硼镁在铁矿粉造块中的行为和作用规律
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摘要
铁前造块是钢铁企业的能耗大户，磁铁矿又是我国主要的铁矿产资源，而磁铁矿粉造块中存在着诸多问题，含铁品位低，SiO_2含量高，成球性能差，致使产品强度低，易粉化，冶金性能差。围绕这些问题，本文综合了大量文献，掌握了国内外铁矿粉造块的发展动态，尤其在铁矿粉造块中添加有关硼镁添加剂的全部情况及存在的问题，并针对这些问题进行系统的研究，以寻求新的解决方法。
本文研究的主要内容包括：硼、镁在烧结矿中的分布规律；磁铁矿粉烧结过程中铁酸钙、正硅酸钙的形成机理及硼镁对其的作用规律；硼、镁对玻璃相的形成及成分的影响规律；硼、镁对球团矿焙烧温度和氧化速率的影响机理等。本论文的研究借助了矿相显微镜、电子显微镜、X—射线衍射仪、能谱分析仪等微观测试手段。
本文在研究过程中，首先摸索出以下两个新的实验方法，一是采用间断式烧结方法，实现了用静态方法对高温反应瞬间动态过程的研究；二是采用铍试剂Ⅲ隐色分光光度法进行了烧结矿中全硼含量的测定，并对烧结矿矿相进行了逐步分离，从而解决了单纯物理方法所不能解决的难题。
通过对硼、镁在铁矿粉造块中的行为和作用规律的研究发现：硼在烧结矿中主要分布于玻璃相中，镁在烧结矿中的分布与含镁添加物的种类和烧结矿碱度有关，添加物种类和烧结矿的碱度不同，镁在烧结矿中的分布规律不同；磁铁矿粉烧结时铁酸钙和正硅酸钙的形成机理与赤铁矿粉烧结时不同，磁铁矿粉烧结过程中初期液相不是CaO-Fe_2O_3系而是FeO_n-SiO_2系；加入硼镁的作用，首先改善了原料的混匀和造球，降低了烧结料的熔点和初期液相的粘度，有利于铁酸钙的形成，并且抑制了正硅酸钙的生成，而且在烧结过程中，硼可以激活惰性状态下的镁，从而使MgO溶入正硅酸钙取代CaO发生类质同象反应，生成钙镁橄榄石，更加降低了正硅酸钙的生成量；此外，发现了烧结过程中玻璃相成分的变化规律和强度—碱度低凹区的形成机理，并且硼镁同时加入后，可以改变玻璃相的结构和物理性能，提高玻璃相的强度，从而改善了烧结矿的质量；硼镁对球团矿焙烧温度和氧化速率的作用是不同的，球团矿加镁后，强化了磁铁矿的稳定性，其氧化受阻，导致磁铁矿氧化不完全，球团矿强度下降，焙烧温度提高，而硼可以促进磁铁矿的氧化，改变磁铁矿的反应活性，使氧化速率提高，并降低了焙烧温度，所以硼镁适当复合加入，有利于改善球团矿质量。
The agglomeration before ironmaking is a main energy-consuming procedure for iron and steel enterprises. Magnetite is main iron ore resources in China, but there are many problems on the agglomeration of iron ore powders, such as the ore being of the low iron and high SiO2 contents and the poor pelletizing performance, and the sinter being of the low strength, the poor metallurgical performance and easily pulverizing. Considering these problems, this thesis has synthesized a lot of references, and mastered the developments in the agglomeration of the iron ore powders at home and abroad, especially in the present situation and the existing problems of boron and magnesium additives used in the agglomeration of the iron ore powders. According to these problems, a systemic study has been made to seek for some new methods of solving them.
This thesis mainly studies the rules of the boron and magnesium distributions in the sinter, the formation mechanism of calcium ferrite and dicalcium silicate and the effects of boron and magnesium in the sintering process of the magnetite, the effects of boron and magnesium on the formation and composition of the glassiness, the mechanism in which boron and magnesium affect the baking temperature and the oxidation rate of the pellet etc. In this thesis, the analysis instruments such as mineral phase microscope, scanning electron microscope attached with X-ray energy dispersive spectrum and X-ray diffractionmeter are used.
