Me～（2+）-NH_4～+-SO_4～（2-）-H_2O体系相平衡及直接法制备锰锌软磁粉料研究
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摘要
针对“陶瓷法”和“共沉淀法”存在的问题，我们将无机化工、湿法冶金和磁性材料等学科进行交叉，成功开发出“直接法”制备锰锌软磁铁氧体材料新技术。本论文通过三元Me~(2+)-NH_4~+-SO_4~(2-)-H_2O体系(Me代表Fe、Mn及Zn，以下同)相平衡的研究，奠定了直接法制备锰锌软磁铁氧体材料技术的关键步骤——溶液深度净化的理论基础，据此开发成功硫酸盐溶液体系中Me~(2+)的深度净化方法——复盐沉淀净化法，从而将直接法的产品质量提升一个档次。经过实验室小试、扩大试验及工业性试验，实现了直接法的工业应用，可生产出质量与日本TDK公司PC30产品相当的锰锌软磁粉料。
1．三元体系Me~(2+)-NH_4~+-SO_4~(2-)-H_2O相平衡研究
1) 用等温溶解平衡法，研究了三元体系Me~(2+)-NH_4~+-SO_4~(2-)-H_2O 298K的溶解度，并绘制其平衡相图。实验结果表明，在Mn~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中，有MnSO_4·H_2O，(NH_4)_2Mn(SO_4)_2·6H_2O和(NH_4)_2SO_4的三条饱和曲线，组成为MnSO_4·H_2O和(NH_4)_2Mn(SO_4)_2·6H_2O，(NH_4)_2Mn(SO_4)_2·6H_2O和(NH_4)_2SO_4的两个共饱和点，以及平衡固相为(NH_4)_2SO_4，(NH_4)_2Mn(SO_4)_2·6H_2O和MnSO_4·H_2O的三个纯盐结晶区。在Zn~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中，有(NH_4)_2Zn(SO_4)_2·6H_2O，ZnSO_4·7H_2O与(NH_4)_2SO_4的三条饱和曲线，组成为(NH_4)_2Zn(SO_4)_2·6H_2O和ZnSO_4·7H_2O，(NH_4)_2SO_4和(NH_4)_2Zn(SO_4)_2·6H_2O的两个共饱和点，以及平衡固相为(NH_4)_2Zn(SO_4)_2·6H_2O，ZnSO_4·7H_2O和(NH_4)_2SO_4的三个纯盐结晶区。在Fe~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中，有(NH_4)_2Fe(SO_4)_2·6H_2O，FeSO_4·7H_2O和(NH_4)_2SO_4的三条饱和曲线，组成为(NH_4)_2Fe(SO_4)_2·6H_2O和FeSO_4·7H_2O，(NH_4)_2Fe(SO_4)_2·6H_2O和(NH_4)_2SO_4的两个共饱和点，以及平衡固相为(NH_4)_2Fe(SO_4)_2·6H_2O，FeSO_4·7H_2O和(NH_4)_2SO_4的三个纯盐结晶区。研究成果可为Me~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中的Me~(2+)的复盐沉淀深度净化提供理论指导。
2) 研究了Me~(2+)-NH_4~+-SO_4~(2-)-H_2O三元体系的饱和溶液密度、pH值和折光率，绘制了密度-组成、折光率-组成和pH-组成图。实验结果表明，随着溶液组分的变化，饱和溶液的密度和折光率在其共饱和点处均产生突变；但溶液组分的变化，对pH的影响不大。饱和溶液物化性质的研究成果，可为复盐沉淀深度净化工艺条件控制提供了理论依据。
In order to overcome the disadvantages of ceramics method and co-precipitation method on the preparation of Mn-Zn soft magnetic ferrite materials, we combined hydrometallurgy and inorganic chemical engineering with ferrite technology, and the direct-method on the preparation of Mn-Zn soft magnetic ferrite has been successfully developed. In this thesis, through the studies on the phase equilibrium in the ternary Me~(2+)-NH_4~+-SO_4~(2-)-H_2O systems, the basic theories being the key factors of the simultaneous deep purification process of Fe~(2+), Mn~(2+) and Zn~(2+) in the leached solution containing Fe~(2+), Mn~(2+), Zn~(2+), Pb~(2+), Ca~(2+), Mg~(2+) and et al were resolved. Therefore, a novel purification method of double salt precipitation method having the capacity of purification for many kinds metal ions in solution was developed. And when the double salt precipitation technology is applied in the deep purification process of direct method, the qualities of Mn-Zn soft magnetic ferrite samples can be improved greatly. After the table and bench and industry scale experimental studies, the direct method on the preparation of Mn-Zn soft magnetic ferrite has been successfully industrialized and soft magnetic powders being similar to PC30 produced by Japan TDK company can be produced by the direct method.
