CN105693561B - A kind of preparation method of trifluoromethane sulfonic acid - Google Patents
A kind of preparation method of trifluoromethane sulfonic acid Download PDFInfo
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- CN105693561B CN105693561B CN201610155298.2A CN201610155298A CN105693561B CN 105693561 B CN105693561 B CN 105693561B CN 201610155298 A CN201610155298 A CN 201610155298A CN 105693561 B CN105693561 B CN 105693561B
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- 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 present invention relates to a kind of preparation method of trifluoromethane sulfonic acid, by trimethyl fluoride sulfonyl fluorine and alkali metal hydroxide in the presence of fluorine fixing material, carries out neutralizing hydrolysis reaction, after the completion of reaction, reaction solution is filtered, is dried to obtain trifluoromethane sulfonic acid alkali metal salt；Trifluoromethane sulfonic acid alkali metal salt and oleum are subjected to acidification, then obtain the trifluoromethane sulfonic acid of high-purity through multiple rectifying.The present invention improves operating flexibility, production efficiency, product stability and comprehensive yield, product purity is adapted to industrialized production up to more than 99.90% by the improvement to preparation method.
Description
Technical field
Present invention relates particularly to a kind of preparation method of trifluoromethane sulfonic acid.
Background technology
Trifluoromethane sulfonic acid is a kind of with very strong to proton (H+) super organic acid, its trifluoromethyl sulfonate radical
(CF3SO3 -) there is extremely strong thermodynamics and chemical stability, C-F keys will not also occur in the presence of strong nucleopilic reagent
Dissociation, trifluoromethane sulfonic acid has in the fields such as Industrial Catalysis, organic synthesis, bio-pharmaceuticals, high performance material, new energy
Very extensive application.
Simons electrofluorinations are at present by methyl (CH at present3 -) synthesis trifluoromethyl (CF3 -) maximally effective industrialization
Process route, it is using methylsufonyl chloride or methanesulfonyl fluoride as raw material, and electrosynthesis glyoxal is carried out in anhydrous liquid hydrogen fluoride
Trimethyl fluoride sulfonyl fluorine, then absorbed using the alkali metal aqueous solution, then be acidified with the concentrated sulfuric acid to obtain crude product fluoroform
Base sulfonic acid, further rectifying obtain high-purity trifluoromethane sulfonic acid., should compared to patent CN102911087A and CN104725283A
Without using organic solvent in synthetic route, also nodeless mesh technique, has the characteristics of safe.And in patent CN101885691A
It can be ionized largely from caused potassium fluoride during trimethyl fluoride sulfonyl fluorine synthesis trifluoromethane sulfonic acid aqueous solution of alkali metal salt
Fluorine ion, fluorine ion is the basic reason of etching apparatus, is handled in the patent by the way of crystallization, increased technique
Complexity, while crystallization processes are limited to the removal ability of potassium fluoride；And the potassium fluoride remained is same in the acidification technique stage
Sample is serious to equipment corrosion, and the hydrogen fluoride formed in acidization causes fluorine ion in product inclined into follow-up workshop section
Height, reduce product stability and quality；Only trifluoromethane sulfonic acid alkali metal salt is acidified using only the concentrated sulfuric acid in the patent,
Its water content is up to 2% ~ 5%, and higher moisture content is to cause another principal element that product stability is poor, equipment corrosion is serious.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of corrosivity to equipment is small and product stability is high three
The preparation method of methyl fluoride sulfonic acid.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
A kind of preparation method of trifluoromethane sulfonic acid, it comprises the following steps：
Step（1）, by trimethyl fluoride sulfonyl fluorine and alkali metal hydroxide in the presence of fluorine fixing material, carry out neutralizing hydrolysis
Reaction, after the completion of reaction, reaction solution is filtered, is dried to obtain trifluoromethane sulfonic acid alkali metal salt；
Step（2）, by step（1）Obtained trifluoromethane sulfonic acid alkali metal salt carries out acidification with oleum, so
The trifluoromethane sulfonic acid of high-purity is obtained by multiple rectifying.
Preferably, in step (1), described alkali metal hydroxide is selected from lithium hydroxide, sodium hydroxide, potassium hydroxide
In one or more.
