OALib Journal期刊
醇洗法纯化乙交酯的工艺及对开环聚合反应的影响
DOI: 10.16085/j.issn.1000-6613.2015.04.0027
Keywords: 醇洗工艺 ,重结晶 ,异丙醇 ,乙交酯 ,开环聚合
Abstract:
对本体解聚制备的乙交酯粗品进行醇洗纯化,研究了醇洗次数、溶剂用量、醇洗时间对乙交酯中游离酸、水含量及收率的影响;考察了醇洗后乙交酯中总氢质子含量对聚合反应的影响.筛选了不同醇类溶剂,优选异丙醇为合适的溶剂进行乙交酯粗品纯化,辅以抽滤、真空干燥等手段最终得到纯化的乙交酯.研究结果表明,醇洗次数3次,溶剂用量即V(醇)/M(乙交酯)=2mL/g,洗涤时间30min,乙交酯中的游离酸、水含量分别降低到1.7×10-5mol/g、468mg/L,总氢质子含量为43×10-6mol/g,通过双螺杆挤出机进行开环聚合,得到聚乙醇酸(PGA)特性黏度高达0.81dL/g;收率可达82%,比重结晶法纯化收率高.通过差示扫描量热法(DSC)测定醇洗后乙交酯纯度,得均值99.93%,满足聚合纯度的要求.
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