微波辐射固体超强酸CuSO_4·AlCl_3催化合成氯乙酸乙酯
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摘要
以氯乙酸和无水乙醇为原料,选用固体超强酸CuSO_4·AlCl_3做催化剂,不使用带水剂,采用微波辐射技术合成氯乙酸乙酯,考察了多种因素对产率的影响.优化的反应条件为:氯乙酸与无水乙醇的摩尔比为1∶1.3,催化剂为1.50 g无水硫酸铜和1.25 g无水氯化铝制成的固体超强酸,微波辐射功率为420 W,微波辐射时间为8min,在此条件下收率可达82.6%.此方法简便、高效、无腐蚀、无废酸污染.
In this paper, ethyl chloroacetate is synthesized by using microwave radiation technology, taking chloroacetic acid and anhydrous ethyl alcohol as raw materials, choosing solid super acid CuSO_4?AlCl_3 as catalyst, and canceling water-carrying agent. The effect of various factors on the yield was studied and came to the conclusion of the optimum reaction conditions: the?molar?ratio?of?chloroacetic acid and anhydrous ethyl alcohol is 1:1.3, the catalyst is solid super acid which made up of 1.25 g anhydrous aluminum chloride and 1.50 g anhydrous copper sulfate, microwave power is 420 W and irradiation time is 8 minutes, on which condition the yield can reach 82.6%. This method is simple, high efficiency and with no corrosion and no waste acid pollution.
In this paper, ethyl chloroacetate is synthesized by using microwave radiation technology, taking chloroacetic acid and anhydrous ethyl alcohol as raw materials, choosing solid super acid CuSO_4?AlCl_3 as catalyst, and canceling water-carrying agent. The effect of various factors on the yield was studied and came to the conclusion of the optimum reaction conditions: the?molar?ratio?of?chloroacetic acid and anhydrous ethyl alcohol is 1:1.3, the catalyst is solid super acid which made up of 1.25 g anhydrous aluminum chloride and 1.50 g anhydrous copper sulfate, microwave power is 420 W and irradiation time is 8 minutes, on which condition the yield can reach 82.6%. This method is simple, high efficiency and with no corrosion and no waste acid pollution.
引文
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[2]赵志娟.氯乙酸乙酯合成工艺研究[J].煤炭与化工,2013,36(4):92-93.
[3]杨良准,杜立芬,施玉梅.硫酸高铈催化合成氯乙酸乙酯[J].化学世界,2000,(8):436-438.
[4]蒋文伟.超强酸催化剂的研究进展[J].精细化工,1997,(1):47-49.
[5]郑纯智,张国华,王普力.磷钼酸催化合成氯乙酸乙酯[J].应用化工,2001,30(1):30-31.
[6]黄慧,陈理,柳金章.固体超强酸催化合成氯乙酸乙酯新工艺研究[J].应用化工,2003,32(5):36-38.
[7]中国医药公司上海化学试剂采购供应站.试剂手册[M].第2版.上海:上海科技出版社,1985:570.