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 is thrown in the form of alkali metal hydroxide aqueous solution
Material, the mass concentration of described alkali metal hydroxide aqueous solution is 10 ~ 50%.
Preferably, in step (1), described fluorine fixing material is one kind or more in calcium hydroxide, calcium oxide, calcium carbonate
The combination of kind.
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), described trimethyl fluoride sulfonyl fluorine and described alkali metal hydroxide feed intake mole
Than for 1：1~1.1.
It is further preferred that in step (1), the throwing of described trimethyl fluoride sulfonyl fluorine and described alkali metal hydroxide
It is 1 to expect mol ratio:1.08~1.09.
Preferably, in step (1), the molar ratio 1 of described alkali metal hydroxide and described fluorine fixing material:0.8~
2。
Preferably, in step (1), under 0.2 ~ 1.0MPa pressure, carry out at a temperature of 70 ~ 120 DEG C it is described in
And hydrolysis.
Preferably, in step (1), described trimethyl fluoride sulfonyl fluorine is passed through in gaseous form, described trifluoromethyl sulphur
The speed that is passed through of acyl fluorides is 240 ~ 350g/h.
Preferably, step（2）In, the quality that feeds intake of described trifluoromethane sulfonic acid alkali metal salt and described oleum
Than for 1:0.9~1:2.
It is further preferred that step（2）In, the throwing of described trifluoromethane sulfonic acid alkali metal salt and described oleum
It is 1 to expect mass ratio：1.
Preferably, step（2）In, 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 be added in reactor, be warming up to 70 ~ 120 DEG C, mix
1 ~ 3h of stirring is closed, then passes to trimethyl fluoride sulfonyl fluorine gas, it is 0.2 ~ 1.0MPa to control reaction pressure, after ventilation terminates, is protected
Temperature 1 ~ 3 h of reaction, is then cooled to 10 ~ 30 DEG C, reaction solution is filtered, it is water-soluble to obtain trifluoromethane sulfonic acid alkali metal salt
Liquid, described trifluoromethane sulfonic acid aqueous solution of alkali metal salt is evaporated to obtain trifluoromethane sulfonic acid alkali metal salt；
Step（2）, by step（1）Obtained trifluoromethane sulfonic acid alkali metal salt carries out acidification with oleum, so
First time rectifying is carried out afterwards and obtains trifluoromethane sulfonic acid crude product, and described trifluoromethane sulfonic acid crude product is carried out into second of rectifying obtains
To the trifluoromethane sulfonic acid of high-purity.
Because above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
Fluorine fixing material in the present invention can effective fluorine removal, fluorine ion in course of reaction is reduced within 20ppm, Neng Gouyou
Effect reduces corrosion of the fluorine ion to equipment；It is acidified in the present invention using oleum, the sulfur trioxide energy in oleum
Moisture content in enough rapid and trifluoromethane sulfonic acid metal salts carries out reaction and produces sulfuric acid, reduces to trifluoromethane sulfonic acid metal salt
Water removal of drying require, while can also reduce equipment corrosion caused by moisture content, the service life of reactor can be greatly prolonged；
In addition, the present invention improves operating flexibility, production efficiency, product stability and comprehensive yield by the improvement to preparation method,
Product purity is adapted to industrialized production up to more than 99.90%.
Embodiment
The reaction scheme of the present invention is as follows：
Technical solutions according to the invention are elaborated with reference to embodiment, the operation of unexplained reference in the present invention
Method is conventional method, and the reaction condition of unexplained reference is normal condition, and the % of unexplained reference is mass percent.
Embodiment 1
The potassium hydroxide aqueous solution that 793g concentration is 49.4%, 560g hydroxides are sequentially added in 304 stainless steel cauldrons
Calcium and 774g high purity waters, 70 DEG C are warming up to, mixed 2 hours；Then quantitative continuous is passed through trimethyl fluoride sulfonyl fluorine gas, control
Reaction pressure processed is between 0.2MPa ~ 1.0MPa；Stop ventilating after quality of ventilating be 980g trimethyl fluoride sulfonyl fluorine, during ventilation
Between 3 hours, then insulation reaction 2 hours, are then cooled to 25 DEG C；Above-mentioned reaction solution is filtered, obtains trifluoromethyl sulphur
Sour aqueous solutions of potassium, the concentration of trifluoromethane sulfonic acid potassium is 46.81%, pH=14, F-=5ppm, ICP are detected：Fe：0.5ppm, Ni：
0.1ppm.Fluorinion concentration<10ppm, Fe<1ppm, Ni<1ppm, this illustrates that the reaction is not corroded to 304 stainless steels, the method
The corrosivity of equipment is greatly reduced, the service life and maintenance cost of equipment can be greatly prolonged.
