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CN102847448B - Allyloxy trimethylsilane and vinyl acetate copolymer gas separation membrane - Google Patents

Allyloxy trimethylsilane and vinyl acetate copolymer gas separation membrane Download PDF

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Publication number
CN102847448B
CN102847448B CN201210334475.5A CN201210334475A CN102847448B CN 102847448 B CN102847448 B CN 102847448B CN 201210334475 A CN201210334475 A CN 201210334475A CN 102847448 B CN102847448 B CN 102847448B
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China
Prior art keywords
gas separation
vinyl acetate
separation membrane
allyloxytrimethylsilane
acetate copolymer
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Expired - Fee Related
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CN201210334475.5A
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Chinese (zh)
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CN102847448A (en
Inventor
贾宏葛
马立群
王雅珍
陈密山
滕杰
胡丹丹
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Qiqihar University
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Qiqihar University
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Publication of CN102847448A publication Critical patent/CN102847448A/en
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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

本发明属于高分子材料与工程领域,特别涉及一种烯丙氧基三甲基硅烷与乙酸乙烯酯的共聚物气体分离膜,解决现有高分子型气体分离膜在气体的透过性和选择性方面相互制约关系的问题。本发明专利以烯丙氧基三甲基硅烷与乙酸乙烯酯共聚制备气体分离膜。采用本体两步聚合法,在玻璃上涂膜,制得的复合高分子型气体分离膜,具有足够的稳定性、对二氧化碳具有良好的选择性和透过性。The invention belongs to the field of polymer materials and engineering, in particular to a copolymer gas separation membrane of allyloxytrimethylsilane and vinyl acetate, which solves the problem of gas permeability and selection of existing polymer gas separation membranes. issues of mutual constraints on sexuality. The invention patent prepares gas separation membrane by copolymerization of allyloxytrimethylsilane and vinyl acetate. The composite polymer gas separation membrane prepared by coating the glass with a two-step bulk polymerization method has sufficient stability and good selectivity and permeability to carbon dioxide.

Description

Allyloxy trimethyl silane and vinyl acetate copolymer gas separation membrane
The invention belongs to macromolecular material and engineering field, be particularly related to the preparation method of a kind of allyloxy trimethyl silane and vinyl acetate copolymer gas separation membrane, solved existing polymer electrolyte gas separation membrane the permeability of gas and selective aspect the problem of mutual restricting relation
It is a kind of " green technology " that gas film separates, and due to it have advantages of that separative efficiency is high, it is low to consume energy, simple to operate.With the competition of traditional isolation technics in demonstrate unique advantage, its research and application development are very rapid.The macromolecule member material that has been applied to gas film separation field has polyimides (PI), cellulose acetate (CA), dimethyl silicone polymer (PDMS), polysulfones (PS), Merlon (PC) etc., but the permeability of existing polymer electrolyte gas separation membrane gas and selective aspect all exist the relation of mutual restriction, unstable chemcial property, does not also possess industrialized condition.
Selectively will relative mistake in the time that gas-premeable is good a little in order to overcome existing polymer electrolyte gas separation membrane, selective good time, the permeability of gas this problem that will be affected, patent of the present invention provides a kind of new polymer electrolyte gas separation membrane, has improved the selective and permeability of carbon dioxide.
The technical scheme that patent of the present invention adopts is: adopt polymerisation in bulk to make polymer, obtain polymer film at film on glass, concrete technology is as follows: first in there-necked flask, add successively vinyl acetate 100 parts of (molal quantity), allyloxy trimethyl silane 40-70 parts (molal quantity), 0.1~0.4 part of initator azodiisobutyronitrile (molal quantity).Then add lesser trochanter, use spherical condensation tube cooling for reflux.At 50 DEG C~70 DEG C, react 15h~25h.After pre-polymerization completes, pour reactant liquor into bottle, little bottle cap is tightened and proceeded in baking oven, continue polymerization 20h~28h at 60 DEG C~80 DEG C.Again polyvinylidene fluoride microporous film is laid on glass plate.In the time that reactant liquor becomes faint yellow sticking liquid, diluted with oxolane, be poured on polyvinylidene fluoride microporous film, through 5~8 hours, on glass plate, there will be a transparent film, taken and make off allyloxy trimethyl silane and vinyl acetate copolymer gas separation membrane.
Patent beneficial effect of the present invention is that the novel high polymer gas separation membrane making not melting under the condition of heating also just has enough stability in solvent, has preferably selectively well water-fast, heatproof and weather-proof, CO 2/ N 2mist sees through middle N 2/ CO 2separation reaches 11.5, CO 2infiltration coefficient can reach 40 barrers more than; CO 2/ CH 4mist sees through middle CO 2/ CH 4separation reaches more than 3, CO 2infiltration coefficient can reach 18 barrers more than, can meet to a certain extent N 2/ CO 2separation requirement.

