Preparation method for co-production of 1, 1-bis(trifluoromethoxy)difluoroethylene and 1, 2-bis(trifluoromethoxy)difluoroethylene
A technology of trifluoromethoxy and difluoroethylene is applied in the field of preparation of 1,1-difluoroethylene co-producing 1,2-difluoroethylene, which can solve the problem that by-products are difficult to utilize, waste liquid is difficult to treat, and Raw materials are not easy to obtain and other problems, to achieve the effect of simple separation and purification, low production equipment requirements, and high efficiency
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Embodiment 1～4
[0034] A Reaction—Prepare a 1L autoclave with stirring, pressure gauge and temperature control device and complete airtightness. First, add 500g of 1,2-dichloroethylene (mixture of cis and trans isomers, cis ratio figure 1 shown), and a small amount of protective agent; subsequently, carry out N to the autoclave 2 Replace three times, control the oxygen content to be less than 15mg / L, and pass high-purity CF at -50°C to -10°C 3 OF, control the reaction pressure 0.1MPa~0.5MPa, and the reaction time 0.5h~2h; finally, the sampling analysis is qualified, the reaction is completed, the pressure is released, the nitrogen is replaced once, the lye is neutralized, layered, washed, dried, and purified by rectification. Get ClCF 3 OCHCHClF pure product, the test results of different conditions are shown in the following table 1.
[0035] Table 1: ClCFs 3 OCHCHClF preparation test results
[0036]
[0037]
Embodiment 5～8
[0039] Reaction B—Prepare a 1L autoclave with stirring, pressure gauge and temperature control device and complete airtightness. First, add 500g ClCF 3 OCHCHClF, 40% concentration alkali liquor and 0.25g phase transfer catalyst; Subsequently, carry out N to autoclave 2 After three replacements, the temperature of the stuffy kettle was raised to 50°C-100°C, and the reaction time was 2h-4h; finally, the sampling analysis was qualified, and the reaction ended. cooling, layering, washing with water, and drying to obtain mixture a, which includes CF 3 OCH=CCIF and ClCF 3 OC=CHF, the test results under different conditions are shown in Table 2 below.
[0040] Table 2: Preparation test results of mixture a
[0041]
Embodiment 9～13
[0043] C Reaction—Prepare a 1L autoclave with stirring, pressure gauge and temperature control device and complete airtightness. First, add 500 g of mixture a, which includes CF 3 OCH=CCIF and ClCF 3 OC=CHF, and 0.25g protective agent; Subsequently, carry out N to autoclave 2 Replace three times, control the oxygen content to be less than 15mg / L, and pass high-purity CF at -40°C to 10°C 3 OF, control the reaction pressure 0.3MPa~0.6MPa, and the reaction time 0.5h~2h; finally, the sampling analysis is qualified, the reaction is completed, the pressure is released, the nitrogen is replaced once, the lye is neutralized, separated, washed with water, and dried to obtain the crude product mixture b , mixture b includes (CF 3 O) 2 CHCCIF 2 、CF 3 OFCHClFOCF 3 、FClCF 3 OCCHFOCF 3 , (CF 3 O) 2 ClCCHF 2 . The test results under different conditions are shown in Table 3 below.
[0044] Table 3: Preparation test results of mixture b
[0045]
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