Method for removing unsaturated impurities in crude products of 1,1,2,3,3,3-hexafluoropropyl hydrofluoroether
A hexafluoropropyl hydrofluoroether, unsaturated technology, applied in ether preparation, ether separation/purification, organic chemistry, etc., can solve the problem of high cost of n-hexylamine, and achieve low cost, low risk, and mild reaction conditions Effect
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Embodiment 1
[0033] Embodiment 1: Preparation of crude product of 1,1,2,3,3,3-hexafluoropropyl ethyl ether
[0034] In the autoclave, add 200g of sodium hydroxide and 460g of absolute ethanol, close the autoclave, replace the air in the autoclave with nitrogen, cool the autoclave to 0°C, and feed a total of 1500g of hexafluoropropylene into the autoclave, during which the feeding of hexafluoropropylene is controlled. Speed, so that the reaction temperature does not exceed 40 ° C, after passing a specified amount of hexafluoropropylene, keep stirring until the reaction temperature and pressure no longer change, collect the reaction solution, wash with water to obtain 1,1,2,3,3,3-hexafluoro Propyl ethyl ether crude product 1460g. GC analysis results showed that in the crude product of 1,1,2,3,3,3-hexafluoropropyl ethyl ether, CF 3 CHFCF 2 -O-CH 2 CH 3 The content of 77.8%, C 3 f 5 -O-CH 2 CH 3 Content 12.4%, other impurity content 9.8%.
[0035]This method is a general method for th...
Embodiment 2
[0036] Example 2: Removal of unsaturated impurities in the crude product of 1,1,2,3,3,3-hexafluoropropyl ethyl ether
[0037] In a three-necked flask equipped with a stirring device, 2850 g of crude 1,1,2,3,3,3-hexafluoropropyl ethyl ether prepared by the method described in Example 1 was added. After testing, the total content of unsaturated impurities in the crude 1,1,2,3,3,3-hexafluoropropyl ethyl ether is 12.4% (about 2mol), wherein CF 3 CF=CF-O-CH 2 CH 3 Content is 7.9%, CF 2 = CFCF 2 -O-CH 2 CH 3 4.5%. Then add 322 g (7 mol) of ethanol and 120 g (3 mol) of sodium hydroxide into the three-necked flask, stir and raise the temperature to 50° C., and keep the reaction for 4 h. After the reaction is complete, filter out the insoluble solids in the three-necked flask, and carry out rectification. Control the rectification temperature at 80-120°C, the rectification pressure at normal pressure, the number of theoretical plates in the rectification column is 10, and collec...
Embodiment 3
[0041] Example 3: Removal of unsaturated impurities in the crude product of 1,1,2,3,3,3-hexafluoropropyl methyl ether
[0042] In a three-necked flask equipped with a stirring device, 1310 g of crude 1,1,2,3,3,3-hexafluoropropyl methyl ether prepared by the method described in Example 1 was added. After testing, the total content of unsaturated impurities in the crude 1,1,2,3,3,3-hexafluoropropyl methyl ether is 8.7% (about 0.7mol), wherein CF 3 CF=CF-O-CH 3 Content is 5.7%, CF 2 = CFCF 2 -O-CH 3 3.0%. Then, 70 g (2.2 mol) of methanol and 40 g (1.0 mol) of sodium hydroxide were added into the three-necked flask, stirred and heated to 40° C., and kept for 2 h. After the reaction is complete, filter out the insoluble solids and carry out rectification. Control the rectification temperature to 65-100°C, the rectification pressure to normal pressure, and the number of theoretical plates in the rectification column to be 10. Collect fractions at 53-55°C to obtain the target pr...
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