复杂低品位锰矿及含锰烟尘加压酸浸—净化—萃取工艺研究
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摘要
我国锰矿资源的贫乏正制约着锰系产品的生产以及可持续发展。在我国一些锰系产品生产集中的地区,所使用碳酸锰矿的品位已经由含锰18%～20%降低到只有12%～15%,而另一方面,大量含锰在20%～25%的软锰矿,却因为还原过程成本过高,或者污染环境严重等问题而得不到利用。由此可见,研究如何经济、合理地利用我国的锰矿资源,对缓解我国当前锰矿资源紧缺的矛盾、确保锰系产品行业的可持续发展,以及促进西部地区经济的发展都具有十分重要的战略意义。本论文以难处理的复杂低品位锰矿和含锰烟尘为原料,开发出加压酸浸-净化-萃取的新工艺。
首先采用化学多元素分析、物相分析、XRD分析、微观形貌和能谱分析等分析手段对复杂低品位锰矿、含锰烟尘及还原剂硫铁矿进行了矿物学分析。分析结果表明,复杂低品位锰矿中的锰主要以高价氧化锰(Mn3O4和MnO1.88)的物相形态存在,锰的品位为17.64%,该矿中主要的脉石矿物是CaO,其次是SiO2、Al2O3及MgO。含锰烟尘中的锰主要分布在高价氧化物MnO2和MnO1.88中,锰的品位为33.5%,烟尘中的主要脉石矿物是SiO2,其次是Al2O3。还原剂硫铁矿的主要物相成分为FeS2,BaSO4,SiO2,ZnS和Al2Si4O10(OH)2。
对复杂低品位锰矿和含锰烟尘加压浸出过程进行了热力学及机理分析,锰浸出的化学反应在373K下的ΔG373Kθ值均为负值。通过对酸性溶液中锰的电位-氧化态-ΔG图以及298K和373K时的Mn-H2O系、Fe-S-H2O系与Mn-H2O系、S-H2O系φ-pH图的分析可知,无论是在常温条件还是在高温条件下,理论上用硫铁矿还原浸出高价氧化锰矿都是可行的。在高温条件下进行加压浸出主要是出于动力学的考虑,同时有利于硫铁矿中的硫和铁分别转变为SO42-或H2SO4和Fe2O3,从而达到浸出速度快,酸耗低,铁溶出率低的效果。
通过对低品位锰矿加压酸浸工艺进行正交实验和单因素实验研究得到优化浸出工艺条件为：低品位氧化锰矿粉100g,初始硫酸浓度120g/L,反应温度120℃,硫铁矿量50g,液固比5：1,浸出时间100min,压力0.7MPa,搅拌转速350r/min。本工艺具有良好的稳定性,在优化浸出条件下,锰的浸出率为96%,而铝和铁的浸出率分别为38.7%和7.12%,浸出液中锰、铁和铝的浓度分别为19.87g/L、2.34g/L和0.74g/L。其中温度、压力和时间对铝的行为影响较大。
含锰烟尘加压浸出较优的工艺条件为：含锰烟尘100g,初始硫酸浓度120g/L,液固比5：1,浸出温度120℃,压力0.8MPa,浸出时间2h,搅拌转速350r/min。锰浸出率可达96.1%以上,铁浸出率仅7%左右,终酸残余率35%左右。浸出液中锰和铁的浓度分别为44.74g/L和2.52g/L。
对加压浸出复杂低品位锰矿动力学进行了研究。考察了搅拌速度、矿粉粒度、温度、压力、硫酸浓度和固体矿物中的硫铁矿量等因素对锰浸出速率的影响。实验结果表明,搅拌速度对反应过程基本没有影响。锰的浸出率随着矿粉粒度的减小而增大,随着温度、压力、硫酸浓度和硫铁矿量的增大而增大。结果表明,浸出反应遵循界面化学反应控制的核收缩模型,反应的表观活化能为43.4kJ/mol。硫酸浓度、压力以及硫铁矿量的表观反应级数分别为1.428、0.864和2.58。得到加压酸浸复杂低品位锰矿的宏观动力学方程为：
1-(1-x)1/3=(3824.8/HAir0.864·r0).exp(-43.4×103/RT)·C1.428·P0.864·[FeS2]2.58·t并最终验证了计算值与实验值基本吻合。
从生产角度出发,对硫酸锰的加压浸出液进行了净化除杂试验研究。采用氧化中和法脱除Fe3+和Al3+等离子,得到的中和液中的Fe3+和A13+离子的浓度分别小于lmg/L和0.18mg/L,Cu2+和Zn2+离子的浓度分别为0.27mg/L和0.082mg/L；然后采用硫化铵为沉淀剂进行重金属离子的脱除,控制溶液pH<6.0即可以使重金属离子沉淀析出而不会生成MnS沉淀,所得滤液中的Co2+、Ni2+和Cu2+的浓度分别为0.253mg/L、0.637mg/L和0.071mg/L；最后采用浓缩静置法对Ca2+和Mg2+脱除后,溶液中Ca2+和Mg2+离子的浓度和脱除率分别为0.08g/L和85.63%、0.36g/L和83.22%。
考虑到低品位锰矿及含锰烟尘浸出液中的锰离子浓度很低,因此采用了萃取-反萃技术。由于浸出液不能直接萃取锰,直接萃取时铁更容易被萃取,且钙和镁易造成乳化现象,因此选择净化除杂后进行萃取。所得优化萃取工艺条件为：萃取剂P2O4的皂化率为80%,萃取相比(O/A)为1：1,萃取剂(P2O4)浓度为40%,萃取平衡pH值为5.0左右,萃取温度为30～40℃,萃取平衡时间为5min,萃取级数为一级。对于含锰21.20g/L的净化液而言,锰的萃取率可达95%以上。反萃优化工艺条件为：反萃酸度为120g/L,反萃温度为室温,反萃混合时间为3min,反萃相比为2：1-3：1,反萃级数为一级,锰的反萃率为96.9%,反萃液中锰离子浓度为42.16g/L,其他杂质离子的浓度均达到电解锰要求。
