1,3-丙二醇单烯丙基醚的合成及工艺优化

Synthesis and optimization of 1,3-propylene glycol monoallyl ether

摘要:

以1,3-丙二醇、氢氧化钾和烯丙基氯为原料，1,3-丙二醇自身作反应介质，在相转移催化剂四丁基溴化铵作用下合成了1,3-丙二醇单烯丙基醚。实验讨论了反应物料摩尔比、碱加入量、催化剂用量、反应温度和反应时间等因素对产品收率的影响。采用三因素五水平的响应面分析法对工艺条件进行了优化，得到了合成的最佳工艺条件。结果表明：四丁基溴化铵为烯丙基氯的5%，n（1,3-丙二醇）：n（KOH）：n（烯丙基氯）=6.3:1.2:1，反应温度72℃，反应时间3h时，收率可达82.48%。通过对1,3-丙二醇的回收套用大大降低了成本。此工艺具有毒性小、副产少、反应时间短、收率高的优点。

Abstract:

The synthesis of 1,3-propylene glycol monoallyl ether was investigated with 1,3-propylene glycol, solid potassium hydroxide and allyl chloride as raw materials, 1,3-propylene glycol as the reaction medium and tetrabutylammonium bromide as phase transfer catalyst. The effects of materials mole ratio, alkali dosage, the mount of catalyst, reaction temperature and time on yield of product were studied. The reaction conditions were optimized by using response surface methodology with three factors and five levels. The optimum conditions were as follows: m(tetrabutylammonium bromide):m(allyl chloride)=5%, n(1,3- propylene glycol):n(potassium hydroxide):n(allyl chloride) =6.3:1.2:1, at 72℃ for 3h. The yield could reach 82.48%. The recovery and reuse of 1,3-propylene glycol could reduce the economic costs. This process has the advantages of low toxicity, low content of by-products, short reaction time and high yield.