废油脂生物柴油副产甘油制备环氧氯丙烷的研究

李惠文, 苗长林, 杨铃梅, 吕鹏梅, 王忠铭, 袁振宏

现代化工 ›› 2020, Vol. 40 ›› Issue (8) : 78 -82.

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现代化工 ›› 2020, Vol. 40 ›› Issue (8) : 78-82. DOI: 10.16606/j.cnki.issn0253-4320.2020.08.017
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废油脂生物柴油副产甘油制备环氧氯丙烷的研究

    李惠文, 苗长林, 杨铃梅, 吕鹏梅, 王忠铭, 袁振宏
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Preparation of epichlorohydrin from by-product glycerine of waste oil biodiesel

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摘要

为了延长生物柴油产业链,以废油脂生物柴油副产物粗甘油为原料,高值化利用生产衍生物环氧氯丙烷(ECH)。粗甘油原料被提纯成工业级甘油,经氯化反应和环化反应制备了环氧氯丙烷。以200 mL/min的氯化氢气体为氯化剂、己二酸为催化剂,在反应温度为105℃、己二酸质量分数为7.5%的条件下,通过降温真空除水3次,制得二氯丙醇(DCP),氯化收率达93.2%,甘油转化率达96.7%。在氢氧化钠催化下二氯丙醇环化制得环氧氯丙烷。通过单因素实验得到环化反应的最佳工艺条件为:反应时间为30 min、氢氧化钠与二氯丙醇摩尔比为1.2∶1、反应温度为90℃,在此条件下的环化收率为89.5%。

Abstract

In order to extend the industrial chain of biodiesel,epichlorohydrin (ECH) is produced from crude glycerol,a by-product of biodiesel from waste oils.Crude glycerol is firstly purified into industrial grade glycerol and then ECH is prepared from industrial grade glycerol through chlorination and cyclization.Using a flow of 200 mL/min HCL gas as chlorinating agent and adipic acid as catalyst,dichloropropanol (DCP) is synthesized by three times of vacuum dehydration under the optimum conditions that the reaction temperature maintains at 105℃ and the mass content of adipic acid is 7.5%.The chlorination yield reaches 93.2% and the conversion of glycerol is 96.7%.ECH is obtained through cyclization of DCP over sodium hydroxide.Through single factor experiments,the optimum conditions of cyclization reaction are obtained as follows:the reaction lasts for 30 min,the molar ratio of sodium hydroxide to DCP is 1.2:1,and reaction temperature maintains at 90℃.Under these conditions,the yield of cyclization can achieve 89.5%.

关键词

生物柴油副产物 / 环氧氯丙烷 / 二氯丙醇 / 粗甘油

Key words

biodiesel by-products / epichlorohydrin / dichloropropanol / crude glycerine

Author summay

李惠文(1979-),男,硕士,高级工程师,主要从事生物质资源化利用及工程推广方面的研究,huiwl@ms.giec.ac.c

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废油脂生物柴油副产甘油制备环氧氯丙烷的研究[J]. , 2020, 40(8): 78-82 DOI:10.16606/j.cnki.issn0253-4320.2020.08.017

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