The production and sustainable development of manganese series products were restricted by poor resources of manganese ore in China. At the area of some manganese series products production concentrated in our country, the grade of manganese carbonate has been reduced from18%～20%to only12%～15%, and on the other hand, a large number of pyrolusite of manganese content in20%～25%can't be used, because of the cost of reduction process is too high or the environmental pollution problems serious. Therefore, it has important strategic significance to research how to use the resources of manganese ore economically and legitimately in China for easing the contradiction of manganese ore resources short supply in our country, ensuring the sustainable development of manganese series products industry, and promoting the economic development of western region. In this thesis, the unmanageable complex low-grade manganese ore and manganese-containing dust as raw material, a new technology of pressure acid leaching-purification-extraction was developed.
First of all, The analysis approaches such as chemical multielement analysis, physical phase analysis, XRD analysis, SEM images and energy spectrum analysis were used for the mineralogy analysis of complex low-grade manganese ore, manganese-containing dust and pyrite. The analysis results showed that manganese of complex low-grade manganese mainly existed in high valence manganese oxide (Mn3O4and MnO1.88), the content of manganese was17.64%. The major gangue mineral of complex low-grade manganese ore is CaO, followed by SiO2, Al2O3and MgO. The manganese of manganese-containing dust mainly distributed in the high valence manganese oxide MnO2and MnO1.88, the content of manganese was33.5%. The major gangue mineral of manganese-containing dust is SiO2, followed by Al2O3. The main phase composition of pyrite were FeS2, BaSO4, SiO2, ZnS and Al2Si4O10(OH)2.
Thermodynamics and mechanism analysis were studied for the pressure leaching process of complex low-grade manganese and manganese-containing dust, the values of chemical reaction were negative. The potential-oxidation state-AG diagram of manganese in acid solution, the φ-pH diagram of Mn-H2O system, Fe-S-H2O system and Mn-H2O system, S-H2O system at298K and373K were analyzed. The analysis results showed that high valence manganese oxide was reducted and leaching by pyrite theoretically whether in room temperature or high temperature conditions. Pressure leaching in high temperature is based on the needs of the dynamics primarily, and it is helpful for the sulfur and iron of pyrite were translated into SO42-or H2SO4and Fe2O3respectively, thus the effect of increasing the leaching speed, decreasing the acid consumption and iron dissolving rate were achieved.
