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机构地区:[1]安阳工学院化学工程系,河南安阳455000 [2]天津大学精细化工系,天津300072 [3]江苏南通柏盛化工有限公司,江苏南通226236
出 处:《化学试剂》2005年第8期507-509,共3页Chemical Reagents
基 金:教育部留学回国人员科研启动基金。
摘 要:以邻二氯苯为溶剂,苯酚、硫酸为原料,通过添加催化剂亚磷酸合成2,4′-二羟基二苯砜(2,4′-BPS),确定了较好工艺条件:n苯酚∶n100%硫酸=2.2∶1,亚磷酸16g,回流时间8.0h,2,4′-BPS含量为47.42%,粗收率为70.0%,产品为白色的结晶。同时还研究了以较便宜二氯甲苯为溶剂合成2,4′-BPS的工艺条件:n苯酚∶n100%硫酸=2.2∶1,不加催化剂,反应时间5.0h,二氯甲苯200g,2,4′-BPS含量为42·21%,粗收率为91.7%,产品为浅粉色结晶。2.4'-Dihydroxydiphenylsulfnne ( 2.4'-BPS ) was prepared by reaction of phenol anti H2SO4 in o-dichlorohenzene as solvent in the presence of phosphorous acid as catalyst. The optimum technologies tbr synthesis were obtained:nphenol:nB2SO4 = 2.2 : 1, phosphorous acid 16g. reflux time 8.0h. The purity of 2. 4'-BPS(white crystal) was 47.42% in the erude mixture synthesized and the crude yield of 2.4'-BPS was 70.0% (based on H2SO4 used ), Furthermore .the synthesis of 2.4'-BPS in dichlorotoluene as a soh, ent was also studied. The better technological conditions for synthesis were as follows: nphenol: nH2SO4 = 2.2:1 , reflux time 5.0h, toluene dichloride 200g. The purity of 2,4'-BPS (pink c .rystal) was 42.21% and the yield was 91.7%(based on H2SO4 used),
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