Method for preparing polyacrylonitrile (PAN)-base microporous membrane
A technology based on polyacrylonitrile and acrylonitrile, which is applied in the field of film preparation, can solve the problems of high price of polyvinylidene fluoride, poor weather resistance, high low temperature brittleness, etc., and achieve more diverse products, excellent mechanical properties, and production efficiency high effect
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[0012] The preparation method of the polyacrylonitrile-based microporous membrane designed by the present invention (referred to as the preparation method), the preparation method adopts the TIPS process method, including the following process steps:
[0013] 1. Prepare meltable acrylonitrile-based copolymers (referred to as copolymers). The copolymer is prepared from an acrylonitrile monomer and a second monomer through an emulsion polymerization process, an aqueous phase precipitation polymerization process, a solution polymerization process or a template polymerization process, and the glass transition temperature in the polymerization process is controlled at 70-150°C; The molar ratio of the acrylonitrile monomer to the second monomer is 95 / 5 to 70 / 30, and the sum of the molar contents of the two monomers is 100%; add 0.01 to 2 wt% of dodecane in the total amount of the monomer or copolymer Mercaptan is a chain transfer agent; the polymerization temperature is 20-80°C, the...
Embodiment 1
[0029] The meltable acrylonitrile / vinyl acetate copolymer is prepared by the aqueous phase precipitation polymerization method. The specific process is: in the polymerization kettle equipped with a mechanical stirrer and a reflux condenser, add deionized water as the reaction medium, and rinse the reaction kettle with dry nitrogen. Finally, add acrylonitrile and vinyl acetate monomers respectively, the feeding molar ratio is 80 / 20, and then add 5mmol% of the total amount of monomers of sodium bisulfite and 2wt% of the total amount of monomers of chain transfer agent - dodecyl Mercaptan, after stirring evenly, add potassium persulfate of 2.5mmol% of the total amount of monomers, stir and react at 80°C for 3 hours, stop stirring, filter to remove the water in the system, wash with deionized water for 3 times, at 80°C Dry in a vacuum oven to constant weight, remove water, and obtain a meltable acrylonitrile / vinyl acetate copolymer.
[0030] Add meltable acrylonitrile / vinyl acetat...
Embodiment 2
[0033] The meltable acrylonitrile / propyl methacrylate copolymer is prepared by the aqueous phase precipitation polymerization method. The specific process is: in the polymerization kettle equipped with a mechanical stirrer and a reflux condenser, add deionized water as the reaction medium, and rinse with dry nitrogen. After the reactor, first add 3mmol% sodium bisulfite of the total amount of monomers and 0.01wt% chain transfer agent-dodecyl mercaptan of the total amount of monomers into the reactor, and then add the total amount of monomers after stirring evenly. Amount of 0.5mmol% potassium persulfate, acrylonitrile and propyl methacrylate monomer (feeding molar ratio is 88 / 12) are mixed evenly and then added to the reactor in 5 times, 20wt% each time, the time interval is 36min, The reaction temperature is 20°C, continue to react for 1 hour after the addition, stop stirring, remove the water in the system by filtration, wash with deionized water for 3 times, dry to constant ...
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