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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。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质量的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3 h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。该工艺具有毒性小、副产少、反应时间短、收率高的优点。
Using 1,3-propanediol, potassium hydroxide and allyl chloride as raw materials, 1,3-propanediol itself as a reaction medium, under the action of the phase transfer catalyst tetrabutylammonium bromide synthesized 1,3-propanediol monoallyl Ether. The effects of molar ratio of reactants, base addition, catalyst dosage, reaction temperature and reaction time on the yield of the product were discussed. The three-factor five-level response surface analysis method was used to optimize the process conditions, and the optimum process conditions were obtained. The results showed that tetrabutylammonium bromide was 5% of allyl chloride, n (1,3-propanediol): n (KOH): n (allyl chloride) = 6.3:1.2:1, reaction temperature 72 ℃, reaction time 3 h, the yield can reach 82.48%. Through the 1,3-propanediol recovery applied greatly reduced costs. The process has the advantages of low toxicity, less byproduct, short reaction time and high yield.