Preparation method and application of perfluoro hexanone
The technology of perfluorohexanone and fluorine ring is applied in the field of preparation of perfluorohexanone, and can solve the problems of complex production process of perfluorohexanone, low relative volatility of perfluorohexanone, influence on the purity of perfluorohexanone finished product, etc. , to achieve the fire-extinguishing effect of green environmental protection, good fire-extinguishing effect, and the effect of improving yield and purity
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[0018] The preparation method of the perfluorohexanone of the present embodiment may comprise the following steps:
[0019] Mix 90-100 parts by weight of hexachloropropene with 94-118 parts by weight of catalyst (solution form), then react at 30-40°C and 0.1-0.15 MPa, and collect the reaction product with the largest specific gravity, for example, statically The layers were separated, and the lower layer was collected to obtain a dimer of hexafluoropropylene.
[0020] As an option, the catalyst includes 90-110 parts by weight of acetonitrile, 3-5 parts by weight of amine catalyst and 1-3 parts by weight of fluorine-containing salt. Among them, the amine catalyst is preferably tetramethylethylenediamine. The fluorine-containing salt includes at least one of sodium fluoride, potassium fluoride, cesium fluoride, potassium bifluoride, phosphorus pentafluoride and sulfur tetrafluoride, preferably potassium fluoride.
[0021] Specifically, 90-100 parts by weight of acetonitrile, 3...
Embodiment 1
[0040] Mix 90 kg of acetonitrile, 3 kg of tetramethylethylenediamine, and 1 kg of a mixture of sodium fluoride and cesium fluoride, blow in nitrogen gas, and react with stirring at 35° C. for 1.2 h to obtain a yellow catalyst solution. Then add 18 kilograms of hexachloropropene per hour in the catalyst solution, adding 90 kilograms of hexachloropropene in total. React under the conditions of 30°C and 0.1MPa, stand still for 6min every 0.8h, collect the lower layer, and obtain a hexafluoropropylene dimer containing perfluoro-2-methyl-2-pentene with a purity of 88%.
[0041] Add 250 kg of the above-mentioned hexafluoropropylene dimer and 40 kg of 1,1,2-trichlorotrifluoroethane into the reactor, stir and cool to 13°C, and then add 500 kg of calcium hypochlorite solution dropwise , the length of dropping is 7.5h. Wherein, the mass concentration of active chlorine contained in the calcium hypochlorite solution is 8%. Adjust the temperature of the reaction system after adding the ...
Embodiment 2
[0044] Mix 100 kilograms of acetonitrile, 5 kilograms of tetramethylethylenediamine and 3 kilograms of potassium hydrofluoride, phosphorus pentafluoride and sulfur tetrafluoride mixture, feed nitrogen, and stir the reaction at 45 ° C for 0.8 h, to obtain a yellow catalyst solution. Then add 22 kilograms of hexachloropropene per hour in the catalyst solution, adding 110 kilograms of hexachloropropene in total. React under the conditions of 40°C and 0.15MPa, stand still for 4min every 1.2h, collect the lower layer, and obtain a hexafluoropropylene dimer containing perfluoro-2-methyl-2-pentene with a purity of 90%.
[0045] Add 130 kg of the above-mentioned hexafluoropropylene dimer to the reactor, then add 90 kg of acetonitrile and 1,1,2-trichlorotrifluoroethane mixture, 3 kg of 15-crown-5 amine and 0.8 Kg of powdered potassium fluoride was stirred and reacted at 40°C for 15 hours. After standing still for 15 min, the lower layer was collected to obtain perfluoro-2-methyl-2-pe...
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