In the course of the study, two breadthroughs on the experimental methods have been made. On the one hand, the static process of an interrupted sintering method used hi the experiment simulates the instant dynamic process of the reaction at a high temperature. On the other hand, the total boron content in the sinter and the boron contents in the different separated mineral phases have been successfully measured by Beryllium reagent III spectrophotometer showing non-color, which solves a difficult problem that can not be solved by physical methods.
After studying the behaviors and effects of boron and magnesium in the agglomeration of the iron ore powders, we find that the most of boron in the sinter is in the glassiness and the distribution of magnesium in the sinter relates to the type of the additive and the basicity of the sinter. The distribution rules of magnesium in the sinter are different when the different additives and basicity of the sinter are used. The formation mechanism of both calcium ferritie and dicalcium silicate in the sintering processes of magnetite is different from those in the sintering processes of hematite. The primary liquid
phase in the sintering processes of the magnetite is from FeOn-Si02 system instead of CaO-Fe2O3 system in the sintering processes of the hematite. The addition of boron and magnesium improve the homogenous degree in the mixing of the raw material and the ability in the pelletizing, and decrease the melting point of the sinter and the viscidity of the primary liquid phase, which favor the formation of the calcium ferrite and restrain the formation of the dicalcium silicate. Meanwhile, boron can activate magnesium in the state of inert in the sintering process, the monticellite is formed because of the isomorphism reaction resulted from the dissolution of magnesia into the dicalium silicate instead of the calcium silicate. In addition, the changing trends in the glossiness composition and the formation mechanism of the low concave area in the relationship between strength and basicity of the sinter are found. The additions of boron and magnesium together in the sinter can alter the structure and physical prope
rties of the glossiness, increase the strength of the glassiness and improve the quality of the sinter. Magnesium and boron play very different roles in affecting the baking temperature and the oxidation rate of the pellet. The addition of magnesium in the pellet enhances the stability of the magnetite and restrains its oxidation, which result in its incomplete oxidation, the decrease in the strengt
本文研究的主要内容包括：硼、镁在烧结矿中的分布规律；磁铁矿粉烧结过程中铁酸钙、正硅酸钙的形成机理及硼镁对其的作用规律；硼、镁对玻璃相的形成及成分的影响规律；硼、镁对球团矿焙烧温度和氧化速率的影响机理等。本论文的研究借助了矿相显微镜、电子显微镜、X—射线衍射仪、能谱分析仪等微观测试手段。
本文在研究过程中，首先摸索出以下两个新的实验方法，一是采用间断式烧结方法，实现了用静态方法对高温反应瞬间动态过程的研究；二是采用铍试剂Ⅲ隐色分光光度法进行了烧结矿中全硼含量的测定，并对烧结矿矿相进行了逐步分离，从而解决了单纯物理方法所不能解决的难题。
通过对硼、镁在铁矿粉造块中的行为和作用规律的研究发现：硼在烧结矿中主要分布于玻璃相中，镁在烧结矿中的分布与含镁添加物的种类和烧结矿碱度有关，添加物种类和烧结矿的碱度不同，镁在烧结矿中的分布规律不同；磁铁矿粉烧结时铁酸钙和正硅酸钙的形成机理与赤铁矿粉烧结时不同，磁铁矿粉烧结过程中初期液相不是CaO-Fe_2O_3系而是FeO_n-SiO_2系；加入硼镁的作用，首先改善了原料的混匀和造球，降低了烧结料的熔点和初期液相的粘度，有利于铁酸钙的形成，并且抑制了正硅酸钙的生成，而且在烧结过程中，硼可以激活惰性状态下的镁，从而使MgO溶入正硅酸钙取代CaO发生类质同象反应，生成钙镁橄榄石，更加降低了正硅酸钙的生成量；此外，发现了烧结过程中玻璃相成分的变化规律和强度—碱度低凹区的形成机理，并且硼镁同时加入后，可以改变玻璃相的结构和物理性能，提高玻璃相的强度，从而改善了烧结矿的质量；硼镁对球团矿焙烧温度和氧化速率的作用是不同的，球团矿加镁后，强化了磁铁矿的稳定性，其氧化受阻，导致磁铁矿氧化不完全，球团矿强度下降，焙烧温度提高，而硼可以促进磁铁矿的氧化，改变磁铁矿的反应活性，使氧化速率提高，并降低了焙烧温度，所以硼镁适当复合加入，有利于改善球团矿质量。
The agglomeration before ironmaking is a main energy-consuming procedure for iron and steel enterprises. Magnetite is main iron ore resources in China, but there are many problems on the agglomeration of iron ore powders, such as the ore being of the low iron and high SiO2 contents and the poor pelletizing performance, and the sinter being of the low strength, the poor metallurgical performance and easily pulverizing. Considering these problems, this thesis has synthesized a lot of references, and mastered the developments in the agglomeration of the iron ore powders at home and abroad, especially in the present situation and the existing problems of boron and magnesium additives used in the agglomeration of the iron ore powders. According to these problems, a systemic study has been made to seek for some new methods of solving them.
