MACA体系中处理低品位氧化锌矿制取电锌的理论与工艺研究
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摘要
我国现有储量巨大的高碱性脉石型低品位氧化锌矿,用传统的炼锌方法无法处理。本文开拓新的途径,采用MACA法即在Me-NH_4Cl-NH_3-H_2O体系中处理这种氧化锌矿制取电锌。论文系统深入地研究了MACA法处理高碱性脉石型氧化锌矿的理论和工艺,得出了一些有意义的结果。
首先采用双平衡法(质量平衡和电荷平衡),分析了Zn(Ⅱ)-NH_3-Cl~--CO_3~(2-)-H_2O体系中Zn(Ⅱ)配合平衡热力学,求出了氨和氯化铵浓度在0-5mol/L范围内变化时,体系中各物种的平衡浓度,绘制了多种热力学关系图。结果表明,体系中有CO_3~(2-)存在时,适当提高氨浓度有利于提高溶液中的总锌浓度。这些现象与不考虑CO_3~(2-)的Zn-NH_4Cl-NH_3体系有较大差异。用试验验证了上述热力学计算结果,试验结果和计算结果彼此符合较好,两者平均相对误差仅为7.47%。这说明热力学模型适用可行,所选数据准确性较好。
系统地分析了Cu、Cd、Co、Ni、Pb、Mg等主要杂质元素在Zn(Ⅱ)-NH_4Cl-NH_3-H_2O体系处理氧化锌矿过程中的溶解行为和平衡规律,它们均能与NH_3、OH~-、Cl~-形成配合物,因此在NH_4Cl-NH_3-H_2O体系中浸出氧化锌矿时,这些杂质元素部分或全部进入浸出液中,对锌的提取产生不利影响,需要净化除去。
绘制了Me(Ⅱ)-NH_4Cl-NH_3-H_2O体系的电位-浓度图,揭示了各主要杂质除去的难易程度。在Me-NH_4Cl-NH_3-H_2O体系中,当氨和氯化铵浓度在0-5mol/L范围内时,E_(Cu~(2+)/Cu)、E_(Ni~(2+)/Ni)、E_(Pb~(2+)/Pb)及E_(Co~(2+)/Co)与E_(Zn~(2+)/Zn)的差均大于0.4v,因此锌粉可以彻底置换它们。在高氨高氯化铵浓度区域内,E_(Cu~(2+)/Cu)、E_(Cd~(2+)/Cd)与E_(Zn~(2+)/Zn)相差较小,最小仅为0.16v。E_(Cd~(2+)/Cd)E_(Co~(2+)/Co)与E_(H~+/H_2)比较接近,在常温下,不会发生酸性体系锌粉置换过程中镉的返溶现象。
研究了MACA法浸出氧化锌矿过程的动力学,发现浸出过程受通过固体膜层扩散过程控制,浸出速率可用收缩核模型描述,浸出反应的表观活化能为7.057 kJ/mol。动力学方程可表示为:
首次提出“(循环)浸出-净化-电积”MACA法处理高碱性脉石氧化锌矿的新工艺,该工艺不需要富集过程即可电积,废电解液返回配制浸出剂,而且常温操作,直流电耗低,实属一种清洁和低能耗的湿法炼锌新方法。分别以云南兰坪中、低品位氧化锌矿为原料,对新工艺进行了系统研究,获得良好结果。
MACA法处理兰坪中等品位氧化锌矿,在总氨浓度7.5 mol/L、NH_4Cl/NH_3=2:1、液固体积质量比4:1、常温、机械搅拌(300 rpm)、浸出时间60 min的优化条件下,锌平均浸出率为88.57%,浸出液中平均Zn~(2+)浓度为43.20 g/L。采用相同的浸出剂成分,在液固体积质量比2.5:1,在常温下,经过30 d柱浸,锌浸出率达到92.19%。
采用胶体共沉淀法脱除As和Sb,其含量均降到0.3 mg/L。采用锌粉两段逆流置换法除去Cu、Cd、Co、Ni、Pb等杂质,其含量均可降至1 mg/L以下,净化后液的化学组成完全满足锌电积要求。
添加剂对阴极锌的形貌有较大影响,净化后液如果不加入添加剂而直接电积,只能得到海绵状锌粉;单独添加骨胶、T-B、T-C,或者仅添加任意两种,同样不能得到致密锌板;在骨胶、T-B添加量为100 mg/L、T-C为2 ml/L的条件下电积,可以得到致密平整的锌板。
在异极距3 cm、电流密度400A/m~2、温度40℃、电解废液锌离子浓度>15 g/L的优化条件下电积,添加剂用量如上所述,电锌质量达到国标1#电锌标准,电流效率>90%,直流电耗为2882 kWh/t锌,氨耗约0.2 t/t锌。
废电解液调整成分后返回浸出,结果证明对工艺技术经济指标不产生影响。
MACA法处理兰坪低品位氧化锌矿,采用循环浸出方式使锌离子在浸出液中富集,在总氨浓度6 mol/L、NH_4~+/NH_3=1:1、液固体积质量比等于4:1的优化条件下,常温浸出3 h,随着浸出过程的进行适当调整浸出剂成分,经过5次循环浸出,浸出液中Zn~(2+)浓度可富集到37.37 g/L,氨可浸锌浸出率98.47%,总锌浸出率73.66%。
浸出液的净化和电积采用与处理中等品位氧化锌矿浸出液同样的工艺条件,经过净化操作,各杂质含量可降到1 mg/L以下,净化后液完全满足锌电积要求。净化后液经过电积,所得电锌质量达到国标1#电锌标准,平均电流效率>90%,直流电耗为2991 kwh/t锌,氨耗约0.2 t/t锌。废电解液调整成分后返回浸出,与前相同,对技术经济指标不产生影响。
