CN101885691A - Processing technology of trifloromethanesulfonic acid - Google Patents
Processing technology of trifloromethanesulfonic acid Download PDFInfo
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- CN101885691A CN101885691A CN2009100276398A CN200910027639A CN101885691A CN 101885691 A CN101885691 A CN 101885691A CN 2009100276398 A CN2009100276398 A CN 2009100276398A CN 200910027639 A CN200910027639 A CN 200910027639A CN 101885691 A CN101885691 A CN 101885691A
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- vitriol oil
- fluoride
- potassium hydroxide
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Abstract
The invention relates to a processing technology of trifloromethanesulfonic acid (TFSA) which is generated by the reaction of raw materials, i.e. anhydrous hydrogen fluoride (AHF), fnmette, potassium hydroxide and concentrated sulfuric acid with the molar ratio of 10-40:1-1.2:2-4:5-8; fluoroform sulfuryl fluoride gas is obtained through a special electrolyzer device; and the collected substances are transferred to an atmospheric distillation reactor after repeated reactions, and the trifloromethanesulfonic acid is collected from a tower top at the temperature of 158-162 DEG C with the content being more than 99%. The invention has the characteristics of simple technology, convenient production and the like.
Description
Technical field: the present invention relates to a kind of organic acid, particularly relate to nucleosides, microbiotic, steroid, protein, join carbohydrate, the synthetic complete processings of products such as VITAMIN is synthetic, silicon rubber modification as the required trifluoromethanesulfonic acid of raw material.
Technical background: trifluoromethanesulfonic acid is a kind of known strong organic acid, is omnipotent synthetics, is widely used in industries such as medicine, chemical industry.At present, when synthesizing trifluoromethanesulfonic acid at home, generally adopt with dithiocarbonic anhydride is raw material, generate trifluoromethyl disulphide with the iodine pentafluoride reaction, again with mercury react trifluoromethylthio mercury (CF3S) 2Hg, the latter promptly gets trifluoromethanesulfonic acid through the hydrogen peroxide oxidation, entire reaction exists the cost height, it is big to pollute, product purity and yield are low, defectives such as complex process, step length have seriously influenced the development space that derived product is used.Purpose of the present invention is exactly the complete processing that a kind of trifluoromethanesulfonic acid will be provided, and is synthetic as various medicines, joins carbohydrate, VITAMIN is synthetic, can improve the yield of target product during the silicon rubber modification significantly, reduces the production cost of target product.
Summary of the invention: the object of the present invention is achieved like this, the complete processing of trifluoromethanesulfonic acid, be by the raw material anhydrous hydrogen fluoride, Fumette, potassium hydroxide, generation that the vitriol oil reacts is characterized in that: described raw material anhydrous hydrogen fluoride, methylsulfonyl chloride, potassium hydroxide, the vitriol oil are respectively in molar ratio: 10-40: 1-1.2: 2-4: 5-8; By special electrolytic cell equipment, anhydrous hydrogen fluoride and methylsulfonyl chloride joined in-30 ℃～20 ℃ the electrolyzer, the control molar ratio of material is a hydrogen fluoride: methylsulfonyl chloride is 10-40: 1-1.2, control current 2A～6A, voltage: 2V～12V, electrolyzer temperature is-30 ℃～20 ℃ situation, electrolysis 72 hours, the fluoroform sulfonic acid fluoride gas that gets separates by low-temperature separator, absorb unnecessary hydrogen fluoride again through the Sodium Fluoride absorption tower, in the