1. Studies on solubility phase equilibrium in the ternary Me~(2+)-NH_4~+-SO_4~(2-)-H_2O systems.
1) The phase equilibrium in the ternary system of Me~(2+)-NH_4~+-SO_4~(2-)-H_2O at 298 K was studied by isothermal equilibrium method and many significant experiment results were obtained. In the ternary system of Mn~(2+)-NH_4~+-SO_4~(2-)-H_2O, there were three saturation curves given by MnSO_4·H_2O, (NH_4)_2Mn(SO_4)_2·6H_2O and (NH_4)_2SO_4, respectively. There were two co-saturation points A having the composition of MnSO_4·H_2O and (NH_4)_2Mn(SO_4)_2·6H_2O and B given by (NH_4)_2Mn(SO_4)_2·6H_2O and (NH_4)_2SO_4. There were three purification crystal areas given by MnSO_4·H_2O (NH_4)_2Mn(SO_4)_2·6H_2O, and (NH_4)_2SO_4, respectively. In the ternary system of Zn~(2+)-NH_4~+-SO_4~(2-)-H_2O, there were three saturation curves given by ZnSO_4-7H_2O (NH_4)_2Zn(SO_4)_2·6H_2O, and (NH_4)_2SO_4, respectively. There were two co-saturation points C having the composition of (NH_4)_2Zn(SO_4)_2·6H_2O and ZnSO_4·7H_2O and D given by (NH_4)_2SO_4 and (NH_4)_2Zn(SO_4)_2·6H_2O, respectively. There were three purification crystal areas given by (NH_4)_2Zn(SO_4)_2·6H_2O, ZnSO_4·7H_2O and (NH_4)_2SO_4, respectively. In the ternary system of Fe~(2+)-NH_4~+-SO_4~(2-)-H_2O, there were three saturation curves given by (NH_4)_2Fe(SO_4)_2·6H_2O, FeSO_4·7H_2O and (NH_4)_2SO_4,
1．三元体系Me~(2+)-NH_4~+-SO_4~(2-)-H_2O相平衡研究
1) 用等温溶解平衡法，研究了三元体系Me~(2+)-NH_4~+-SO_4~(2-)-H_2O 298K的溶解度，并绘制其平衡相图。实验结果表明，在Mn~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中，有MnSO_4·H_2O，(NH_4)_2Mn(SO_4)_2·6H_2O和(NH_4)_2SO_4的三条饱和曲线，组成为MnSO_4·H_2O和(NH_4)_2Mn(SO_4)_2·6H_2O，(NH_4)_2Mn(SO_4)_2·6H_2O和(NH_4)_2SO_4的两个共饱和点，以及平衡固相为(NH_4)_2SO_4，(NH_4)_2Mn(SO_4)_2·6H_2O和MnSO_4·H_2O的三个纯盐结晶区。在Zn~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中，有(NH_4)_2Zn(SO_4)_2·6H_2O，ZnSO_4·7H_2O与(NH_4)_2SO_4的三条饱和曲线，组成为(NH_4)_2Zn(SO_4)_2·6H_2O和ZnSO_4·7H_2O，(NH_4)_2SO_4和(NH_4)_2Zn(SO_4)_2·6H_2O的两个共饱和点，以及平衡固相为(NH_4)_2Zn(SO_4)_2·6H_2O，ZnSO_4·7H_2O和(NH_4)_2SO_4的三个纯盐结晶区。在Fe~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中，有(NH_4)_2Fe(SO_4)_2·6H_2O，FeSO_4·7H_2O和(NH_4)_2SO_4的三条饱和曲线，组成为(NH_4)_2Fe(SO_4)_2·6H_2O和FeSO_4·7H_2O，(NH_4)_2Fe(SO_4)_2·6H_2O和(NH_4)_2SO_4的两个共饱和点，以及平衡固相为(NH_4)_2Fe(SO_4)_2·6H_2O，FeSO_4·7H_2O和(NH_4)_2SO_4的三个纯盐结晶区。研究成果可为Me~(2+)-NH_4~+-SO_4~(2-)-H_2O体系中的Me~(2+)的复盐沉淀深度净化提供理论指导。
2) 研究了Me~(2+)-NH_4~+-SO_4~(2-)-H_2O三元体系的饱和溶液密度、pH值和折光率，绘制了密度-组成、折光率-组成和pH-组成图。实验结果表明，随着溶液组分的变化，饱和溶液的密度和折光率在其共饱和点处均产生突变；但溶液组分的变化，对pH的影响不大。饱和溶液物化性质的研究成果，可为复盐沉淀深度净化工艺条件控制提供了理论依据。
