富钴和富硒物料湿法处理工艺及理论基础研究
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摘要
近年来随着钴、硒的广泛应用,需求量急剧增加。而我国钴、硒资源相对匮乏,如何从复杂二次资源中提高回收率已迫在眉睫。湿法冶金因具有选择性好和能耗低等优点,已成为回收钴、硒的主要工艺。同时在实际生产模拟及优化工艺过程中建立准确可靠的控制对象模型具有重要意义,但实际收入项和支出项的比较、模型设计参数的合理计算以及终点成分的预测仍是难点。本文针对富钴和富硒物料的特性,深入进行湿法处理过程中的热力学、动力学分析和优化工艺实验设计等研究,构建了湿法处理两种物料过程中的有价元素分配模型,对有价元素的具体走向及分布状况进行分析,为该类湿法工艺开发提供理论和技术依据,结论如下：
系统分析了富钻物料和富硒物料湿法处理过程的热力学。硫酸浸出富钻物料中的金属氧化物反应趋势为：MnO>CoO>NiO> ZnO>Cd2O3> CuO> Fe2O3;控制pH值和温度可实现优先沉铜；沉锰铁过程中,过硫酸钠优先氧化铁,可实现锰、铁的选择性沉淀；提高pH值和温度,有利于钴的沉淀回收。煤油脱除富硒物料中的单质硫,温度应达到95℃以上；提高pH值和温度,有利于硒的氧化浸出；亚硫酸钠还原过程中,溶液初始酸度越大,亚硫酸钠还原硒的趋势越大,越有利于硒的还原析出。
系统研究了富钻物料和富硒物料湿法处理优化工艺。硫酸浸出富钴物料,Co、Zn、Cd、Ni、Cu、Mn、Fe和Pb的浸出率分别达到97.99%、91.79%、96.20%、87.31%、91.20%、89.19%、67.09%和0.14%；硫化钠除铜,Cu的沉淀率达到99.93%；过硫酸钠氧化水解沉锰铁,Mn和Fe的浓度分别降至0.0005g/L和0.0018g/L；过硫酸钠沉钴,Co的沉淀率达到99.81%,沉钴产品为CoO(OH)(羟基氧化钴),Co含量高达45.56%。整个富钴物料处理工艺过程中,Cu、Mn、Fe和Co的直收率分别为88.58%、89.09%、70.01%和93.58%。煤油脱硫富硒物料,单质硫的脱除率达到97.8%；氧化酸浸脱硫富硒物料,Se和Fe的浸出率分别为97.76%和12.20%；亚硫酸钠还原沉硒,Se的还原率为99.7%,沉硒产品为单质Se,其含量高达99.63%。整个富硒物料处理工艺过程中,S、Fe和Se的直收率为97.8%、92.84%和98.46%。
系统研究了酸浸富钴物料和富硒物料的动力学及其机理。结果表明：富钴物料中Co、Zn和Cu的浸出反应为未反应收缩核扩散控制过程,三者有较强的关联性。Co、Zn和Cu的表观活化能分别为11.69kJ/mol、6.69kJ/mol和5.98kJ/mol,化学反应级数分别为0.74、0.41和0.32；粒度级数分别为-1.44、-1.04和-0.84；Co、Zn和Cu的浸出动力学方程分别为：
富硒物料中Se的浸出反应为化学反应控制过程,Fe的浸出曲线不符合化学反应控制模型,两者关联性不强。Se的表观活化能为39.50kJ/mol,化学反应级数n1为0.15,化学反应级数n2为0.95,粒度级数为-0.16。Se的浸出动力学方程为：
构建了富钴和富硒物料在湿法处理过程中的有价元素分配模型,模型预测的整体分配质量和整体分配比例可以定量预估实验结果,表明有价元素分配模型可用于该类湿法工艺模拟优化控制；有价元素在富钴和富硒物料湿法处理过程中的具体分配走向如下：富钴物料中已回收铜、锰、铁、钻元素的单步工序回收率和直收率分别为99.93%和89.36%、99.95%和89.89%、99.69%和70.16%、99.98%和95.38%,铅元素均为99.88%。铅、铜、锰、铁和钴的分配比例分别为99.88%、89.36%、89.85%、70.16%和95.38%。未回收的95.66%的锌、93.35%的镉和85.80%的镍存于沉钻后液中,10.74%的镍进入到硫酸浸出渣中。富硒物料中已回收铁、硒元素的单步工序回收率和直收率分别为93.03%和92.78%、99.93%和98.05%,硫元素均为99.90%,铁、硒和硫的分配比例分别为92.77%、98.06%和98.06%。本论文图153幅,表61个,参考文献303篇。
In recent years, the demanding of cobalt and selenium is increasing dramatically with its wide applications. However, the resources of cobalt and selenium are relatively scarce in China, so how to increase the recovery of cobalt and selenium from complex secondary materials becomes imperative. Hydrometallurgical processes which are the main technologies of recovery of cobalt and selenium have many advantages including excellent selectivity, low energy consumption and so on; Meanwhile, the accurate and reliable object controlling model in hydrometallurgical process is established for practical production simulation and optimization control while its comparison of input and output, parameters calculation of model and the final composition are all difficult to predict. Based on the analysis of cobalt and selenium metallurgical residue properties and characteristics, combination of thermodynamics analysis, kinetic analysis and optimization design of experiment research in the hydrometallurgical processes, the quality of value element allocation model of hydrometallurgical technological process of cobalt and selenium metallurgical residue was proposed, meanwhile the flow analysis of the value element in the technological process was analyzed which provide the theoretical and technological basis for the industrial processing of cobalt and selenium metallurgical residue, the main conclusions are as follows:
