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机构地区:[1]广西工学院生物与化学工程系,广西柳州545006
出 处:《广东化工》2011年第1期41-42,48,共3页Guangdong Chemical Industry
摘 要:以一氯乙酸与异辛醇为原料合成氯乙酸异辛酯,经巯基取代,酸解,还原合成巯基乙酸异辛酯。结果表明,最佳工艺为:酯化反应中异辛醇与氯乙酸之比为1.1∶1,催化剂为80%硫酸溶液1.4 g,环己烷18 mL,反应温度为96℃。巯基化反应中以甲醇-水体系作溶剂,PTC加入量0.36 g;酸化水解过程中80%硫酸用量10 mL,水解温度100℃;还原时锌粉用量为2.3 g。此工艺下以氯乙酸计总收率为83.3%,减压精馏后产品纯度大于97%(GC)。Isooctyl chloroacetate was synthesized from chloroacetic acid and 2-ethylhexanol. via sulfhydrylation, acidolysis and reduction reaction,converted into isooctyl mercaptoacetate. The results showed that the optimum technological conditions should be that, fur esterification, n(2-ethylhexanol) : n(chloroacetic acid)- 1. 1 : 1.0. Amount of 80 % sulfuric acid catalyst was 1.4 g, volume of cyclohexane was 18 mL, and the reaction temperature was 96 . For creation of isooctyl mercaptoacetate. Solvent used was methanol and water, amount of PTC was 0.36 g; volume of 80 % sulfuric acid 10 mL, and the acidolysis reaction temperature was 100℃; amount of zinc powder was 2.3 g of the reduction reaction. The overall yield was 83.3 % to chloroacetic acid under these conditions, the product purity was 97 %(GC) by vacuum distillation.
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