Method for preparing perfluor alkyl ethide phosphite ester
A technology of perfluoroalkyl ethyl phosphite and perfluoroalkyl ethanol is applied in the field of preparation of perfluoroalkyl ethyl phosphite, which can solve the problem of electrochemical instability of flame retardant additives and negative performance of lithium ion batteries. Influence and other issues, to achieve the effects of good electrochemical stability and thermodynamic stability, obvious flame retardant effect, and good comprehensive performance
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[0037] Step 1 Synthesis
[0038] In a 2000mL four-neck flask, configure a cold bath with a freezing temperature of less than -10°C, a thermometer with a range of -50°C to +150°C, with stirring, and a condensing reflux tube with a freezing temperature of less than -10°C (exhaust gas discharge ), equipped with HCl tail gas absorption device. 1681g of CF with a content greater than 99% 3 CH 2 Put OH into a four-neck flask, stir, turn on the freezer, cool down to -10°C, slowly add 770g of PCl with a content greater than 99% dropwise through a constant pressure titration funnel 3 , The dropping process continued for 5h, and the generated HCl gas was absorbed and removed by the absorption device. When no HCl gas is generated, turn on a small amount of N 2 , bubbling to drive away free HCl, use acid-base extensive pH test to release gas, when it is weakly acidic, stop bubbling N 2 ;
[0039] Step 2 neutralizes and removes impurities (CF 3 CH 2 O) 2 POH and Filtration
[004...
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