finate
Sodium trifluoromethanesulfinate
CAS: 2926-29-6
Molecular Formula: CF3NaO2S
finate - Names and Identifiers
| Name | Sodium trifluoromethanesulfinate |
| Synonyms | finate SODIUM TRIFLUOROMETHANESULFINATE Sodium trifluoromethanesulfinate Sodium Trifluoromethanesulfinate SODIUM TRIFLUOROMETHANESULPHINATE TRIFLUOROMETHANESULFINIC ACID SODIUM SALT sodium trifluoromethanesulfinate CF3NaO2S Trifluoromethanesulphinic acid, sodium salt Methanesulfinic acid,1,1,1-trifluoro-, sodiuM salt |
| CAS | 2926-29-6 |
| EINECS | 423-490-1 |
| InChI | InChI=1/CHF3O2S.Na/c2-1(3,4)7(5)6;/h(H,5,6);/q;+1/p-1 |
| InChIKey | KAVUKAXLXGRUCD-UHFFFAOYSA-M |
finate - Physico-chemical Properties
| Molecular Formula | CF3NaO2S |
| Molar Mass | 156.06 |
| Melting Point | <325°C |
| Boling Point | 222.8°C at 760 mmHg |
| Flash Point | 88.5°C |
| Solubility | Water (Sparingly) |
| Vapor Presure | 0.0369mmHg at 25°C |
| Appearance | powder |
| Color | white |
| BRN | 3723394 |
| Storage Condition | Keep in dark place,Inert atmosphere,Room temperature |
| MDL | MFCD03092989 |
finate - Risk and Safety
| Hazard Symbols | Xi - Irritant |
| Risk Codes | R36/37/38 - Irritating to eyes, respiratory system and skin. R36/38 - Irritating to eyes and skin. |
| Safety Description | S26 - In case of contact with eyes, rinse immediately with plenty of water and seek medical advice. S36/37/39 - Wear suitable protective clothing, gloves and eye/face protection. |
| WGK Germany | 3 |
| TSCA | No |
| HS Code | 29309090 |
| Hazard Class | IRRITANT |
finate - Reference Information
| Application | Sodium trifluoromethane sulfonate is a sulfonate compound that can be used as an intermediate in organic synthesis. |
| overview | sodium trifluoromethyl sulfonate (CF3NaO2S) is the main raw material for the production of lithium bistrifluoromethanesulfonium. its production method is mainly obtained by reaction synthesis under high pressure in an autoclave with trifluorobromomethane as raw material, hydrosulfite as dehalogenation agent, sodium dihydrogen phosphate as neutralizer, water and acetonitrile at the same time. |
| prepare | 1. first, vacuum 1625kg of water is drawn into a 5000L stainless steel high-pressure reactor, the manhole cover is opened, stirring is started, 120kg of flake alkali is added and stirred for 30 minutes, then 1100kg of trisodium phosphate and 600kg of sodium hydrosulfite are successively added, and the manhole cover is tightened. Use vacuum to pump 1100kg of acetonitrile to-0.08MPa to raise the temperature. 2. When the temperature rises to 40 ℃, the residual gas in the reaction kettle after the reaction is completed shall be passed first, and the trifluorobromomethane gas in the recovery tank shall be passed after the pressure of the reaction kettle and the recovery tank is balanced. After the pressure of the reaction kettle and the recovery tank is balanced, the steel cylinder shall be opened to 310kg of trifluorobromomethane gas in the steel cylinder, and the temperature shall be raised to 55 ℃ for heat preservation. 3. Keep the temperature at 55~60 ℃ for 4~5 hours, press the material into a 5000L layered kettle and let it stand for layering. 4. Let stand for 60 minutes and layer, the acetonitrile layer is divided into a desolysis kettle, the foot material layer is added with acetonitrile, and the foot material layer is extracted 3 times, 100kg of acetonitrile each time, the extraction material is pumped into the desolysis kettle and dissolved together, and the foot material is packed into a barrel. 5. Desolubilization, slow heating, negative pressure desolubilization, pressure maintenance-0.085Mpa, temperature removal to 60 ℃, intermediate is weighed in a barrel, and spray drying is entered into the next process. 6. The dedissolved acetonitrile is pumped into the distillation kettle and 7kg of potassium permanganate is added to the distillation kettle, and the temperature is heated and distilled. The normal reflux is about 10 hours at 80 degrees. The distillation is finished when the temperature rises. To be recovered acetonitrile sampling analysis, the next feeding. 7. The intermediate is spray dried to obtain sodium trifluoromethyl sulfinate. The spray drying temperature is controlled to not exceed 180 ℃, and the dry temperature weight is not more than 1%. The purity of the obtained sodium trifluoromethyl sulfinate is 98%, and the yield is as high as 80%. |
| purification | in a 2000ml three-mouth flask equipped with a stirrer, add 300g of 60-70% sodium trifluoromethyl sulfonate industrial product, 20g of anhydrous magnesium sulfate, 500g of ethyl acetate solvent, stirring at 20-30 ℃ for 0.5h, stop stirring, discharge filtration, filtrate collection, filter cake return to the flask, and add 500g of ethyl acetate solvent to the flask, stir at 20-30 ℃ for 0.5h, stop stirring, filter out of material, collect filtrate, put the filter cake back into the flask, add 300g of ethyl acetate solvent, stir at 20-30 ℃ for 0.5h, stop stirring, filter out of material, collect filtrate, rinse the filter cake with a small amount of ethyl acetate solvent, remove the filter cake, collect the filter liquid and rinse filtrate solution for three times, evaporate to dry with rotary steam negative pressure, recover ethyl acetate solvent, and recycle, add 1000g of deionized water to the kettle, dissolve sodium trifluoromethyl sulfinate solid to obtain sodium trifluoromethyl sulfinate aqueous solution, and send sodium trifluoromethyl sulfinate aqueous solution to a dryer for spray drying to obtain sodium trifluoromethyl sulfinate products with a content of more than 95%. |
Last Update：2024-04-10 22:29:15
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