The aqueous solution of above-mentioned trifluoromethane sulfonic acid potassium is evaporated to obtain trifluoromethane sulfonic acid potassium 1201g, moisture content
10000ppm, F-=8ppm；Then 105% oleum for adding 1201g carries out acidification；By the trifluoromethane sulfonic acid of acidifying
Potassium carries out rectifying in 316L stainless steel rectifying columns, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F-=3ppm, Fe=
0.01ppm, Ni=0.01ppm, purity 99.0%, yield 98%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out into secondary rectifying to obtain
High-purity trifluoromethane sulfonic acid product, F-=1ppm, ICP are determined：K=0.1ppm, Na=0.09ppm, Fe=0.01ppm, Ca are not detected,
Pb is not detected, and Ni=0.01ppm, Cu is not detected, and Zn is not detected, and Al is not detected, Cr=0.08ppm, purity 99.98%, comprehensive to receive
Rate 95%, therefore this method illustrates that its corrosion of stainless steel equipment to 316L is low, permanently effective can run, equipment operating cost is low,
Product purity and stability are high, are adapted to industrialized production.
Embodiment 2
The potassium hydroxide aqueous solution that 793g concentration is 49.4%, 434g hydroxides are sequentially added in 304 stainless steel cauldrons
Calcium and 774g high purity waters, 70 DEG C are warming up to, mixed 2 hours；Then quantitative continuous is passed through trimethyl fluoride sulfonyl fluorine gas, control
Reaction pressure processed is between 0.2MPa ~ 1.0MPa；Stop ventilating after quality of ventilating be 980g trimethyl fluoride sulfonyl fluorine, during ventilation
Between 3 hours, then insulation reaction 2 hours, are then cooled to 25 DEG C；Above-mentioned reaction solution is filtered, obtains trifluoromethyl sulphur
Sour aqueous solutions of potassium, the concentration of trifluoromethane sulfonic acid potassium is 48.74%, pH=14, F-=4ppm, ICP are detected：Fe：0.4ppm, Ni：
0.09ppm.Fluorinion concentration<10ppm, Fe<1ppm, Ni<1ppm, this illustrates that the reaction is not corroded to 304 stainless steels, the method
The corrosivity of equipment is greatly reduced, the service life and maintenance cost of equipment can be greatly prolonged.
The aqueous solution of above-mentioned trifluoromethane sulfonic acid potassium is evaporated to obtain trifluoromethane sulfonic acid potassium 1210g, moisture content
8000ppm, F-=9ppm；Then 114% oleum for adding 1210g carries out acidification；By the trifluoromethane sulfonic acid of acidifying
Potassium carries out rectifying in 316L stainless steel rectifying columns, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F-=2.5ppm,
Fe=0.09ppm, Ni=0.1ppm, purity 99.1%, yield 97.5%；Above-mentioned crude product trifluoromethane sulfonic acid is subjected to secondary rectifying
Obtain high-purity trifluoromethane sulfonic acid product, F-=1.2ppm, ICP are determined：K=0.09ppm, Na=0.08ppm, Fe=0.01ppm, Ca
Do not detect, Pb is not detected, and Ni=0.01ppm, Cu is not detected, and Zn is not detected, and Al is not detected, Cr=0.09ppm, and purity is
99.99%, comprehensive yield 95.8%, therefore this method illustrates that its corrosion of stainless steel equipment to 316L is low, permanently effective can run,
Equipment operating cost is low, and product stability is high, is adapted to industrialized production.
