铅锌冶炼渣硫化处理新方法研究
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摘要
铅锌冶炼企业每年会产生大量的重金属废渣,历年的堆存量已经过亿吨,此类重金属废渣的治理一直是环保领域的重大课题。然而,现有处理技术难以同时实现废渣中重金属的资源化和稳定化,例如浸出等回收技术在提取金属的同时会产生大量的废水和浸出渣；而水泥固化等稳定化技术又难以将废渣中的金属提取,造成资源的浪费,因此,迫切需要一种兼顾重金属资源化和稳定化的处理方法。硫化技术处理废渣不仅能将其中的重金属转化为硫化物通过浮选的方式加以回收,同时处理后的重金属也具有良好的稳定性,是重金属废渣处理的一种新思路。基于对铅锌冶炼企业废渣产生情况调研及废渣组分分析结果,本文采用三种堆置类废渣(挥发窑渣,常压富氧浸锌渣,重金属废水中和渣)为主要研究对象。首次采用干磨自蔓延硫化、湿式球磨硫化以及水热硫化法对上述废渣进行硫化处理,并对三种新型硫化方法的反应机制及过程特征进行探讨。
三种堆置类废渣的化学成分及环境活性分析结果表明：挥发窑渣中Zn, Pb等重金属含量为2%-3%,且Pb、Cd等金属的浸出毒性存在超标风险；锌浸出渣的Zn含量为5%,Pb含量为5%,其金属的浸出毒性远远超过国家标准；中和渣的Zn含量在15-20%之间,但其中的重金属性质较稳定,且浸出毒性低于国家标准。根据上述分析结果,并结合重金属氧化物的硫化探索性实验,本文确定了以上三种堆置类废渣的硫化工艺：挥发窑渣采用干式球磨硫化-硫磺固化处理,采用硫磺作为硫化剂；常压富氧浸锌渣采用湿式球磨硫化-浮选分离稳定化处理,以硫化钠为硫化剂；中和渣采用水热硫化-浮选回收处理,以硫磺为硫化剂。
系统地研究了重金属的机械诱发的自蔓延硫化反应机制,实现了挥发窑渣的稳定化转变。研究结果表明,机械干磨挥发窑渣的最佳工艺参数为：硫磺添加量为4.5%,球磨时间为1小时,球料比为20：1,最优情况下Zn的硫化率可达95.4%,Pb的硫化率可达94.2%,处理后各重金属浸出毒性达标。通过分析球磨过程中重金属化合物晶体结构变化以及废渣中其他组分的行为特征,研究认为反应体系的绝热温度(Tad)是机械力诱发白蔓延硫化反应的主要决定因素,而球磨过程中晶体性质的变化仅起到促进或阻碍硫化反应的作用。挥发窑中的Fe等单质是诱发ZnO的实现自蔓延硫化反应的主要原因,其作用机制是提高了整个反应体系的绝热温度。硫化后的废渣可以制备成硫磺建材,最优的制备工艺为：采用分步投加方式加热,硫磺添加量40%,原料粒径小于150μm,骨料添加量控制在15%以内,在最优制备条件下,硫磺固化体的抗压强度为35MPa,吸水率为4%,满足建材要求。
利用湿式球磨的界面活化作用,实现了常压富氧浸锌渣的深度硫化,废渣中铅硫化率可达73.2%。湿式球磨硫化的最佳工艺为：Na2S·9H2O添加量为8.4%,球料比10：1,硫化时间1小时。利用收缩核模型揭示了机械力促进重金属硫化的原因。研究认为,PbSO4硫化反应受内扩散控制,球磨作用可以通过降低颗粒粒径,提高硫化剂进入反应物内核的速率。后续的浮选处理可以分离废渣中50%以上的Pb, Cu, Cd等重金属,然而废渣硫磺含量大、生成硫化物粒径细小是影响浮选回收率提高的主要原因。TCLP和连续淋洗实验表明,处理后的常压富氧浸锌渣重金属浸出毒性低于相关标准,并且具有长期稳定性。
利用水热条件下的溶解-再结晶机制,实现了重金属废水中和渣中重金属的高效硫化。其水热硫化的最佳工艺条件为：水热硫化温度200℃；水热硫化时间2小时；硫磺添加量15%；矿浆浓度300g·L-1；pH大于10。在此最优条件下,中和渣的锌硫化率可以达到85%以上,铅的硫化率可以达到75.4%以上。水热硫化中和渣的反应历程包括硫磺歧化、重金属溶解、CaSO4的生成、重金属含硫配合物的生成、降温结晶等阶段。水热硫化处理后锌的浮选回收率为33.3%,铅为58.9%,铜为68.8%。锌的可浮性较差主要是由其晶体性质造成的。水热合成的ZnS晶粒较小,团聚严重,表面粗糙,呈球状,这些性质都将降低其可浮性。为了提高ZnS的可浮性,实验考察了ZnS的晶型调控技术及其对可浮性的影响,结果表明,提高反应温度至260℃,延长反应时间至4小时,控制初始锌含量为10%后,ZnS回收率由33.3%提高至72.8%。重金属的稳定性检测结果表明,经过水热硫化-浮选处理后,废渣中的重金属浸出毒性低于国家标准,且重金属具有长期稳定性。
研制了“重金属废渣硫化-浮选处理中试系统”,并开展水热硫化-浮选技术处理废水中和渣的中试实验研究。实验结果表明该系统具有运行稳定,硫化率高,二次污染小等优点。现有的实验结果表明,处理后,中和渣中Zn的重金属硫化率达到87.34%,浮选处理可以从废水中和渣中回收铅锌综合品位为40%的人造硫化物精矿,回收率达65%。
Tons of heavy metal containing wastes are generated every year by zinc-lead smelters, whose total amount is more than100million tons. The management of these wastes is one of the great subject in environmental protection field. However, current methods are difficult to realize the resourcelization and stablization of heavy metals. For example, the widely-used direct extraction technique leads to a large quantity of wastewater and residue containing unstable state heavy metals; while cement solidification often causes the losses of heavy metal. Sulfidation treatment is a novel method to deal with heavy metal containing wastes. Through this approach the heavy metal can be converted into metal sulfide, the metal in which, subsequently, can be separated and recycled by means of floatation technique, and moreover the managed wastes are fairly stabilized after