Method for recycling trifluoromethanesulfonic acid from trifluoromethanesulfonic acid amine salt waste water
A technology of ammonium trifluoromethanesulfonate and ammonium trifluoromethanesulfonate, which is applied in the field of recycling trifluoromethanesulfonic acid, can solve the problem of high temperature resistance and corrosion resistance of equipment, poor production and operation safety, trifluoromethanesulfonic acid Difficulty in repeated use and other problems, to achieve the effect of low temperature and improved safety
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Embodiment 1
[0026] (1) Get 300g trifluoromethanesulfonic acid triethylamine salt waste water in the flask, contain trifluoromethanesulfonic acid triethylamine salt 80.4g (0.32mol) in the waste water, under distillation temperature 60 ℃, 5kPa condition, water Evaporated to obtain 101.4g of dark liquid, which was washed three times with 200ml petroleum ether respectively to obtain 83.8g of dark liquid.
[0027] (2) Add Ba(OH) to 83.8g dark liquid 2 ·8H 2 O45.4g (0.144mol) and 400g water, stirring reaction at 50°C for 2h, filtering, evaporating the solvent, and crystallizing the crude product of barium trifluoromethanesulfonate, recrystallizing the crude product with ethanol 3 times, drying to obtain barium trifluoromethanesulfonate 55.3 g of crystals.
[0028] (3) Add 600 g of acetic acid to 55.3 g of barium trifluoromethanesulfonate crystals, dissolve at 30° C., then add dropwise 11.9 g (0.121 mol) of anhydrous sulfuric acid, stir, and filter to obtain an acid solution. The number of re...
Embodiment 2
[0030] (1) Get 300g trifluoromethanesulfonic acid triethylamine salt waste water in the flask, contain trifluoromethanesulfonic acid triethylamine salt 80.4g (0.32mol) in the waste water, under distillation temperature 60 ℃, 5kPa condition, water Evaporated to obtain 101.4 g of dark liquid, which were washed three times with 200 ml of dichloromethane respectively to obtain 81.4 g of dark liquid.
[0031] (2) Add Ca(OH) to 81.4g dark liquid 2 9.5g (0.128mol)) and 400g water, stirred and reacted at 20°C for 2h, filtered, evaporated the solvent, and the crude product of barium trifluoromethanesulfonate was crystallized, and the crude product was recrystallized 3 times with acetone, dried to obtain calcium trifluoromethanesulfonate 39.3 g of crystals.
[0032] (3) Add 200 g of acetonitrile to 39.3 g of calcium trifluoromethanesulfonate crystals, dissolve at 30° C., add dropwise 10.2 g (0.104 mol) of anhydrous sulfuric acid, stir, and filter to obtain an acid solution. The number...
Embodiment 3
[0034] (1) Get 300g trifluoromethanesulfonic acid triethylamine salt waste water in the flask, contain trifluoromethanesulfonic acid triethylamine salt 80.4g (0.32mol) in the waste water, under distillation temperature 60 ℃, 5kPa condition, water Evaporated to obtain 101.4 g of dark liquid, which were washed three times with 200 ml of hexane respectively to obtain 82.8 g of dark liquid.
[0035] (2) Add Sr(OH) to 82.8g dark liquid 2 19.5g (0.160mol) and 400g water, stirred and reacted at 90°C for 2h, filtered, evaporated the solvent, crystallized the crude product of strontium trifluoromethanesulfonate, recrystallized the crude product three times with distilled water, dried to obtain strontium trifluoromethanesulfonate crystal 52.7g.
[0036] (3) Add 1050 g of isopropanol to 52.7 g of strontium trifluoromethanesulfonate crystals, dissolve at 30° C., add dropwise 13.3 g (0.136 mol) of anhydrous sulfuric acid, stir, and filter to obtain an acid solution. The number of rectify...
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