The fundamental thermodynamics analysis of cobalt metallurgical residue in the hydrometallurgical process was studied. The metal acidic leaching trend of cobalt metallurgy sluge were as follows: MnO>CoO>NiO>ZnO>Cd2O3>CuO>Fe2O3; Copper was preferentially removed by controling pH value and tempature of acidic leaching solution; In the process of oxidizing and hydrolysis precipitation(pH<4), by adding sodium persulfate in the purification solution after copper precipitation, iron was first oxidized, then manganese which could realize selective precipitation; The higher it increase temperature and pH value of solution after iron and manganese precipitation, the more beneficial to precipitation rate of cobalt it was.
The thermodynamics analysis of selenium metallurgical residue show that the kerosene desulfurization temperature should achieve above sulfur melting point; The higher it increase temperature and pH value of oxidization acid leaching solution solution after kerosene desulfurization, the more beneficial to leaching rate of selenium it was. In the selenium reduction process, the greater the initial acidity of solution it had, the more beneficial to precipitation rate of selenium it was.
The optimization conditions on treatment of cobalt and selenium metallurgical residue were studied. In the process of acid leaching, the leaching rates of cobalt, zinc, cadmium, nickel, copper, manganese, iron and lead are97.99%,91.79%,96.20%,87.31%,91.20%,89.19%,67.09%and0.14%, respectively.99.93%of copper was preferentially removed with Na2S. During the oxidizing and hydrolysis precipitation, iron and manganese residual amount of solution are about0.0005g/L and0.0018g/L respectively. In the process of cobalt oxidizing precipitation with Na2S2O8,99.81%of cobalt was precipitated. The phase of cobalt product is CoO(OH),which content of cobalt is45.56%. In the whole process, the direct yield recovery rate of copper, manganese, iron and cobalt were88.58%,89.09%,70.01%and93.58%, respectively.
The experimental design for optimization of kerosene desulfurization process was done, and the results show that the rate of desulphurization was lager than97%. During the process of oxidization leaching, the leaching efficiencies of selenium and iron are97.76%and12.20%, respectively.99.7%of selenium was precipited with Na2SO3in the leaching solution. The phase of selenium product is Se, which content of selenium is99.63%. In the whole processes, the direct recoveries of surfur, iron and selenium are97.8%,92.84%and98.46%, respectively.
