Method for preparing polyacrylonitrile (PAN)-base microporous membrane

A polyacrylonitrile-based and acrylonitrile-based technology, 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 diversified products, excellent mechanical properties, and preparation efficiency. high effect

Active Publication Date: 2012-12-05
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyethylene has poor oxidation resistance and UV resistance, polypropylene has high low temperature brittleness and poor weather resistance, polyvinylidene fluoride is expensive, and has poor stability in negative ion solutions, which are not as good as PAN microporous membranes.
However, due to the strong dipole force between the cyano group and the cyano group on the main chain of the PAN macromolecule, it decomposes without melting when heated, so there is no relevant report on the preparation of PAN-based microporous membranes by the TIPS method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[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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Abstract

The invention discloses a method for preparing a polyacrylonitrile (PAN)-base microporous membrane, which adopts a thermally induced phase separation (TIPS) technology and comprises the steps of: 1, preparing meltable acrylonitrile-base copolymer: adopting a mixture of acrylonitrile monomer and second monomer, which has the mixing molar ratio of 95:5-70:30, and preparing the meltable acrylonitrile-base copolymer through a polymerization technology; 2, preparing acrylonitrile-base casting film liquid: adding the copolymer and diluent into a reactor according to a weight ratio of 1:9-5:5wt%, heating to 140-230 DEG C, forming the uniform solution, then defoaming for 10-60 minutes, and producing PAN-base casting film liquid; and 3, preparing a microporous membrane: adopting a flat membrane preparation method which comprises of pouring the casting film liquid into a mould which is preheated to 150-230 DEG C, calendaring molding, cooling, solidifying, and extracting to obtain the product; adopting a hollow membrane preparation method which comprises of pouring the casting film liquid into a spinning machine, extruding at 150-230 DEG C, and extracting the diluent to obtain the product.

Description

technical field [0001] The invention belongs to membrane preparation technology, in particular to a method for preparing polyacrylonitrile (PAN)-based microporous membranes by adopting a heat-induced phase separation process. Background technique [0002] Membrane separation technology is currently the most widely used separation membrane with the largest total sales due to its functions of separation, concentration, purification and refining, as well as high efficiency, energy saving, environmental protection, molecular level filtration and simple filtration process, easy to control, etc. , are widely used in food, medicine, biology, environmental protection, water treatment, electronics and bionics and other fields, have produced huge economic and social benefits, and have received widespread attention. PAN microporous membrane has the characteristics of low cost, easy film formation, high mechanical strength, solvent resistance, UV resistance, corrosion resistance, hydrop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/42B01D69/06B01D69/08B01D67/00
Inventor 韩娜张兴祥王宁熊俊诚彭伟伟
Owner TIANJIN POLYTECHNIC UNIV
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