Embodiment 3
The sodium hydrate aqueous solution that 875g concentration is 32.0%, 424g oxidations are sequentially added in 316L stainless steel cauldrons
Calcium and 580g high purity waters, 85 DEG C are warming up to, mixed 3 hours；Then quantitative continuous is passed through trimethyl fluoride sulfonyl fluorine gas, control
Reaction pressure processed is between 0.2MPa ~ 1.0MPa；Stop ventilating after quality of ventilating be 980g trimethyl fluoride sulfonyl fluorine, during ventilation
Between 4 hours, then insulation reaction 2.5 hours, are then cooled to 25 DEG C；Above-mentioned reaction solution is filtered, obtains trifluoromethyl
Sulfonic acid sodium water solution, the concentration of trifluoromethyl sulfonate is 47.55%, pH=14, F-=7ppm, ICP are detected：Fe：0.5ppm, Ni：
0.14ppm.Fluorinion concentration<10ppm, Fe<1ppm, Ni<1ppm, this illustrates that the reaction is not corroded to 316L stainless steels, should
Method greatly reduces the corrosivity of equipment, can greatly prolong the service life and maintenance cost of equipment.
The aqueous solution of above-mentioned trifluoromethyl sulfonate is evaporated to obtain trifluoromethyl sulfonate 1100g, moisture content
9200ppm, F-=15ppm；Then 105% oleum for adding 1100g carries out acidification；By the trifluoromethane sulfonic acid of acidifying
Sodium carries out rectifying in 316L stainless steel rectifying columns, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F-=3.1ppm,
Fe=0.08ppm, Ni=0.08ppm, purity 99.3%, yield 97.1%；Above-mentioned crude product trifluoromethane sulfonic acid is subjected to secondary fine
Evaporate to obtain high-purity trifluoromethane sulfonic acid product, F-=1.0ppm, ICP are determined：K=0.02ppm, Na=0.04ppm, Fe=0.01ppm,
Ca is not detected, and Pb is not detected, and Ni=0.02ppm, Cu is not detected, and Zn is not detected, and Al is not detected, Cr=0.04ppm, and purity is
99.99%, comprehensive yield 95.2%, therefore this method illustrates that its corrosion of stainless steel equipment to 316L is low, permanently effective can run,
Equipment operating cost is low, and product stability is high, is adapted to industrialized production.
Embodiment 4
The lithium hydroxide aqueous solution that 1678g concentration is 10.0%, 424g oxidations are sequentially added in 316L stainless steel cauldrons
Calcium, 85 DEG C are warming up to, mixed 3 hours；Then quantitative continuous is passed through trimethyl fluoride sulfonyl fluorine gas, controls the reaction pressure to be
Between 0.2MPa ~ 1.0MPa；Stop ventilating after quality of ventilating is 980g trimethyl fluoride sulfonyl fluorine, duration of ventilation 3.5 hours, so
Insulation reaction 3 hours afterwards, then it is cooled to 25 DEG C；Above-mentioned reaction solution is filtered, obtains the trifluoromethyl sulfonic acid lithium aqueous solution,
The concentration of trifluoromethyl sulfonic acid lithium is 40.05%, pH=14, F-=5ppm, ICP are detected：Fe：0.3ppm, Ni：0.12ppm.Fluorine from
Sub- concentration<10ppm, Fe<1ppm, Ni<1ppm, this illustrates that the reaction is not corroded to 316L stainless steels, and the method greatly reduces
The corrosivity of equipment, the service life and maintenance cost of equipment can be greatly prolonged.
The aqueous solution of above-mentioned trifluoromethyl sulfonic acid lithium is evaporated to obtain trifluoromethyl sulfonic acid lithium 1001g, moisture content
10000ppm, F-=11ppm；Then 105% oleum for adding 1001g carries out acidification；By the trifluoromethyl sulphur of acidifying
Sour lithium carries out rectifying in 316L stainless steel rectifying columns, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F-=
1.1ppm, Fe=0.04ppm, Ni=0.02ppm, purity 99.6%, yield 96.8%；Above-mentioned crude product trifluoromethane sulfonic acid is carried out
Secondary rectifying obtains high-purity trifluoromethane sulfonic acid product, F-=0.8ppm, ICP are determined：K=0.01ppm, Na=0.05ppm, Fe=
0.02ppm, Ca are not detected, and Pb is not detected, and Ni=0.02ppm, Cu is not detected, and Zn is not detected, and Al is not detected, and Cr=0.04ppm is pure
Spend for 99.98%, comprehensive yield 96.2%, therefore this method illustrates that its corrosion of stainless steel equipment to 316L is low, can be permanently effective
Operation, equipment operating cost is low, and product stability is high, is adapted to industrialized production.