This thesis mainly studies the rules of the boron and magnesium distributions in the sinter, the formation mechanism of calcium ferrite and dicalcium silicate and the effects of boron and magnesium in the sintering process of the magnetite, the effects of boron and magnesium on the formation and composition of the glassiness, the mechanism in which boron and magnesium affect the baking temperature and the oxidation rate of the pellet etc. In this thesis, the analysis instruments such as mineral phase microscope, scanning electron microscope attached with X-ray energy dispersive spectrum and X-ray diffractionmeter are used.
In the course of the study, two breadthroughs on the experimental methods have been made. On the one hand, the static process of an interrupted sintering method used hi the experiment simulates the instant dynamic process of the reaction at a high temperature. On the other hand, the total boron content in the sinter and the boron contents in the different separated mineral phases have been successfully measured by Beryllium reagent III spectrophotometer showing non-color, which solves a difficult problem that can not be solved by physical methods.
After studying the behaviors and effects of boron and magnesium in the agglomeration of the iron ore powders, we find that the most of boron in the sinter is in the glassiness and the distribution of magnesium in the sinter relates to the type of the additive and the basicity of the sinter. The distribution rules of magnesium in the sinter are different when the different additives and basicity of the sinter are used. The formation mechanism of both calcium ferritie and dicalcium silicate in the sintering processes of magnetite is different from those in the sintering processes of hematite. The primary liquid
phase in the sintering processes of the magnetite is from FeOn-Si02 system instead of CaO-Fe2O3 system in the sintering processes of the hematite. The addition of boron and magnesium improve the homogenous degree in the mixing of the raw material and the ability in the pelletizing, and decrease the melting point of the sinter and the viscidity of the primary liquid phase, which favor the formation of the calcium ferrite and restrain the formation of the dicalcium silicate. Meanwhile, boron can activate magnesium in the state of inert in the sintering process, the monticellite is formed because of the isomorphism reaction resulted from the dissolution of magnesia into the dicalium silicate instead of the calcium silicate. In addition, the changing trends in the glossiness composition and the formation mechanism of the low concave area in the relationship between strength and basicity of the sinter are found. The additions of boron and magnesium together in the sinter can alter the structure and physical prope
rties of the glossiness, increase the strength of the glassiness and improve the quality of the sinter. Magnesium and boron play very different roles in affecting the baking temperature and the oxidation rate of the pellet. The addition of magnesium in the pellet enhances the stability of the magnetite and restrains its oxidation, which result in its incomplete oxidation, the decrease in the strengt
