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作 者:韩金铭[1] 徐晓波 李宏峰 Han Jinming;Xu Xiaobo;Li Hongfeng(Electrochemical Plant, Zhejiang Juhua Co.,Ltd;Juhua Group Technology Center: Quzhou, Zhejiang 324004)
机构地区:[1]浙江巨化股份有限公司电化厂 [2]巨化集团技术中心,浙江衢州324004
出 处:《化工生产与技术》2016年第5期4-6,9,共4页Chemical Production and Technology
摘 要:用2步法合成制备2,2-二氟乙醇,探讨了该方法的优化工艺条件。结果表明,第1步合成2,2-二氟乙基乙酸酯中间体,1-氯-2,2-二氟乙烷与乙酸钾摩尔比为1:1.5,反应时间2 h、温度为120℃,溶剂DMSO质量是反应原料的2倍时,在适量催化剂A作用下,1-氯-2,2-二氟乙烷转化率为99.7%,2,2-二氟乙基乙酸酯收率为95.8%;第2步合成2,2-二氟乙醇时,甲醇与2,2-二氟乙基乙酸酯中间体摩尔比4:1,反应温度90℃、时间为2 h时,在适量催化剂B作用下,2,2-二氟乙基乙酸酯转化率可达92.6%,2,2-二氟乙醇收率可达92.5%。该法原料来源方便、成本低廉。2,2-Difluoroethanol was synthesized by two-step reaction in this article,and the optimization conditions were studied.Results showed that in the first step for2,2-difluoroethyl acetate intermediate synthesis,when the mole ratio of1-chloro-2,2-difuoroethane to potassium acetate was1:1.5,reaction temperature and time were120丈and2h respectively,DMSO solvent quality was the double amount of reaction materials,a suitable amount of catalyst A was used,1-chloro-2,2-difuoroethane conversion was about99.7%and the yield of2,2-difluoroethyl acetate was95.8%.In the second step for2,2-difluoroethanol synthesis,when the mole ratio of methanol to2,2-difluoroethyl acetate was4:1,reaction temperature and time were90丈and2h respectively,a suitable amount of catalyst B was used,2,2-difluoroethyl acetate conversion was92.6%,the yield of2,2-difluoroethanol was up to about92.5%.The raw material source was convenient and the cost was low.
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