Embodiment 5
The sodium hydrate aqueous solution that 875g concentration is 32.0%, 757g oxidations are sequentially added in 316L stainless steel cauldrons
Calcium and 580g high purity waters, 95 DEG C are warming up to, mixed 3 hours；Then quantitative continuous is passed through trimethyl fluoride sulfonyl fluorine gas, control
Reaction pressure processed is between 0.2MPa ~ 1.0MPa；Stop ventilating after quality of ventilating be 980g trimethyl fluoride sulfonyl fluorine, during ventilation
Between 4 hours, then insulation reaction 2.5 hours, are then cooled to 25 DEG C；Above-mentioned reaction solution is filtered, obtains trifluoromethyl
Sulfonic acid sodium water solution, the concentration of trifluoromethyl sulfonate is 47.0%, pH=14, F-=4ppm, ICP are detected：Fe：0.8ppm, Ni：
0.16ppm.Fluorinion concentration<10ppm, Fe<1ppm, Ni<1ppm, this illustrates that the reaction is not corroded to 316L stainless steels, should
Method greatly reduces the corrosivity of equipment, can greatly prolong the service life and maintenance cost of equipment.
The aqueous solution of above-mentioned trifluoromethyl sulfonate is evaporated to obtain trifluoromethyl sulfonate 1100g, moisture content
7800ppm, F-=11ppm；Then 105% oleum for adding 1100g carries out acidification；By the trifluoromethane sulfonic acid of acidifying
Sodium carries out rectifying in 316L stainless steel rectifying columns, obtains colourless crude product trifluoromethane sulfonic acid, after measured its F-=2.5ppm,
Fe=0.04ppm, Ni=0.07ppm, purity 99.4%, yield 96.9%；Above-mentioned crude product trifluoromethane sulfonic acid is subjected to secondary fine
Evaporate to obtain high-purity trifluoromethane sulfonic acid product, F-=1.7ppm, ICP are determined：K=0.02ppm, Na=0.03ppm, Fe=0.02ppm,
Ca is not detected, and Pb is not detected, and Ni=0.02ppm, Cu is not detected, and Zn is not detected, and Al is not detected, Cr=0.04ppm, and purity is
99.99%, comprehensive yield 96.2%, therefore this method illustrates that its corrosion of stainless steel equipment to 316L is low, permanently effective can run,
Equipment operating cost is low, and product stability is high, is adapted to industrialized production.
Comparative example
Potassium hydroxide aqueous solution that 1982.5g concentration is 49.4% is added in 304 stainless steel cauldrons and 774g is high-purity is
70 DEG C are warming up to, is mixed 2 hours；Then quantitative continuous is passed through trimethyl fluoride sulfonyl fluorine gas, controls the reaction pressure to be
Between 0.2MPa ~ 1.0MPa；Stop ventilating after quality of ventilating is 980g trimethyl fluoride sulfonyl fluorine, duration of ventilation 10 hours, so
Insulation reaction 4 hours afterwards, then it is cooled to 25 DEG C；Above-mentioned reaction solution is filtered, obtains trifluoromethane sulfonic acid aqueous solutions of potassium,
The concentration of trifluoromethane sulfonic acid potassium is 45%, pH=14, F-=102800ppm, ICP are detected：Fe：100ppm, Ni：20ppm.