the treatment. According to the survey and the analysis of the heavy metal containing wastes from zinc-lead smelters, the stockpile wastes—namely volatilization kiln slag (VKS), atmospheric enriched-oxygen leaching residue (AELR) and neutralization (NZ)—are determined as research contents. In this research, three methods of dry-milling sulfidation, wet-milling sulfidation and hydrothermal sulfidation are firstly applied to deal with these wastes and the reaction mechanism of the three methods and the characteristics of reaction process are discussed.
The analysis on chemical composition and on environmental activation of the three categories reveals that the total composition of Zn&Pb in VKS is up to2%-3%and its heavy metal leaching concentration exceeds the national limits; the AELR contains5%of Zn and5%of Pb, in which the leaching concentration is also far beyond the national requirement. Though in NS, the contents of zinc is as high as15%-20%, the leaching concentration, however, can stay under the national limits since the heavy metal remains a stable property. Based on the results gained above together with the exploratory experiments on sulfidation of heavy metal oxide, three sulfidation technologies are introduced respectively to manage the three kinds of stockpiles. The dry-milling sulfidation is suitable for VKS with sulfur as sulfidizer, the wet-milling sulfidation is for AELR with sodium sulfide (Na2S) as sulfidizer and the hydrothermal sulfidation for NS with sulfur as sulfidizer.
The mechanism of the mechanically induced self-propagating sulfidation reaction (MSR) is systematically investigated in this research and the conversion of VKS is stabilized. The result of the dry-milling method shows that the optimum parameter is:sulfur:4.5%; milling time:1hour; ball-to-material ratio:20:1, and after the treatment95.4%of Zn and94.2%of Pb can be vulcanized, and the heavy metal concentration in leachate of the treated waste is under the allowable limit. The research also goes to study the crystal oxide structure variation of the heavy metal compounds as well as the features of other components. It is found that the vital factor to determine the mechanically induced self-propagating sulfidation reaction is adiabatic temperature (Tad) in the reactor, while the variation of crystal structure during the milling process can promote or hinder the reaction. The existence of iron powder (Fe) can induce the self-propagating sulfidation reaction, whose mechanism can be explained by the increasing of the Tad. The treated VKS can be used to make prefabricated sulfur materials for building. The optimal approach to solidification is heating step by step with40%of sulfur addition, particle size less than150μm and15%of aggregate in the filler. Under the conditions above, the compressive strength of solidified stuff can reach up to35MPa, and water absorption up to4%.
