4 from halogen, returning and reutilizing halogen, gas-phase purifying, liquefying and filling. The halogen fluoride has synthetic reaction with pure industrial brim stone proportionally in a reactor, with reacting temperature of 110deg.C-500deg.C, reacting pressure 0.1-1.0MPs, the mole ratio of halogen fluoride to S = 4-5:5 and the excess of the halogen fluoride = 0-25%. It achieves low cost, simple process and higher efficiency.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a continuous production method of sulfur tetrafluoride.
Background
Sulfur tetrafluoride is a very specific fluorinating agent with irreplaceable effects on the fluorination of oxygen, sulfur and nitrogen containing genes (U.S. Pat. No. 2,992,073), and has particular utility in the deoxofluorination of aldehydes, ketones and carboxylic acids according to the current data of the largest global sulfur tetrafluoride supplier AIR PRODUCTS ANDCHEMICALS, INC..
At present, sulfur tetrafluoride has several synthesis methods, and the most representative methods are as follows:
1. the synthesis of sulfur tetrafluoride from alkali metal fluorides, chlorine and sulfur containing reactants is taught in U.S. Pat. No. 2,992,073 (1961).
2. U.S. Pat. No. 3,950,498(1976) describes the reaction of sulfur tetrachloride (or a mixture of sulfur dichloride and chlorine) with hydrogen fluoride in a carbon tetrahalide medium.
3. U.S. Pat. No. 3,399,036(1968) and U.S. Pat. No. 2,823276 (1981) describe processes for the production of sulfur tetrafluoride by the reaction of fluorine and sulfur at a carefully controlled temperature, but until now large scale commercial production has not been achieved due to the fact that fluorine and sulfur react too vigorously to be controlled, the temperature is not well controlled, and sulfur hexafluoride or fluoride is produced instead of sulfur tetrafluoride.
4. Japanese ASAHI GLASS co ltd (asahi glass) is also published (u.s.pat No.4,372,938) (1982) by am.nhf and SCl2Preparation of SF by reaction4. Nhf is a complex of HF with an organic amine, Am is often pyridine or trialkylamine, and n is 1-4. The reaction is carried out in a solvent. After reaction SF4Is distilled off under vacuum to obtain by-product S2Cl2Can be re-chlorinated to SCl2The am.hcl can be reprocessed with HF to am.3hf for recycle.
5. Newly published references to SF4The synthesis method is described in U.S. Pat. No. 5,639,435(1997) which uses metal fluorides (AgF, CuF)2，HgF2) Synthetic route to sulfur hexafluoride, SF4Only as intermediates and not as final products. The method has no industrial reports, and the described process steps and reaction modes are too complex and have a large amount of byproducts to be treated.
Currently only AIR PRODUCTS AND CHEMICALS, INC. is in use for SF4The commercial production of (1) has the annual output of only a few tons, the purity of the supplied commodity is not high (94%), andthe impurity in the product is S2F2，SE6，SOF2And is expensive, severely restricting SF4Downstream product development applications.
Disclosure of Invention
Aiming at the problems of the existing sulfur tetrafluoride production method, the invention provides a method for continuously producing sulfur tetrafluoride.
The invention mainly relates to a synthetic method for producing sulfur tetrafluoride gas by using halogen fluoride as fluorinating agent to react with industrial sulfur and application thereof in actual production.
It is believed that the reaction of a halogen fluoride (including bromine trifluoride, bromine pentafluoride, iodine heptafluoride, chlorine monofluoride and chlorine trifluoride) with sulfur will result in the fluorination of sulfur toThe highest price generates sulfur hexafluoride (ISBN 7-5025-0842-2/TQ.487 encyclopedia of chemical engineering, volume five, P74, 1 st edition of 11 months 1993), and multiple scientific experiments show that the sulfur in the reaction is only fluorinated to quadrivalence to generate sulfur tetrafluoride instead of sulfur hexafluoride. Based on this finding, the present invention proposes a novel SF4A continuous process for the production of sulfur from sulfur and fluorine compounds by reacting sulfur with a halogen fluoride at a temperature of from 110 ℃ to 500 ℃ above the upper limit temperature SF4Pyrolysis into SF6. The reaction can be rapidly carried out under certain temperature and pressure conditions, and the used halogen fluoride is bromine trifluoride and iodine pentafluoride. The reaction formula is as follows:
wherein n is 1, 3, 5, 7, which is the valence of halogen and fluorine, and X is one element of chlorine, bromine and iodine.
