仲丁醇铝水解制备高纯拟薄水铝石  

Preparation of high purity pseudo⁃boehmite by hydrolysis of aluminium sec⁃butoxide

作　　者：李凡 杨雨哲 田朋 李伟[1] 宁桂玲[1] LI Fan;YANG Yuzhe;TIAN Peng;LI Wei;NING Guiling(School of Chemical Engineering,Dalian University of Technology,Dalian 116023,China)

机构地区：[1]大连理工大学化工学院,辽宁大连116023

出　　处：《无机盐工业》2022年第7期78-84,104,共8页Inorganic Chemicals Industry

基　　金：大连市高层次人才创新支持计划(青年科技之星)(2018RQ15);国家重点研发计划(2021YFA1500300)。

摘　　要：采用仲丁醇铝为原料水解制备高纯拟薄水铝石,研究水解温度、水用量、水解时间、干燥温度对拟薄水铝石胶溶指数的影响,并结合X射线衍射(XRD)和红外光谱(IR)分析产物的结构。研究结果表明:水解温度、水用量、水解时间以及干燥温度的改变都会影响拟薄水铝石的胶溶指数,其中水解温度和水用量的影响最为明显;水解温度的提高有益于拟薄水铝石结晶,低温产物无法胶溶,当水用量不断增大时,产物的晶型从最初的无定形态过渡到拟薄水铝石相,结晶度增加,相应产物的胶溶指数也增大;水解时间的延长,有利于水解产物的晶粒长大,胶溶指数增加;提高干燥温度对产物结晶和胶溶指数的影响均较小。实验最终得到周期短、残水量少、残碳量低的最优水解条件:仲丁醇铝与水物质的量比为1∶4.0,水解搅拌时间为2 h,水解温度和干燥温度均为110℃。为进一步提高产物的胶溶指数,采用将水解后产物再水化法对其进行优化,胶溶指数高达99.6%,优化后产物的各项技术参数均可与商用高纯拟薄水铝石(SB粉)相媲美。该研究为仲丁醇铝水解制备拟薄水铝石的工业化提供了相应基础。High purity pseudo⁃boehmite was prepared by hydrolysis of aluminium sec⁃butoxide.The effect of hydrolysis tem⁃perature,water dosage,hydrolysis time,and drying temperature on dispersion index was investigated.The X-ray diffraction(XRD)and infrared spectroscopy(IR)characterization were carried on to analyze the structure of product.The results showed that hydrolysis temperature,water dosage,hydrolysis time and drying temperature affected the dispersion index of the product,and the effect of hydrolysis temperature and water dosage were more obvious.The increase of hydrolysis tem⁃perature was beneficial to the growth of pseudo⁃boehmite crystal,and the peptizing property of products at low temperature was poor.With the increase of water dosage,the crystal form of the product was continuously improved,from the initial amor⁃phous form to the pseudo⁃boehmite phase,respectively crystalline rises and the dispersion index of the product increased accordingly.Prolonging the hydrolysis time was beneficial to the grain growth of pseudo⁃boehmite and the increase of disper⁃sion index.And the drying temperature had less effect on the crystallization and dispersion index.The optimal hydrolysis con⁃ditions were obtained as follows:the molar ratio of aluminum sec⁃butoxide to water was 1∶4.0,the hydrolysis stirring time was 2 h,and the hydrolysis temperature and drying temperature were 110℃.In order to further improve the dispersion in⁃dex index of the product,hydration of the hydrolyzed product was used to optimize the dispersion index up to 99.6%.At the same time,other technical parameters of the optimized product were comparable with SB powder.This study provided a re⁃search basis for the industrialization of the preparation of pseudo⁃boehmite by the hydrolysis of aluminium sec⁃butoxide.

关 键 词：仲丁醇铝 高纯拟薄水铝石 胶溶指数 

分 类 号：TQ133.1[化学工程—无机化工]