cold-trap of the collection and confinement of gases to 0 that obtains～80 ℃, liquefaction for content greater than 97% fluoroform sulfonic acid fluoride liquid, this liquid is slowly heated up, in the solution of the potassium hydroxide of 10～40 ℃ of feedings a certain amount of 20%～50% of controlled temperature, molar ratio of material example control 1-1.2: 2-4,10～100 ℃ of temperature controls, ventilation moves to concentration kettle with this liquid after finishing, the control negative pressure is under the situation of-0.08Mpa～0.1Mpa, temperature is a terminal point for 70～100 ℃, leftover materials are cooled to 20 ℃ of crystallizations, after the solid-liquid separation, solid is delivered to baking oven, control 80 ℃～120 ℃, dried by the fire 10～12 hours, the gained solids adds in the acidifying still, drip a certain amount of vitriol oil, the quality of material ratio is solid: the vitriol oil is 1-1.2: 5-8, temperature is controlled at 30～80 ℃, drip and finish 80 ℃～120 ℃ of back intensifications, reacted 3～8 hours, moving to still kettle vacuum distillation pressure then is-0.08Mpa～0.01Mpa to collect the finished product of 50 ℃～100 ℃ of tower top temperatures, the material of collecting moves to the atmospheric distillation still again, and what collect 158 ℃～162 ℃ of cats head is product content greater than 99% trifluoromethanesulfonic acid.Institute's synthetic trifluoromethanesulfonic acid, its molecular formula is: CF3SO2OH.Its synthetic chemical equation is:
CH3SO2F+3HF→CF3SO2F+3H2
CF3SO2F+2KOH→CF3SO2OK+KF+H2O
CF3SO2OK+H2SO4→CF3SO3H+KHSO4
Concrete embodiment: trifluoromethanesulfonic acid, its molecular formula is: CF3SO2OH is a kind of known strong organic acid, omnipotent synthetics.It is by the raw material anhydrous hydrogen fluoride, Fumette, and potassium hydroxide, generation that the vitriol oil reacts is characterized in that: described raw material anhydrous hydrogen fluoride, methylsulfonyl chloride, potassium hydroxide, the vitriol oil are respectively in molar ratio: 10-40: 1-1.2: 2-4: 5-8.Institute's synthetic trifluoromethanesulfonic acid, its molecular formula is: CF3SO2OH.Pass through special electrolytic cell equipment when synthetic, anhydrous hydrogen fluoride and Fumette are measured in the electrolyzer that joins-30 ℃～20 ℃, control current 2A～6A, voltage: 2V～12V, electrolyzer temperature is-30 ℃～20 ℃ situation, electrolysis 72 hours, the fluoroform sulfonic acid fluoride gas that gets separates by low-temperature separator, absorb unnecessary hydrogen fluoride again through the Sodium Fluoride absorption tower, in the cold-trap of the collection and confinement of gases to 0 that obtains～80 ℃, liquefaction for content greater than 97% fluoroform sulfonic acid fluoride liquid, this liquid is slowly heated up, in the solution of the potassium hydroxide of 10～40 ℃ of feedings a certain amount of 20%～50% of controlled temperature, 10～100 ℃ of temperature controls, ventilation moves to concentration kettle with this liquid after finishing, under the control negative pressure-situation of 0.08Mpa～0.1Mpa under, temperature is a terminal point for 70～100 ℃, leftover materials are cooled to 20 ℃ of crystallizations, after the solid-liquid separation, solid is to baking oven, control 80 ℃～120 ℃, dried by the fire 10～12 hours, the gained solids adds in the acidifying still, drip a certain amount of vitriol oil, temperature is controlled at 30～80 ℃, drips to finish 80 ℃～120 ℃ of back intensifications, reacts 3～8 hours, moving to still kettle vacuum distillation pressure then is-0.08Mpa～0.01Mpa, collect the finished product of 50 ℃～100 ℃ of tower top temperatures, the material of collection moves to the atmospheric distillation still again, and what collect 158 ℃～162 ℃ of cats head is the product trifluoromethanesulfonic acid.