The kinetics and its mechanism of leaching cobalt metallurgical residue in sulfur acid system were investigated, the results show that the leaching behavior of cobalt, zinc and copper which have high correlation between them fit well with the kinetic models of unreacted shrinking core reactions. The apparent activation energies for cobalt, zinc and copper extraction are11.69KJ/mol,6.69KJ/mol and5.98KJ/mol, respectively, which indicates that the leaching rate of cobalt, zinc and copper were controlled by diffusion through a porous product layer with chemical reaction rate order of0.74,0.41and0.74respectively and particle size rate order of-1.44,-1.04and-0.84respectively; The leaching kinetic equations of cobalt, zinc and copper are as follows:
The kinetics of leaching desulfurization residue in sodium chlorate and sulfur acid system show that the leaching behavior of selenium fit well with the kinetic models of surface chemical reactions control, while iron was not affected. So selenium and iron have low correlation between them. The apparent activation energies for selenium extraction were39.50KJ/mol, which indicated that the leaching rate of selenium was controlled by surface chemical reactions with chemical reaction rate orders:n1of0.15, n2of0.95respectively and particle size rate order of-0.16; The leaching kinetic equation of selenium is as follows:
The quality of value element allocation model of technological process of cobalt and selenium metallurgical residue was established based on the analysis of treatment process of cobalt and selenium metallurgical residue and material balance to determine the algorithms of model coefficient. The distribution of overall quality and overall allocation proportion of the prediction model can be quantitatively estimated technological process result. It shows that quality of value element allocation model of technological process can be used for industrial production. The flow analysis of the value element in the technological process of cobalt metallurgical residue are as follows:the single step process and direct yield recovery rate of copper, lead, manganese, iron and cobalt are99.93%and89.36%,99.95%and89.89%,99.69%and70.16%,99.98%and95.38%, which of lead are all both99.88%.The allocation proportion of lead, copper, manganese, iron and cobalt are99.88%,89.36%,89.85%,70.16%and95.38%, respectively. About95.66%of unrecovered zinc,93.35%of unrecovered cadmium,85.80%of unrecovered nickel are existed in the cobalt precipitated solution.
The flow analysis of the value element in the technological process of selenium metallurgical residue are as follows:the single step process and direct yield recovery rate of iron and selenium are93.03%and92.78%,99.93%and98.05%, which of surfur are all both99.90%.The allocation proportion of iron, selenium and surfur are92.77%,98.06%and98.06%, respectively. The overall of figures, tables and inferences are153,61,303, respectively.
系统分析了富钻物料和富硒物料湿法处理过程的热力学。硫酸浸出富钻物料中的金属氧化物反应趋势为：MnO>CoO>NiO> ZnO>Cd2O3> CuO> Fe2O3;控制pH值和温度可实现优先沉铜；沉锰铁过程中,过硫酸钠优先氧化铁,可实现锰、铁的选择性沉淀；提高pH值和温度,有利于钴的沉淀回收。煤油脱除富硒物料中的单质硫,温度应达到95℃以上；提高pH值和温度,有利于硒的氧化浸出；亚硫酸钠还原过程中,溶液初始酸度越大,亚硫酸钠还原硒的趋势越大,越有利于硒的还原析出。