Claims (1)

1.一种烯丙氧基三甲基硅烷与乙酸乙烯酯共聚物气体分离膜制备方法,其特征在于采用本体两步聚合法,首先是预聚,在三口瓶中依次按摩尔量加入乙酸乙烯酯100份、烯丙氧基三甲基硅烷40-70份、引发剂偶氮二异丁腈0.1~0.4份,然后加入小转子,在50℃~70℃下反应15h~25h,预聚完成后,将反应液倒入小瓶,将小瓶盖拧紧转入烘箱中,在60℃~80℃继续聚合20h~28h,当反应液变为淡黄色有粘性的液体时,用四氢呋喃将其稀释,倒在铺有聚偏氟乙烯微孔膜的玻璃板上,经过5~8个小时,玻璃板上会出现一张透明的薄膜,将其揭下即制得烯丙氧基三甲基硅烷与乙酸乙烯酯共聚物气体分离膜。 1. a kind of allyloxytrimethylsilane and vinyl acetate copolymer gas separation membrane preparation method, it is characterized in that adopt bulk two-step polymerization method, at first be prepolymerization, in there-necked bottle, add vinyl acetate in molar quantity successively 100 parts of ester, 40-70 parts of allyloxytrimethylsilane, 0.1-0.4 parts of initiator azobisisobutyronitrile, then add small rotor, react at 50℃~70℃ for 15h-25h, prepolymerization is completed Finally, pour the reaction liquid into a small bottle, tighten the cap of the small bottle and transfer it to an oven, and continue to polymerize at 60°C to 80°C for 20h to 28h. When the reaction liquid turns into a light yellow viscous liquid, dilute it with tetrahydrofuran. Pour it on a glass plate covered with polyvinylidene fluoride microporous membrane, after 5 to 8 hours, a transparent film will appear on the glass plate, which can be peeled off to obtain allyloxytrimethylsilane and Vinyl acetate copolymer gas separation membrane.
CN201210334475.5A 2012-09-12 2012-09-12 Allyloxy trimethylsilane and vinyl acetate copolymer gas separation membrane Expired - Fee Related CN102847448B (en)

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CN102847448B true CN102847448B (en) 2014-07-02

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108479435A (en) * 2018-04-16 2018-09-04 哈尔滨工业大学 A kind of preparation method of ceramic base polyvinyl acetate composite membrane

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101733029A (en) * 2008-11-14 2010-06-16 中国科学院大连化学物理研究所 Method for preparing CO2 separation membrane material and composite membrane
CN102008909A (en) * 2010-12-13 2011-04-13 大连欧科膜技术工程有限公司 Preparation method for gas separation composite membrane
JP2011224553A (en) * 2010-03-29 2011-11-10 Fujifilm Corp Gas separation membrane, method for producing the same, method for separating gas mixture using them, gas separation membrane module, and gas separation device

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101733029A (en) * 2008-11-14 2010-06-16 中国科学院大连化学物理研究所 Method for preparing CO2 separation membrane material and composite membrane
JP2011224553A (en) * 2010-03-29 2011-11-10 Fujifilm Corp Gas separation membrane, method for producing the same, method for separating gas mixture using them, gas separation membrane module, and gas separation device
CN102008909A (en) * 2010-12-13 2011-04-13 大连欧科膜技术工程有限公司 Preparation method for gas separation composite membrane

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