In our country large reserves of low grade zinc oxide ores bearing high basic gangues can not be treated by traditional zinc metallurgical process. In this dissertation, a new process named as MACA method was proposed to produce cathode zinc from these zinc oxide ores in the system of Me-NH_4Cl-NH_3-H_2O.Theoretical and technical studies on the extraction zinc in Me-NH_4Cl-NH_3-H_2O (MACA) system were carried out in detail and some meaningful conclusions were obtained.
Thermodynamics of Zn(Ⅱ) complex equilibria in Zn(Ⅱ)-NH_3-Cl~--CO_3~(2-)-H_2O system was studied based on the conservation of mass and charge neutrality. When the concentration of ammonia and ammonium chloride is variable in range of 0-5mol/L, the equilibrium concentrations of all species were calculated, respectively, and thermodynamic diagrams were plotted. It indicated that the total equilibrium concentration of zinc is enhanced with the increasing of ammonia concentration in presence of CO_3~(2-) ion. The theoretical calculation results were testified by solubility experiments. The results show that the average relative error is less than 8%, which indicates that the thermodynamic models and critical data are feasible and reliable.
The behavior and equilibrium law of major impurities, such as Cu, Cd, Co, Ni, Pb and Mg, during the leaching of zinc oxide ores in Zn(Ⅱ)-NH_4Cl-NH_3-H_2O system were detailedly analyzed. Cu, Cd, Co, Ni and Mg in raw material can be leached out with certain rate due to the formation of metallic complex like Me(NH_3)_i~(n+),Me(OH)_j~(n-j),or MeCl_k~(n-k). The impurities in leaching solution have adverse effect on zincelectrowinning, and must be removed.
The difficulties or ease of removal major impurities from Zn(Ⅱ)-NH_4Cl-NH_3-H_2O system were systematically revealed by potential-concentration diagrams. The potential differences between E_(Me~(2+)/Me)(Me represent Cu~(2+),Ni~(2+),Pb~(2+),Co~(2+)) and E_(Zn~(2+)/Zn) are higher than0.4V when the concentration of ammonia and ammonium chloride is variable in range of 0-5mol/L, respectively. So they can be cemented thoroughly by zinc powder. When the concentration of ammonia and ammonium chloride is higher,the potential differences between E_(Me~(2+)/Me) (Me represent Cu~+,Cd~(2+)) and E_(Zn~(2+)/Zn) are low, and the minimum value is 0.16V.E_(Cd~(2+)/Cd)、E_(Co~(2+)/Co) is close to E_(H~+/H_2),cadmium and cobaltcemented will not resolve in Zn(Ⅱ)-NH_4Cl-NH_3-H_2O system at ambient temperature.