The pressure leaching process of complex low-grade manganese ore in a sulfuric acid medium was studied by orthogonal experiments and single-factor experiments. And the optimum leaching conditions were determined to be:low grade manganese powdered ore of100g, initial acidity of120g/L, leaching temperature of120℃, pyrite amount of50g, liquid-to-solid ratio of5:1, leaching time of100min, pressure of0.7Mpa, the agitation speed of350r/min. The results of experiments indicated that this craft had good stability. Under the optimized leaching condition, the leaching rate of manganese was96%, and the leaching rates of Al and Fe were38.7%and7.12%. The concentration of Mn、Fe and Al in leaching liquid were19.87g/L、2.34g/L and0.74g/L respectively. The temperature, pressure and time had a great important on the behavior of aluminum.
The optimum operating parameters of pressure leaching of manganese-containing dust were established as follows:the manganese-containing dust of100g; pyrite amount of50g; the liquid to solid ratio of5:1; the initial sulfuric acid concentration of120g/L, leaching temperature of120℃, pressure of0.8MPa, leaching time of2h, the agitation speed of350r/min. Under these conditions, the leaching rates of Mn and Fe arrive at96.1%and7%, the residual rate of final acid is about35%. The concentration of manganese and iron in leaching liquid were44.74g/L and2.52g/L.
The kinetics of pressure leaching low grade manganese ore was studied. The effects of agitation rate, particle size,temperature, pressure, initial acid concentration and pyrite content in solid mineral on the leaching rate of manganese were examined. The experiment results indicate that the agitation rate had no effect basically on the reaction process, manganese leaching rate increases with a decrease of particle size and an increase of temperature, total pressure, sulfuric acid concentration and pyrite content in solid mineral. It was found that the reaction kinetic model follows the shrinking core model of chemical reaction control and the apparent activation energy was determined as43.4kJ/mol. The reaction orders with respect to sulphuric acid concentration total pressure and pyrite content were1.428、0.864and2.58, respectively. The kinetic equations for the effect of particle size, leaching temperature, total pressure, sulfuric acid concentration and pyrite content were obtained and a mathematical model of manganese leaching from low grade manganese ore was developed as:
1-(1-x)1/3=(3824.8/HAir0.864·r0)·exp(-43.4×103/RT)·C1.428·P0.864·[FeS2]2.58·t This equation estimates the leaching of manganese with very good agreement between the experimental and calculated values.
Considering the production, the purification process of manganese sulfate pressure leaching liquid has been studied. The method of oxidation and neutralization was used for removing Fe3+and Al3+ions, the concentration of Fe3+and Al3+ions in neutralization liquid were less than1mg/L and0.18mg/L respectively, the concentration of Cu2+and Zn2+ion were0.27mg/L and0.082mg/L respectively; Removal heavy metal ion by ammonium sulphide as the precipitating agent, the pH of the neutralization fluid was controlled less than6.0, the heavy metal ions were precipitate out and MnS precipitation was not generated, the concentration of Co2+Ni2+and Cu2+in filtrate were0.253mg/L、0.637mg/L and0.071mg/L; After concentration and standing for a long time, the concentration and removal rate of Ca2+and Mg2+ion were0.08g/L and85.63%、0.36g/L and83.22%.
In view of the low concentration of manganese ions in leaching solution of low-grade manganese ore and manganese-containing dust, the technique of extraction-back extraction was used. Manganese can not be directly extracted from the leaching solution because of iron is extracted easily, and calcium and magnesium would lead to the emulsification of extracting agent. Therefore, the purification process was carried out before the process of extraction-back extraction.The optimum extraction conditions were determined to be:the saponification rate of extraction agent P204was80%, the extraction phase ratio (O/A) was1:1, the concentration of extraction agent (P204) was40%, the extraction pH value was5.0, the temperature was30～40℃, the extraction time was5min, the extraction stages was level1. In terms of the purification liquid that the concentration of manganese ion is21.20g/L, Mn extraction rate was above95%. The optimum back-extraction conditions were determined to be:the acidity of back-extraction was120g/L, the temperature of back-extraction was room temperature, the mixing time of back-extraction was3min, the phase ratio of back-extraction was2:1-3:1, the stages of back-extraction was level1. The back-extraction rate and the concentration of manganese were96.9%and42.16g/L respectively, and the concentration of other impurities has reached the requirement of electrolytic manganese.
