混合溶剂法精制双酚S的工艺研究

Process for the Purification of Bisphenol S by Mixed Solvents

研究了醇-四氯乙烷或醇-苯甲醚混合溶剂法精制粗品双酚S。将粗品双酚S在醇中溶解,加入四氯乙烷或苯甲醚,加热条件下活性炭脱色,蒸馏除去醇,过滤得到高质量分数的双酚S精制产品。醇-四氯乙烷精制的最佳工艺条件为:10 g粗品于40 g异戊醇中溶解,加入100 g四氯乙烷,1 g活性炭,50℃搅拌脱色1 h,过滤得滤液,蒸馏除去醇,降温、过滤、干燥,所得精制产品中双酚S的质量分数为99.50%,收率为82%;醇-苯甲醚精制的最佳工艺条件为:10 g粗品于40 g异丁醇或异戊醇中溶解,加入60 g苯甲醚,1 g活性炭。50℃搅拌脱色1 h,过滤,滤液蒸馏除去醇,降温、过滤、干燥,所得精制产品质量分数达99.80%以上,收率在83%左右。

In order to reduce the wastewater and improve the quality of the product,crude bisphenol S is purified by mixed solvents system of alcohol-tetrachloroethane or alcohol-anisole. Crude bisphenol S is dissolved in an alcohol. Then active carbon is added with tetrachloroethane or anisole under heating conditions. After a period of time of decolorization,the alcohol is removed by distillation. The high quality bisphenol S is obtained by filtration. The optimum conditions of the alcohol-tetrachloroethane system are as follows. Firstly 10 g crude bisphenol S is dissolved in 40 g isoamyl alcohol. Then 100 g tetrachloroethane and 1 g active carbon are added under stirring and the whole system is heated at 50℃ for 1 hour. The alcohol can be removed from the filtrate by distillation after filtration. High quality bisphenol S can be obtained after the rest of the filtrate being cooled,filtered and dried. The mass fraction and yield of bisphenol S obtained by alcohol-tetrachloroethane are 99. 50% and 82%respectively. The optimum conditions of alcohol-anisole system are as follows. Firstly 10 g crude bisphenol S is dissolved in 40 g isobutanol or isoamylalcohol. Then 60 g anisole and 1 g active carbon are added under stirring and the whole system is heated at 50 ℃ for 1 hour. The alcohol can be removed from the filtrate by distillation after filtration. High quality bisphenol S can be obtained after the rest of the filtrate being cooled,filtered and dried. The mass fraction of bisphenol S obtained by alcohol-anisole is more than 99. 80%,and the yield of which is about 83%.