Heavy metal in AELR can be efficiently converted into metal sulfide when the surface active effect is caused by wet-milling sulfidation. The optimum parameters in operating process of the wet-milling sulfidation are established as the following:the reagent dosage of Na2S:8.4%, B/M:10:1, ball-milling time:1hour. Under these experimental conditions,73.2%of Pb in leaching residue can be converted to PbS. The shrinking core model discloses the cause that mechanic force can promote the heavy metal sulfidation, and the research shows that the sulfidation of PbSO4is controlled by inner diffusion of the reactants and the intensive mechanical stressing would result in faster kinetics by using fine particles to minimize diffusion problems. Flotation test indicates that up to50%of Pb, Cu and Cd could be recovered from the sludge. But the amount of sulfur in the sludge and the size of sulfide particles generated will determine the recovery during the process of flotation. TCLP and continuous leaching test reveal that the heavy metal concentration in leachate from the treated sludge is lower than the allowable limit. And the heavy metal left in the tailings is in a long-term stable state.
The Zn in the NS can efficiently be converted to zinc sulfide through dissolution-recrystallization process under hydrothermal conditions. The optimum parameters of operating process for hydrothermal sulfidation are: reaction time:2hours; temperature:200℃; sulfur concentration:15%; pulp density:300g·L-1; pH value:10plus. The result of the above shows that85%of Zn and75.4%of Pb in the sludge can be vulcanized. The entire course of hydrothermal sulfidation consists of the following stages: disproportionation reaction of sulfur, dissolution of metals, formation of CaSO4, synthesis of complexes with ligands containing sulphur atoms, and crystallization.33.3%of Zn,58.9%of Pb and68.8%of Cu can be recovered from the sludge by floatation. The lower recovery of ZnS is due to the small ball-shaped and heavily clustered particles with rough surface, which decline the floatability. But the poor floatability of ZnS can be improved by crystal modification. With an increase of temperature to260℃, reaction time to4hours, and adjusting initial Zn concentration to10%, the recovery is raised from33.3%to72.8%. The TCLP results indicate that all the leached heavy metal concentrations form floatation tailings are under the allowable limit. And the heavy metal in the tailings possesses a property of a long-term stability.
During the research, the "Hydrothermal Sulfidation and Floatation Treatment of Heavy-Metal-Containing Waste Pilot Experimental System" is developed and the pilot sulfidation experiment on NS is implemented as well. A series of experiments have witnessed that this pilot system is very well-functioning in terms of operative stability, a high rate of sulfdation and low secondary pollution. After floatation, the Zn sulfidation extent can reach up to87.34%. NS can produce Zn&Pb sulfide concentrate with a grade about40%and a recovery above65%.
