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机构地区:[1]南通大学化学化工学院,南通226019 [2]南通惠康国际企业有限公司,南通226009
出 处:《塑料助剂》2012年第1期24-27,共4页Plastics Additives
基 金:江苏省南通市科技局自然科学基金资助项目(项目编号:ZS12010058;TBA2010023)
摘 要:以石油醚为溶剂,颗粒状活性炭负载四丁基钛酸酯为催化剂,-定比例的癸二酸二甲酯和1.2.2.6,6-五甲基-4-羟基哌啶在110~120qC下缩合反应2~5h。然后水洗、活性炭脱色、脱溶齐4等后处理操作。-步合成了产物受阻胺光稳定剂(HALS)UV-292,其中1-甲基-8-(1,2,2,6.6-五甲基-4-哌啶)癸二酸酯(单酯)质量分数为15%~30%和双(1,2,2,6,6-五甲基-4-哌啶基1癸二酸酯(双酯1质量分数为65%~80%),收率超过97%.纯度不低于96%。得到了优化的工艺条件:反应时间为2.5h,在癸二酸二甲酯为0.1IYIOl的情况下,n(癸二酸二甲酯):n(1。2,2,6,6-五甲基-4-羟基哌啶)为0.1:0.165,催化剂用量为1.0g、溶剂的用量为40g。催化剂不经处理可循环使用多次,The hindered amine light stabilizers(HALS) UV-292 is synthesized in one step through react- ing dimethyl sebacate with 1,2,2,6,6,-pentamethyl-4-piperidinol at 110-120℃ for 2.5h by using petroleum ether as solvent , tetra-tert-butyl titanate supported on granule activated carbon as catalyst. The obtained mixture is washed with water at first, then decolorized with activated carbon and finally with solvent to give HALS UV-292. Contents of 1-methyl-8(1,2,2,6,6- pentamethyl-4-piperidinyl)sebacate(single ester) and bis (1,2,2,6,6-pentamethyl-4-piperidinyl)sebacate (two ester) in products can reach 15-30% (mass fraction)and 65-80% respectively,The yield of HALS UV-292 can reach over 97%,purity of the stearate 2,2,6,6-tetram- ethyl-4-piperidinyl ester (single ester and two ester) is over 96%~The optimal technological conditions were given as follows:reaction time 2.5 h,n (dimethyl sebacate):n (1,2,2,6,6,-pentamethyl-4-piperidinol) equal to 0.1:0.165.the amounts of catalysts is 1.0 g,the amounts of solvent is 40 g(when dimethyl sebacate is 0.1 tool). The catalyst could be used for times without any treatments.
关 键 词:双(1 2 2 6 6-五甲基-4-哌啶)癸二酸酯 1-甲基-8-(1 2 2 6 6-五甲基-4-哌啶)癸二酸酯 癸二酸二甲酯 1 2 2 6 6-五甲基-4-羟基哌啶 受阻胺光稳定剂 合成
分 类 号:TQ314.245[化学工程—高聚物工业]
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