CN105693561A - Preparation method of trifluoromethane sulfonic acid - Google Patents
Preparation method of trifluoromethane sulfonic acid Download PDFInfo
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- CN105693561A CN105693561A CN201610155298.2A CN201610155298A CN105693561A CN 105693561 A CN105693561 A CN 105693561A CN 201610155298 A CN201610155298 A CN 201610155298A CN 105693561 A CN105693561 A CN 105693561A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
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Abstract
The invention relates to a preparation method of trifluoromethane sulfonic acid. According to the preparation method, trifluoromethanesulphonyl fluoride and alkali metal hydroxide are subjected to a neutralizing hydrolysis reaction under existence of a fluorine fixing agent, after the reaction is completed, reaction liquid is filtered and dried, and fluorinated methyl sulfonic acid alkali metal salt is obtained; the fluorinated methyl sulfonic acid alkali metal salt and fuming sulphuric acid are subjected to acidizing treatment, then rectification is conducted multiple times, and high-purity trifluoromethane sulfonic acid is obtained. Through improvement of the preparation method, operating flexibility, production efficiency and product stability are improved, the comprehensive yield is raised, product purity can reach 99.90% or above, and the preparation method is suitable for industrial production.
Description
Technical field
The preparation method that present invention relates particularly to a kind of trifluoromethane sulfonic acid。
Background technology
Trifluoromethane sulfonic acid is that one has very by force to proton (H
+
) super organic acid, its trifluoromethane sulfonic acid root (CF
3
SO
3
-
) there is extremely strong thermodynamics and chemical stability, even if without there is dissociating of C-F key under the effect of strong nucleopilic reagent, trifluoromethane sulfonic acid has application widely in the fields such as Industrial Catalysis, organic synthesis, bio-pharmaceuticals, high performance material, new forms of energy。
Current Simons electrofluorination is at present by methyl (CH
3
-
) synthesis trifluoromethyl (CF
3
-
) maximally effective industrialization process route, it is with methylsufonyl chloride or methanesulfonyl fluoride for raw material, anhydrous liquid hydrogen fluoride carries out electrolytic synthesis trimethyl fluoride sulfonyl fluorine, then alkali metal aqueous solution is used to absorb, carrying out acidifying with concentrated sulphuric acid again and obtain crude product trifluoromethane sulfonic acid, further rectification obtains high-purity trifluoromethane sulfonic acid。Compared to patent CN102911087A and CN104725283A, this synthetic route does not use organic solvent, nodeless mesh technique yet, has the advantages that safety is high。And the potassium fluoride produced from trimethyl fluoride sulfonyl fluoro one-tenth trifluoromethane sulfonic acid aqueous solution of alkali metal salt process in patent CN101885691A can ionize substantial amounts of fluorion, fluorion is the basic reason of etching apparatus, the mode adopting crystallization in this patent processes, the complexity of the technique increased, crystallization processes is limited to the removal ability of potassium fluoride simultaneously；And the potassium fluoride remained is serious to equipment corrosion equally in the acidification technique stage, and the fluohydric acid gas formed in acidization enters follow-up workshop section and causes fluorion in product higher, reduces product stability and quality；Simply using concentrated sulphuric acid in this patent and trifluoromethane sulfonic acid alkali metal salt is carried out acidifying, its water content is up to 2% ~ 5%, and moisture content is higher is cause another principal element that product stability is poor, equipment corrosion is serious。
Summary of the invention
The preparation method that the technical problem to be solved is to provide a kind of trifluoromethane sulfonic acid that the corrosivity to equipment is little and product stability is high。