At IF5For example, the reaction formula is as follows:
reaction of halogen fluoride with sulfur to form SF4The halogen is replaced, the reaction pressure is 0.1-1.0 MPa, and IF is controlled5The molar ratio of S to S is 4-5: 5, fluoride is excessive by 0-25%, and after the obtained product is cooled to solidify and separate iodine, a gas-phase product contains SF except for the product60.2-1.0 percent, the total amount of other impurities can be controlled within 3 percent, and SF4The product can reach 94% without purification. If the sulfur content in the reactants is excessive, the impurities (mainly sulfur subfluoride) in the reaction products are increased.
The method comprises the steps of feeding, reacting, synthesizing, separating gas from liquid or gas from solid by cooling, recycling halogen and excessive fluoride halide, purifying gas phase, liquefying, filling and the like.
Several methods can be used in the feed reaction synthesis step. Starting material of halogen fluoride by IF5For example, the following steps are carried out:
1. the raw materials can be continuously fed according to the proportionFeeding into a reactor, and controlling the reaction temperature to be I2The reaction product is continuously discharged above the boiling point of the iodine, the iodine is solidified and separated from the gas product by a cooling system, the gas enters a purification, liquefaction and filling system, and the iodine is recovered and made into IFagain5Can be recycled.
2. Gaseous IF5The reactor containing sulfur is continuously charged, the sulfur can be continuously supplemented in a liquid state, and the rest is the same as above.
3. A special reactor with a heating device is made, the reactor is divided into a left chamber and a right chamber by a partition plate, and a channel is reserved at the bottom of the partition plate to ensure that liquefied sulfur can pass through. Solid sulphur is continuously fed from the top of the right chamber and kept in a molten state, IF5Continuously injecting into the left chamber, maintaining the reaction temperature above the boiling point of iodine, continuously discharging the reaction product, maintaining the sulfur liquid level higher than the bottom channel of the partition plate, and preventing IF in the left chamber of the reactor5And the reaction product into the right chamber, thus allowing continuous production.
The method for synthesizing the sulfur tetrafluoride has the following advantages: can continuously and efficiently produce high-quality products. Because the raw materials used in the method only consume fluorine element and industrial sulfur actually, fluorine gas is introduced to prepare halogen fluoride again after halogen is recoveredThe raw materials used in the method only consume fluorine element and industrial sulfur actually, and fluorine gas is introduced to prepare halogen fluoride again after halogen is recovered, so the cost is low. Because the process is simple, the equipment investment is reduced, the production can be continuously and efficiently carried out, the production safety is improved, and the number of using operators is reduced. The invention better solves the problems of transportation and storage, and can generate SF on site by using the bittern fluoride and the sulfur which are convenient for safe transportation and storage due to simple reaction and simple and convenient operation4When the fluorinating agent is used, the sulfur and the raw material to be fluorinated can be uniformly mixed according to a reasonable proportion, and then the fluorinating process can be completed by introducing halogen fluoride under certain pressure and temperature. In these methods, the halogen or halide must be separated from the reaction product and recycled.
The production and use of sulfur tetrafluoride may also be further simplified due to the disclosed mechanism of sulfur tetrafluoride formation. Fluorine gas and halogen are firstly used for synthesizing halogen fluoride, and the halogen fluoride is then reacted with sulfur to generate sulfur tetrafluoride. The sulfur tetrafluoride can also be generated by the reaction of fluorine gas and sulfur in the presence of halogen, and in the aspect of sulfur tetrafluoride application, a simplified method is that under the condition of not influencing the chemical reaction property, the fluorine gas and the halogen according to a certain molar ratio, and the sulfur which is uniformly mixed according to a reasonable proportion can be used together with the raw material to be fluorinated under a certain temperature and pressure to complete the fluorination process.
Detailed Description
Example 1: a1.8 liter stainless steel reactor, a top cover and a kettle body are connected by a flange and provided with a vacuum pressure gauge, a thermometer with digital display is inserted into the bottom of the kettle, and the feeding and discharging are controlled by a valve. Firstly, 8 g of sulfur is put into a reactor, a top cover is fixed, then the reactor is vacuumized, and 45 g of liquid IF5The reactor was fed by differential pressure and head through a valve. And closing the valve after vacuumizing again. The reactor was placed in an oil bath and warmed to 300 ℃ for two hours and maintained at this temperature for three hours. Cooling the reactor to 10 deg.C, the pressure gauge shows pressure of 0.22MPa, the gas product is tested by gas chromatograph (Propak Q packed column, TCD detector, both temperatures are 85 deg.C, helium as carrier gas, flow rate of 20ml/min, and 120mA as bridge flow), and the test result is SF491.7% content, 3% air, SF60.20 percent of high boiling point gas S, and the balance of 3.9 percent2F2. 26 g of gas-phase product obtained, SF in sulphur4The yield thereof was found to be about 88.3%. Air is caused by system contamination during the inspection process. When the reactor was opened, white smoke was emitted from the inside, indicating that there was some IF5Not reacted completely, also has a small part of SF4The adhesion to the inner wall of the reactor was not calculated to be within the above yield (due to incomplete evacuation). The iodine displaced is 24 g, IF5The conversion was calculated to be about 94.5%.
