Synthetic method of polymerizable total-fluorine polyether monomer
A technology of perfluoropolyether and synthesis method, applied in the field of coatings, can solve the problems of complex preparation method, increased operation difficulty, explosion, etc., and achieve the effects of simple synthesis method, strong environmental protection performance and strong applicability
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[0027] A kind of polymerizable perfluoropolyether monomer synthesis method of the present invention comprises the following steps:
[0028] Step 1, synthetic perfluoropolyether fluoride (CF 3 CF 2 [CF 2 OCF (CF 3 )] n COF):
[0029] The following components are prepared according to the following weight percentages: 90-95% of hexafluoropropylene oxide, 0.14-0.27% of fluorine salt, and 4.88-9.77% of aprotic polar solvent;
[0030] Add metal sodium wire to the aprotic polar solvent, let it stand until no hydrogen is generated, and obtain the aprotic polar solvent after water removal;
[0031] Provide a stainless steel pressure vessel with a stirrer, pass nitrogen gas into the pressure vessel for leak detection, then add the fluoride salt and the dewatered aprotic polar solvent into the pressure vessel, and cool to -60 ~20°C, and vacuum;
[0032] Start the agitator, adjust the temperature in the pressure vessel to -10-20°C, add the hexafluoropropylene oxide into the pressu...
Embodiment 1
[0050] Put 74.00g of QF-1 in a 250ml three-neck round-bottomed flask with a magnetic stirrer and a condenser tube, add 10.00g of anhydrous methanol (CH3OH) dropwise, and shake slightly to make the anhydrous methanol and QF-1 mix evenly and release After the three-neck flask was naturally cooled and the mixture was separated into layers, about 2 g of NaHCO3 was added, and magnetically stirred at room temperature for 18 h.
[0051] Take out the three-neck bottle and let it stand, remove the upper layer after the mixture is clearly separated, add about 800ml of secondary deionized water to the lower layer in batches, wash away the HF generated by the reaction, until the washing liquid is neutral.
[0052] Add 20g of methanol to the oil phase, shake it fully to dissolve the remaining water into the methanol, then let it stand for stratification, remove the upper layer, repeat this step three times, after the last oscillation, fully reflux the mixture in a 70°C oil bath for 20min, ...
Embodiment 2
[0054] Put 50g of QF-2 in a 250ml three-necked round-bottomed flask with a magnetic stirrer and a condenser tube, purged with nitrogen to remove the air, put the three-necked flask in a water bath at 30°C, and added 4g of ethanolamine (NH2CH2CH2OH) and 50g of trifluorotrifluorotri Ethyl chloride (F113), the mixture was stirred for 3 h, then 50 ml of F113 and about 50 ml of 5% HCl solution were added, and the lower layer was washed twice to remove unreacted ethanolamine and generated methanol.
[0055] The lower oil phase was rotary evaporated under reduced pressure at 40°C and -0.1MPa to remove trifluorotrichloroethane, and a light yellow transparent viscous liquid was obtained.
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