Preparation method of fluorocarbon polyether compound
The technology of polyether compound and fluorocarbon polyether is applied in the field of preparation of fluorocarbon polyether compound, can solve the problems of increased cost, high price of antimony pentafluoride, poor conversion effect, etc., and achieves excellent high temperature stability, low cost effect
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Embodiment 1
[0018] 0.05mol C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF(CF 3 )COOH (average weight-average molecular weight 3000) and 0.005mol of antimony trifluoride dried at 200°C for 2 hours were added to a 250ml Monel alloy autoclave, vacuum-nitrogen replaced three times, and then fluorine gas containing 0.1mol of fluorine gas was added / Nitrogen (volume ratio 40 / 60) mixed gas, start stirring, heat up to 160°C within 15 minutes and react for 6 hours, then vent the autoclave, filter to remove metal fluorides, distill off low boiling point components, and the residue weighs 142.6g. Infrared detection showed that the fluorocarbon polyether carboxylic acid was completely converted into the product C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF 2 CF 3 , yield 95.1%.
Embodiment 2
[0020] 0.05mol C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF(CF 3 )COOH (average weight-average molecular weight 3000) and 0.02mol of antimony trifluoride dried at 200°C for 2 hours were added to a 250ml Monel alloy autoclave, vacuum-nitrogen replaced three times, and then fluorine gas containing 0.2mol of fluorine gas / Nitrogen (volume ratio 40 / 60) mixed gas, start stirring, heat up to 120°C within 10 minutes and react for 10 hours, vent the autoclave, filter to remove metal fluorides, distill off low boiling point components, the residue weighs 139.2g, Infrared detection showed that the fluorocarbon polyether carboxylic acid was completely converted into the product C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF 2 CF 3 , yield 92.8%.
Embodiment 3
[0022] 0.05mol C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF(CF 3 )COOH (average weight-average molecular weight 3000) and 0.006mol of silver fluoride dried at 200°C for 2 hours were added to a 250ml Monel alloy autoclave, vacuum-nitrogen replaced three times, and then fluorine / nitrogen containing 0.2mol of fluorine was added (Volume ratio 30 / 70) Mixed gas, heat up while stirring, heat up to 200°C within 20 minutes, react for 6 hours, empty the autoclave, filter to remove metal fluorides, distill off low boiling point components, and the residue weighs 143.1g , Infrared detection showed that the fluorocarbon polyether carboxylic acid was completely converted into the product C 3 f 7 O(CF(CF 3 ) CF 2 O) p CF 2 CF 3 , yield 95.4%.
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