In order to overcome the disadvantages of ceramics method and co-precipitation method on the preparation of Mn-Zn soft magnetic ferrite materials, we combined hydrometallurgy and inorganic chemical engineering with ferrite technology, and the direct-method on the preparation of Mn-Zn soft magnetic ferrite has been successfully developed. In this thesis, through the studies on the phase equilibrium in the ternary Me~(2+)-NH_4~+-SO_4~(2-)-H_2O systems, the basic theories being the key factors of the simultaneous deep purification process of Fe~(2+), Mn~(2+) and Zn~(2+) in the leached solution containing Fe~(2+), Mn~(2+), Zn~(2+), Pb~(2+), Ca~(2+), Mg~(2+) and et al were resolved. Therefore, a novel purification method of double salt precipitation method having the capacity of purification for many kinds metal ions in solution was developed. And when the double salt precipitation technology is applied in the deep purification process of direct method, the qualities of Mn-Zn soft magnetic ferrite samples can be improved greatly. After the table and bench and industry scale experimental studies, the direct method on the preparation of Mn-Zn soft magnetic ferrite has been successfully industrialized and soft magnetic powders being similar to PC30 produced by Japan TDK company can be produced by the direct method.
1. Studies on solubility phase equilibrium in the ternary Me~(2+)-NH_4~+-SO_4~(2-)-H_2O systems.
1) The phase equilibrium in the ternary system of Me~(2+)-NH_4~+-SO_4~(2-)-H_2O at 298 K was studied by isothermal equilibrium method and many significant experiment results were obtained. In the ternary system of Mn~(2+)-NH_4~+-SO_4~(2-)-H_2O, there were three saturation curves given by MnSO_4·H_2O, (NH_4)_2Mn(SO_4)_2·6H_2O and (NH_4)_2SO_4, respectively. There were two co-saturation points A having the composition of MnSO_4·H_2O and (NH_4)_2Mn(SO_4)_2·6H_2O and B given by (NH_4)_2Mn(SO_4)_2·6H_2O and (NH_4)_2SO_4. There were three purification crystal areas given by MnSO_4·H_2O (NH_4)_2Mn(SO_4)_2·6H_2O, and (NH_4)_2SO_4, respectively. In the ternary system of Zn~(2+)-NH_4~+-SO_4~(2-)-H_2O, there were three saturation curves given by ZnSO_4-7H_2O (NH_4)_2Zn(SO_4)_2·6H_2O, and (NH_4)_2SO_4, respectively. There were two co-saturation points C having the composition of (NH_4)_2Zn(SO_4)_2·6H_2O and ZnSO_4·7H_2O and D given by (NH_4)_2SO_4 and (NH_4)_2Zn(SO_4)_2·6H_2O, respectively. There were three purification crystal areas given by (NH_4)_2Zn(SO_4)_2·6H_2O, ZnSO_4·7H_2O and (NH_4)_2SO_4, respectively. In the ternary system of Fe~(2+)-NH_4~+-SO_4~(2-)-H_2O, there were three saturation curves given by (NH_4)_2Fe(SO_4)_2·6H_2O, FeSO_4·7H_2O and (NH_4)_2SO_4,
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