葡萄糖水热碳化催化热处理制备石墨微球  

Preparation of Graphitic Carbon Spheres by Hydrothermal Carbonization and Catalytic Graphitization Method Using Glucose as Starting Material

作　　者：李赛赛[1] 王军凯[1] 王慧芳[1] 黄亮[1] 张海军[1] 

机构地区：[1]武汉科技大学,省部共建耐火材料与冶金国家重点实验室,武汉430081

出　　处：《硅酸盐学报》2017年第12期1843-1852,共10页Journal of The Chinese Ceramic Society

基　　金：国家自然科学基金面上项目(51272188,51472184,51472185)资助

摘　　要：以葡萄糖为碳源、聚丙烯酸钠为分散剂、硝酸镍为催化剂的前驱体,采用水热碳化法一步制备了负载有Ni O催化剂的碳微球,再在氩气气氛下催化热处理制备了平均粒径约2μm的石墨化程度高、球形度及分散性好的石墨微球。研究了催化剂用量、热处理温度以及保温时间对合成石墨微球的影响。结果表明:当催化剂Ni的加入量为1.5%(质量分数)、热处理温度为1 200℃、保温时间为3 h时,所得石墨微球的石墨化程度最高。继续升高热处理温度或延长保温时间,石墨微球的石墨化程度反而降低,其原因可能是过高的温度或者过长的保温时间导致了催化剂的团聚及失活。碳微球的催化石墨化过程由溶解–析出机理决定。此外,石墨微球具有与鳞片石墨几乎相当的抗氧化性能,且远高于碳微球。Graphitic carbon spheres with an average size of 2 μm, good sphericity, narrow size distribution and high graphitization degree were synthesized via a hydrothermal carbonization and catalytic graphitization process in Ar atmosphere using glucose as a carbon source, sodium polyacrylate（PAANa） as a dispersant and nickel nitrate（Ni（NO3）2·6 H2O） as a catalyst precursor. The effects of catalyst amount, firing temperature and soaking time on the preparation of graphitic carbon spheres were investigated. The results show that the graphitic carbon spheres can be obtained under the optimal experimental conditions（i.e., holding time of 3 h, sintering temperature of 1 200 ℃ and 1.5%Ni）. The graphitization degree of as-prepared graphitic carbon spheres decreases with increasing the heat-treatment temperature or the soaking time, which might result from the aggregration and deactivation of Ni nanoparticle catalysts. In addition, dissolution-precipitation mechanism for the formation of graphitic carbon spheres was also discussed. In addition, graphite carbon spheres have almost identical oxidation resistance compared with flake graphite, and much higher oxidation resistance than carbon spheres.

关 键 词：水热碳化法 葡萄糖 催化剂 石墨微球 溶解–析出 

分 类 号：TB35[一般工业技术—材料科学与工程]