聚二乙烯苯基炭微球的制备  

Preparation of a novel type of carbon bead from polydivinylbenzene(PDVB) microspheres

作　　者：李立朝[1] 宋怀河[1] 陈晓红[1] 

机构地区：[1]北京化工大学化工资源有效利用国家重点实验室,北京100029

出　　处：《北京化工大学学报（自然科学版）》2007年第3期279-282,286,共5页Journal of Beijing University of Chemical Technology(Natural Science Edition)

基　　金：北京市科技新星计划(954811400/B200309);高等学校新世纪优秀人才支持计划(NCET-04-0122)

摘　　要：采用分散聚合的方法合成了粒径0．5～1．5μm的聚二乙烯苯（PDVB）微球。惰性气氛下对其进行炭化研究，结果表明：纯PDVB微球在700℃下会软化熔融，炭化收率为31．2％；空气中250～320℃的氧化处理有效提高-pPDVB微球的热稳定性，经后续炭化处理得到了炭化收率大于40％的PDVB基炭微球，石墨化后得到了晶化程度提高的炭微球。用扫描电镜、透射电镜、红外光谱和X-射线衍射对样品的形貌和结构变化进行了表征，可能的交联反应机理为：在热空气中，氧气与PDVB中的悬垂双键发生反应，分子链中有羟基和羧基基团出现，羟基和羧基的酯化反应增加了PDVB的交联程度，使其能在700℃下保持球形。PDVB microspheres with an average size in the range 0.5-1.5μm have been synthesized by dispersion polymerization. A novel type of carbon bead was subsequently prepared from the PDVB microspheres by oxidation in hot air and subsequent carbonization. Whereas untreated PDVB microspheres melt below 700℃ with a carbon yield of 31.2%, it was found that their thermal stability was enhanced by oxidation treatment in the temperature range 250℃ to 320 ℃ and their spherical shape was preserved up to 700 ℃. The carbon yield of the pre-treated beads was over 40% and the crystal structure of the resulting carbon beads was improved by a graphitization process. The influence of oxidation parameters such as temperature and oxidation time on the morphologies and structures of the carbon beads was investigated by SEM, TEM, IR and XRD measurements. Finally, a possible cross-linking mechanism for PDVB under hot air is proposed, involving generation of carboxyl and hydroxyl groups by reaction between O2 and pendant ethylene groups on PDVB. It is proposed that preservation of the spherical shape is due to the ester cross-linking structure formed by reaction between carboxyl and hydroxyl groups.

关 键 词：聚二乙烯苯微球 热氧化处理 交联反应 炭微球 

分 类 号：TM912.9[电气工程—电力电子与电力传动]