Leaching kinetics of zinc oxide ore in the system of NH_4Cl-NH_3-H_2O was studied. It is indicated that diffusion through the inert ash film is the controlling step. The leaching kinetics follows shrinking-core model, and the apparent activation energy is about 7.057 kJ/mol. Dynamical equation can be expressed as follow:
A new process of "cycle leaching-purification-electrowinning" in the system of Zn(Ⅱ)-NH_4Cl-NH_3-H_2O was proposed for extracting zinc from the zinc oxide ores bearing high basic gangue. Zinc concentrations in the obtained pregnant solution may be met the case of zinc electrowinning. Spent electrolyte was recycled to leaching operation. The whole process was carried out at ambient temperature and the direct-current consumption was low. So it is a cleaning and energy-saving process for zinc hydrometallurgy. Middle and low grade zinc oxide ores from Lan-ping in Yunnan province were used as raw materials in present dissertation and wonderful results were obtained.
Middle-grade zinc oxide ores from Lan-ping were leached under the following optimum conditions: total ammonium concentration of 7.5 mol/L,n_(NH_4Cl)/n_(NH_3)=2:1,the ratio of liquid to solid being 4, mechanically stirring speed of 300 rpm, leaching time for 60min at ambient temperature. The average leaching rate was 88.57%, and the average concentration of zinc in pregnant solution was 43.20g/L. During heaping leaching, the composition of lixiviant was the same as bottle leaching, and the leaching rate of zinc was 92.19% after 30 days at ambient temperature when the ratio of liquid to solid is 2.5.
The concentration of As and Sb in pregnant solution can be decreased to 0.3 mg/L by colloid coprecipitation method. After two-stage of counter-current cementation by zinc powder, the concentration of impurities, such as Cu, Cd, Co, Ni and Pb, may be less than 1 mg/L, respectively. The obtained purificatory solution meets the requirements of zinc electrowinning.
The additives have significant influence on the surface morphology of cathode zinc. Sponge zinc was produced during zinc electrowinning without additives. Compact zinc plate can not be obtained when electrowinning adding any one or two of additives as bone glue, T-B and T-C. Compact zinc plate was obtained when the amount of bone glue, T-B and T-C is 100mg/L,100mg/L and 2ml/L, respectively.
According to the results of single-factor experiments, the optimum conditions of zinc electrowinning was determined as follow: electrode space of 3 cm, current density of 400A/m~2,zinc concentration in spent electrolyte >15g/L, bone glue of 100mg/L, T-B of 100mg/L, T-C of 2ml/L,and at 40℃.Cathode zinc obtained under optimum conditions meets the requirements of first-grade zinc in GB 470-1997 1~# standard. Current efficiency was higher than 90%. The power and ammonia consumption was about 2882 kWh/t zinc and 0.2 t/t-zinc, respectively. Spent electrolyte was recycled to leaching operation after its composition adjusted. The results show that spent electrolyte circulation hasn't adverse influences on the technical and economic indexes of the process.
During leaching low-grade zinc oxide ores, the concentration of zinc in leaching solution was enriched continuously by the method of circulation leaching. After five-cycle of lixiviant, the concentration of zinc in leachate was higher than 37g/L under the conditions that total ammonium concentration is 6 mol/L,n_(NH_4Cl)/n_(NH_3)=1:1,the ratio of liquid to solid is 4, mechanically stirring speed is 300rpm, and leaching time for 3h at ambient temperature. The average leaching rate of zinc was 98.47%. The purification and electrowinning of obtained leachate was carried out under the above-mentioned optimum conditions. The concentration of impurities, such as As, Sb, Cu, Cd, Co, Ni and Pb in purificatory solution may be less than 1mg/L. Cathode zinc obtained meets the requirements of first-grade zinc in GB 470-1997 1# standard. Current efficiency was higher than 90%. The power and ammonia consumption was about 2991 kWh/t·zinc and 0.2 t/t-zinc, respectively.
