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机构地区:[1]先进土木工程材料教育部重点实验室,上海200092 [2]同济大学材料科学与工程学院,上海200092
出 处:《工程塑料应用》2007年第12期14-17,共4页Engineering Plastics Application
摘 要:采用溴/过氧化物法和NBS法对五溴甲苯进行苄位溴化,合成了五溴苄基溴,比较了两种方法的优缺点。结果表明,采用溴/过氧化物法时,产物的产率和溴含量都较高;进一步在乙二醇甲醚溶剂中与丙烯酸钠反应得到了新型阻燃剂单体五溴苯基丙烯酸酯。考察了原料配比、反应条件和产品后处理方法等工艺参数对合成产物的影响。结果表明,当溴与五溴甲苯的物质的量之比为0.9∶1时,五溴苄基溴的产率为94.4%,溴含量为84.61%;丙烯酸与无水碳酸钠的物质的量之比为2.04∶1时,五溴苯基丙烯酸酯的产率为93.5%,溴含量达72.90%。对五溴苯基丙烯酸酯进行聚合所得产物的产率为69.5%,溴含量达71.20%,与理论值相当。Brominated pentabromobenzyl was prepared from pentabrominated toluene by using bromine/peroxides method and NBS method. The experimental results showed that there were higher yield and bromine content when the bromine/peroxides method was used. Then a new flame-retandants pentabromobenzyl acrylate was prepared by the reaction of brominated pentabromobenzyl and acrylic sodium with methoxyethanol as the solvent. The influence of the dosage of reagents, the reaction condition and the purification method on the yield and bromine content of products was studied. The experimental results showed that the yield of brominated pent- abromobenzyl came up to 94.4% and the bromine contents reached 84.61% when the ratio ofbromine to pentabrominated toluene equals 0.9: 1. The yield of pentabromobenzyl acrylate came up to 93.5% and the bromine contents reached 72.90% when the ratio of acrylic acid to sodium carbonate equals 2.04: 1. The yield of polymerization of pentabromobenzyl acrylate came up to 69.5%, while the bromine contents reached 71.20%, which was consonant with the theoretical value.
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