三种堆置类废渣的化学成分及环境活性分析结果表明：挥发窑渣中Zn, Pb等重金属含量为2%-3%,且Pb、Cd等金属的浸出毒性存在超标风险；锌浸出渣的Zn含量为5%,Pb含量为5%,其金属的浸出毒性远远超过国家标准；中和渣的Zn含量在15-20%之间,但其中的重金属性质较稳定,且浸出毒性低于国家标准。根据上述分析结果,并结合重金属氧化物的硫化探索性实验,本文确定了以上三种堆置类废渣的硫化工艺：挥发窑渣采用干式球磨硫化-硫磺固化处理,采用硫磺作为硫化剂；常压富氧浸锌渣采用湿式球磨硫化-浮选分离稳定化处理,以硫化钠为硫化剂；中和渣采用水热硫化-浮选回收处理,以硫磺为硫化剂。
系统地研究了重金属的机械诱发的自蔓延硫化反应机制,实现了挥发窑渣的稳定化转变。研究结果表明,机械干磨挥发窑渣的最佳工艺参数为：硫磺添加量为4.5%,球磨时间为1小时,球料比为20：1,最优情况下Zn的硫化率可达95.4%,Pb的硫化率可达94.2%,处理后各重金属浸出毒性达标。通过分析球磨过程中重金属化合物晶体结构变化以及废渣中其他组分的行为特征,研究认为反应体系的绝热温度(Tad)是机械力诱发白蔓延硫化反应的主要决定因素,而球磨过程中晶体性质的变化仅起到促进或阻碍硫化反应的作用。挥发窑中的Fe等单质是诱发ZnO的实现自蔓延硫化反应的主要原因,其作用机制是提高了整个反应体系的绝热温度。硫化后的废渣可以制备成硫磺建材,最优的制备工艺为：采用分步投加方式加热,硫磺添加量40%,原料粒径小于150μm,骨料添加量控制在15%以内,在最优制备条件下,硫磺固化体的抗压强度为35MPa,吸水率为4%,满足建材要求。
利用湿式球磨的界面活化作用,实现了常压富氧浸锌渣的深度硫化,废渣中铅硫化率可达73.2%。湿式球磨硫化的最佳工艺为：Na2S·9H2O添加量为8.4%,球料比10：1,硫化时间1小时。利用收缩核模型揭示了机械力促进重金属硫化的原因。研究认为,PbSO4硫化反应受内扩散控制,球磨作用可以通过降低颗粒粒径,提高硫化剂进入反应物内核的速率。后续的浮选处理可以分离废渣中50%以上的Pb, Cu, Cd等重金属,然而废渣硫磺含量大、生成硫化物粒径细小是影响浮选回收率提高的主要原因。TCLP和连续淋洗实验表明,处理后的常压富氧浸锌渣重金属浸出毒性低于相关标准,并且具有长期稳定性。
利用水热条件下的溶解-再结晶机制,实现了重金属废水中和渣中重金属的高效硫化。其水热硫化的最佳工艺条件为：水热硫化温度200℃；水热硫化时间2小时；硫磺添加量15%；矿浆浓度300g·L-1；pH大于10。在此最优条件下,中和渣的锌硫化率可以达到85%以上,铅的硫化率可以达到75.4%以上。水热硫化中和渣的反应历程包括硫磺歧化、重金属溶解、CaSO4的生成、重金属含硫配合物的生成、降温结晶等阶段。水热硫化处理后锌的浮选回收率为33.3%,铅为58.9%,铜为68.8%。锌的可浮性较差主要是由其晶体性质造成的。水热合成的ZnS晶粒较小,团聚严重,表面粗糙,呈球状,这些性质都将降低其可浮性。为了提高ZnS的可浮性,实验考察了ZnS的晶型调控技术及其对可浮性的影响,结果表明,提高反应温度至260℃,延长反应时间至4小时,控制初始锌含量为10%后,ZnS回收率由33.3%提高至72.8%。重金属的稳定性检测结果表明,经过水热硫化-浮选处理后,废渣中的重金属浸出毒性低于国家标准,且重金属具有长期稳定性。
研制了“重金属废渣硫化-浮选处理中试系统”,并开展水热硫化-浮选技术处理废水中和渣的中试实验研究。实验结果表明该系统具有运行稳定,硫化率高,二次污染小等优点。现有的实验结果表明,处理后,中和渣中Zn的重金属硫化率达到87.34%,浮选处理可以从废水中和渣中回收铅锌综合品位为40%的人造硫化物精矿,回收率达65%。
Tons of heavy metal containing wastes are generated every year by zinc-lead smelters, whose total amount is more than100million tons. The management of these wastes is one of the great subject in environmental protection field. However, current methods are difficult to realize the resourcelization and stablization of heavy metals. For example, the widely-used direct extraction technique leads to a large quantity of wastewater and residue containing unstable state heavy metals; while cement solidification often causes the losses of heavy metal. Sulfidation treatment is a novel method to deal with heavy metal containing wastes. Through this approach the heavy metal can be converted into metal sulfide, the metal in which, subsequently, can be separated and recycled by means of floatation technique, and moreover the managed wastes are fairly stabilized after the treatment. According to the survey and the analysis of the heavy metal containing wastes from zinc-lead smelters, the stockpile wastes—namely volatilization kiln slag (VKS), atmospheric enriched-oxygen leaching residue (AELR) and neutralization (NZ)—are determined as research contents. In this research, three methods of dry-milling sulfidation, wet-milling sulfidation and hydrothermal sulfidation are firstly applied to deal with these wastes and the reaction mechanism of the three methods and the characteristics of reaction process are discussed.