首先采用化学多元素分析、物相分析、XRD分析、微观形貌和能谱分析等分析手段对复杂低品位锰矿、含锰烟尘及还原剂硫铁矿进行了矿物学分析。分析结果表明,复杂低品位锰矿中的锰主要以高价氧化锰(Mn3O4和MnO1.88)的物相形态存在,锰的品位为17.64%,该矿中主要的脉石矿物是CaO,其次是SiO2、Al2O3及MgO。含锰烟尘中的锰主要分布在高价氧化物MnO2和MnO1.88中,锰的品位为33.5%,烟尘中的主要脉石矿物是SiO2,其次是Al2O3。还原剂硫铁矿的主要物相成分为FeS2,BaSO4,SiO2,ZnS和Al2Si4O10(OH)2。
对复杂低品位锰矿和含锰烟尘加压浸出过程进行了热力学及机理分析,锰浸出的化学反应在373K下的ΔG373Kθ值均为负值。通过对酸性溶液中锰的电位-氧化态-ΔG图以及298K和373K时的Mn-H2O系、Fe-S-H2O系与Mn-H2O系、S-H2O系φ-pH图的分析可知,无论是在常温条件还是在高温条件下,理论上用硫铁矿还原浸出高价氧化锰矿都是可行的。在高温条件下进行加压浸出主要是出于动力学的考虑,同时有利于硫铁矿中的硫和铁分别转变为SO42-或H2SO4和Fe2O3,从而达到浸出速度快,酸耗低,铁溶出率低的效果。
通过对低品位锰矿加压酸浸工艺进行正交实验和单因素实验研究得到优化浸出工艺条件为：低品位氧化锰矿粉100g,初始硫酸浓度120g/L,反应温度120℃,硫铁矿量50g,液固比5：1,浸出时间100min,压力0.7MPa,搅拌转速350r/min。本工艺具有良好的稳定性,在优化浸出条件下,锰的浸出率为96%,而铝和铁的浸出率分别为38.7%和7.12%,浸出液中锰、铁和铝的浓度分别为19.87g/L、2.34g/L和0.74g/L。其中温度、压力和时间对铝的行为影响较大。
含锰烟尘加压浸出较优的工艺条件为：含锰烟尘100g,初始硫酸浓度120g/L,液固比5：1,浸出温度120℃,压力0.8MPa,浸出时间2h,搅拌转速350r/min。锰浸出率可达96.1%以上,铁浸出率仅7%左右,终酸残余率35%左右。浸出液中锰和铁的浓度分别为44.74g/L和2.52g/L。
对加压浸出复杂低品位锰矿动力学进行了研究。考察了搅拌速度、矿粉粒度、温度、压力、硫酸浓度和固体矿物中的硫铁矿量等因素对锰浸出速率的影响。实验结果表明,搅拌速度对反应过程基本没有影响。锰的浸出率随着矿粉粒度的减小而增大,随着温度、压力、硫酸浓度和硫铁矿量的增大而增大。结果表明,浸出反应遵循界面化学反应控制的核收缩模型,反应的表观活化能为43.4kJ/mol。硫酸浓度、压力以及硫铁矿量的表观反应级数分别为1.428、0.864和2.58。得到加压酸浸复杂低品位锰矿的宏观动力学方程为：
1-(1-x)1/3=(3824.8/HAir0.864·r0).exp(-43.4×103/RT)·C1.428·P0.864·[FeS2]2.58·t并最终验证了计算值与实验值基本吻合。
从生产角度出发,对硫酸锰的加压浸出液进行了净化除杂试验研究。采用氧化中和法脱除Fe3+和Al3+等离子,得到的中和液中的Fe3+和A13+离子的浓度分别小于lmg/L和0.18mg/L,Cu2+和Zn2+离子的浓度分别为0.27mg/L和0.082mg/L；然后采用硫化铵为沉淀剂进行重金属离子的脱除,控制溶液pH<6.0即可以使重金属离子沉淀析出而不会生成MnS沉淀,所得滤液中的Co2+、Ni2+和Cu2+的浓度分别为0.253mg/L、0.637mg/L和0.071mg/L；最后采用浓缩静置法对Ca2+和Mg2+脱除后,溶液中Ca2+和Mg2+离子的浓度和脱除率分别为0.08g/L和85.63%、0.36g/L和83.22%。
考虑到低品位锰矿及含锰烟尘浸出液中的锰离子浓度很低,因此采用了萃取-反萃技术。由于浸出液不能直接萃取锰,直接萃取时铁更容易被萃取,且钙和镁易造成乳化现象,因此选择净化除杂后进行萃取。所得优化萃取工艺条件为：萃取剂P2O4的皂化率为80%,萃取相比(O/A)为1：1,萃取剂(P2O4)浓度为40%,萃取平衡pH值为5.0左右,萃取温度为30～40℃,萃取平衡时间为5min,萃取级数为一级。对于含锰21.20g/L的净化液而言,锰的萃取率可达95%以上。反萃优化工艺条件为：反萃酸度为120g/L,反萃温度为室温,反萃混合时间为3min,反萃相比为2：1-3：1,反萃级数为一级,锰的反萃率为96.9%,反萃液中锰离子浓度为42.16g/L,其他杂质离子的浓度均达到电解锰要求。
The production and sustainable development of manganese series products were restricted by poor resources of manganese ore in China. At the area of some manganese series products production concentrated in our country, the grade of manganese carbonate has been reduced from18%～20%to only12%～15%, and on the other hand, a large number of pyrolusite of manganese content in20%～25%can't be used, because of the cost of reduction process