Claims (1)
1. the complete processing of trifluoromethanesulfonic acid, be by raw material anhydrous hydrogen fluoride, Fumette, potassium hydroxide, generation that the vitriol oil reacts is characterized in that: described raw material anhydrous hydrogen fluoride, methylsulfonyl chloride, potassium hydroxide, the vitriol oil are respectively in molar ratio: 10-40: 1-1.2: 2-4: 5-8; By special electrolytic cell equipment, anhydrous hydrogen fluoride and methylsulfonyl chloride joined in-30 ℃～20 ℃ the electrolyzer, the control molar ratio of material is a hydrogen fluoride: methylsulfonyl chloride is 10-40: 1-1.2, control current 2A～6A, voltage: 2V～12V, electrolyzer temperature is-30 ℃～20 ℃ situation, electrolysis 72 hours, the fluoroform sulfonic acid fluoride gas that gets separates by low-temperature separator, absorb unnecessary hydrogen fluoride again through the Sodium Fluoride absorption tower, in the cold-trap of the collection and confinement of gases to 0 that obtains～80 ℃, liquefaction for content greater than 97% fluoroform sulfonic acid fluoride liquid, this liquid is slowly heated up, in the solution of the potassium hydroxide of 10～40 ℃ of feedings a certain amount of 20%～50% of controlled temperature, molar ratio of material example control 1-1.2: 2-4,10～100 ℃ of temperature controls, ventilation moves to concentration kettle with this liquid after finishing, the control negative pressure is under the situation of-0.08Mpa～0.1Mpa, temperature is a terminal point for 70～100 ℃, leftover materials are cooled to 20 ℃ of crystallizations, after the solid-liquid separation, solid is delivered to baking oven, controls 80 ℃～120 ℃, dries by the fire 10～12 hours, the gained solids adds in the acidifying still, drip a certain amount of vitriol oil, the quality of material ratio is solid: the vitriol oil is 1-1.2: 5-8, and temperature is controlled at 30～80 ℃, drip and finish 80 ℃～120 ℃ of back intensifications, reacted 3～8 hours, moving to still kettle vacuum distillation pressure then is-0.08Mpa～0.01Mpa to collect the finished product of 50 ℃～100 ℃ of tower top temperatures, the material of collecting moves to the atmospheric distillation still again, and what collect 158 ℃～162 ℃ of cats head is the product trifluoromethanesulfonic acid.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100276398A CN101885691A (en) | 2009-05-15 | 2009-05-15 | Processing technology of trifloromethanesulfonic acid |
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| CN2009100276398A CN101885691A (en) | 2009-05-15 | 2009-05-15 | Processing technology of trifloromethanesulfonic acid |
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| CN2009100276398A Pending CN101885691A (en) | 2009-05-15 | 2009-05-15 | Processing technology of trifloromethanesulfonic acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387300A (en) * | 2014-11-11 | 2015-03-04 | 中国船舶重工集团公司第七一八研究所 | Purification method of trifluoromathanesulfonyl fluoride |
| CN104725283A (en) * | 2015-04-14 | 2015-06-24 | 江西国化实业有限公司 | Trifluoromethanesulfonic acid preparation method |
| 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 |
| CN113860943A (en) * | 2021-09-24 | 2021-12-31 | 中船重工（邯郸）派瑞特种气体有限公司 | Comprehensive treatment method for kettle residues in preparation of trifluoromethanesulfonic acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2732398A (en) * | 1953-01-29 | 1956-01-24 | cafiicfzsojk | |
| CN1126502A (en) * | 1993-06-30 | 1996-07-10 | 美国3M公司 | Process for preparing perfluoroalkanesulfonyl fluorides |
-
2009
- 2009-05-15 CN CN2009100276398A patent/CN101885691A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2732398A (en) * | 1953-01-29 | 1956-01-24 | cafiicfzsojk | |
| CN1126502A (en) * | 1993-06-30 | 1996-07-10 | 美国3M公司 | Process for preparing perfluoroalkanesulfonyl fluorides |
Non-Patent Citations (2)
| Title |
|---|
| 吕灵华等: ""三氟甲基磺酸的生产工艺总数"", 《化学工程与装备》 * |
| 吕灵华等: ""三氟甲基磺酸的生产工艺总数"", 《舰船防化》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387300A (en) * | 2014-11-11 | 2015-03-04 | 中国船舶重工集团公司第七一八研究所 | Purification method of trifluoromathanesulfonyl fluoride |
| CN104387300B (en) * | 2014-11-11 | 2015-09-23 | 中国船舶重工集团公司第七一八研究所 | A kind of purification process of fluoroform sulfonic acid fluoride |
| CN104725283A (en) * | 2015-04-14 | 2015-06-24 | 江西国化实业有限公司 | Trifluoromethanesulfonic acid preparation method |
| 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 |
| CN113860943A (en) * | 2021-09-24 | 2021-12-31 | 中船重工（邯郸）派瑞特种气体有限公司 | Comprehensive treatment method for kettle residues in preparation of trifluoromethanesulfonic acid |
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Application publication date: 20101117 |