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作 者:孟照成[1] 崔志华[1] 陈维国[1] 曹益宁[1] 方颂[1]
机构地区:[1]浙江理工大学先进纺织材料与制备技术教育部重点实验室,杭州310018
出 处:《浙江理工大学学报(自然科学版)》2010年第6期874-879,共6页Journal of Zhejiang Sci-Tech University(Natural Sciences)
基 金:浙江省自然科学基金项目(Y4090227)
摘 要:以三聚氯氰、乙醇和间苯二酚为主要原料,分两步合成得到一种均三嗪类紫外线吸收剂2,4-二乙氧基-6-(2’,4’-二羟基苯基)-1,3,5-三嗪,并对该物质以及其中间体2,4-二乙氧基-6-氯-1,3,5-三嗪进行了表征。在优化合成工艺的基础上,试验确定其中间体合成优化工艺为:反应温度35℃,反应时间24 h,以碳酸氢钠为缚酸剂,其用量为原料三聚氯氰摩尔量的3倍;最终产物紫外线吸收剂的合成优化工艺为:反应温度110℃、反应时间8 h、相对于中间体2,4-二乙氧基-6-氯-1,3,5-三嗪催化剂无水三氯化铝用量为0.9 mol。A s-type ultraviolet absorber 2,4-diethoxyl-6-(2,4-dihydroxylphenyl)-1,3,5-triazine has been synthesized from cyanuric chloride,ethanol and resorcinol through two-step reaction,this ultraviolet absorber and its intermediate 2,4-diethoxyl-6-chloro-1,3,5-triazine have been characterized by FT-IR,1H-NMR,Mass Spectrum and ultraviolet-absorb spectrum in this article.The synthesizing processes of these two compounds have also been discussed in this article,and it is found that in the best synthesis process for the intermediate: the reaction uses 50mL ethanol and 5mL water as the solvent system with 3 equivalents of sodium bicarbonate as the hydrogen chloride scavenger compared to 0.1 mol cyanuric chloride,the reaction temperature is controlled at 35℃,and lasted for 24 hours;as for the ultraviolet absorber,the best synthesis process is 0.9 equivalent of anhydrous aluminium trichloride compared to intermediate 2,4-diethoxyl-6-chloro-1,3,5-triazine as catalyst,and the reaction temperature is controlled at 110℃,the reaction time is controlled for 8 hours.
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