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机构地区:[1]南京师范大学化学与环境科学学院,江苏南京210097
出 处:《南京师大学报(自然科学版)》2009年第2期65-68,共4页Journal of Nanjing Normal University(Natural Science Edition)
基 金:江苏省科技攻关(BE2007050)资助项目
摘 要:用三氯氧磷与苯酚反应制得磷酸三苯酯(TPP),再由TPP与对苯二酚反应制得四苯基对苯二酚双磷酸酯.采用单因素法分别对物料比、反应温度、催化剂进行讨论,确定了适宜的工艺条件:磷酸三苯酯(TPP)与对苯二酚物质的量之比为2.1:1,第一步反应温度为130~140℃,反应时间为0.5h;第二步反应温度为160~170℃,反应时间为0.5h;催化剂为无水三氯化铝,产品收率达92%.产品经红外光谱验证,与四苯基对苯二酚双磷酸酯的特征峰完全一致;通过热重分析表明产品耐热性能良好;且经过技术质量指标检测,产品的外观、酸值、粘度、磷含量等技术质量指标均达到国外同类产品标准.Quinol bis(diphenyl phosphate) was synthesized from phosphous oxychloride, p-dihydroxybenzene and phenol. Triphenyl phosphate (TPP) was prepared by the reaction of phenol with phosphous oxychloride. TPP was then allowed to react with quinol to give the product. The effects of process parameters, such as molar ratio, reaction tempereture and catalyst on the yield were studied respectively, and the suitable synthesis conditions were defined as follows: the molar ratio of triphenyl phosphate and quinol is 2. 1: 1. In the first step, the reaction temperature was 130 - 140℃, and the reaction time was 0. 5 hour. In the second step, the reaction temperature was 160 - 170℃, and the reaction time was 0. 5 hour. AIC13 was the best catalyst, and its dosage was 1% of the amount of quinol. The yield reached 92%. The structure of the product was defined by FT - IR. The quality indexes of the product can reach the indexes of the oversea product.
关 键 词:对苯二酚 四苯基对苯二酚双磷酸酯 阻燃剂 合成
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