Synthetic method of perfluoropolyether
A technology of perfluoropolyether and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of high cost, high degree of danger, complex process of metal hydride, etc., and achieve the effects of avoiding the use of diluent, low cost and simple process
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[0018] The invention provides a kind of synthetic method of perfluoropolyether, comprising:
[0019] A) react the first volume part of purified hexafluoropropylene oxide gas with alkali metal fluoride in an aprotic solvent at 0°C to 50°C to obtain an oligomer;
[0020] B) Lower the temperature of the oligomer obtained in step A) to -40°C to -20°C, add the second volume part of purified hexafluoropropylene oxide gas to it, and react to obtain perfluoropolyether.
[0021] The present invention adopts a synthesis process of feeding materials and temperature control in stages to prepare perfluoropolyether. Firstly, the first volume part of purified hexafluoropropylene oxide gas and alkali metal fluoride are carried out in an aprotic solvent at 0°C to 50°C. Reaction to obtain oligomers; then lower the temperature of the obtained oligomers to -40°C to -20°C, add the second volume of purified hexafluoropropylene oxide gas to it, and react to obtain perfluoropolyether, so that six Th...
Embodiment 1
[0033] The raw material hexafluoropropylene oxide gas is passed into two groups of adsorption towers filled with purifying agents, wherein the first group of adsorption towers is filled with aluminum hydroxide, and the second group of adsorption towers is filled with silica gel; when the pressure in the adsorption tower rises to 0.2 At MPa, discharge the purified hexafluoropropylene oxide gas from the end of the adsorption tower at a gas velocity of 4L / h. After stabilizing for 2 hours, the gas purification in the tower reaches an equilibrium state. After testing, the purified hexafluoropropylene oxide gas is , the acid gas content is 0.01wt%, the water content is 5ppm, and the hexafluoroacetone content is 0.006wt%.
[0034] Under the protection of high-purity nitrogen, 10g of cesium fluoride powder and 200g of tetraethylene glycol dimethyl ether, which have been strictly dewatered, were quickly added to a 2L stainless steel reaction kettle, and then the reaction kettle was seal...
Embodiment 2
[0036] The raw material hexafluoropropylene oxide gas is passed into two groups of adsorption towers filled with purifiers, wherein the first group of adsorption towers is filled with soda lime, and the second group of adsorption towers is filled with silica gel; when the pressure in the adsorption tower rises to 0.1MPa , discharge the purified hexafluoropropylene oxide gas from the end of the adsorption tower at a gas velocity of 4L / h. After stabilizing for 2 hours, the gas purification in the tower reaches an equilibrium state. After testing, in the purified hexafluoropropylene oxide gas, The acid gas content is 0.06wt%, the water content is 0.5ppm, and the hexafluoroacetone content is 0.004wt%.
[0037] Under the protection of high-purity nitrogen, 12g of cesium fluoride powder and 160g of tetraethylene glycol dimethyl ether, which have been strictly dewatered, were quickly added to a 2L stainless steel reaction kettle, and then the reaction kettle was sealed and the system ...
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