首先采用双平衡法(质量平衡和电荷平衡),分析了Zn(Ⅱ)-NH_3-Cl~--CO_3~(2-)-H_2O体系中Zn(Ⅱ)配合平衡热力学,求出了氨和氯化铵浓度在0-5mol/L范围内变化时,体系中各物种的平衡浓度,绘制了多种热力学关系图。结果表明,体系中有CO_3~(2-)存在时,适当提高氨浓度有利于提高溶液中的总锌浓度。这些现象与不考虑CO_3~(2-)的Zn-NH_4Cl-NH_3体系有较大差异。用试验验证了上述热力学计算结果,试验结果和计算结果彼此符合较好,两者平均相对误差仅为7.47%。这说明热力学模型适用可行,所选数据准确性较好。
系统地分析了Cu、Cd、Co、Ni、Pb、Mg等主要杂质元素在Zn(Ⅱ)-NH_4Cl-NH_3-H_2O体系处理氧化锌矿过程中的溶解行为和平衡规律,它们均能与NH_3、OH~-、Cl~-形成配合物,因此在NH_4Cl-NH_3-H_2O体系中浸出氧化锌矿时,这些杂质元素部分或全部进入浸出液中,对锌的提取产生不利影响,需要净化除去。
绘制了Me(Ⅱ)-NH_4Cl-NH_3-H_2O体系的电位-浓度图,揭示了各主要杂质除去的难易程度。在Me-NH_4Cl-NH_3-H_2O体系中,当氨和氯化铵浓度在0-5mol/L范围内时,E_(Cu~(2+)/Cu)、E_(Ni~(2+)/Ni)、E_(Pb~(2+)/Pb)及E_(Co~(2+)/Co)与E_(Zn~(2+)/Zn)的差均大于0.4v,因此锌粉可以彻底置换它们。在高氨高氯化铵浓度区域内,E_(Cu~(2+)/Cu)、E_(Cd~(2+)/Cd)与E_(Zn~(2+)/Zn)相差较小,最小仅为0.16v。E_(Cd~(2+)/Cd)E_(Co~(2+)/Co)与E_(H~+/H_2)比较接近,在常温下,不会发生酸性体系锌粉置换过程中镉的返溶现象。
研究了MACA法浸出氧化锌矿过程的动力学,发现浸出过程受通过固体膜层扩散过程控制,浸出速率可用收缩核模型描述,浸出反应的表观活化能为7.057 kJ/mol。动力学方程可表示为:
首次提出“(循环)浸出-净化-电积”MACA法处理高碱性脉石氧化锌矿的新工艺,该工艺不需要富集过程即可电积,废电解液返回配制浸出剂,而且常温操作,直流电耗低,实属一种清洁和低能耗的湿法炼锌新方法。分别以云南兰坪中、低品位氧化锌矿为原料,对新工艺进行了系统研究,获得良好结果。
MACA法处理兰坪中等品位氧化锌矿,在总氨浓度7.5 mol/L、NH_4Cl/NH_3=2:1、液固体积质量比4:1、常温、机械搅拌(300 rpm)、浸出时间60 min的优化条件下,锌平均浸出率为88.57%,浸出液中平均Zn~(2+)浓度为43.20 g/L。采用相同的浸出剂成分,在液固体积质量比2.5:1,在常温下,经过30 d柱浸,锌浸出率达到92.19%。
采用胶体共沉淀法脱除As和Sb,其含量均降到0.3 mg/L。采用锌粉两段逆流置换法除去Cu、Cd、Co、Ni、Pb等杂质,其含量均可降至1 mg/L以下,净化后液的化学组成完全满足锌电积要求。
添加剂对阴极锌的形貌有较大影响,净化后液如果不加入添加剂而直接电积,只能得到海绵状锌粉;单独添加骨胶、T-B、T-C,或者仅添加任意两种,同样不能得到致密锌板;在骨胶、T-B添加量为100 mg/L、T-C为2 ml/L的条件下电积,可以得到致密平整的锌板。
在异极距3 cm、电流密度400A/m~2、温度40℃、电解废液锌离子浓度>15 g/L的优化条件下电积,添加剂用量如上所述,电锌质量达到国标1#电锌标准,电流效率>90%,直流电耗为2882 kWh/t锌,氨耗约0.2 t/t锌。
废电解液调整成分后返回浸出,结果证明对工艺技术经济指标不产生影响。
MACA法处理兰坪低品位氧化锌矿,采用循环浸出方式使锌离子在浸出液中富集,在总氨浓度6 mol/L、NH_4~+/NH_3=1:1、液固体积质量比等于4:1的优化条件下,常温浸出3 h,随着浸出过程的进行适当调整浸出剂成分,经过5次循环浸出,浸出液中Zn~(2+)浓度可富集到37.37 g/L,氨可浸锌浸出率98.47%,总锌浸出率73.66%。
浸出液的净化和电积采用与处理中等品位氧化锌矿浸出液同样的工艺条件,经过净化操作,各杂质含量可降到1 mg/L以下,净化后液完全满足锌电积要求。净化后液经过电积,所得电锌质量达到国标1#电锌标准,平均电流效率>90%,直流电耗为2991 kwh/t锌,氨耗约0.2 t/t锌。废电解液调整成分后返回浸出,与前相同,对技术经济指标不产生影响。
In our country large reserves of low grade zinc oxide ores bearing high basic gangues can not be treated by traditional zinc metallurgical process. In this dissertation, a new process named as MACA method was proposed to produce cathode zinc from these zinc oxide ores in the system of Me-NH_4Cl-NH_3-H_2O.Theoretical and technical studies on the extraction zinc in Me-NH_4Cl-NH_3-H_2O (MACA) system were carried out in detail and some meaningful conclusions were obtained.
