工艺参数对高压氢液相还原法制备超细钴粉粒度和实收率的影响  

Effect of Process Parameters on Particle Size and Yield of Ultrafine Cobalt Powder Prepared by High Pressure Hydrogen Liquid-Phase Reduction

作　　者：李成 王朝安 张志平 侯玉成 朱治军 Li Cheng;Wang Chao’an;Zhang Zhiping;Hou Yucheng;Zhu Zhijun(Anhui Hanrui New Material Co.,Ltd.,Chuzhou Anhui 239000,China)

机构地区：[1]安徽寒锐新材料有限公司,安徽滁州239000

出　　处：《硬质合金》2024年第5期400-407,共8页Cemented Carbides

摘　　要：以七水合硫酸钴为原料,氨水为络合剂,通过加入催化剂、有机聚合分散剂和引发剂,制备出钴氨络合物前驱体,然后将其转入高压搅拌反应釜中,加热、搅拌,到达设定温度后,通入一定压力的氢气进行反应,用去离子水和甲醇离心洗涤反应产物,真空干燥后得到超细钴粉。研究了反应温度、钴氨络合比、氢气压力对超细钴粉实收率和引发剂用量、催化剂用量、分散剂用量对超细钴粉费氏粒度的影响规律。研究结果表明:当反应温度为140℃,氢气压力为2.5 MPa,n(Co)∶n(NH_(3))为1∶2.3时,通过控制引发剂、催化剂、分散剂的加入量,能合成出费氏粒度小于0.6μm,粒度分布均匀且实收率大于99.5%的超细球形钴粉。超细钴粉成分符合某国外公司超细钴粉成分要求。In this paper,the precursor of the cobalt-ammonia complex was prepared by adding catalysts,organic polymerization dispersants,and initiators with cobalt sulfate heptahydrate as raw material and ammonia water as a complexing agent.It was then transferred into a high-pressure stirred reactor,heated,and stirred.After reaching the set temperature,hydrogen at a certain pressure was introduced for the reaction.The reaction product was centrifuged with deionized water and methanol,and the ultrafine cobalt powder was obtained after vacuum drying.The effects of reaction temperature,cobalt-ammonia complex ratio,and hydrogen pressure on the actual yield of ultrafine cobalt powder,as well as those of initiator,catalyst,and dispersant dosages on the Fisher particle size of ultrafine cobalt powder were studied.The results show that ultrafine spherical cobalt powder with Fisher particle size of less than 0.6µm,uniform particle size distribution,and actual yield of greater than 99.5% can be synthesized by controlling the amount of initiator,catalyst,and dispersant when the reaction temperature is 140℃;the hydrogen pressure is 2.5 MPa,and n(Co)∶n(NH_(3))is 1∶2.3.

关 键 词：高压氢液相还原 超细钴粉 球形 费氏粒度 实收率 粒度分布 钴粉成分 

分 类 号：TQ2[化学工程—有机化工]