Copolymerization of N-phenylmaleimide and propylene oxide initiated with organozinc compounds
Copolymerization of N-phenylmaleimide and propylene oxide initiated with organozinc compounds
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DOI：
10.1021/ma00194a090
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发表时间：
1989-07
期刊：
影响因子：
5.5
通讯作者：
T. Hagiwara;Masahiko Takeda;H. Hamana;T. Narita
中科院分区：
文献类型：
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作者：
T. Hagiwara;Masahiko Takeda;H. Hamana;T. Narita
将纯化的IV-PMI和PO在封闭式玻璃瓶中，在纯氮气氛下进行聚合。11用盐酸/甲醇终止反应，将反应混合物倒入甲醇中。将沉淀物(不溶于甲醇的部分)过滤出来，在110℃的真空下干燥，通过蒸发甲醇(沉淀剂)，用苯提取，然后将苯溶液冷冻干燥，收集甲醇可溶聚合物。表2总结了IV-PMI(3 Mmo1)和PO(59 Mmo1)与有机锌化合物的共聚结果。只有3个给出了IV-PMI和PO作为不溶于甲醇的聚合物的可观产率。图1显示了通过与表II中的3进行共聚得到的不溶于甲醇的聚合物的NMR12。在1.2(E)、1.8(D)和3.8ppm(B)处的吸收分别是聚合物中PO单元的甲基、亚甲基和亚甲基的可分配基团。分别将7.2ppm(A)的峰和3.0-5.3ppm的宽峰(c：用虚线表示与PO单元的亚甲基团重叠的信号)指认给苯基和亚甲基团
Polymerizations were carried out with purified IV-PMI and PO in sealedglass ampules under purified nitrogen atmosphere. 11 The reaction was terminated with hydro-chloric acid/methanol and the reaction mixture was poured into methanol. The precipitate (methanol-insoluble part) was filtered off and dried under vacuum at 110 C. The methanol-soluble polymer was collected by evaporation of methanol (precipitant) and extraction with benzene, fol-lowed by freeze-drying of the benzene solution. Results of copolymerization of IV-PMI (3 mmol) and PO (59 mmol) with organozinc compounds are summarized in Table II. Only 3 gives an appreciable yield of copolymer from IV-PMI andPO as methanol-insoluble polymer. Figure 1 shows NMR12 of the methanol-insoluble polymer obtained by the copolymerization with 3 in Table II. Absorptions at 1.2 (e), 1.8 (d) and 3.8 ppm (b) are assignable tomethyl, methylene and methine groups of PO units in the polymer, respectively. A peak at 7.2 ppm (a) and broad one from 3.0 to 5.3 ppm (c: shown bydotted line with the overlapping signal of methine groups of PO units) are assigned, respectively, to phenyl and methine