Thermodynamics of Zn(Ⅱ) complex equilibria in Zn(Ⅱ)-NH_3-Cl~--CO_3~(2-)-H_2O system was studied based on the conservation of mass and charge neutrality. When the concentration of ammonia and ammonium chloride is variable in range of 0-5mol/L, the equilibrium concentrations of all species were calculated, respectively, and thermodynamic diagrams were plotted. It indicated that the total equilibrium concentration of zinc is enhanced with the increasing of ammonia concentration in presence of CO_3~(2-) ion. The theoretical calculation results were testified by solubility experiments. The results show that the average relative error is less than 8%, which indicates that the thermodynamic models and critical data are feasible and reliable.
The behavior and equilibrium law of major impurities, such as Cu, Cd, Co, Ni, Pb and Mg, during the leaching of zinc oxide ores in Zn(Ⅱ)-NH_4Cl-NH_3-H_2O system were detailedly analyzed. Cu, Cd, Co, Ni and Mg in raw material can be leached out with certain rate due to the formation of metallic complex like Me(NH_3)_i~(n+),Me(OH)_j~(n-j),or MeCl_k~(n-k). The impurities in leaching solution have adverse effect on zincelectrowinning, and must be removed.
The difficulties or ease of removal major impurities from Zn(Ⅱ)-NH_4Cl-NH_3-H_2O system were systematically revealed by potential-concentration diagrams. The potential differences between E_(Me~(2+)/Me)(Me represent Cu~(2+),Ni~(2+),Pb~(2+),Co~(2+)) and E_(Zn~(2+)/Zn) are higher than0.4V when the concentration of ammonia and ammonium chloride is variable in range of 0-5mol/L, respectively. So they can be cemented thoroughly by zinc powder. When the concentration of ammonia and ammonium chloride is higher,the potential differences between E_(Me~(2+)/Me) (Me represent Cu~+,Cd~(2+)) and E_(Zn~(2+)/Zn) are low, and the minimum value is 0.16V.E_(Cd~(2+)/Cd)、E_(Co~(2+)/Co) is close to E_(H~+/H_2),cadmium and cobaltcemented will not resolve in Zn(Ⅱ)-NH_4Cl-NH_3-H_2O system at ambient temperature.
