腐植酸基铁矿球团粘结剂的构效关系研究
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摘要
摘要：粘结剂是生产铁矿球团的关键性辅助原料,其性能优劣直接关系到球团矿质量的好坏。腐植酸类物质是含有羧基、羟基以及苯环结构的有机高分子聚合物,已成功应用于直接还原球团的生产。目前,腐植酸基粘结剂在铁精矿表面的作用机理尚不完全明确。此外,由于对粘结剂的物化特性特别是其结构特征缺乏系统的认识和研究,尚未建立粘结剂的结构与性能关系。
本论文利用我国不同低阶变质煤资源(褐煤和风化煤),制备出了以黄腐酸、胡敏酸为功能组分的腐植酸基粘结剂；采用红外光谱(FTIR)、环境扫描电镜(ESEM)、原子力显微镜(AFM)、热重-差热(TG-DSC)、X射线光电子能谱(XPS)等手段,深入研究了粘结剂功能组分的性质及其在铁矿表面的吸附行为；运用量子化学中的密度泛函理论(DFT),定量计算了粘结剂与不同类型铁精矿中铁矿物作用的能量判据△ETRT,揭示了粘结剂分子空间因素对其亲固能力的影响；根据粘结剂功能组分的结构与性能关系,建立了铁矿球团用腐植酸基粘结剂的技术要求。本论文的主要结论如下：
(1)黄腐酸和胡敏酸之间的理化性质存在明显差异。黄腐酸分散性好、芳构化程度低、分子量小,而含氧官能团含量较高。胡敏酸的非极性芳香官能团含量高,而含氧官能团含量较低。胡敏酸的热稳定性好,热分解区间较宽。
(2)黄腐酸和胡敏酸在铁精矿表面发生化学吸附,且前者的吸附作用较强。黄腐酸、胡敏酸在铁精矿表面的吸附符合Freundlich式和二级动力学模型,理论最大吸附量分别为8.92×10-3mg·cm-2和2.70×10-3mg·cm-2。吸附黄腐酸或胡敏酸后,铁精矿中Fe2p3/2的电子结合能变化量分别为-1.12eV和-0.57eV,净脱附热分别为-87.0J·g-1和-26.7J·g-1。粘结剂功能组分在铁精矿表面呈网状、纤维状或堆簇状吸附。黄腐酸的存在能够促进胡敏酸在铁精矿表面的吸附。
(3)DFT计算表明,羧基的亲固能力大于酚羟基。随着极性基团数量的增加,粘结剂的亲固能力提高。对粘结剂分子来说,非极性芳香烃基越大,其化学作用越强,但其静电力作用越弱。
粘结剂主要通过化学作用与矿物表面发生亲固反应。粘结剂与矿物晶胞表面的亲固能力从强到弱依次为FeTiO3、Fe3O4、Fe2O3.对于粘结剂与矿物晶胞表面之间的作用力来说,正配键共价作用△E2RT对能量判据△TRT的贡献最大,静电力作用△E1RT的贡献最小。
(4)黄腐酸的吸附性能、粘结性能与其光密度比(E4/E6)呈负相关性。黄腐酸分子量越大或芳构化程度越高,其吸附、粘结性能越强。胡敏酸的吸附性能、粘结性能与其E4/E6呈正相关性。胡敏酸分子量越小或芳构化程度越低,其吸附、粘结性能越强。腐植酸分子量过大或过小均不利于其吸附、粘结性能。当黄腐酸、胡敏酸的分子量分别接近600Da和1500Da时,二者的吸附、粘结性能最好。当黄腐酸、胡敏酸的分子量为最优值时,腐植酸分子量趋于1410～1490Da。
铁矿球团用腐植酸基粘结剂的技术要求为：1)腐植酸的E4/E6接近3.86；2)腐植酸含量(容量法)为40%～50%；3)适宜的胡富比因铁精矿类型不同而异,对于普通磁铁精矿、钒钛磁铁精矿、赤铁精矿来说,最佳胡富比分别接近8：2、7：3和6：4。
(5)针对普通磁铁精矿、钒钛磁铁精矿和赤铁精矿,制备出3种腐植酸基粘结剂。粘结剂用量为0.75%的球团矿的抗压强度超过膨润土用量为2.0%的球团矿,与膨润土球团相比铁品位提高1.0%以上、冶金性能相当。图88幅,表44个,参考文献198篇
Abstract:Binder is indispensable in the production of iron ore pellets, which can dramaticly influence the quality of finished products. Humic substances as a type of organic macromolecule polymer consist of carboxyl groups and hydroxyl groups, which should be further researched because of their ideal adhesive molecular conformation. At present, functional mechanisms of humic substances on the surface of iron ore is not fully clear. Furthermore, structure-performance relationships of humic substances based binder have not yet been clearly established because of few researches on their physical and chemical properties especially on the structure characteristics.
