1,3-二氯丙酮的合成工艺研究

Synthesis of 1,3-Dichloroacetone

采用氧化1，3-二氯-2-丙醇的方法制备1，3-二氯丙酮。通过优化操作条件，探索出了适用于实验室制备纯品的工艺条件，并可放大于工业生产。将硫酸水溶液滴加到1，3-二氯-2-丙醇与重铬酸钠水溶液的混合物中，在温度23～27℃的条件下搅拌反应5h，重铬酸钠：1，3．二氯-2-丙醇=1：2（摩尔比），此条件下收率为79．6％。与文献方法相比．1，3-二氯丙酮的收率提高了约10％，而反应时间缩短了约4／5，并有易于操作的优点。

1,3-dichloroacetone had been prepared by the oxidation of 1,3-dichloro-2-propanol. A technical process which was fit for the laboratory had been found. It also could be used in the industry. The solution of sulfuric acid was added dropwise to the reaction vessel contained 1,3-dichloro-2-propanol, sodium dichromate and water. The mixture was stirred at 23- 27℃ for 5 hours. The molar ratio of sodium dichromate to 1,3-dichloro-2- propanol was 1：2. Under the above conditions, pure 1,3-dichloroacetone was obtained with a yield of 79.6%. Compared with other technology, the yield was improved by about 10%, and the reactive time was reduced by about four fifth.