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作 者:张天永[1,2,3] 朱佳佑[1] 李彬[1,2,4] 姜爽[1] 陈松[1,3] 王树华
机构地区:[1]天津大学化工学院,天津300072 [2]天津市应用催化科学与工程重点实验室,天津300072 [3]天津市绿色橡胶助剂企业重点实验室(筹),天津300270 [4]大连理工大学精细化工国家重点实验室,辽宁大连116024 [5]科迈化工股份有限公司,天津300270
出 处:《现代化工》2014年第2期113-116,共4页Modern Chemical Industry
基 金:国家自然科学基金(21103121;21276187);教育部高等学校博士学科点专项科研基金(20110032120011);天津市应用基础与前沿技术研究计划(13JCQNJC05800);精细化工国家重点实验室开放基金(KF1101)
摘 要:将双酚S粗品在氨水-活性炭体系中脱色提纯得到初精制产品,再置于苯甲醚溶剂中回流萃取去除异构体2,4'-二羟基二苯砜,得到高纯度精制产品。较好的工艺条件为:m(粗品)∶m(ω=3%氨水)=1∶10,m(粗品)∶m(糖用活性炭)=10∶1,搅拌脱色1 h,过滤后滤液酸析得初精制产品,纯度为98.30%,收率为88.4%;m(初精制产品)∶m(苯甲醚)=1∶20,回流搅拌1 h,降温过滤得精制产品,纯度为99.93%,收率为94.5%。该工艺精制产品纯度高,经济环保,操作简便,易于工业化。Crude 4,4'-dihydroxydiphenylsulfone is decolored and purified by the ammonia-activated carbon system to obtain primary purified product.Then the primary purified product is refluxed and extracted in boiling anisole to remove isomer 2,4'-dihydroxydiphenylsulfone to obtain the high-purity product.The improved process is applied as follow:1 ∶ 10 of m(crude product) ∶ m (ω =3% ammonia),10∶1 of m (crude product) ∶ m (activated carbon for sugar industry) and 1 hour of decoloration.Then the primary purified product is precipitated out by adding sulfuric acid to the filtrate after activated carbon is filtered off.The purity of primary product reaches 98.30% and the yield is 88.4%.When the ratio of m (the primary purified product) and m (anisole) is 1 ∶ 20,and the mixture is stirred at refluxing temperature for 1 hour,the high-purity can be obtained by cooling and being filtered.The purity of final product can reach 99.93% and the yield is 94.5%.The product purity obtained by the process is high.The improved process is relatively cost-effective and environmental benign,and is easy to be operated and industrialized.
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