Example 2: IF (intermediate frequency) circuit5The usage amount is 50 g (excess 10%), the reactor is quickly heated to 400 ℃ by a heating jacket and then is naturally cooled to 10 ℃, the other conditions are the same as example 1, and the detection result is SF494.4% content, 3% air (also brought in during the detection), SF60.28% of S2F2The content was 2.1%. 27 g of gas-phase product obtained, SF in sulphur4The yield thereof was found to be about 94%. Due to excessive IF5Mixing with the displaced iodine makes it impossible to measure the iodine.
Example 3: BrF352 g of sulfur and 8 g of sulfur are used, the temperature is raised to 250 ℃ by using oil bath, the rest is the same as example 1, 27 g of gas-phase product, 3 percent of air and SF are obtained60.30% of S2F20.19% of SF4SF in sulfur content 94.2%4The yield thereof was found to be about 94%. Due to excess BrF3Mixed with the bromine being displaced, and is not metered in.
Claims (6)
1. A method for continuously producing sulfur tetrafluoride is characterized by comprising a synthetic reaction and separation of SF by cooling4And returning halogen and halogen for reuse, gas-phase purification, liquefaction and filling, wherein the synthetic reaction is to place halogen fluoride and industrial pure sulfur in a reactor according to a proportion for synthetic reaction, the reaction temperature is 110-500 ℃, the reaction pressure is 0.1-1.0 MPa, the molar ratio of the halogen fluoride to S is 4-5: 5, and the halogen fluoride is excessive by 0-25%.
2. The method for continuously producing sulfur tetrafluoride according to claim 1, wherein the halogen fluoride used is bromine trifluoride or iodine pentafluoride.
3. The method for continuously producing sulfur tetrafluoride according to claim 1, wherein the step of the synthesis reaction is performed by:
a. continuously adding the raw materials into a reactor according to the proportion;
b. continuously introducing gaseous halogen fluoride into a reactor filled with sulfur, and continuously supplementing the sulfur in a liquid state;
c. the reactor is provided with a heating device, the reactor is divided into a left chamber and a right chamber by a partition board, a channel is reserved at the bottom of the partition board to enable liquefied sulfur to pass through, solid sulfur is continuously added from the top of the right chamber and keeps a molten state, fluoride halide is continuously injected from the left chamber, and the liquid level of the sulfur is maintained to be higher than the channel at the bottom of the partition board.
4. The method for continuously producing sulfur tetrafluoride according to claim 1, wherein the synthesis reaction step uses a halogen fluoride as a fluorinating agent to react with sulfur and a raw material to be fluorinated when applied on site.
5. The method for continuously producing sulfur tetrafluoride according to claim 1, wherein the step of synthesizing reaction is reacting halogen fluoride with sulfur to form SF when applied on site4Then reacting with the raw materials to be reacted.
6. The method of claim 1, wherein the synthesis reaction is performed in the presence of halogen to directly produce SF from the reaction of fluorine and sulfur4。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101004415A CN1301211C (en) | 2004-12-22 | 2004-12-22 | Continuous production of sulfur tetrafluoride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101004415A CN1301211C (en) | 2004-12-22 | 2004-12-22 | Continuous production of sulfur tetrafluoride |
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| CN1644490A true CN1644490A (en) | 2005-07-27 |
| CN1301211C CN1301211C (en) | 2007-02-21 |
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| CNB2004101004415A Expired - Fee Related CN1301211C (en) | 2004-12-22 | 2004-12-22 | Continuous production of sulfur tetrafluoride |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079509A (en) * | 2011-03-14 | 2011-06-01 | 李学庆 | Automatic control of sulfur tetrafluoride production process |
| CN102107857A (en) * | 2011-03-14 | 2011-06-29 | 李学庆 | Process for purifying and rectifying sulfur tetrafluoride |
| CN102173393A (en) * | 2011-03-14 | 2011-09-07 | 李学庆 | Sulfur tetrafluoride production technique |