系统研究了富钻物料和富硒物料湿法处理优化工艺。硫酸浸出富钴物料,Co、Zn、Cd、Ni、Cu、Mn、Fe和Pb的浸出率分别达到97.99%、91.79%、96.20%、87.31%、91.20%、89.19%、67.09%和0.14%；硫化钠除铜,Cu的沉淀率达到99.93%；过硫酸钠氧化水解沉锰铁,Mn和Fe的浓度分别降至0.0005g/L和0.0018g/L；过硫酸钠沉钴,Co的沉淀率达到99.81%,沉钴产品为CoO(OH)(羟基氧化钴),Co含量高达45.56%。整个富钴物料处理工艺过程中,Cu、Mn、Fe和Co的直收率分别为88.58%、89.09%、70.01%和93.58%。煤油脱硫富硒物料,单质硫的脱除率达到97.8%；氧化酸浸脱硫富硒物料,Se和Fe的浸出率分别为97.76%和12.20%；亚硫酸钠还原沉硒,Se的还原率为99.7%,沉硒产品为单质Se,其含量高达99.63%。整个富硒物料处理工艺过程中,S、Fe和Se的直收率为97.8%、92.84%和98.46%。
系统研究了酸浸富钴物料和富硒物料的动力学及其机理。结果表明：富钴物料中Co、Zn和Cu的浸出反应为未反应收缩核扩散控制过程,三者有较强的关联性。Co、Zn和Cu的表观活化能分别为11.69kJ/mol、6.69kJ/mol和5.98kJ/mol,化学反应级数分别为0.74、0.41和0.32；粒度级数分别为-1.44、-1.04和-0.84；Co、Zn和Cu的浸出动力学方程分别为：
富硒物料中Se的浸出反应为化学反应控制过程,Fe的浸出曲线不符合化学反应控制模型,两者关联性不强。Se的表观活化能为39.50kJ/mol,化学反应级数n1为0.15,化学反应级数n2为0.95,粒度级数为-0.16。Se的浸出动力学方程为：
构建了富钴和富硒物料在湿法处理过程中的有价元素分配模型,模型预测的整体分配质量和整体分配比例可以定量预估实验结果,表明有价元素分配模型可用于该类湿法工艺模拟优化控制；有价元素在富钴和富硒物料湿法处理过程中的具体分配走向如下：富钴物料中已回收铜、锰、铁、钻元素的单步工序回收率和直收率分别为99.93%和89.36%、99.95%和89.89%、99.69%和70.16%、99.98%和95.38%,铅元素均为99.88%。铅、铜、锰、铁和钴的分配比例分别为99.88%、89.36%、89.85%、70.16%和95.38%。未回收的95.66%的锌、93.35%的镉和85.80%的镍存于沉钻后液中,10.74%的镍进入到硫酸浸出渣中。富硒物料中已回收铁、硒元素的单步工序回收率和直收率分别为93.03%和92.78%、99.93%和98.05%,硫元素均为99.90%,铁、硒和硫的分配比例分别为92.77%、98.06%和98.06%。本论文图153幅,表61个,参考文献303篇。
In recent years, the demanding of cobalt and selenium is increasing dramatically with its wide applications. However, the resources of cobalt and selenium are relatively scarce in China, so how to increase the recovery of cobalt and selenium from complex secondary materials becomes imperative. Hydrometallurgical processes which are the main technologies of recovery of cobalt and selenium have many advantages including excellent selectivity, low energy consumption and so on; Meanwhile, the accurate and reliable object controlling model in hydrometallurgical process is established for practical production simulation and optimization control while its comparison of input and output, parameters calculation of model and the final composition are all difficult to predict. Based on the analysis of cobalt and selenium metallurgical residue properties and characteristics, combination of thermodynamics analysis, kinetic analysis and optimization design of experiment research in the hydrometallurgical processes, the quality of value element allocation model of hydrometallurgical technological process of cobalt and selenium metallurgical residue was proposed, meanwhile the flow analysis of the value element in the technological process was analyzed which provide the theoretical and technological basis for the industrial processing of cobalt and selenium metallurgical residue, the main conclusions are as follows:
The fundamental thermodynamics analysis of cobalt metallurgical residue in the hydrometallurgical process was studied. The metal acidic leaching trend of cobalt metallurgy sluge were as follows: MnO>CoO>NiO>ZnO>Cd2O3>CuO>Fe2O3; Copper was preferentially removed by controling pH value and tempature of acidic leaching solution; In the process of oxidizing and hydrolysis precipitation(pH<4), by adding sodium persulfate in the purification solution after copper precipitation, iron was first oxidized, then manganese which could realize selective precipitation; The higher it increase temperature and pH value of solution after iron and manganese precipitation, the more beneficial to precipitation rate of cobalt it was.
