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作 者:曹文全[1] 马喜平[1] 吕本莲[2] 韩晓兰[1]
机构地区:[1]西南石油大学化学化工学院,成都610500 [2]河南科技大学化工与制药学院,洛阳471003
出 处:《精细石油化工进展》2008年第2期35-38,共4页Advances in Fine Petrochemicals
摘 要:以氯苯为溶剂,在氯化锌的催化作用下,苯甲酸与间苯二酚反应,制得酰化产物,再用浓硫酸磺化,合成了水溶性紫外线吸收剂2,4-二羟基-5-磺酸基二苯甲酮。确定了酰化反应的最佳条件:间苯二酚与苯甲酸摩尔比为1∶2.5,反应温度为110℃,反应时间为7h,催化剂与间苯二酚的质量比为3∶20,酰化产品收率为90.2%;磺化反应最佳条件:酰化产物与浓硫酸的质量比为1∶10,磺化温度为70℃,磺化时间为2h,磺化产物收率为94.0%。产物经红外光谱、紫外光谱进行了表征,证明为二苯甲酮类物质,可用做紫外线吸收剂。A water- soluble ultraviolet absorbent 2,4 - dihydroxy - 5 - sulfo - benzophenone was synthesized by sulfonating 2,4- dihydroxy- benzophenone intermediate, which was synthesized by acidylation of benzoic acid and resorcinol with chlorobenzene as solvent and zinc chloride as catalyst. The optimum condition of the acidylation was determined as follows:The molar ratio of resorcinol to benzoic acid 1:2.5, reaction temperature 110 ℃, reaction time 7 h, mass ratio of zinc chloride to resorcinol 3:20. The optimum condition of the sulfonation was mass ratio of 2,4- dihydroxy- benzophenone to concentrated sulfuric acid 1:10, temperature 70 ℃, time 2 h. The yields of of 2,4 - dihydroxy - benzophenone and 2,4 - dihydroxy - 5 - sulfo - benzophenone were 90.2% and 94.0% respec- tively under the optimum conditions. The sulfonating product was confirmed as a benzophenone substance by infrared spectrum and ultraviolet spectrum characterizations and could used as an ultraviolet absorbent.
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