聚乙交酯公斤级生产途径探索

Pilot Production of Polyglycolide

探索聚乙交酯的工业化生产途径 .以氯乙酸为原料 ,与氢氧化钠成盐后在真空下热解制得乙交酯单体 ,纯化后进行开环聚合成功地获得了高相对分子质量聚乙交酯 .研究了聚乙交酯的制备以及催化剂和引发剂用量对聚合反应的影响 .以苯酚 /1,1,2 ,2 -四氯乙烷 (m/m=1∶ 1)作溶剂 ,在 30℃下测定了聚乙交酯溶液的特性粘数 .结果表明 ,合成出的聚乙交酯特性粘数 [η]在 0 .64～ 1.36d

Bulk polymerization of glycolide (GA) was conducted. Potassium chloroacetate was first prepared from the reaction of chloroacetic acid with potassium hydroxide. The chloroacetate was then pyrolyzed to produce glycolide monomer under high vacuum and high temperature. Finally, the glycolide was twice purified and polymerized into polyglycolide by a ring opening polymerization. Following this a pilot line for the production of polyglycolide was designed and manufactured. Techniques in the preparation and purification of glycolide were investigated in some detail, and influences of catalysts and initiators on the polymerization were examined. The structure and properties of the resulting polymer were analysed by 1H NMR and differential scanning calorimetry (DSC). With phenol and 1,1,2,2 tetrachloroethane ( m∶m =1∶1) as solvent, inherent viscosity of the polyglycolide solution was measured at 30 ℃. It can be adjusted in the range of 0 64～1 36 dL/g.