For reaching above-mentioned purpose, the technical solution used in the present invention is:
The preparation method of a kind of trifluoromethane sulfonic acid, it comprises the steps:
Step (1), by trimethyl fluoride sulfonyl fluorine and alkali metal hydroxide under the existence of fluorine fixing material, be neutralized hydrolysis, after react, reactant liquor obtains trifluoromethane sulfonic acid alkali metal salt through filtering, drying；
Step (2), trifluoromethane sulfonic acid alkali metal salt step (1) prepared carry out acidification with oleum, then obtain highly purified trifluoromethane sulfonic acid through repeatedly rectification。
Preferably, in step (1), described alkali metal hydroxide is one or more in Lithium hydrate, sodium hydroxide, potassium hydroxide。
It is further preferred that in step (1), described alkali metal hydroxide is sodium hydroxide or potassium hydroxide。
Most preferably, in step (1), described alkali metal hydroxide is potassium hydroxide。
Preferably, in step (1), described alkali metal hydroxide feeds intake with the form of alkali metal hydroxide aqueous solution, and the mass concentration of described alkali metal hydroxide aqueous solution is 10 ~ 50%。
Preferably, in step (1), described fluorine fixing material is one or more the combination in calcium hydroxide, calcium oxide, calcium carbonate。
It is further preferred that in step (1), described fluorine fixing material is calcium hydroxide or calcium oxide。
Most preferably, in step (1), described fluorine fixing material is calcium hydroxide。
Preferably, in step (1), the molar ratio of described trimethyl fluoride sulfonyl fluorine and described alkali metal hydroxide is 1:1 ~ 1.1。
It is further preferred that in step (1), the molar ratio of described trimethyl fluoride sulfonyl fluorine and described alkali metal hydroxide is 1:1.08 ~ 1.09。
Preferably, in step (1), molar ratio 1:0.8 ~ 2 of described alkali metal hydroxide and described fluorine fixing material。
Preferably, in step (1), under the pressure of 0.2 ~ 1.0MPa, at the temperature of 70 ~ 120 DEG C, carry out described neutralizing hydrolysis reaction。
Preferably, in step (1), described trimethyl fluoride sulfonyl fluorine passes in gaseous form, and the speed that passes into of described trimethyl fluoride sulfonyl fluorine is 240 ~ 350g/h。
Preferably, in step (2), the mass ratio that feeds intake of described trifluoromethane sulfonic acid alkali metal salt and described oleum is 1:0.9 ~ 1:2。
It is further preferred that in step (2), the mass ratio that feeds intake of described trifluoromethane sulfonic acid alkali metal salt and described oleum is 1:1。
Preferably, in step (2), the mass concentration of described oleum is 105% ~ 114%。
Specifically, the concrete operations of the preparation method of described trifluoromethane sulfonic acid are:
Step (1), alkali metal hydroxide aqueous solution, fluorine fixing material are joined in reactor, it is warming up to 70 ~ 120 DEG C, mix and blend 1 ~ 3h, then passes to trimethyl fluoride sulfonyl fluorine gas, and control reaction pressure is 0.2 ~ 1.0MPa, after ventilation terminates, insulation reaction 1 ~ 3h, is then cooled to 10 ~ 30 DEG C, is filtered by reactant liquor, obtain trifluoromethane sulfonic acid aqueous solution of alkali metal salt, described trifluoromethane sulfonic acid aqueous solution of alkali metal salt is evaporated and obtains trifluoromethane sulfonic acid alkali metal salt；
Step (2), trifluoromethane sulfonic acid alkali metal salt step (1) prepared carry out acidification with oleum, then carry out first time rectification and obtain trifluoromethane sulfonic acid crude product, described trifluoromethane sulfonic acid crude product is carried out second time rectification and obtains highly purified trifluoromethane sulfonic acid。
Owing to technique scheme is used, the present invention compared with prior art has the advantage that
