Novel process for industrially synthesizing perfluoromethyl vinyl ether and 1, 1, 2, 2-tetrafluoro-1-trifluoromethoxyethane
A technology of perfluoromethyl vinyl ether and trifluoromethoxy, applied in industrial synthesis of perfluoromethyl vinyl ether and 1,1,2,2-tetrafluoro-1-trifluoromethoxyethane It can solve the problems of sub-optimal process, high energy consumption, salt formation, etc.
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Embodiment 1
[0395] with diluted F 2 The gas fluorinated HFE-254 to E227(TFTFME) in a countercurrent system (first step), and E227(TFTFME) was subjected to base-induced HF elimination to obtain PFMVE (second step).
[0396] equipment:
[0397] Columns made of Hastelloy C4, 30 cm in length, filled with HDPTFE, 5 cm in diameter were used according to the diagram below. The volume of the reservoir is 2l. The pump is a centrifugal pump from Schmitt. A pressure valve is installed at the top of the tower to regulate the pressure. Heat exchangers for heating and cooling are installed in loops such as figure 1 shown.
Embodiment 1a
[0398] Embodiment 1a (first step):
[0399] Selective direct fluorination of HFE-254 to E 227 (TFTFME).
[0400]The reservoir was filled with 1000 g (7.57 mol) of HFE-254 (1,1,2,2-tetrafluoro-1-(methoxy)ethane) and the pump was started (flow ca. 1500 l / h). 10%F 2 Gas (in N 2 medium dilution) was fed into the column through a Bronkhorst mass flow meter so that the reaction temperature was kept at 30°C, while the pressure on the column was kept at 10 bar absolute through a pressure valve. After 1 hour, 893 g (23.5 mol) F 2 (N as an inert gas 2 10% F in 2 ) is fed into the system, while the inert N 2 Along with some traces of HF formed and traces of E 227, it exited the unit through a pressure valve above the top into the high-efficiency scrubber. After a further 10 minutes of reflux without any dose, stop the pump. Samples were withdrawn from the reservoir using a high-grade stainless steel cylinder into which all material fell after the pump was stopped. The reservoir ...
Embodiment 1b
[0403] Example 1b (second step):
[0404] Base-induced HF elimination was performed on E 227 (TFTFME) to obtain PFMVE.
[0405] In the next step, the pump was restarted and 921 g (9.1 mol) NEt was dosed by using a piston metering pump before the heat exchanger 3 Feed into the refluxing reaction mixture.
[0406] For NEt used in this example 3 Note on the amount (9.1 mol): Since in Example 1a, 3 mol of HF formed in the fluorination step had been removed with ice water, based on 1000 g (7.57 mol) amount of HFE-254, considering the (1 mol) of the HF elimination step : 1) Stoichiometric, itself only needs 7.57mol NEt 3 . Due to NEt 3 Even three HFs can be absorbed (complex formation), theoretically requiring only 2.52mol NEt 3 instead of 7.57mol NEt 3 Stoichiometric (1:1). However, since phase separation is required here, the base NEt compared to (1:1) stoichiometry 3 with high excess NEt 3 use.
[0407] For this second step, the pressure was reduced to 7 bar absolute. ...
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