The aqueous solution of above-mentioned trifluoromethane sulfonic acid potassium is evaporated to obtain trifluoromethane sulfonic acid potassium and potassium fluoride mixture
1221g, moisture content 10000ppm；Then 98% concentrated sulfuric acid for adding 1221g carries out acidification, finds in acidization to have larger
The white smoke of amount produces, and is determined to HF gases；The trifluoromethane sulfonic acid potassium of acidifying is entered in 316L stainless steel rectifying columns
Row rectifying, the crude product trifluoromethane sulfonic acid to be turned to be yellow, after measured its F-=10000ppm, Fe=50ppm, Ni=10ppm, purity
For 97.2%, yield 94.5%, the rise of Fe ions and Ni ions is the important indicator of equipment corrosion；By above-mentioned crude product trifluoromethyl
Sulfonic acid carries out secondary rectifying and obtains high-purity trifluoromethane sulfonic acid product, F-=4000ppm, ICP are determined：K=5ppm, Na=2ppm, Fe
=30ppm, Ca are not detected, Pb=3ppm, Ni=13ppm, and Cu is not detected, and Zn is not detected, and Al is not detected, Cr=18ppm, and purity is
98.2%, comprehensive yield 93.8%, the rise of Fe ions, Ni ions and Cr ions is the important indicator therefore this method of equipment corrosion
Substantially 304 and 316L stainless steel equipment is corroded, longtime running has very big hidden danger, and equipment operating cost is high, product
Stability is poor, is unfavorable for industrialized production.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, all according to the present invention
The equivalent change or modification that Spirit Essence is made should be all included within the scope of the present invention.
Claims (5)
- A kind of 1. preparation method of trifluoromethane sulfonic acid, it is characterised in that：It comprises the following steps：Step（1）, by trimethyl fluoride sulfonyl fluorine and alkali metal hydroxide in the presence of fluorine fixing material, 0.2 ~ 1.0MPa's Under pressure, neutralizing hydrolysis reaction is carried out at a temperature of 70 ~ 120 DEG C, after the completion of reaction, reaction solution is filtered, is dried to obtain three Methyl fluoride sulfonic acid alkali metal salts；Described fluorine fixing material is one or more groups in calcium hydroxide, calcium oxide, calcium carbonate Close；The molar ratio 1 of described alkali metal hydroxide and described fluorine fixing material:0.8~2；Described trimethyl fluoride sulfonyl fluorine It is passed through in gaseous form, the speed that is passed through of described trimethyl fluoride sulfonyl fluorine is 240 ~ 350g/h；Step（2）, by step（1）System The trifluoromethane sulfonic acid alkali metal salt obtained carries out acidification with oleum, then obtains the trifluoro of high-purity through multiple rectifying Pyrovinic acid；The mass concentration of described oleum is 105% ~ 114%.
- 2. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that：In step (1), described alkali Metal hydroxides is the one or more in lithium hydroxide, sodium hydroxide, potassium hydroxide.
- 3. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that：In step (1), described alkali Metal hydroxides is fed intake in the form of alkali metal hydroxide aqueous solution, the quality of described alkali metal hydroxide aqueous solution Concentration is 10 ~ 50%.
- 4. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that：In step (1), described three The molar ratio of methyl fluoride sulfuryl fluoride and described alkali metal hydroxide is 1：1~1.1.
- 5. the preparation method of trifluoromethane sulfonic acid according to claim 1, it is characterised in that：Step（2）In, described three Methyl fluoride sulfonic acid alkali metal salts and the mass ratio that feeds intake of described oleum are 1:0.9~1.2.
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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 |
| CN111116424B (en) * | 2019-12-28 | 2022-08-09 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing trifluoromethanesulfonic acid by continuous hydrolysis |
| CN112679392A (en) * | 2020-12-30 | 2021-04-20 | 中船重工（邯郸）派瑞特种气体有限公司 | Production device and method of trifluoromethanesulfonic acid |
| CN112778170B (en) * | 2020-12-30 | 2022-12-27 | 中船(邯郸)派瑞特种气体股份有限公司 | Method and device for preparing lithium trifluoromethanesulfonate |
| CN113845446B (en) * | 2021-10-26 | 2023-03-14 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method of trifluoromethanesulfonic acid |
| CN113929601B (en) * | 2021-11-15 | 2023-07-18 | 苏州湘园新材料股份有限公司 | Preparation method of zirconium triflate oxide |
| CN115894308B (en) * | 2022-11-04 | 2024-04-05 | 中船(邯郸)派瑞特种气体股份有限公司 | Technological method for preparing trifluoromethanesulfonic acid |
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