| CN102173394A (en) * | 2011-03-14 | 2011-09-07 | 李学庆 | Material recycling technique used during sulfur tetrafluoride production |
| CN109704291A (en) * | 2019-03-01 | 2019-05-03 | 绵阳华鑫瑞建筑劳务有限公司 | A kind of purification rectification process of sulfur tetrafluoride |
| CN110114304A (en) * | 2016-12-26 | 2019-08-09 | 大金工业株式会社 | The manufacturing method of sulfur tetrafluoride |
| CN113353893A (en) * | 2021-06-29 | 2021-09-07 | 鹤壁德瑞科技有限公司 | Sulfur tetrafluoride synthesis method and reaction system |
| CN113371681A (en) * | 2021-06-29 | 2021-09-10 | 鹤壁德瑞科技有限公司 | Purification method and preparation method of high-purity chlorine trifluoride |
| CN114348971A (en) * | 2022-02-17 | 2022-04-15 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method and device of sulfur tetrafluoride |
| CN114405035A (en) * | 2022-02-09 | 2022-04-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Reaction equipment and reaction process for preparing high-purity sulfur tetrafluoride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3399036A (en) * | 1966-04-20 | 1968-08-27 | Air Prod & Chem | Sulfur tetrafluoride |
| DE2363679A1 (en) * | 1973-12-21 | 1975-07-03 | Rolf Prof Dr Appel | PROCESS FOR THE PRODUCTION OF SULFUR TRAFLUORIDE |
| CA1066022A (en) * | 1975-07-02 | 1979-11-13 | Allied Chemical Corporation | Preparation of sulfur fluorides |
| IT1150046B (en) * | 1979-10-12 | 1986-12-10 | Asahi Glass Co Ltd | PROCEDURE FOR THE PRODUCTION OF SULFUR THEATRAFLUORIDE |
| JPS5761604A (en) * | 1980-09-30 | 1982-04-14 | Asahi Glass Co Ltd | Preparation of sulfur tetrafluoride |
| SU971785A1 (en) * | 1981-02-27 | 1982-11-07 | Волгоградский Ордена Трудового Красного Знамени Политехнический Институт | Process for producing sulphur tetrachloride |
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- 2004-12-22 CN CNB2004101004415A patent/CN1301211C/en not_active Expired - Fee Related
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| CN102107857A (en) * | 2011-03-14 | 2011-06-29 | 李学庆 | Process for purifying and rectifying sulfur tetrafluoride |
| CN102173393A (en) * | 2011-03-14 | 2011-09-07 | 李学庆 | Sulfur tetrafluoride production technique |
| CN102173394A (en) * | 2011-03-14 | 2011-09-07 | 李学庆 | Material recycling technique used during sulfur tetrafluoride production |
| CN102107857B (en) * | 2011-03-14 | 2012-05-09 | 李学庆 | Process for purifying and rectifying sulfur tetrafluoride |
| CN102079509B (en) * | 2011-03-14 | 2012-07-04 | 李学庆 | Automatic control of sulfur tetrafluoride production process |
| CN102079509A (en) * | 2011-03-14 | 2011-06-01 | 李学庆 | Automatic control of sulfur tetrafluoride production process |
| CN102173393B (en) * | 2011-03-14 | 2013-01-02 | 李学庆 | Sulfur tetrafluoride production technique |
| US11718524B2 (en) | 2016-12-26 | 2023-08-08 | Daikin Industries, Ltd. | Method for manufacturing sulfur tetrafluoride |
| CN110114304A (en) * | 2016-12-26 | 2019-08-09 | 大金工业株式会社 | The manufacturing method of sulfur tetrafluoride |
| EP3560889A4 (en) * | 2016-12-26 | 2020-07-29 | Daikin Industries, Ltd. | METHOD FOR PRODUCING SULFUR TETRAFLUORIDE |
| TWI735700B (en) * | 2016-12-26 | 2021-08-11 | 日商大金工業股份有限公司 | Manufacturing method of sulfur tetrafluoride |
| US11339052B2 (en) | 2016-12-26 | 2022-05-24 | Daikin Industries, Ltd. | Method for manufacturing sulfur tetrafluoride |
| CN110114304B (en) * | 2016-12-26 | 2023-02-17 | 大金工业株式会社 | Process for producing sulfur tetrafluoride |
| CN109704291A (en) * | 2019-03-01 | 2019-05-03 | 绵阳华鑫瑞建筑劳务有限公司 | A kind of purification rectification process of sulfur tetrafluoride |
| CN113371681A (en) * | 2021-06-29 | 2021-09-10 | 鹤壁德瑞科技有限公司 | Purification method and preparation method of high-purity chlorine trifluoride |
| CN113353893A (en) * | 2021-06-29 | 2021-09-07 | 鹤壁德瑞科技有限公司 | Sulfur tetrafluoride synthesis method and reaction system |
| CN114405035A (en) * | 2022-02-09 | 2022-04-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Reaction equipment and reaction process for preparing high-purity sulfur tetrafluoride |
| CN114348971A (en) * | 2022-02-17 | 2022-04-15 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method and device of sulfur tetrafluoride |
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