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机构地区:[1]大连理工大学精细化工国家重点实验室,辽宁大连116024
出 处:《精细化工》2011年第10期999-1003,1013,共6页Fine Chemicals
基 金:国家自然科学基金(20806013;20923006);教育部高等学校博士学科点专项科研基金(200801411011);国家科技支撑计划(2011BAE07B05)~~
摘 要:合成了一类以2-羟基二苯甲酮为紫外线吸收功能基,以聚乙烯胺(PVAm)为接枝骨架的新型水溶性大分子紫外线吸收剂PVAm-g-BP-4。PVAm-g-BP-4的合成分两步,首先,将2-羟基-4-甲氧基-5-磺酸基二苯甲酮(BP-4)结构中的磺酸基转变为磺酰氯,合成了反应中间体2-羟基-4-甲氧基-5-氯磺酰基二苯甲酮(CBP-4),采用二氯亚砜为反应溶剂和氯代试剂,N,N-二甲基甲酰胺(DMF)为催化剂,产率达94.5%;然后,将CBP-4接枝到聚乙烯胺(PVAm)骨架上,合成了PVAm-g-BP-4。目标产物经过TLC、IR、UV分析证明,CBP-4已接枝到PVAm上。通过实验优化了催化剂用量、反应温度、反应时间、溶剂体积比等反应条件。在棉织物上的初步应用结果表明,PVAm-BP-4可赋予棉织物良好的紫外线防护功能,而且耐洗牢度优异。A novel type of water-soluble macromolecular UV absorber PVAm-g-BP-4 was synthesized with 2-hydroxybenzophenone as UV absorbing group and polyvinylamine (PVAm) as backbone. PVAm- g-BP-4 was synthesized in two steps. Reactive intermediate 2-hydroxy-4-methoxy-5- chlorosulfonylbenzophenone (CBP-4) was first synthesized from 2-hydroxy-4-methoxy-5-sulfo- benzophenone (BP-4) with thionyl chloride as chlorination agent and solvent and N, N- dimethylformamide (DMF) as catalyst : the yield of the intermediate could reach 94. 5%. And then, PVAm-g-BP-4 was synthesized by grafting CBP-4 onto PVAm. CBP-4 was confirmed to be grafted onto PVAm through TLC, IR and UV spectroscopy. The preparation conditions of the intermediate and the target products were optimized by studying the dosage of catalyst, reaction temperature, reaction time, solvents volume ratio, etc. The application of PVAm-BP-4 on cotton fibers shows that it can furnish the fibers with good anti-UV property and its wash fastness was exceptional.
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