The thermodynamics analysis of selenium metallurgical residue show that the kerosene desulfurization temperature should achieve above sulfur melting point; The higher it increase temperature and pH value of oxidization acid leaching solution solution after kerosene desulfurization, the more beneficial to leaching rate of selenium it was. In the selenium reduction process, the greater the initial acidity of solution it had, the more beneficial to precipitation rate of selenium it was.
The optimization conditions on treatment of cobalt and selenium metallurgical residue were studied. In the process of acid leaching, the leaching rates of cobalt, zinc, cadmium, nickel, copper, manganese, iron and lead are97.99%,91.79%,96.20%,87.31%,91.20%,89.19%,67.09%and0.14%, respectively.99.93%of copper was preferentially removed with Na2S. During the oxidizing and hydrolysis precipitation, iron and manganese residual amount of solution are about0.0005g/L and0.0018g/L respectively. In the process of cobalt oxidizing precipitation with Na2S2O8,99.81%of cobalt was precipitated. The phase of cobalt product is CoO(OH),which content of cobalt is45.56%. In the whole process, the direct yield recovery rate of copper, manganese, iron and cobalt were88.58%,89.09%,70.01%and93.58%, respectively.
The experimental design for optimization of kerosene desulfurization process was done, and the results show that the rate of desulphurization was lager than97%. During the process of oxidization leaching, the leaching efficiencies of selenium and iron are97.76%and12.20%, respectively.99.7%of selenium was precipited with Na2SO3in the leaching solution. The phase of selenium product is Se, which content of selenium is99.63%. In the whole processes, the direct recoveries of surfur, iron and selenium are97.8%,92.84%and98.46%, respectively.
The kinetics and its mechanism of leaching cobalt metallurgical residue in sulfur acid system were investigated, the results show that the leaching behavior of cobalt, zinc and copper which have high correlation between them fit well with the kinetic models of unreacted shrinking core reactions. The apparent activation energies for cobalt, zinc and copper extraction are11.69KJ/mol,6.69KJ/mol and5.98KJ/mol, respectively, which indicates that the leaching rate of cobalt, zinc and copper were controlled by diffusion through a porous product layer with chemical reaction rate order of0.74,0.41and0.74respectively and particle size rate order of-1.44,-1.04and-0.84respectively; The leaching kinetic equations of cobalt, zinc and copper are as follows:
The kinetics of leaching desulfurization residue in sodium chlorate and sulfur acid system show that the leaching behavior of selenium fit well with the kinetic models of surface chemical reactions control, while iron was not affected. So selenium and iron have low correlation between them. The apparent activation energies for selenium extraction were39.50KJ/mol, which indicated that the leaching rate of selenium was controlled by surface chemical reactions with chemical reaction rate orders:n1of0.15, n2of0.95respectively and particle size rate order of-0.16; The leaching kinetic equation of selenium is as follows:
The quality of value element allocation model of technological process of cobalt and selenium metallurgical residue was established based on the analysis of treatment process of cobalt and selenium metallurgical residue and material balance to determine the algorithms of model coefficient. The distribution of overall quality and overall allocation proportion of the prediction model can be quantitatively estimated technological process result. It shows that quality of value element allocation model of technological process can be used for industrial production. The flow analysis of the value element in the technological process of cobalt metallurgical residue are as follows:the single step process and direct yield recovery rate of copper, lead, manganese, iron and cobalt are99.93%and89.36%,99.95%and89.89%,99.69%and70.16%,99.98%and95.38%, which of lead are all both99.88%.The allocation proportion of lead, copper, manganese, iron and cobalt are99.88%,89.36%,89.85%,70.16%and95.38%, respectively. About95.66%of unrecovered zinc,93.35%of unrecovered cadmium,85.80%of unrecovered nickel are existed in the cobalt precipitated solution.
The flow analysis of the value element in the technological process of selenium metallurgical residue are as follows:the single step process and direct yield recovery rate of iron and selenium are93.03%and92.78%,99.93%and98.05%, which of surfur are all both99.90%.The allocation proportion of iron, selenium and surfur are92.77%,98.06%and98.06%, respectively. The overall of figures, tables and inferences are153,61,303, respectively.
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