精铁矿粉除硅及制备超高纯α-Fe_2O_3工艺和应用研究
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摘要
以铁氧体原料α-Fe_2O_3的国家标准分析方法为基础，得到了精铁矿粉中微量SiO_2含量测定的一种新方法，重点探讨了操作过程和条件，通过与仪器分析结果对比可知：本法具有精确度高、重复性好、操作简便和测定范围宽等优点，为精铁矿粉的除硅加工提供了分析上的保证；以精铁矿粉为原料，研究出了通过碱洗除硅、再经催化氧化制备高质量α-Fe_2O_3的工艺，并通过正交实验得到了优化的工艺条件，产品主要指标为：Fe_2O_3≥99.82％，SiO_2≤0.0028％，粒径＜1μm，达到了电子工业所要求的超高纯级质量标准；以精铁矿粉催化氧化过程的实验数据为基础，通过数学方法处理，得到了该反应过程的动力学模型，为该过程的进一步放大和优化操作提供了可靠的依据；在前期实验和理论研究的基础上，在江苏宜兴建了一套500t／a α-Fe_2O_3中试生产装置，在西安周至建立了一套2000t／a的生产装置，对该过程进行了工业化放大研究，其结果与扩大试验结果吻合良好；详细地探讨了以染料工业废铁泥为原料经催化氧化制备铁红颜料的工艺过程及其优化工艺条件，应用实验表明该产品可用于油漆、涂料和地板砖的生产，具有显著的经济效益、社会效益和环境效益。
A new method of trace silica test in refined iron ore powder has been successfully researched on the basis of chemical analysis methods, introduced in the GB, of raw materials used in ferrite materials. The research is focused on probing into the optimum technological conditions. Compared with the test result of modern analytic apparatus, it is known that this method possesses some properties such as high accuracy and good repetition and other advantages of operating simply and having wide test range which are contrary to the traditional methods. All above mentioned ensure processing refined iron ore powder.
With the raw material of high-grade ore powder from Chengde in Hebei province and east Qinling Mountain in Shannxi, a new technology of preparing higher-grade a - Fe2O3 has been successfully studied by way of first removing silicon with dissolution of sodium hydroxide and then catalytically oxidating. The study mainly inquires into the optimum technological conditions of removing silicon, the production have some good indexes ,for example, Fe2O3 > 99.82%; SiO2< 0.0028%; size: < 1um, which certainly meets the needs of the raw materials for producing high-grade ferrite.
With the same raw material as the former, on the basis of the data achieved from the experiment ,the chemical kinetics formula of producing a - Fe2O3 by catalytic oxidation has been built by means of mathematics techniques according to the process mechanism reported. It could service as the basis by which the process will be amplified further and is controlled better.
According to the achievements in theoretic and experimental research of catalytic oxidation of high-grade magnetite, two set of production installations have been set up, the one in Yixing city with the capacity of 500 tons of a -Fe2O3 per year ,and the other in Zhouzhi of Xian with the capacity of 2000 tons. This research show the industrial results of the process are in good accordance with the results of primary and medium experiments.
The technology of preparing red ferric oxide and its optimum technological conditions have been inquired with the raw material of waste iron mud from chemical industry by catalytic oxidation, and through the applied research, the facts that this production red ferric oxide can be fit to make coating, paint and floor brick, being with great economic , social and environmental profits are showed.
A new method of trace silica test in refined iron ore powder has been successfully researched on the basis of chemical analysis methods, introduced in the GB, of raw materials used in ferrite materials. The research is focused on probing into the optimum technological conditions. Compared with the test result of modern analytic apparatus, it is known that this method possesses some properties such as high accuracy and good repetition and other advantages of operating simply and having wide test range which are contrary to the traditional methods. All above mentioned ensure processing refined iron ore powder.
With the raw material of high-grade ore powder from Chengde in Hebei province and east Qinling Mountain in Shannxi, a new technology of preparing higher-grade a - Fe2O3 has been successfully studied by way of first removing silicon with dissolution of sodium hydroxide and then catalytically oxidating. The study mainly inquires into the optimum technological conditions of removing silicon, the production have some good indexes ,for example, Fe2O3 > 99.82%; SiO2< 0.0028%; size: < 1um, which certainly meets the needs of the raw materials for producing high-grade ferrite.