The analysis on chemical composition and on environmental activation of the three categories reveals that the total composition of Zn&Pb in VKS is up to2%-3%and its heavy metal leaching concentration exceeds the national limits; the AELR contains5%of Zn and5%of Pb, in which the leaching concentration is also far beyond the national requirement. Though in NS, the contents of zinc is as high as15%-20%, the leaching concentration, however, can stay under the national limits since the heavy metal remains a stable property. Based on the results gained above together with the exploratory experiments on sulfidation of heavy metal oxide, three sulfidation technologies are introduced respectively to manage the three kinds of stockpiles. The dry-milling sulfidation is suitable for VKS with sulfur as sulfidizer, the wet-milling sulfidation is for AELR with sodium sulfide (Na2S) as sulfidizer and the hydrothermal sulfidation for NS with sulfur as sulfidizer.
The mechanism of the mechanically induced self-propagating sulfidation reaction (MSR) is systematically investigated in this research and the conversion of VKS is stabilized. The result of the dry-milling method shows that the optimum parameter is:sulfur:4.5%; milling time:1hour; ball-to-material ratio:20:1, and after the treatment95.4%of Zn and94.2%of Pb can be vulcanized, and the heavy metal concentration in leachate of the treated waste is under the allowable limit. The research also goes to study the crystal oxide structure variation of the heavy metal compounds as well as the features of other components. It is found that the vital factor to determine the mechanically induced self-propagating sulfidation reaction is adiabatic temperature (Tad) in the reactor, while the variation of crystal structure during the milling process can promote or hinder the reaction. The existence of iron powder (Fe) can induce the self-propagating sulfidation reaction, whose mechanism can be explained by the increasing of the Tad. The treated VKS can be used to make prefabricated sulfur materials for building. The optimal approach to solidification is heating step by step with40%of sulfur addition, particle size less than150μm and15%of aggregate in the filler. Under the conditions above, the compressive strength of solidified stuff can reach up to35MPa, and water absorption up to4%.
Heavy metal in AELR can be efficiently converted into metal sulfide when the surface active effect is caused by wet-milling sulfidation. The optimum parameters in operating process of the wet-milling sulfidation are established as the following:the reagent dosage of Na2S:8.4%, B/M:10:1, ball-milling time:1hour. Under these experimental conditions,73.2%of Pb in leaching residue can be converted to PbS. The shrinking core model discloses the cause that mechanic force can promote the heavy metal sulfidation, and the research shows that the sulfidation of PbSO4is controlled by inner diffusion of the reactants and the intensive mechanical stressing would result in faster kinetics by using fine particles to minimize diffusion problems. Flotation test indicates that up to50%of Pb, Cu and Cd could be recovered from the sludge. But the amount of sulfur in the sludge and the size of sulfide particles generated will determine the recovery during the process of flotation. TCLP and continuous leaching test reveal that the heavy metal concentration in leachate from the treated sludge is lower than the allowable limit. And the heavy metal left in the tailings is in a long-term stable state.
The Zn in the NS can efficiently be converted to zinc sulfide through dissolution-recrystallization process under hydrothermal conditions. The optimum parameters of operating process for hydrothermal sulfidation are: reaction time:2hours; temperature:200℃; sulfur concentration:15%; pulp density:300g·L-1; pH value:10plus. The result of the above shows that85%of Zn and75.4%of Pb in the sludge can be vulcanized. The entire course of hydrothermal sulfidation consists of the following stages: disproportionation reaction of sulfur, dissolution of metals, formation of CaSO4, synthesis of complexes with ligands containing sulphur atoms, and crystallization.33.3%of Zn,58.9%of Pb and68.8%of Cu can be recovered from the sludge by floatation. The lower recovery of ZnS is due to the small ball-shaped and heavily clustered particles with rough surface, which decline the floatability. But the poor floatability of ZnS can be improved by crystal modification. With an increase of temperature to260℃, reaction time to4hours, and adjusting initial Zn concentration to10%, the recovery is raised from33.3%to72.8%. The TCLP results indicate that all the leached heavy metal concentrations form floatation tailings are under the allowable limit. And the heavy metal in the tailings possesses a property of a long-term stability.
During the research, the "Hydrothermal Sulfidation and Floatation Treatment of Heavy-Metal-Containing Waste Pilot Experimental System" is developed and the pilot sulfidation experiment on NS is implemented as well. A series of experiments have witnessed that this pilot system is very well-functioning in terms of operative stability, a high rate of sulfdation and low secondary pollution. After floatation, the Zn sulfidation extent can reach up to87.34%. NS can produce Zn&Pb sulfide concentrate with a grade about40%and a recovery above65%.
引文
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