基于水热法制备改性聚磷酸钙的工艺调控、表征及性能  

Processing,Characterization and Performance of Modified Calcium Polyphosphate Prepared by Hydrothermal Method

作　　者：王琛 刘静 王亮 路思娴 WANG Chen;LIU Jing;WANG Liang;LU Sixian(School of Materials Science&Engineering,Xi’an Polytechnic University,Xi’an 710048,China)

机构地区：[1]西安工程大学材料工程学院,西安710048

出　　处：《硅酸盐学报》2020年第5期745-752,共8页Journal of The Chinese Ceramic Society

基　　金：陕西省自然科学基础研究计划(2019JQ-844);陕西省教育厅专项科研计划项目(19JK0378);2018年中国纺织工业联合会科技指导项目(2018059);西安工程大学博士科研启动基金项目(BS201861);西安工程大学研究生创新基金项目(chx2019062)。

摘　　要：以12-氨基十二烷酸(12-AA)、丙烯酰氯为主要原料,通过Schotton-Baumann酰化反应对聚磷酸钙(CPP)进行改性。探究了水热反应时间和12-AA用量对CPP改性工艺的影响,并利用Fourier红外、X射线衍射、扫描电子显微镜对产物进行了表征,同时研究了CPP的粒度、接触角和热稳定性能。结果表明:随着水热反应时间与12-AA含量的增加,CPP的产率呈增长趋势,酰化反应过程中体系pH值随反应时间的增加呈减小趋势直至平稳(呈弱酸性,pH=6.2)。当反应时间为12 h,CPP与12-AA的摩尔比为1:3时,产率可达56.70%,粒径较小(588.3±119.7 nm);改性前后接触角由2°提高至61.41°;未改性CPP无明显失重(分解温度为592.92℃),热稳定性良好。改性CPP出现明显失重,分解温度在426.68~461.66℃范围内,仍保持良好的热稳定性。Calcium polyphosphate(CPP)was modified via the Schotton-Baumann acylation reaction using 12-aminododecanoic acid(12-AA)and acryloyl chloride as main raw materials.The effects of hydrothermal reaction time and 12-AA dosage on the modification process of CPP were investigated.They were characterized by Fourier infrared spectroscopy,X-ray diffraction and scanning electron microscopy.The particle size,contact angle and thermal stability of CPP were also determined.The results show that the yield of CPP-modified increases with increasing the hydrothermal reaction time and 12-AA content.In the acylation process,the pH value decreases as the reaction time increases until stable(i.e.,a weak acidity,pH 6.2).A greater yield(i.e.,56.70%)and the smaller particle size(i.e.,588.3±119.7 nm)of modified CPP are obtained when a molar ratio of CPP to 12-AA is 1:3 and the reaction time is 12 h.The contact angle before and after the modification increases from 2 to 61.41 degrees.Based on the results by thermogravimetric analysis,the CPP has a good thermal stability with little mass loss at<592.92℃.However,the modified CPP still has a good thermal stability and shows an obvious mass loss at 426.68-461.66℃.

关 键 词：聚磷酸钙 改性 水热合成 热稳定性能 

分 类 号：O635[理学—高分子化学]