is too high or the environmental pollution problems serious. Therefore, it has important strategic significance to research how to use the resources of manganese ore economically and legitimately in China for easing the contradiction of manganese ore resources short supply in our country, ensuring the sustainable development of manganese series products industry, and promoting the economic development of western region. In this thesis, the unmanageable complex low-grade manganese ore and manganese-containing dust as raw material, a new technology of pressure acid leaching-purification-extraction was developed.
First of all, The analysis approaches such as chemical multielement analysis, physical phase analysis, XRD analysis, SEM images and energy spectrum analysis were used for the mineralogy analysis of complex low-grade manganese ore, manganese-containing dust and pyrite. The analysis results showed that manganese of complex low-grade manganese mainly existed in high valence manganese oxide (Mn3O4and MnO1.88), the content of manganese was17.64%. The major gangue mineral of complex low-grade manganese ore is CaO, followed by SiO2, Al2O3and MgO. The manganese of manganese-containing dust mainly distributed in the high valence manganese oxide MnO2and MnO1.88, the content of manganese was33.5%. The major gangue mineral of manganese-containing dust is SiO2, followed by Al2O3. The main phase composition of pyrite were FeS2, BaSO4, SiO2, ZnS and Al2Si4O10(OH)2.
Thermodynamics and mechanism analysis were studied for the pressure leaching process of complex low-grade manganese and manganese-containing dust, the values of chemical reaction were negative. The potential-oxidation state-AG diagram of manganese in acid solution, the φ-pH diagram of Mn-H2O system, Fe-S-H2O system and Mn-H2O system, S-H2O system at298K and373K were analyzed. The analysis results showed that high valence manganese oxide was reducted and leaching by pyrite theoretically whether in room temperature or high temperature conditions. Pressure leaching in high temperature is based on the needs of the dynamics primarily, and it is helpful for the sulfur and iron of pyrite were translated into SO42-or H2SO4and Fe2O3respectively, thus the effect of increasing the leaching speed, decreasing the acid consumption and iron dissolving rate were achieved.