A type of humic substances based binders are prepared from lignite and weather coals. The binders mainly consist of two active fractions including fulvic acid and humic acid. The properties of binder active fractions and their functional mechanisms were studied by adopting infrared spectroscopy (FTIR), environment scanning electron microscope (ESEM), atomic force microscope (AFM), thermogravimetric-differential thermal analysis (TG-DSC) and X-ray photoelectron spectroscopy (XPS) et.al; The energy criterion△ETRT between binder and target minerals were calculated using the density functional theory (DFT), molecular functional assembly and binder molecular model; And most of all, the technical requirements for humic substances based binder are proposed based on the structure-performance relationships of binder active fractions. The main conclusions of this research are summaried as follows:
(1) There are obvious differences in physical and chemical properties between binder active fractions (fulvic and humic aicds). Compared to humic acid, Fulvic acid is characterized by better dispersibility, relatively low degree of aromatization and small molecular weight but relatively high content of oxygen-containing functional groups. Humic acid processes good thermal stability and wider thermal decomposition range.
(2) Chemical adsorption occurs between binder active fractions and iron concentrate surface, indicating the adsorption of fulvic acid is stronger. The adsorption of binder is more accord with Freundlich model and second order kinetics. The theoretical maximum adsorption amount of fulvic and humic acids is respectively8.92×10-3mg·cm-2and2.70×10-3mg·cm-2. Electronic binding energy variation of Fe2p3/2after adsorption of fulvic and humic acids are-1.12eV and-0.57eV, respectively. The net desorption energy of fulvic and humic acids is respectively-87.0J/g and-26.7J/g. The active fractions adsorbs on the surface of iron concentrates in the shape of net, fibrous or clusters. The adsorption of humic acid can be enhanced by fulvic acid.
(3) DFT calculation demonstrates that, compared to phenolic hydroxyl group, carboxyl group performs better solid-affinitive capability. The solid-affinitive capability of binder increases with the increase of the number of polar groups. For binder molecule, the enlargement of non-polar aromatic hydrocarbon can enhance the capacity of chemical adsorption, but also result in decrease of electrostatic forcing.
Reagent active equation and energy criterion demonstrates that binder molecule adsorbs on mineral surface with chemical reaction as deciding effort. The order of solid affinitive capability of binder with three target minerals follows FeTiO3> Fe3O4> Fe2O3. For interaction between binder and target minerals, the contribution of positive covalent coordination bond△E2RTT to energy criterion△ETRT is biggest, while electrostatic forcing△E1RT is smallest.
(4) The adsorption and subsequent binding strengths are negative correlation with E4/E6of fulvic acid. The performance of fulvic acid is increased with increasing its molecular weight. The adsorption and binding strengths are positive correlation with E4/E6of humic acid. The performance of humic acid is increased with decreasing its molecular weight. The molecular weight which is too large or too small is unfavorable to the adsorption and binding strengths of humic substances. The performance of active fractions performs better when the molecular weight of fulvic acid and humic acids is respectively600Da and1500Da. The idea range of molecular weight of humic substances is from1410Da to1490Da.
The technical requirements for humic substances based binder are proposed by following:1) E4/E6of humicsubstances should be close to3.86;2) The content of humic substances should be in the range of40%to50%;3) For magnetite, V-Ti containing magnetite and hematite, the mass ratio of humic acid to fulvic acid should be close to8:2,7:3and6:4.
