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作 者:牛睿祺[1] 王俊凤[1] 张军[1] 张学龙 李素芹[1] 李举[1]
机构地区:[1]河南科技大学化工与制药学院,河南洛阳471003 [2]山东鲁碧建材有限公司,山东莱芜271103
出 处:《应用化工》2008年第2期158-161,共4页Applied Chemical Industry
基 金:河南省科技攻关项目(0524240014);河南科技大学重大科技预研专项项目(2004ZD005)
摘 要:为了提高D,L-丙交酯的收率,研究了D,L-乳酸为单体,低真空条件下使乳酸单体先缩聚后解聚制备D,L-丙交酯的工艺条件。考察了制备过程中脱水温度、脱水率、催化剂量、聚合温度和解聚温度对丙交酯产率的影响。结果表明,以ZnO为催化剂,用量为1.2%,在全程低真空条件下,乳酸分别在120—160℃脱水和220—250℃解聚,以无水乙醇和乙酸乙酯作为溶剂改进了粗产品的提纯方法,可得到产率达40.2%的丙交酯。毛细管熔点法测定了产物的熔点,并用红外光谱、差示扫描量热法、X-射线衍射分析对产物进行了分析表征。所得产物为高纯的环状丙交酯。With D, L-lactic acid as monomer, D, L-lactide has been synthesized by polymerization and depolymerization in low vacuum level condition. The effects of dehydration temperature, ratio of dehydration, catalyst dosage, polymerization and depolymerization temperature on the yield of D, L-lactide were stud- ied. It is showed that the optimal conditions were as follows: amount of catalyst zinc oxide (ZnO) was 1.2% ;dehydration temperature was 120-160℃, depolymerization temperature was 220 - 250℃, the purification method from coarse product was improved by using absolute ethyl alcohol and ethyl acetate as solvents. Under this optimal conditions, the yield of D, L-lactide reached 40.2%. Melting point of product was measured by capiUary tube method and the ring lactide with high purity was identified by IR, DSC and XRD.
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