引文
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66 陈国珍等．紫外—可见光分光光度法(上下、册)．北京：原子能出版社，1983
67 朱玉伦等．硼特效树脂分离分光光度法测定岩石矿物中痕量硼．岩矿测试．1989(3)：21-25
68 朱玉伦等．分光光度法中过量显色剂隐色的研究(Ⅰ)．分析化学．1986(6)：17-21
69 张孙伟等．有色试剂在分析中的应用．北京：科学出版社，1981
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75 Eva Dudrova, Marcela Selecka, Radovan Rures. Effect of Boron Addition on Microstucture and Properties of Sintered Fe-1.5 Mo Powder Materials. ISIJ International. 1997(37): 59-64
76 K.A.Zimmermann, K.H.Peters. Mischbett and Sinter-technik bet der Mollervorberitung in Werk Schwelgern der Thyssen Stahl AG. Stahl und Eisen. 1983,103: 697-702
77 A.Muan, E.F.Osborn. Preprint of General Meeting of American Iron and Steel Institute. New York, 1951(3): 23-24
78 Ichiro Shigaki, Mineo Sawada, Masahiro Maekawa. Melting Property of MgO Containing Sinter. Transactions ISIJ. 1981(21): 862-869
79 K.H.Peters, H.Beer. Verfahrenstechnische Mabnahmen zur Erhohung der Sinterleistung im Werk Schwelgern der Thyssen Stahl AG. Stahl und Eisen. 1986(106): 763-767
80 Moustafa, S.F. Morsi, M.B. Formation of Mg ferrite by mechanical alloying and sintering. Materials Letters. 1998,(34):241-247
81 Haga, Tetsuzo Kasama, Shunji Kozono, Takuma Oga. Evaluation of Melting Characteristics of Fine Iron Ores by the Tablet Sintering Test. Tetsu-To-Hagane/Journal of The Iron and Steel Institute of Japan. 1996,82(12):981-986
82 P.R.Dawson. Research Studies on Sintering and Sinter Quality. Ironmaking and Steelmaking. 1993,20(2): 137-142
83 Eiki Kasai, Shengli Wu, Yasuo Omori. Factors Gonerning the Strength of Agglomerated Granules affter Sintering. ISIJ International. 1991(1): 17-23
84 Kawai, Jun Takahasi, Hideyuki Hayshi, Kouichi. Magnesium K X-ray Emission Spectra of Mg, MgO and Oliving [(Mg, Fe)2(SiO4)] by EPMA and XRF. Tetsu-To-Hagane. 1999,85(2): 164-168
85 Xingmin Guo, Yoichi Oho. Memoirs of the Faculty of Engineering Kyushu Univerity. 1992(52): 1-7
86 F.Matsuno, T.Harada. Changes of mineral phase during the sintering of iron ore-lime stone systems. Transactions ISIJ. 1981(21): 318
87 张玉柱，郎建峰，李振国．B2O3对磁铁矿烧结过程铁酸钙形成的影响．河北理工学院学报．1999(4)：13-18
88 张玉柱，郎建峰，李振国．含硼添加剂改善烧结矿质量机理及硼镁复合添加剂的研究．矿产综合利用．2000(1)：29-32
89 Ohtsuki, Chikara Kobayashi, Yukio Tsuru, Kanji. Compositional dependence of bioactivity of glasses in the system CaO-B_2O_3-SiO_2: Its in vitro evaluation. Zairyo/Journal of the Society of Materials Science, 1995(44):693-699
90 Yang, Cheng-Fu Cheng, Chien-Min. Influence of B2O3 on the Sintering of MgO-CaO-Al_2O_3-SiO_2 powder. Compsite glass Powder. Ceramics International. 1999(4): 383-387
91 Lo, Sh.-H. Yang, Ch.-F. Sintering Characteristics of B_2O_3 added MgO-CaO-Al_2O_3-SiO_2 glass Powder. Ceramics International. 1998(2): 139-144
92 Cheng, Chien-Min Yang, Cheng-Fu Lo, Shi-Hong. Influence of crystallization on the flexural strength of MgO-CaO-Al_2O_3-SiO_2 composite glass. Ceramics International. 1999(6):581-586
