有机磷阻燃剂插层钙基蒙脱土纳米复合物的制备和表征  

Preparation and characterization of intercalated calcium-based montmorillonite nanocompounds with organophosphorus flame retardants

作　　者：秦建雨 赵翰鹏 姚金雨 张文超 杨荣杰 QIN Jianyu;ZHAO Hanpeng;YAO Jinyu;ZHANG Wenchao;YANG Rongjie(National Engineering Technology Research Center of Flame Retardant Materials,School of Materials Science&Engineering,Beijing Institute of Technology,Beijing 100081,China;Beijing System Design Institute of Electro-mechanic Engineering,Beijing 100854,China;Standards&Metrology Research Institute,China Academy of Railway Sciences Co.,Ltd.,Beijing 100081,China;Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China)

机构地区：[1]北京理工大学材料学院国家阻燃材料工程技术研究中心,北京100081 [2]北京机电工程总体设计部,北京100854 [3]中国铁道科学研究院集团有限公司标准计量研究所,北京100081 [4]中国科学院过程工程研究所,北京100190

出　　处：《材料工程》2022年第9期78-88,共11页Journal of Materials Engineering

基　　金：国家重点研究发展规划项目(2016YFB0302101)。

摘　　要：采用一种简单直接、绿色无溶剂的制备方法,将三种有机磷小分子阻燃剂(9,10-二氢-9-氧杂-10-膦菲-10-氧杂(DOPO)、磷酸三苯酯(TPP)、季戊四醇磷酸酯(PEPA))分别插层进入到钙基蒙脱土(CaMMT)的片层中,制备了三种有机磷阻燃剂的蒙脱土纳米复合物(DOPO-CaMMT,TPP-CaMMT和PEPA-CaMMT)。X射线衍射(XRD)表明三种含磷小分子成功插层进入了蒙脱土的片层中,透射电子显微镜(TEM)验证了三种蒙脱土纳米复合物中蒙脱土的层间距表现出不同程度的增加,热重分析(TGA)表征了纳米复合物热稳定性的变化。对三种纳米复合物的形成机理进行研究。结果表明,TPP和PEPA均以一步插入到蒙脱土片层中;DOPO按照两步插层蒙脱土,且层间距更大。三种有机磷阻燃剂在插层进入蒙脱土层间形成的纳米复合物,实现了蒙脱土在聚合物中更好的分散性及磷硅协同的阻燃效应。Three organophosphorus flame retardants(9,10-dihydro-9-oxa-10-phosphophenanthrene-10-oxa(DOPO),triphenyl phosphate(TPP)and pentaerythritol phosphate(PEPA))were intercalated into the layer of calcium-based montmorillonite(CaMMT)by a simple,direct and solvent-free method,and three organophosphorus flame retardant montmorillonite nanocompounds(DOPO-CaMMT,TPP-CaMMT and PEPA-CaMMT)were prepared.X-ray diffraction(XRD)shows that the three phosphorus-containing small molecules are successfully intercalated into the layer of CaMMT.It was verified by transmission electron microscope(TEM)that the interlayer spacing of CaMMT in the three nanocompounds shows different degrees of increase.The change of thermal stability of the nanocompounds was characterized by thermogravimetric analysis(TGA).The formation mechanism of the three nanocompounds was studied.The results show that TPP and PEPA are intercalated into CaMMT in one step,while DOPO is intercalated into CaMMT in two steps with a larger interlayer spacing.The nanocompounds formed by the intercalation of three organophosphorus flame retardants into CaMMT layer are expected to achieve better dispersion of CaMMT in polymer and synergistic flame retardant effect of phosphorus and silicon.

关 键 词：钙基蒙脱土 9 10-二氢-9-氧杂-10-膦菲-10-氧杂 磷酸三苯酯 季戊四醇磷酸酯 纳米复合物 插层 

分 类 号：TB332[一般工业技术—材料科学与工程]