The pressure leaching process of complex low-grade manganese ore in a sulfuric acid medium was studied by orthogonal experiments and single-factor experiments. And the optimum leaching conditions were determined to be:low grade manganese powdered ore of100g, initial acidity of120g/L, leaching temperature of120℃, pyrite amount of50g, liquid-to-solid ratio of5:1, leaching time of100min, pressure of0.7Mpa, the agitation speed of350r/min. The results of experiments indicated that this craft had good stability. Under the optimized leaching condition, the leaching rate of manganese was96%, and the leaching rates of Al and Fe were38.7%and7.12%. The concentration of Mn、Fe and Al in leaching liquid were19.87g/L、2.34g/L and0.74g/L respectively. The temperature, pressure and time had a great important on the behavior of aluminum.
The optimum operating parameters of pressure leaching of manganese-containing dust were established as follows:the manganese-containing dust of100g; pyrite amount of50g; the liquid to solid ratio of5:1; the initial sulfuric acid concentration of120g/L, leaching temperature of120℃, pressure of0.8MPa, leaching time of2h, the agitation speed of350r/min. Under these conditions, the leaching rates of Mn and Fe arrive at96.1%and7%, the residual rate of final acid is about35%. The concentration of manganese and iron in leaching liquid were44.74g/L and2.52g/L.
The kinetics of pressure leaching low grade manganese ore was studied. The effects of agitation rate, particle size,temperature, pressure, initial acid concentration and pyrite content in solid mineral on the leaching rate of manganese were examined. The experiment results indicate that the agitation rate had no effect basically on the reaction process, manganese leaching rate increases with a decrease of particle size and an increase of temperature, total pressure, sulfuric acid concentration and pyrite content in solid mineral. It was found that the reaction kinetic model follows the shrinking core model of chemical reaction control and the apparent activation energy was determined as43.4kJ/mol. The reaction orders with respect to sulphuric acid concentration total pressure and pyrite content were1.428、0.864and2.58, respectively. The kinetic equations for the effect of particle size, leaching temperature, total pressure, sulfuric acid concentration and pyrite content were obtained and a mathematical model of manganese leaching from low grade manganese ore was developed as:
1-(1-x)1/3=(3824.8/HAir0.864·r0)·exp(-43.4×103/RT)·C1.428·P0.864·[FeS2]2.58·t This equation estimates the leaching of manganese with very good agreement between the experimental and calculated values.
Considering the production, the purification process of manganese sulfate pressure leaching liquid has been studied. The method of oxidation and neutralization was used for removing Fe3+and Al3+ions, the concentration of Fe3+and Al3+ions in neutralization liquid were less than1mg/L and0.18mg/L respectively, the concentration of Cu2+and Zn2+ion were0.27mg/L and0.082mg/L respectively; Removal heavy metal ion by ammonium sulphide as the precipitating agent, the pH of the neutralization fluid was controlled less than6.0, the heavy metal ions were precipitate out and MnS precipitation was not generated, the concentration of Co2+Ni2+and Cu2+in filtrate were0.253mg/L、0.637mg/L and0.071mg/L; After concentration and standing for a long time, the concentration and removal rate of Ca2+and Mg2+ion were0.08g/L and85.63%、0.36g/L and83.22%.
In view of the low concentration of manganese ions in leaching solution of low-grade manganese ore and manganese-containing dust, the technique of extraction-back extraction was used. Manganese can not be directly extracted from the leaching solution because of iron is extracted easily, and calcium and magnesium would lead to the emulsification of extracting agent. Therefore, the purification process was carried out before the process of extraction-back extraction.The optimum extraction conditions were determined to be:the saponification rate of extraction agent P204was80%, the extraction phase ratio (O/A) was1:1, the concentration of extraction agent (P204) was40%, the extraction pH value was5.0, the temperature was30～40℃, the extraction time was5min, the extraction stages was level1. In terms of the purification liquid that the concentration of manganese ion is21.20g/L, Mn extraction rate was above95%. The optimum back-extraction conditions were determined to be:the acidity of back-extraction was120g/L, the temperature of back-extraction was room temperature, the mixing time of back-extraction was3min, the phase ratio of back-extraction was2:1-3:1, the stages of back-extraction was level1. The back-extraction rate and the concentration of manganese were96.9%and42.16g/L respectively, and the concentration of other impurities has reached the requirement of electrolytic manganese.
引文
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