(5) For magnetite, V-Ti containing magnetite and hematite concentrates, three kinds of binders are prepared. Compared to those pellets prepared with2.0%bentonite, the pellets with0.75%novel binder are characterized by1.0%higher TFe grade, better compression strength and the similar metallurgical properties.
本论文利用我国不同低阶变质煤资源(褐煤和风化煤),制备出了以黄腐酸、胡敏酸为功能组分的腐植酸基粘结剂；采用红外光谱(FTIR)、环境扫描电镜(ESEM)、原子力显微镜(AFM)、热重-差热(TG-DSC)、X射线光电子能谱(XPS)等手段,深入研究了粘结剂功能组分的性质及其在铁矿表面的吸附行为；运用量子化学中的密度泛函理论(DFT),定量计算了粘结剂与不同类型铁精矿中铁矿物作用的能量判据△ETRT,揭示了粘结剂分子空间因素对其亲固能力的影响；根据粘结剂功能组分的结构与性能关系,建立了铁矿球团用腐植酸基粘结剂的技术要求。本论文的主要结论如下：
(1)黄腐酸和胡敏酸之间的理化性质存在明显差异。黄腐酸分散性好、芳构化程度低、分子量小,而含氧官能团含量较高。胡敏酸的非极性芳香官能团含量高,而含氧官能团含量较低。胡敏酸的热稳定性好,热分解区间较宽。
(2)黄腐酸和胡敏酸在铁精矿表面发生化学吸附,且前者的吸附作用较强。黄腐酸、胡敏酸在铁精矿表面的吸附符合Freundlich式和二级动力学模型,理论最大吸附量分别为8.92×10-3mg·cm-2和2.70×10-3mg·cm-2。吸附黄腐酸或胡敏酸后,铁精矿中Fe2p3/2的电子结合能变化量分别为-1.12eV和-0.57eV,净脱附热分别为-87.0J·g-1和-26.7J·g-1。粘结剂功能组分在铁精矿表面呈网状、纤维状或堆簇状吸附。黄腐酸的存在能够促进胡敏酸在铁精矿表面的吸附。
(3)DFT计算表明,羧基的亲固能力大于酚羟基。随着极性基团数量的增加,粘结剂的亲固能力提高。对粘结剂分子来说,非极性芳香烃基越大,其化学作用越强,但其静电力作用越弱。
粘结剂主要通过化学作用与矿物表面发生亲固反应。粘结剂与矿物晶胞表面的亲固能力从强到弱依次为FeTiO3、Fe3O4、Fe2O3.对于粘结剂与矿物晶胞表面之间的作用力来说,正配键共价作用△E2RT对能量判据△TRT的贡献最大,静电力作用△E1RT的贡献最小。
(4)黄腐酸的吸附性能、粘结性能与其光密度比(E4/E6)呈负相关性。黄腐酸分子量越大或芳构化程度越高,其吸附、粘结性能越强。胡敏酸的吸附性能、粘结性能与其E4/E6呈正相关性。胡敏酸分子量越小或芳构化程度越低,其吸附、粘结性能越强。腐植酸分子量过大或过小均不利于其吸附、粘结性能。当黄腐酸、胡敏酸的分子量分别接近600Da和1500Da时,二者的吸附、粘结性能最好。当黄腐酸、胡敏酸的分子量为最优值时,腐植酸分子量趋于1410～1490Da。
铁矿球团用腐植酸基粘结剂的技术要求为：1)腐植酸的E4/E6接近3.86；2)腐植酸含量(容量法)为40%～50%；3)适宜的胡富比因铁精矿类型不同而异,对于普通磁铁精矿、钒钛磁铁精矿、赤铁精矿来说,最佳胡富比分别接近8：2、7：3和6：4。
(5)针对普通磁铁精矿、钒钛磁铁精矿和赤铁精矿,制备出3种腐植酸基粘结剂。粘结剂用量为0.75%的球团矿的抗压强度超过膨润土用量为2.0%的球团矿,与膨润土球团相比铁品位提高1.0%以上、冶金性能相当。图88幅,表44个,参考文献198篇
Abstract:Binder is indispensable in the production of iron ore pellets, which can dramaticly influence the quality of finished products. Humic substances as a type of organic macromolecule polymer consist of carboxyl groups and hydroxyl groups, which should be further researched because of their ideal adhesive molecular conformation. At present, functional mechanisms of humic substances on the surface of iron ore is not fully clear. Furthermore, structure-performance relationships of humic substances based binder have not yet been clearly established because of few researches on their physical and chemical properties especially on the structure characteristics.