Leaching kinetics of zinc oxide ore in the system of NH_4Cl-NH_3-H_2O was studied. It is indicated that diffusion through the inert ash film is the controlling step. The leaching kinetics follows shrinking-core model, and the apparent activation energy is about 7.057 kJ/mol. Dynamical equation can be expressed as follow:
A new process of "cycle leaching-purification-electrowinning" in the system of Zn(Ⅱ)-NH_4Cl-NH_3-H_2O was proposed for extracting zinc from the zinc oxide ores bearing high basic gangue. Zinc concentrations in the obtained pregnant solution may be met the case of zinc electrowinning. Spent electrolyte was recycled to leaching operation. The whole process was carried out at ambient temperature and the direct-current consumption was low. So it is a cleaning and energy-saving process for zinc hydrometallurgy. Middle and low grade zinc oxide ores from Lan-ping in Yunnan province were used as raw materials in present dissertation and wonderful results were obtained.
Middle-grade zinc oxide ores from Lan-ping were leached under the following optimum conditions: total ammonium concentration of 7.5 mol/L,n_(NH_4Cl)/n_(NH_3)=2:1,the ratio of liquid to solid being 4, mechanically stirring speed of 300 rpm, leaching time for 60min at ambient temperature. The average leaching rate was 88.57%, and the average concentration of zinc in pregnant solution was 43.20g/L. During heaping leaching, the composition of lixiviant was the same as bottle leaching, and the leaching rate of zinc was 92.19% after 30 days at ambient temperature when the ratio of liquid to solid is 2.5.
The concentration of As and Sb in pregnant solution can be decreased to 0.3 mg/L by colloid coprecipitation method. After two-stage of counter-current cementation by zinc powder, the concentration of impurities, such as Cu, Cd, Co, Ni and Pb, may be less than 1 mg/L, respectively. The obtained purificatory solution meets the requirements of zinc electrowinning.
The additives have significant influence on the surface morphology of cathode zinc. Sponge zinc was produced during zinc electrowinning without additives. Compact zinc plate can not be obtained when electrowinning adding any one or two of additives as bone glue, T-B and T-C. Compact zinc plate was obtained when the amount of bone glue, T-B and T-C is 100mg/L,100mg/L and 2ml/L, respectively.
According to the results of single-factor experiments, the optimum conditions of zinc electrowinning was determined as follow: electrode space of 3 cm, current density of 400A/m~2,zinc concentration in spent electrolyte >15g/L, bone glue of 100mg/L, T-B of 100mg/L, T-C of 2ml/L,and at 40℃.Cathode zinc obtained under optimum conditions meets the requirements of first-grade zinc in GB 470-1997 1~# standard. Current efficiency was higher than 90%. The power and ammonia consumption was about 2882 kWh/t zinc and 0.2 t/t-zinc, respectively. Spent electrolyte was recycled to leaching operation after its composition adjusted. The results show that spent electrolyte circulation hasn't adverse influences on the technical and economic indexes of the process.
During leaching low-grade zinc oxide ores, the concentration of zinc in leaching solution was enriched continuously by the method of circulation leaching. After five-cycle of lixiviant, the concentration of zinc in leachate was higher than 37g/L under the conditions that total ammonium concentration is 6 mol/L,n_(NH_4Cl)/n_(NH_3)=1:1,the ratio of liquid to solid is 4, mechanically stirring speed is 300rpm, and leaching time for 3h at ambient temperature. The average leaching rate of zinc was 98.47%. The purification and electrowinning of obtained leachate was carried out under the above-mentioned optimum conditions. The concentration of impurities, such as As, Sb, Cu, Cd, Co, Ni and Pb in purificatory solution may be less than 1mg/L. Cathode zinc obtained meets the requirements of first-grade zinc in GB 470-1997 1# standard. Current efficiency was higher than 90%. The power and ammonia consumption was about 2991 kWh/t·zinc and 0.2 t/t-zinc, respectively.
引文
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