高含量2,4′-二羟基二苯砜的合成

The preparation of 2,4′-dihydroxydiphenylsulfone

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）,