聚(环三磷腈-co-4,4′-二氨基二苯砜)微球的制备及性能研究  

Preparation and Properties of Poly(cyclotriphosphazene-co-4,4′-diaminodiphenylsulfone)Microspheres

作　　者：张心愿 魏欢 熊芸 刘生鹏 ZHANG Xinyuan;WEI Huan;XIONG Yun;LIU Shengpeng(Key Laboratory for Green Chemical Process of Ministry of Education,School of Chemical Engineering and Pharmacy,Wuhan Institute of Technology,Wuhan 430205,China;National Engineering and Technology Center for Development&Utilization of Phosphate Resources,Wuhan Institute of Technology,Wuhan 430205,China)

机构地区：[1]武汉工程大学化工与制药学院绿色化工过程教育部重点实验室,湖北武汉430205 [2]武汉工程大学国家磷资源开发利用工程技术研究中心,湖北武汉430205

出　　处：《化学与生物工程》2021年第6期25-30,共6页Chemistry & Bioengineering

基　　金：湖北省重大科技创新计划(2018ACA155)。

摘　　要：以六氯环三磷腈(HCCP)和4,4′-二氨基二苯砜(DDS)为单体,制备了单分散的聚(环三磷腈-co-4,4′-二氨基二苯砜)(PDS)微球,通过单因素实验对反应方式、反应溶剂、HCCP浓度、HCCP和DDS的官能团物质的量比n(Cl)∶n(NH_(2))、HCCP加料方式等进行了优化,探讨了PDS微球的热稳定性和成炭性能。结果表明,PDS微球的最佳制备工艺为:乙腈为反应溶剂、三乙胺为缚酸剂、HCCP和DDS的官能团物质的量比n(Cl)∶n(NH_(2))为1∶1、一次性加入2 mg·mL^(-1)HCCP、80℃回流反应24 h,所制备的PDS微球分散均匀,粒径均一,直径在1.0μm左右,具有优异的热稳定性和良好的成炭性能,PDS微球残炭具有类石墨烯结构及较完整的石墨晶体结构。Using hexachlorocyclotriphosphazene(HCCP)and 4,4′-diaminodiphenylsulfone(DDS)as monomers,we prepared monodisperse poly(cyclotriphosphazene-co-4,4′-diaminodiphenylsulfone)(PDS)microspheres.Moreover,we optimized the reaction modes,reaction solvent,HCCP concentration,molar ratio of functional group of HCCP and DDS,and HCCP adding way by single-factor experiments,and discussed the thermal stability and char-forming property.The optimal preparation process of PDS microspheres is obtained as follows:acetonitrile as a reaction solvent,triethylamine as an acid-binding agent,the molar ratio of Cl to NH2 is 1∶1,one-shot 2 mg·mL^(-1) HCCP is added,and refluxing reaction at 80℃for 24 h.The prepared PDS microspheres are uniformly dispersed with uniform particle size,and the diameter is about 1.0μm.PDS microspheres have excellent thermal stability and good char-forming property.PDS microspheres carbon residue has graphere-like structure and a relatively complete graphite crystal structure.

关 键 词：聚(环三磷腈-co-4 4′-二氨基二苯砜)(PDS) 微球 热稳定性 成炭性能 工艺优化 

分 类 号：O64[理学—物理化学]