Fluorine fixing material in the present invention can effective fluorine removal, make within course of reaction, fluorion is reduced to 20ppm, it is possible to effectively reduce the fluorion corrosion to equipment；The present invention use oleum carry out acidifying, sulfur trioxide in oleum can react generation sulphuric acid by the moisture content rapidly and in trifluoromethane sulfonic acid slaine, reduce the dry requirement that dewaters to trifluoromethane sulfonic acid slaine, it also is able to reduce the equipment corrosion that moisture content causes, it is possible to be greatly prolonged the service life of reactor simultaneously；Additionally, the present invention is by the improvement to preparation method, improve operating flexibility, production efficiency, product stability and comprehensive yield, product purity, up to more than 99.90%, is suitable for industrialized production。
Detailed description of the invention
The reaction scheme of the present invention is as follows:
Below in conjunction with embodiment, technical solutions according to the invention being elaborated, in the present invention, unexplained operational approach is conventional method, and unexplained reaction condition is normal condition, and unexplained % is mass percent。
Embodiment 1
304 stainless steel cauldrons are sequentially added into the potassium hydroxide aqueous solution that 793g concentration is 49.4%, 560g calcium hydroxide and 774g high purity water, are warming up to 70 DEG C, mix and blend 2 hours；Then quantitative continuous passes into trimethyl fluoride sulfonyl fluorine gas, and controlling reaction pressure is between 0.2MPa ~ 1.0MPa；When ventilation quality stops ventilation, duration of ventilation 3 hours, then insulation reaction 2 hours after being 980g trimethyl fluoride sulfonyl fluorine, it is cooled to 25 DEG C subsequently；Being filtered by above-mentioned reactant liquor, obtain trifluoromethane sulfonic acid aqueous solutions of potassium, the concentration of trifluoromethane sulfonic acid potassium is 46.81%, pH=14, F
-
=5ppm, ICP detect: Fe:0.5ppm, Ni:0.1ppm。< < < 1ppm, this illustrates that 304 rustless steels are not corroded by this reaction to fluorinion concentration, and this method greatly reduces the corrosivity of equipment, it is possible to be greatly prolonged service life and the maintenance cost of equipment for 1ppm, Ni for 10ppm, Fe。
Undertaken being evaporated by the aqueous solution of above-mentioned trifluoromethane sulfonic acid potassium and obtain trifluoromethane sulfonic acid potassium 1201g, moisture content 10000ppm, F
-
=8ppm；105% oleum being subsequently adding 1201g carries out acidification；The trifluoromethane sulfonic acid potassium of acidifying is carried out rectification in 316L rustless steel rectifying column, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F
-
=3ppm, Fe=0.01ppm, Ni=0.01ppm, purity is 99.0%, yield 98%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out secondary rectification and obtains high-purity trifluoromethane sulfonic acid product, F
-
=1ppm, ICP measure: K=0.1ppm, Na=0.09ppm, Fe=0.01ppm, Ca do not detect, and Pb does not detect, Ni=0.01ppm, Cu do not detect, and Zn does not detect, Al does not detect, Cr=0.08ppm, and purity is 99.98%, comprehensive yield 95%, therefore the method illustrates that the stainless steel equipment of 316L is corroded low by it, can permanently effective run, equipment operating cost is low, and product purity and stability are high, are suitable for industrialized production。
Embodiment 2
304 stainless steel cauldrons are sequentially added into the potassium hydroxide aqueous solution that 793g concentration is 49.4%, 434g calcium hydroxide and 774g high purity water, are warming up to 70 DEG C, mix and blend 2 hours；Then quantitative continuous passes into trimethyl fluoride sulfonyl fluorine gas, and controlling reaction pressure is between 0.2MPa ~ 1.0MPa；When ventilation quality stops ventilation, duration of ventilation 3 hours, then insulation reaction 2 hours after being 980g trimethyl fluoride sulfonyl fluorine, it is cooled to 25 DEG C subsequently；Being filtered by above-mentioned reactant liquor, obtain trifluoromethane sulfonic acid aqueous solutions of potassium, the concentration of trifluoromethane sulfonic acid potassium is 48.74%, pH=14, F
