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Preparation of High Purity Lactide Using a High-Boiling-Point Alcohol Immobilization Method
Industrial & Engineering Chemistry Research ( IF 3.8 ) Pub Date : 2018-05-25 , DOI: 10.1021/acs.iecr.8b01088
Guocai Wang , Shigui Tang , Fei Cao 1, 2 , Hongli Wu , Honghua Jia , Ping Wei 1, 2 , Pingkai Ouyang
Affiliation  

During the lactide producing process, volatile impurities, such as lactic acid and its dimer, are simultaneously distilled out with lactide. To remove these impurities, many post-treatments were needed. Herein, we present a novel approach to obtain high purity lactide by adding high-boiling-point alcohols to immobilize these volatile impurities. A series of high-boiling-point alcohols were screened and pentaerythritol was found to be the best immobilization reagent. When the molar ratio of lactic acid’s carboxylic group and pentaerythritol’s hydroxyl group was 15:1, lactide with 99% GC purity was directly distilled out and no traces of lactic acid and its dimer were detected. The results of HPLC-MS revealed that the distillation residues were esters of pentaerythritol with lactic acid or its oligomer. This indicated that volatile impurities were immobilized in distillation residues. The distillation residues were reused for 4 runs, and the purities of lactide were all over 98%.

中文翻译:

高沸点醇固定法制备高纯度丙交酯

在丙交酯的生产过程中,易挥发的杂质(例如乳酸及其二聚体)与丙交酯同时被蒸馏出。为了去除这些杂质,需要许多后处理。在这里,我们提出了一种通过添加高沸点醇来固定这些挥发性杂质来获得高纯度丙交酯的新颖方法。筛选了一系列高沸点醇,发现季戊四醇是最好的固定剂。当乳酸的羧基与季戊四醇的羟基的摩尔比为15:1时,直接蒸馏出纯度为99%GC的丙交酯,没有发现任何痕量的乳酸及其二聚体。HPLC-MS的结果表明,蒸馏残余物是季戊四醇与乳酸或其低聚物的酯。这表明挥发性杂质被固定在蒸馏残余物中。蒸馏残留物可重复使用4次,丙交酯的纯度均超过98%。
更新日期:2018-05-27
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