A type of humic substances based binders are prepared from lignite and weather coals. The binders mainly consist of two active fractions including fulvic acid and humic acid. The properties of binder active fractions and their functional mechanisms were studied by adopting infrared spectroscopy (FTIR), environment scanning electron microscope (ESEM), atomic force microscope (AFM), thermogravimetric-differential thermal analysis (TG-DSC) and X-ray photoelectron spectroscopy (XPS) et.al; The energy criterion△ETRT between binder and target minerals were calculated using the density functional theory (DFT), molecular functional assembly and binder molecular model; And most of all, the technical requirements for humic substances based binder are proposed based on the structure-performance relationships of binder active fractions. The main conclusions of this research are summaried as follows:
(1) There are obvious differences in physical and chemical properties between binder active fractions (fulvic and humic aicds). Compared to humic acid, Fulvic acid is characterized by better dispersibility, relatively low degree of aromatization and small molecular weight but relatively high content of oxygen-containing functional groups. Humic acid processes good thermal stability and wider thermal decomposition range.
(2) Chemical adsorption occurs between binder active fractions and iron concentrate surface, indicating the adsorption of fulvic acid is stronger. The adsorption of binder is more accord with Freundlich model and second order kinetics. The theoretical maximum adsorption amount of fulvic and humic acids is respectively8.92×10-3mg·cm-2and2.70×10-3mg·cm-2. Electronic binding energy variation of Fe2p3/2after adsorption of fulvic and humic acids are-1.12eV and-0.57eV, respectively. The net desorption energy of fulvic and humic acids is respectively-87.0J/g and-26.7J/g. The active fractions adsorbs on the surface of iron concentrates in the shape of net, fibrous or clusters. The adsorption of humic acid can be enhanced by fulvic acid.
(3) DFT calculation demonstrates that, compared to phenolic hydroxyl group, carboxyl group performs better solid-affinitive capability. The solid-affinitive capability of binder increases with the increase of the number of polar groups. For binder molecule, the enlargement of non-polar aromatic hydrocarbon can enhance the capacity of chemical adsorption, but also result in decrease of electrostatic forcing.
Reagent active equation and energy criterion demonstrates that binder molecule adsorbs on mineral surface with chemical reaction as deciding effort. The order of solid affinitive capability of binder with three target minerals follows FeTiO3> Fe3O4> Fe2O3. For interaction between binder and target minerals, the contribution of positive covalent coordination bond△E2RTT to energy criterion△ETRT is biggest, while electrostatic forcing△E1RT is smallest.
(4) The adsorption and subsequent binding strengths are negative correlation with E4/E6of fulvic acid. The performance of fulvic acid is increased with increasing its molecular weight. The adsorption and binding strengths are positive correlation with E4/E6of humic acid. The performance of humic acid is increased with decreasing its molecular weight. The molecular weight which is too large or too small is unfavorable to the adsorption and binding strengths of humic substances. The performance of active fractions performs better when the molecular weight of fulvic acid and humic acids is respectively600Da and1500Da. The idea range of molecular weight of humic substances is from1410Da to1490Da.
The technical requirements for humic substances based binder are proposed by following:1) E4/E6of humicsubstances should be close to3.86;2) The content of humic substances should be in the range of40%to50%;3) For magnetite, V-Ti containing magnetite and hematite, the mass ratio of humic acid to fulvic acid should be close to8:2,7:3and6:4.
(5) For magnetite, V-Ti containing magnetite and hematite concentrates, three kinds of binders are prepared. Compared to those pellets prepared with2.0%bentonite, the pellets with0.75%novel binder are characterized by1.0%higher TFe grade, better compression strength and the similar metallurgical properties.
引文
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