摘要
通过二磷酸哌嗪的催化缩合合成了焦磷酸哌嗪,并通过红外光谱、固体核磁共振磷谱和碳谱表征结构。较佳的合成条件为m(二磷酸哌嗪)∶m(催化剂A)=1∶(0.012~0.015),反应温度和时间分别为210℃和5 h,产品经甲醇洗涤提纯。该条件下,缩合和洗涤的总产率约为88%,产品的水溶性为0.15 g/100 mL水。该方法具有工艺简单、产品产率高、水溶性小及颜色白等优点。热重分析结果表明,合成出的产品具有良好的热稳定性和成炭性。
Piperazine pyrophosphate was synthesized by catalytic condensation of piperazine diphosphate,and its structure was characterized by infrared,solid-state ^(31)P NMR and ^(13)C NMR.The optimal synthesis conditions are as follows:m(piperazine diphosphate)∶m(catalyst A)=1∶(0.012~0.015),the reaction temperature and time are 210℃ and 5 h,respectively,and the product is purified through washing with methanol.Under the above conditions,the overall yield of condensation and washing is about 88%,and the water solubility of the product is 0.15 g/100 mL water.The method has the advantages such as simple process,high yield,low water solubility and white color of product.The results of thermogravimetric analysis show that the synthesized product has good thermal stability and charring properties.
作者
赵震
郭建树
王盛海
冯祥砚
唐林生
ZHAO Zhen;GUO Jianshu;WANG Shenghai;FENG Xiangyan;TANG Linsheng(Shandong Engineering Laboratory of Environment-friendly Macromolecular Flame Retardant Material,Weifang 262715,China;College of Chemical Engineering,Qingdao University of Science and Technology,Qingdao 266042,China)
出处
《化工科技》
CAS
2022年第5期18-21,28,共5页
Science & Technology in Chemical Industry
基金
国家自然科学基金项目(21878165)。
关键词
二磷酸哌嗪
缩合
焦磷酸哌嗪
表征
Piperazine diphosphate
Condensation
Piperazine pyrophosphate
Characterization
