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淤浆法制备聚(异丁烯-co-对甲基苯乙烯)无规共聚物及其溴化与可逆硫化研究

Preparation of BIMS random copolymer by slurry method and its bromination and reversible vulcanization
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摘要 通过正离子聚合淤浆法,以异丁烯和对甲基苯乙烯为原料、二氯乙基铝/2-氯-2,4,4-三甲基戊烷(AlEtCl2/TMPCl)为引发体系,制备了无规共聚物,并使用自由基引发剂偶氮二异庚腈(AVBN)在55℃遮光条件下进行溴化得到主链结构全饱和的溴化聚(异丁烯-co-对甲基苯乙烯)无规共聚物(BIMS),使用四甲基乙二胺(TEMED)与自制的可逆硫化剂双环戊二烯二甲酸钾盐[DCPD(COOK)2]进行硫化加工。结果表明:在-86℃下进行反应,AlEtCl2与TMPCl摩尔比为18时,稳定性及重复性较好,其分子量达到24kg/mol;自由基引发剂AVBN质量含量在0.75×10-3%时,溴化反应效果较好;DCPD(COOK)2与TEMED相比具有更好的效果,二次硫化加工时拉伸强度平均下降10.6%,断裂伸长率平均下降16.5%,在添加5份DCPD(COOK)2时拉伸强度最大,达到4.9MPa,具有较好的再加工性。 Random copolymers were prepared by cationic polymerization slurry method with isobutylene and pmethylstyrene as raw materials and AlEtCl2/TMPCl as initiator.The free radical initiator AVBN was brominated under the shading condition of 55℃to obtain brominated poly(isobutene-co-p-methylstyrene)random copolymer(BIMS)with fully saturated main chain structure.Tetramethylethylenediamine(TEMED)and potassium dicyclopentadienyl dicarboxylate[DCPD(COOK)2],a self-made reversible vulcanizing agent,were used for vulcanization.The results showed that when the molar ratio of AlEtCl2 to TMPCl was 18,the stability and repeatability of the reaction were good,and the molecular weight reached 24 kg/mol.When the dosage of free radical initiator AVBN was 0.75×10-3 wt%,the effect of bromination reaction was better.Compared with TEMED,DCPD(COOK)2 had better effect.The average tensile strength and elongation at break decrease by 10.6%and 16.5%during secondary vulcanization.When adding 5 phr DCPD(COOK)2,the tensile strength reached 4.9 MPa,which had better reprocessability.
作者 田英鑫 商育伟 伍一波 杨丹 李树新 郭文莉 Tian Yingxin;Shang Yuwei;Wu Yibo;Yang Dan;Li Shuxin;Guo Wenli(Beijing Key Lab of Special Elastomeric Composite Materials,Department of Materials Science and Chemical Engineering,Beijing Institute of Petrochemical Technology,Beijing 102617;College of Materials Science and Engineering,Beijing University of Chemical and Technology,Beijing 100029)
出处 《化工新型材料》 CAS CSCD 北大核心 2020年第7期159-163,共5页 New Chemical Materials
关键词 正离子聚合 无规共聚物 异丁烯 溴化 可逆硫化 cationic polymerization random copolymer isobutylene bromination reversible vulcanization
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