-
=4ppm, ICP detect: Fe:0.4ppm, Ni:0.09ppm。< < < 1ppm, this illustrates that 304 rustless steels are not corroded by this reaction to fluorinion concentration, and this method greatly reduces the corrosivity of equipment, it is possible to be greatly prolonged service life and the maintenance cost of equipment for 1ppm, Ni for 10ppm, Fe。
Undertaken being evaporated by the aqueous solution of above-mentioned trifluoromethane sulfonic acid potassium and obtain trifluoromethane sulfonic acid potassium 1210g, moisture content 8000ppm, F
-
=9ppm；114% oleum being subsequently adding 1210g carries out acidification；The trifluoromethane sulfonic acid potassium of acidifying is carried out rectification in 316L rustless steel rectifying column, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F
-
=2.5ppm, Fe=0.09ppm, Ni=0.1ppm, purity is 99.1%, yield 97.5%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out secondary rectification and obtains high-purity trifluoromethane sulfonic acid product, F
-
=1.2ppm, ICP measure: K=0.09ppm, Na=0.08ppm, Fe=0.01ppm, Ca do not detect, and Pb does not detect, Ni=0.01ppm, Cu do not detect, and Zn does not detect, Al does not detect, Cr=0.09ppm, and purity is 99.99%, comprehensive yield 95.8%, therefore the method illustrates that the stainless steel equipment of 316L is corroded low by it, can permanently effective run, equipment operating cost is low, and product stability is high, is suitable for industrialized production。
Embodiment 3
316L stainless steel cauldron is sequentially added into the sodium hydrate aqueous solution that 875g concentration is 32.0%, 424g calcium oxide and 580g high purity water, is warming up to 85 DEG C, mix and blend 3 hours；Then quantitative continuous passes into trimethyl fluoride sulfonyl fluorine gas, and controlling reaction pressure is between 0.2MPa ~ 1.0MPa；When ventilation quality stops ventilation, duration of ventilation 4 hours, then insulation reaction 2.5 hours after being 980g trimethyl fluoride sulfonyl fluorine, it is cooled to 25 DEG C subsequently；Being filtered by above-mentioned reactant liquor, obtain trifluoromethyl sulfonate aqueous solution, the concentration of trifluoromethyl sulfonate is 47.55%, pH=14, F
-
=7ppm, ICP detect: Fe:0.5ppm, Ni:0.14ppm。< < < 1ppm, this illustrates that 316L rustless steel is not corroded by this reaction to fluorinion concentration, and this method greatly reduces the corrosivity of equipment, it is possible to be greatly prolonged service life and the maintenance cost of equipment for 1ppm, Ni for 10ppm, Fe。
Undertaken being evaporated by the aqueous solution of above-mentioned trifluoromethyl sulfonate and obtain trifluoromethyl sulfonate 1100g, moisture content 9200ppm, F
-
=15ppm；105% oleum being subsequently adding 1100g carries out acidification；The trifluoromethyl sulfonate of acidifying is carried out rectification in 316L rustless steel rectifying column, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F
-
=3.1ppm, Fe=0.08ppm, Ni=0.08ppm, purity is 99.3%, yield 97.1%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out secondary rectification and obtains high-purity trifluoromethane sulfonic acid product, F
-
=1.0ppm, ICP measure: K=0.02ppm, Na=0.04ppm, Fe=0.01ppm, Ca do not detect, and Pb does not detect, Ni=0.02ppm, Cu do not detect, and Zn does not detect, Al does not detect, Cr=0.04ppm, and purity is 99.99%, comprehensive yield 95.2%, therefore the method illustrates that the stainless steel equipment of 316L is corroded low by it, can permanently effective run, equipment operating cost is low, and product stability is high, is suitable for industrialized production。
Embodiment 4
