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首页> 外文期刊>繊維学会誌 >Consideration of Solvent Effect on Precipitation Polymerization of Poly(ether-ketone)s via Friedel-Craft Acylation
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Consideration of Solvent Effect on Precipitation Polymerization of Poly(ether-ketone)s via Friedel-Craft Acylation

机译：考虑溶剂对Friedel-Craft酰化聚醚醚沉淀聚合的影响

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Precipitation polymerization of diphenyl ether and isophthaloyl chloride catalyzed by AlCl_3 via Friedel-Crafts acylation was examined in various solvents to clarify the polymerization behavior. Polymerizations were carried out in three categorized solvents based on the solubility to both catalyst and polymer, which were cyclohexane (CH), 1,2-dichloroethane (DCE) and DCE containing 2 wt% nitrobenzene (2%-NB). In DCE which was widely used, the oligomers were precipitated as a form of the complex with AlCl_3 at the early stage of polymerization. The precipitates of the oligomers were swollen by the solvent, in which any short-range regular structure did not exist. The further polymerization proceeded even in the precipitates with eliminating by-produced HCl, and high molecular weight poly(ether-ketone)s (PEK) were finally formed. Nevertheless the reaction in 2%-NB yielded the well-swollen precipitates, the high molecular weight PEK was not synthesized in the precipitates because the reaction was terminated by not only the inefficient elimination of HCl due to the higher solubility of HCl but also the deactivation of catalyst by coordination of NB to AlCl_3. Although the precipitation occurred more readily in CH due to the lower solubility of oligomers, the polymer was not synthesized in the precipitates. The resulting precipitates comprised of the dimers were not swollen in this case, and thereby it was very difficult to react between dimers and eliminate HCl from the precipitates. The solvents having high miscibility to catalyst and the polymers, low solubility of HCl gas, and no basicity are necessary for making high molecular weight polymers via the precipitation polymerization.
机译：在各种溶剂中检查了AlCl_3通过Friedel-Crafts酰化反应催化的二苯醚和间苯二甲酰氯的沉淀聚合反应，以阐明聚合行为。基于对催化剂和聚合物的溶解性，在三种分类的溶剂中进行聚合，所述溶剂为环己烷（CH），1,2-二氯乙烷（DCE）和含有2重量％硝基苯（2％-NB）的DCE。在广泛使用的DCE中，低聚物在聚合初期以与AlCl_3的络合物形式沉淀。低聚物的沉淀物被溶剂溶胀，其中不存在任何短程规则结构。甚至在沉淀物中也进行了进一步的聚合，同时消除了副产的HCl，最终形成了高分子量的聚（醚-酮）（PEK）。然而，在2％-NB中的反应产生了溶胀良好的沉淀物，在沉淀物中未合成高分子量PEK，因为不仅由于HCl的较高溶解度而导致的HCl无效去除导致反应终止，而且失活NB与AlCl_3的配位反应尽管由于低聚物的较低的溶解度，在CH中更容易发生沉淀，但是在沉淀中没有合成聚合物。在这种情况下，所得的由二聚体组成的沉淀没有溶胀，因此很难在二聚体之间反应并从沉淀中除去HCl。对于通过沉淀聚合制备高分子量聚合物而言，与催化剂和聚合物具有高混溶性，HCl气体的溶解度低且没有碱度的溶剂是必需的。

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