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65 周乐光．矿石学基础．北京：冶金工业出版社，1990
66 陈国珍等．紫外—可见光分光光度法(上下、册)．北京：原子能出版社，1983
67 朱玉伦等．硼特效树脂分离分光光度法测定岩石矿物中痕量硼．岩矿测试．1989(3)：21-25
68 朱玉伦等．分光光度法中过量显色剂隐色的研究(Ⅰ)．分析化学．1986(6)：17-21
69 张孙伟等．有色试剂在分析中的应用．北京：科学出版社，1981
70 陈莉华等．硼锑钼杂多酸—丁基罗丹明B四元络合体系分光光度法测钢中硼．冶金分析．1995(3)：19-24
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72 何安元等．硼—苦杏仁酸—孔雀绿三元络合物萃取光度法测定钢中酸溶硼．理化检验．1998(1)：18-23
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74 Hosotani, Yozo Yamaguchi, Kazuyoshi Orimoto, Tak. Development of Evaluation Method for Softening-melting Properties of Sinter. Tetsu-To-Hagane/Journal of the Iron and Steel Institute of Japan. 1997,83(2):97-102
75 Eva Dudrova, Marcela Selecka, Radovan Rures. Effect of Boron Addition on Microstucture and Properties of Sintered Fe-1.5 Mo Powder Materials. ISIJ International. 1997(37): 59-64
76 K.A.Zimmermann, K.H.Peters. Mischbett and Sinter-technik bet der Mollervorberitung in Werk Schwelgern der Thyssen Stahl AG. Stahl und Eisen. 1983,103: 697-702
77 A.Muan, E.F.Osborn. Preprint of General Meeting of American Iron and Steel Institute. New York, 1951(3): 23-24
78 Ichiro Shigaki, Mineo Sawada, Masahiro Maekawa. Melting Property of MgO Containing Sinter. Transactions ISIJ. 1981(21): 862-869
79 K.H.Peters, H.Beer. Verfahrenstechnische Mabnahmen zur Erhohung der Sinterleistung im Werk Schwelgern der Thyssen Stahl AG. Stahl und Eisen. 1986(106): 763-767
80 Moustafa, S.F. Morsi, M.B. Formation of Mg ferrite by mechanical alloying and sintering. Materials Letters. 1998,(34):241-247
81 Haga, Tetsuzo Kasama, Shunji Kozono, Takuma Oga. Evaluation of Melting Characteristics of Fine Iron Ores by the Tablet Sintering Test. Tetsu-To-Hagane/Journal of The Iron and Steel Institute of Japan. 1996,82(12):981-986
82 P.R.Dawson. Research Studies on Sintering and Sinter Quality. Ironmaking and Steelmaking. 1993,20(2): 137-142
83 Eiki Kasai, Shengli Wu, Yasuo Omori. Factors Gonerning the Strength of Agglomerated Granules affter Sintering. ISIJ International. 1991(1): 17-23
84 Kawai, Jun Takahasi, Hideyuki Hayshi, Kouichi. Magnesium K X-ray Emission Spectra of Mg, MgO and Oliving [(Mg, Fe)2(SiO4)] by EPMA and XRF. Tetsu-To-Hagane. 1999,85(2): 164-168
85 Xingmin Guo, Yoichi Oho. Memoirs of the Faculty of Engineering Kyushu Univerity. 1992(52): 1-7
86 F.Matsuno, T.Harada. Changes of mineral phase during the sintering of iron ore-lime stone systems. Transactions ISIJ. 1981(21): 318
87 张玉柱，郎建峰，李振国．B2O3对磁铁矿烧结过程铁酸钙形成的影响．河北理工学院学报．1999(4)：13-18
88 张玉柱，郎建峰，李振国．含硼添加剂改善烧结矿质量机理及硼镁复合添加剂的研究．矿产综合利用．2000(1)：29-32
89 Ohtsuki, Chikara Kobayashi, Yukio Tsuru, Kanji. Compositional dependence of bioactivity of glasses in the system CaO-B_2O_3-SiO_2: Its in vitro evaluation. Zairyo/Journal of the Society of Materials Science, 1995(44):693-699
90 Yang, Cheng-Fu Cheng, Chien-Min. Influence of B2O3 on the Sintering of MgO-CaO-Al_2O_3-SiO_2 powder. Compsite glass Powder. Ceramics International. 1999(4): 383-387
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