316L stainless steel cauldron is sequentially added into the lithium hydroxide aqueous solution that 1678g concentration is 10.0%, 424g calcium oxide, is warming up to 85 DEG C, mix and blend 3 hours；Then quantitative continuous passes into trimethyl fluoride sulfonyl fluorine gas, and controlling reaction pressure is between 0.2MPa ~ 1.0MPa；When ventilation quality stops ventilation, duration of ventilation 3.5 hours, then insulation reaction 3 hours after being 980g trimethyl fluoride sulfonyl fluorine, it is cooled to 25 DEG C subsequently；Being filtered by above-mentioned reactant liquor, obtain trifluoromethyl sulfonic acid lithium aqueous solution, the concentration of trifluoromethyl sulfonic acid lithium is 40.05%, pH=14, F
-
=5ppm, ICP detect: Fe:0.3ppm, Ni:0.12ppm。< < < 1ppm, this illustrates that 316L rustless steel is not corroded by this reaction to fluorinion concentration, and this method greatly reduces the corrosivity of equipment, it is possible to be greatly prolonged service life and the maintenance cost of equipment for 1ppm, Ni for 10ppm, Fe。
Undertaken being evaporated by the aqueous solution of above-mentioned trifluoromethyl sulfonic acid lithium and obtain trifluoromethyl sulfonic acid lithium 1001g, moisture content 10000ppm, F
-
=11ppm；105% oleum being subsequently adding 1001g carries out acidification；The trifluoromethyl sulfonic acid lithium of acidifying is carried out rectification in 316L rustless steel rectifying column, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F
-
=1.1ppm, Fe=0.04ppm, Ni=0.02ppm, purity is 99.6%, yield 96.8%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out secondary rectification and obtains high-purity trifluoromethane sulfonic acid product, F
-
=0.8ppm, ICP measure: K=0.01ppm, Na=0.05ppm, Fe=0.02ppm, Ca do not detect, and Pb does not detect, Ni=0.02ppm, Cu do not detect, and Zn does not detect, Al does not detect, Cr=0.04ppm, and purity is 99.98%, comprehensive yield 96.2%, therefore the method illustrates that the stainless steel equipment of 316L is corroded low by it, can permanently effective run, equipment operating cost is low, and product stability is high, is suitable for industrialized production。
Embodiment 5
316L stainless steel cauldron is sequentially added into the sodium hydrate aqueous solution that 875g concentration is 32.0%, 757g calcium oxide and 580g high purity water, is warming up to 95 DEG C, mix and blend 3 hours；Then quantitative continuous passes into trimethyl fluoride sulfonyl fluorine gas, and controlling reaction pressure is between 0.2MPa ~ 1.0MPa；When ventilation quality stops ventilation, duration of ventilation 4 hours, then insulation reaction 2.5 hours after being 980g trimethyl fluoride sulfonyl fluorine, it is cooled to 25 DEG C subsequently；Being filtered by above-mentioned reactant liquor, obtain trifluoromethyl sulfonate aqueous solution, the concentration of trifluoromethyl sulfonate is 47.0%, pH=14, F
-
=4ppm, ICP detect: Fe:0.8ppm, Ni:0.16ppm。< < < 1ppm, this illustrates that 316L rustless steel is not corroded by this reaction to fluorinion concentration, and this method greatly reduces the corrosivity of equipment, it is possible to be greatly prolonged service life and the maintenance cost of equipment for 1ppm, Ni for 10ppm, Fe。
Undertaken being evaporated by the aqueous solution of above-mentioned trifluoromethyl sulfonate and obtain trifluoromethyl sulfonate 1100g, moisture content 7800ppm, F
-
=11ppm；105% oleum being subsequently adding 1100g carries out acidification；The trifluoromethyl sulfonate of acidifying is carried out rectification in 316L rustless steel rectifying column, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F
-
=2.5ppm, Fe=0.04ppm, Ni=0.07ppm, purity is 99.4%, yield 96.9%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out secondary rectification and obtains high-purity trifluoromethane sulfonic acid product, F
-
