氧化铝制备过程中硫酸根的脱除
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摘要
研究了以工业级硫酸铝铵为原料制备氧化铝的过程中杂质SO_4~(2-)的脱除工艺,并考察了滴加顺序、硫酸铝铵初始浓度、反应温度、滴加速率、终点pH、水热介质和水热温度对SO_4~(2-)脱除的影响。结果表明:在硫酸铝铵初始浓度为0.5 mol/L、反应温度为55℃、滴加速率为4 mL/min、终点pH=9.0、反滴加、水热介质为1 mol/L的精制氨水、水热处理温度为205℃的条件下,可以制得SO_4~(2-)质量分数最低为0.001 5%的Al2O3。水热介质选用氨水可有效增大前驱体粒径,进而大大降低SO_4~(2-)的表面吸附,利于氧化铝中SO_4~(2-)含量的脱除。与传统直接煅烧硫酸铝铵法相比,该工艺煅烧前即洗掉了大量的SO_4~(2-)杂质,有效避免了煅烧不充分造成氧化铝中SO_4~(2-)含量较大的弊端。
Impurity SO_4~(2-)removal was investigated in the process of alumina preparation.It was used the industrial-grade ammonium aluminum sulfate as raw material.The influences of the factors,including the dripping sequence,the initial concentration of ammonium aluminum sulfate,the reaction temperature,the dripping speed rate,the pH at end-point,hydrothermal medium and hydrothermal temperature,on the SO_4~(2-)removal effect were discussed.The results showed that: when the initial concentration of ammonium aluminum sulfate was 0.5 mol/L,the reaction temperature was 55 ℃,the dripping speed rate was4 mL/min,the pH=9.0,hydrothermal medium was 1 mol/L of ammonia,and hydrothermal temperature was 205 ℃,alumina with the lowest SO_4~(2-)mass fraction of 0.001 5% could be obtained.It could effectively increase the precursor particle size when the hydrothermal medium was ammonia.Thus it greatly reduced the surface adsorption of SO_4~(2-),which benefited for the removal of SO_4~(2-)content in alumina.Compared with the traditional method direct calcination ammonium aluminum sulfate,this process washed away a lot of SO_4~(2-)impurities before calcination,which effectively avoided the inadequate calcination causing SO_4~(2-)content larger.
Impurity SO_4~(2-)removal was investigated in the process of alumina preparation.It was used the industrial-grade ammonium aluminum sulfate as raw material.The influences of the factors,including the dripping sequence,the initial concentration of ammonium aluminum sulfate,the reaction temperature,the dripping speed rate,the pH at end-point,hydrothermal medium and hydrothermal temperature,on the SO_4~(2-)removal effect were discussed.The results showed that: when the initial concentration of ammonium aluminum sulfate was 0.5 mol/L,the reaction temperature was 55 ℃,the dripping speed rate was4 mL/min,the pH=9.0,hydrothermal medium was 1 mol/L of ammonia,and hydrothermal temperature was 205 ℃,alumina with the lowest SO_4~(2-)mass fraction of 0.001 5% could be obtained.It could effectively increase the precursor particle size when the hydrothermal medium was ammonia.Thus it greatly reduced the surface adsorption of SO_4~(2-),which benefited for the removal of SO_4~(2-)content in alumina.Compared with the traditional method direct calcination ammonium aluminum sulfate,this process washed away a lot of SO_4~(2-)impurities before calcination,which effectively avoided the inadequate calcination causing SO_4~(2-)content larger.
引文
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[2]Du M X,Chen K L,Xiong Y G,et al.Advances in high-purity alumina and resource distribution[J].Advanced Materials Research,2014,926/927/928/929/930:36-39
[3]王守平,孙俊才,高陇桥,等.硫酸铵盐制备氧化铝粉体及透明氧化铝陶瓷的微观结构[J].硅酸盐学报,2007,35(11):1467-1472.
[4]李来时,翟玉春,秦晋国,等.以粉煤灰为原料制备高纯氧化铝[J].化工学报,2006,57(9):2189-2193.
[5]宋云华,刘欣,陈建铭,等.一种氢氧化铝及氧化铝粉体的制备工艺:中国,105692667A[P].2016-06-22.
[6]蒋快良,龙桂花,谭群英,等.分光比浊法测定氯化钴中硫酸根[J].冶金分析,2012,32(11):72-75.
[7]DZ/T 0064.65—1993地下水质检验方法—比浊法测定硫酸根[S].
[8]张滨,张军.用工业硫酸铝和工业硫酸铵生产高纯硫酸铝铵的方法:中国,103172099A[P].2013-06-26.
[9]范伟东.氢氧化铝粉体制备过程形貌控制研究[D].长沙:中南大学,2005.
[10]段海婷,侯清麟,罗炽,等.正交实验优化Zr O2包覆钛白粉工艺研究[J].功能材料,2013,44(11):1667-1671.
[11]江琦,雷蕾.醇盐水解-水热法制备高结晶度纳米氢氧化铝[J].材料导报,2008,22(s3):23-25.