With the same raw material as the former, on the basis of the data achieved from the experiment ,the chemical kinetics formula of producing a - Fe2O3 by catalytic oxidation has been built by means of mathematics techniques according to the process mechanism reported. It could service as the basis by which the process will be amplified further and is controlled better.
According to the achievements in theoretic and experimental research of catalytic oxidation of high-grade magnetite, two set of production installations have been set up, the one in Yixing city with the capacity of 500 tons of a -Fe2O3 per year ,and the other in Zhouzhi of Xian with the capacity of 2000 tons. This research show the industrial results of the process are in good accordance with the results of primary and medium experiments.
The technology of preparing red ferric oxide and its optimum technological conditions have been inquired with the raw material of waste iron mud from chemical industry by catalytic oxidation, and through the applied research, the facts that this production red ferric oxide can be fit to make coating, paint and floor brick, being with great economic , social and environmental profits are showed.
引文
1．丁绪淮等．工业结晶[M]．北京：化学工业出版社，1985
2．王文亮．结晶化学[M]．北京：人民教育出版社，1961
3. J.W. Mellor. A Comprehensive Treatise on Inorganic and Theoretical Chemistry. Vol. Ⅷ,1934
4．周志刚．等铁氧体磁性材料[M]．北京：科学技术出版社，1981
5．孙来九．精细无机化工工艺学[M]．西安：西北工业大学出版社，1993
6. Gorter, E.W. Saturation Magnetization and Crystal Chemistry and Ferrimagnetic Oxide[J].philips. Res. Rep. 9(1954):295-320;321-365;403-443
7. Guy, A. Introduction to Material Sciece[M].1972
8. Epsteind. FrackiewiezL. Z. Some properties of. Quenched Magnesium Ferrite [J]. App. phys. 29, (1958):376～378
9．朱骥良，吴申年．颜料工艺学[M]．北京：化学工业出版社，1994
10．E．Φ．别达基．颜料化学与工艺学[M]．北京：高等教育出版社，1956
11．曹恩荣，王耕福．我国软磁铁氧体生产之展望[J]．磁性材料及器件，1986，17(1)：37-42
12．王耕福．软磁铁氧体生产、应用、市场预测[J]．磁性材料及器件，1995，26(2)：11-14
13．曾恒兴．铁资源的综合利用[J]．化学世界，1993(12)：619-623
14. Strivens, M.A.,cholG. Ferrite Pro. of the inter, conf[M].239-342
15. Mendelson. M.I.,Particle size Distribution of Coprecipitated Mn-Zn Ferrite Powder[J].J.Amer. Geo. sci. 1976(56):219-221
16．陈彪，陈德乾．Fe_2O_3原料的理化特性对Mn-Zn铁氧体微观结构及性能的影响[J]．磁性材料及器件，1990，21(4)：53-56
17．李永定．利用铁泥生产聚合硫酸铁[J]．化工环保，1991，11(4)：224-226