=1.7ppm, ICP measure: K=0.02ppm, Na=0.03ppm, Fe=0.02ppm, Ca do not detect, and Pb does not detect, Ni=0.02ppm, Cu do not detect, and Zn does not detect, Al does not detect, Cr=0.04ppm, and purity is 99.99%, comprehensive yield 96.2%, therefore the method illustrates that the stainless steel equipment of 316L is corroded low by it, can permanently effective run, equipment operating cost is low, and product stability is high, is suitable for industrialized production。
Comparative example
In 304 stainless steel cauldrons add 1982.5g concentration be 49.4% potassium hydroxide aqueous solution and 774g high-purity be warming up to 70 DEG C, mix and blend 2 hours；Then quantitative continuous passes into trimethyl fluoride sulfonyl fluorine gas, and controlling reaction pressure is between 0.2MPa ~ 1.0MPa；When ventilation quality stops ventilation, duration of ventilation 10 hours, then insulation reaction 4 hours after being 980g trimethyl fluoride sulfonyl fluorine, it is cooled to 25 DEG C subsequently；Being filtered by above-mentioned reactant liquor, obtain trifluoromethane sulfonic acid aqueous solutions of potassium, the concentration of trifluoromethane sulfonic acid potassium is 45%, pH=14, F
-
=102800ppm, ICP detect: Fe:100ppm, Ni:20ppm。
Undertaken being evaporated by the aqueous solution of above-mentioned trifluoromethane sulfonic acid potassium and obtain trifluoromethane sulfonic acid potassium and potassium fluoride mixture 1221g, moisture content 10000ppm；98% concentrated sulphuric acid being subsequently adding 1221g carries out acidification, finds have larger amount of white smoke to produce, be HF gas after measured in acidization；The trifluoromethane sulfonic acid potassium of acidifying is carried out rectification in 316L rustless steel rectifying column, obtains the crude product trifluoromethane sulfonic acid of jaundice, its F after measured
-
=10000ppm, Fe=50ppm, Ni=10ppm, purity is 97.2%, yield 94.5%, and the rising of Fe ion and Ni ion is the important indicator of equipment corrosion；Above-mentioned crude product trifluoromethane sulfonic acid is carried out secondary rectification and obtains high-purity trifluoromethane sulfonic acid product, F
-
=4000ppm, ICP measure: K=5ppm, Na=2ppm, Fe=30ppm, Ca do not detect, Pb=3ppm, Ni=13ppm, Cu do not detect, and Zn does not detect, Al does not detect, Cr=18ppm, and purity is 98.2%, comprehensive yield 93.8%, the stainless steel equipment of 304 and 316L is substantially corroded by important indicator therefore the method that the rising of Fe ion, Ni ion and Cr ion is equipment corrosion, and longtime running has very big hidden danger, equipment operating cost is high, and product stability is poor, is unfavorable for industrialized production。
Above-described embodiment is only for illustrating technology design and the feature of the present invention; its object is to allow person skilled in the art will appreciate that present disclosure and to implement according to this; can not limiting the scope of the invention with this, all equivalences made according to spirit of the invention change or modification all should be encompassed within protection scope of the present invention。
Claims (10)
1. the preparation method of a trifluoromethane sulfonic acid, it is characterised in that: it comprises the steps:
Step (1), by trimethyl fluoride sulfonyl fluorine and alkali metal hydroxide under the existence of fluorine fixing material, be neutralized hydrolysis, after react, reactant liquor obtains trifluoromethane sulfonic acid alkali metal salt through filtering, drying；
Step (2), trifluoromethane sulfonic acid alkali metal salt step (1) prepared carry out acidification with oleum, then obtain highly purified trifluoromethane sulfonic acid through repeatedly rectification。
2. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (1), described alkali metal hydroxide is one or more in Lithium hydrate, sodium hydroxide, potassium hydroxide。
3. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterized in that: in step (1), described alkali metal hydroxide feeds intake with the form of alkali metal hydroxide aqueous solution, and the mass concentration of described alkali metal hydroxide aqueous solution is 10 ~ 50%。
4. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (1), described fluorine fixing material is one or more the combination in calcium hydroxide, calcium oxide, calcium carbonate。
5. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (1), the molar ratio of described trimethyl fluoride sulfonyl fluorine and described alkali metal hydroxide is 1:1 ~ 1.1。
6. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (1), molar ratio 1:0.8 ~ 2 of described alkali metal hydroxide and described fluorine fixing material。
7. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (1), under the pressure of 0.2 ~ 1.0MPa, at the temperature of 70 ~ 120 DEG C, carry out described neutralizing hydrolysis reaction。
8. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (1), described trimethyl fluoride sulfonyl fluorine passes in gaseous form, and the speed that passes into of described trimethyl fluoride sulfonyl fluorine is 240 ~ 350g/h。
9. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (2), the mass ratio that feeds intake of described trifluoromethane sulfonic acid alkali metal salt and described oleum is 1:0.9 ~ 1:2。
10. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that: in step (2), the mass concentration of described oleum is 105% ~ 114%。
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| CN108276315A (en) * | 2017-12-29 | 2018-07-13 | 中国船舶重工集团公司第七八研究所 | A kind of purification process of trifluoromethanesulfonic acid |
| CN109535039A (en) * | 2018-12-18 | 2019-03-29 | 湖北优世达科技股份有限公司 | The method of one-step synthesis method perfluorohexylethyl sulfonic acid |
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| CN114019080A (en) * | 2021-10-28 | 2022-02-08 | 中船重工（邯郸）派瑞特种气体有限公司 | Method for quantitatively analyzing concentration of electrolyte for preparing trifluoromethyl sulfonyl fluoride by ion chromatography |
| CN115894308A (en) * | 2022-11-04 | 2023-04-04 | 中船(邯郸)派瑞特种气体股份有限公司 | Process for preparing trifluoromethanesulfonic acid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03209359A (en) * | 1990-01-10 | 1991-09-12 | Sumikin Chem Co Ltd | Production of naphthalene sulfonic acid salt |
| JP2002114755A (en) * | 2000-10-06 | 2002-04-16 | Sumika Fine Chemicals Co Ltd | Method for producing camostat mesylate |
| CN101402591A (en) * | 2008-11-09 | 2009-04-08 | 中国船舶重工集团公司第七一八研究所 | Process for preparing high-purity trifluoromethyl sulphonic acid |
| CN101747240A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing trifluoromethyl sulfonic acid CF3SO3H by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F |
| CN101878195A (en) * | 2007-11-27 | 2010-11-03 | 罗地亚管理公司 | Method for preparing trifluoromethanesulphinic acid |
| CN102911086A (en) * | 2012-11-19 | 2013-02-06 | 江西国化实业有限公司 | Preparation method of trifluoro methanesulfonic anhydride |
-
2016
- 2016-03-18 CN CN201610155298.2A patent/CN105693561B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03209359A (en) * | 1990-01-10 | 1991-09-12 | Sumikin Chem Co Ltd | Production of naphthalene sulfonic acid salt |
| JP2002114755A (en) * | 2000-10-06 | 2002-04-16 | Sumika Fine Chemicals Co Ltd | Method for producing camostat mesylate |
| CN101878195A (en) * | 2007-11-27 | 2010-11-03 | 罗地亚管理公司 | Method for preparing trifluoromethanesulphinic acid |
| CN101402591A (en) * | 2008-11-09 | 2009-04-08 | 中国船舶重工集团公司第七一八研究所 | Process for preparing high-purity trifluoromethyl sulphonic acid |
| CN101747240A (en) * | 2008-12-11 | 2010-06-23 | 张家港市国泰华荣化工新材料有限公司 | Method for preparing trifluoromethyl sulfonic acid CF3SO3H by electrochemical fluorination gas-phase product of methanesulfonyl fluoride CH3SO2F |
| CN102911086A (en) * | 2012-11-19 | 2013-02-06 | 江西国化实业有限公司 | Preparation method of trifluoro methanesulfonic anhydride |
Non-Patent Citations (1)
| Title |
|---|
| 孙树臣等: "氧化钙对混合稀土精矿分解气相中氟的影响", 《稀有金属》 * |
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| CN109535039A (en) * | 2018-12-18 | 2019-03-29 | 湖北优世达科技股份有限公司 | The method of one-step synthesis method perfluorohexylethyl sulfonic acid |
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