溶胶-凝胶自蔓延燃烧法制备铜铬黑颜料及表征  

Synthesis and structural characterization of copper chromite black pigment by sol-gel self-propagating combustion

作　　者：刘立华[1] 李波[1] 唐安平[1] 徐国荣[1] 

机构地区：[1]湖南科技大学化学化工学院,理论有机化学与功能分子教育部重点实验室,分子构效关系湖南省普通高等学校重点实验室,湖南湘潭411201

出　　处：《湖南科技大学学报（自然科学版）》2014年第3期91-97,共7页Journal of Hunan University of Science And Technology：Natural Science Edition

基　　金：国家自然科学基金资助项目(51078141);湖南省科技计划项目(2010FJ3030)

摘　　要：以硝酸铜和硝酸铬为原料，硬脂酸为胶凝剂，采用溶胶-凝胶自蔓延燃烧法合成了铜铬黑颜料．考察了原料配比对凝胶的制备，煅烧温度和保温时间对铜铬黑颜料晶型形成的影响，并用热重-差热分析和红外光谱对前驱体，以及扫描电镜、能谱分析和X-射线衍射对产物结构进行表征．结果表明，当硝酸铜和硝酸铬的摩尔比为1∶2，硬脂酸与金属盐的摩尔比为1．25～1．50∶1，煅烧温度为800℃，保温时间为3 h时，制备的铜铬黑颜料纯度高、晶型规整、粒度较小且分布较窄，其平均粒径为60～80 nm．比以柠檬酸为胶凝剂的成本低，比高温固相法和醇-水共沉淀法的煅烧温度和能耗低．Copper chromite black pigment was prepared from copper nitrate and chromic nitrate using stearic acid as a gelling agent by sol-gel self-propagating combustion.The effects of raw material ratio on the sol preparation,and calcining temperature and holding time on the formation of copper chromite black crystal were investigated.The precursors prepared were characterized by thermogravimetry-differential thermal analysis （TG-DTA）and infrared spectroscopic analysis （IR）,and the production structures were characterized by scanning electron microscope （SEM）,energy spectrum analysis （ESA）and X-ray diffraction （XRD）.The results show that,when the molar ratio of copper nitrate to chromic nitrate is 1∶2,the molar ratio of stearic acid to metal slats is 1 .25 -1 .50∶1 ,and the calcination temperature is 800 ℃ and the holding time is 3 h,the copper chromite black pigment is of high purification,regular crystal form,and smaller particle size and narrow distribution.Its average particle size is about 60-80 nm.The cost of this method is lower than that using citric acid as a gelling agent,and the calcination temperature and energy consumption are lower than the solid-state method and the alcohol-water co-precipitation method.

关 键 词：铜铬黑颜料 溶胶-凝胶 自蔓延燃烧 硬脂酸 

分 类 号：TQ621.2[化学工程—精细化工]