18．岩石矿物分析编写小组．岩石矿物分析(第一分册)，第三版[M]．北京：地质出版社1991，227-240
19．中华人民共和国国家标准(6730．9—86)．铁矿石化学分析方法
20．中华人民共和国国家标准(GB11434—89)．铁氧体原材料化学分析方法
21．岩矿分解方法编写．组岩矿分解方法[M]．北京：科学出版社，1979，31-52
22．李稳宏，孙道华，樊君．高纯铁矿粉催化氧化法生产α-Fe_2O_3新工艺[J]．西北大学，2002，32(6)：644-646
23．吴宪军．高品位磁铁矿粉催化氧化研究．(硕士论文)．1997
24．孙道华．精铁矿粉催化氧化制备高纯铁氧体原料α-Fe_2O_3的研究．(硕士论文)．2001
25．日本化学会．无机固态反应[M]．董万棠，董绍俊译．北京：科学出版社，1985
26．胡黎明，古宏晨，郑柏存．等超微粒Fe_3O_4氧化反应过程研究[J]．华东化工学院学报，1992，18(4)：495-498
27．李稳宏，樊君，张粉艳．精铁矿粉催化氧化法生产α-Fe_2O发_3应过程研究[J]．化学工程，2002，30(6)：59-66
28．叶大伦等．实用无机物热力学数据手册[M]．北京：冶金工业出版社1981
29．赵新宇，李春忠，郑柏存等．Fe_3O_4氧化制备γ—Fe_2O_3磁粉动力学[J]．华东理工大学学报，1995，21(5)：561-565
30．李仲轩．炼钢烟尘生产氧化铁红的除硅研究[J]．内蒙古石油化工，1997，23(1)：21-23
31．A．C．切尔尼亚科．化学选矿[M]．郑飞译．北京：中国建筑工业出版社，1982
32．张粉艳，李稳宏，樊君等．铁矿粉化学热加工中铁含量的测定[J]．理化检验(化学分册)，2001，38(11)：560-561
33．朱炳辰．无机化工反应工程[M]．北京：化学工业出版社，1985
34．佛明义，贺建勋．数据统计及实验设计[M]．西安：西北大学出版社，1994
35．常弘哲等．燃料与燃烧[M]．上海：上海交通大学出版社，1981
36．化工部工业炉设计技术中心站编．化学工业炉设计手册[M]．北京：化学工业出版社，1988
37．宋世谟，庄公惠，王正烈．物理化学[M]．北京：高等教育出版社，1996
38．山东建筑材料工业学院编．水泥工业热工过程及设备[M]．北京：中国建筑工业出版社，1981
39．W．特林克斯，M．H．莫欣尼．工业炉[M]．尹加禾译．北京：冶金工业出版社，1980
40．化学工业部第八设计院编．化工传热与燃烧[M]．北京：化学工业出版社，1987
41．于遵宏．化工过程开发[M]．上海：华东理工大学出版社，1997
42．陆震维．化工过程开发[M]．北京：化学工业出版社，1984
43．邹光中，叶继雄，程炜．磁铁矿砂直接生产氧化铁红颜料[J]．无机盐工业，1995，27(2)：19-22
44．周苏闽，王红艳．用铁泥制氧化铁红[J]．化工环保，1999，19(6)：357-359
45．天津化工研究院等编．无机盐工艺手册(下)[M]．第二版．北京：化学工业出版社，2000
46．张永志．硫酸尾气的净化[J]．硫酸工业，1996，4：21-24
47. Gallagher K J. Feitknecht W, Mannweiler U. Mechanism of magnetite to γ- Fe_2O_3. Nature, 1968,217:1118-1121
48. Kojima H, Hanada K. Origin of coercivity changes during the oxidation of. Fe_3O_4 to γ- Fe_2O_3.IEEE Tran On Mag, 1980. MAG-16(1):11-13
49．都有为，张毓昌，陆怀先．超细Fe_3O_4的氧化过程[J]．物理学报，1981，30(3)：424-427
50. Giliot B. Rate law versus oxygen pressure in spinel oxidation to γ lacunar spinels .Mat Res Bull,1980,15:31-39
2．王文亮．结晶化学[M]．北京：人民教育出版社，1961
3. J.W. Mellor. A Comprehensive Treatise on Inorganic and Theoretical Chemistry. Vol. Ⅷ,1934
4．周志刚．等铁氧体磁性材料[M]．北京：科学技术出版社，1981
5．孙来九．精细无机化工工艺学[M]．西安：西北工业大学出版社，1993
6. Gorter, E.W. Saturation Magnetization and Crystal Chemistry and Ferrimagnetic Oxide[J].philips. Res. Rep. 9(1954):295-320;321-365;403-443
7. Guy, A. Introduction to Material Sciece[M].1972
8. Epsteind. FrackiewiezL. Z. Some properties of. Quenched Magnesium Ferrite [J]. App. phys. 29, (1958):376～378
9．朱骥良，吴申年．颜料工艺学[M]．北京：化学工业出版社，1994
10．E．Φ．别达基．颜料化学与工艺学[M]．北京：高等教育出版社，1956
11．曹恩荣，王耕福．我国软磁铁氧体生产之展望[J]．磁性材料及器件，1986，17(1)：37-42
12．王耕福．软磁铁氧体生产、应用、市场预测[J]．磁性材料及器件，1995，26(2)：11-14
13．曾恒兴．铁资源的综合利用[J]．化学世界，1993(12)：619-623
14. Strivens, M.A.,cholG. Ferrite Pro. of the inter, conf[M].239-342
15. Mendelson. M.I.,Particle size Distribution of Coprecipitated Mn-Zn Ferrite Powder[J].J.Amer. Geo. sci. 1976(56):219-221
16．陈彪，陈德乾．Fe_2O_3原料的理化特性对Mn-Zn铁氧体微观结构及性能的影响[J]．磁性材料及器件，1990，21(4)：53-56
17．李永定．利用铁泥生产聚合硫酸铁[J]．化工环保，1991，11(4)：224-226
18．岩石矿物分析编写小组．岩石矿物分析(第一分册)，第三版[M]．北京：地质出版社1991，227-240
19．中华人民共和国国家标准(6730．9—86)．铁矿石化学分析方法
20．中华人民共和国国家标准(GB11434—89)．铁氧体原材料化学分析方法
21．岩矿分解方法编写．组岩矿分解方法[M]．北京：科学出版社，1979，31-52
22．李稳宏，孙道华，樊君．高纯铁矿粉催化氧化法生产α-Fe_2O_3新工艺[J]．西北大学，2002，32(6)：644-646
23．吴宪军．高品位磁铁矿粉催化氧化研究．(硕士论文)．1997
24．孙道华．精铁矿粉催化氧化制备高纯铁氧体原料α-Fe_2O_3的研究．(硕士论文)．2001
25．日本化学会．无机固态反应[M]．董万棠，董绍俊译．北京：科学出版社，1985
26．胡黎明，古宏晨，郑柏存．等超微粒Fe_3O_4氧化反应过程研究[J]．华东化工学院学报，1992，18(4)：495-498
27．李稳宏，樊君，张粉艳．精铁矿粉催化氧化法生产α-Fe_2O发_3应过程研究[J]．化学工程，2002，30(6)：59-66
28．叶大伦等．实用无机物热力学数据手册[M]．北京：冶金工业出版社1981
29．赵新宇，李春忠，郑柏存等．Fe_3O_4氧化制备γ—Fe_2O_3磁粉动力学[J]．华东理工大学学报，1995，21(5)：561-565
30．李仲轩．炼钢烟尘生产氧化铁红的除硅研究[J]．内蒙古石油化工，1997，23(1)：21-23
31．A．C．切尔尼亚科．化学选矿[M]．郑飞译．北京：中国建筑工业出版社，1982
32．张粉艳，李稳宏，樊君等．铁矿粉化学热加工中铁含量的测定[J]．理化检验(化学分册)，2001，38(11)：560-561
33．朱炳辰．无机化工反应工程[M]．北京：化学工业出版社，1985
34．佛明义，贺建勋．数据统计及实验设计[M]．西安：西北大学出版社，1994
35．常弘哲等．燃料与燃烧[M]．上海：上海交通大学出版社，1981
36．化工部工业炉设计技术中心站编．化学工业炉设计手册[M]．北京：化学工业出版社，1988
37．宋世谟，庄公惠，王正烈．物理化学[M]．北京：高等教育出版社，1996
38．山东建筑材料工业学院编．水泥工业热工过程及设备[M]．北京：中国建筑工业出版社，1981
39．W．特林克斯，M．H．莫欣尼．工业炉[M]．尹加禾译．北京：冶金工业出版社，1980
40．化学工业部第八设计院编．化工传热与燃烧[M]．北京：化学工业出版社，1987
41．于遵宏．化工过程开发[M]．上海：华东理工大学出版社，1997
42．陆震维．化工过程开发[M]．北京：化学工业出版社，1984
43．邹光中，叶继雄，程炜．磁铁矿砂直接生产氧化铁红颜料[J]．无机盐工业，1995，27(2)：19-22
44．周苏闽，王红艳．用铁泥制氧化铁红[J]．化工环保，1999，19(6)：357-359
45．天津化工研究院等编．无机盐工艺手册(下)[M]．第二版．北京：化学工业出版社，2000
46．张永志．硫酸尾气的净化[J]．硫酸工业，1996，4：21-24
47. Gallagher K J. Feitknecht W, Mannweiler U. Mechanism of magnetite to γ- Fe_2O_3. Nature, 1968,217:1118-1121
48. Kojima H, Hanada K. Origin of coercivity changes during the oxidation of. Fe_3O_4 to γ- Fe_2O_3.IEEE Tran On Mag, 1980. MAG-16(1):11-13
49．都有为，张毓昌，陆怀先．超细Fe_3O_4的氧化过程[J]．物理学报，1981，30(3)：424-427
50. Giliot B. Rate law versus oxygen pressure in spinel oxidation to γ lacunar spinels .Mat Res Bull,1980,15:31-39