氧化锌矿物碱法提取新工艺研究
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摘要
随着硫化锌矿资源的日趋紧缺,氧化锌矿资源正逐步得到开发和利用。针对氧化锌矿物中异极矿难于处理的现状,提出了碱法处理异极矿的新工艺,并对其做了系统的条件和理论研究。其具体研究内容如下：
(一)通过绘制Zn-Si-H2O系的lgC-pH图,分析了苛性钠处理异极矿的热力学条件,得知,异极矿在碱浸出过程中,锌、硅分别以Zn(OH)42-和H2SiO42-的形式进入溶液。苛性钠处理异极矿的动力学研究表明,浸出过程受化学反应控制,其反应活化能E=45.7 kJ/mol,反应级数n=1.4。
(二)设计了碱法处理低硅型异极矿的工艺流程。首先在热球磨中对低硅型异极矿进行苛性钠浸出,并在浸出的同时加CaO抑制矿物中硅的浸出,在CaO用量为理论用量的1倍、NaOH浓度为4.5mol/L、浸出温度为110℃、L：S=10：1、浸出时间1h的条件下,锌的浸出率可达到93%,而只有7%左右的Si02被浸出。然后在浸出液中添加Na2S固体,使S2-与溶液中的ZnO22-反应生成ZnS沉淀,而Na+将与溶液中的OH-结合生成NaOH,在反应温度为60℃、S／Zn摩尔比为0.95：1、时间为15分钟的条件下,沉锌率为93%,沉锌母液返回再次浸矿,在NaOH浓度为5 mol/L、CaO用量为理论用量的1.25倍、浸出温度为110℃、L：S=10：1、浸出时间1h的条件下,锌的浸出率维持在91%左右,而其它元素在循环浸出过程中不会积累。
(三)设计了碱法处理高硅型异极矿的工艺流程。首先在热球磨中对高硅型异极矿进行苛性钠浸出,在NaOH浓度为8mol/L、浸出温度为130℃、L：S=8：1、浸出时间1h的条件下,锌的浸出率为95%,Si02的浸出率为64%。然后在浸出液中添加Na2S固体,在反应温度为60℃、S／Zn摩尔比为0.98、时间为15分钟的条件下,沉锌率可达到95%。接着在沉锌母液中添加CaO固体,在反应温度为75℃、CaO用量为理论量的1.5倍、时间0.5h的条件下,沉硅率达到96%。沉硅母液返回再次浸矿,在氢氧化钠浓度为8.5mol/L、浸出温度为130℃、L：S=8：1、浸出时间1h的条件下,锌的浸出率维持在93%左右,未发现其它元素在循环浸出过程中积累。
With the increasing shortage of Zinc sulfide ore, Zinc oxide resources are gradually developed and utilized. Aiming at the status that hemimorphite in Zinc oxide mine is difficult to deal with, we proposed a new alkaline process to treat hemimorphite, and carried out systematic conditions and theoretical studies. The specific contents are as follows:
1). Drawed the lgC-pH diagram of Zn-Si-H2O system, and analized the thermodynamic conditions with caustic soda to treat hemimorphite. We can learn that in alkaline leaching process of hemimorphite, Zn and silicon entered into solution with Zn (OH)42- and H2SiO42- respectively. We also studied its dynamics mechanism, and determined its activation energy E= 45.7 kJ/mol, the reaction order n= 1.4, which showed that the leaching process was controlled by chemical reaction.
2). Designed the process flow with Alkaline to treat low-silicon hemimorphite. First of all, extract Zn in alkali solution from low-silicon hemimorphite in a hot ball mill reactor. In order to control the leaching of SiO2, CaO was added into NaOH solution during the leaching process. When CaO dosage is 1 time of the theoretical quantity, temperature is 110℃, NaOH concentration is 4.5 mol/L, liquid-solid ratio (L/S) is 10:1 and leaching time is 1h, the recovery of Zn is 93%, but the decomposition rate of SiO2 is only 7.3%. And then, add the solid Na2S into leaching solution, in which the ion of S2- and ZnO22- will be formed as the precipitation ZnS, and the ion of Na+ will be formed as NaOH combined with OH-. When the reaction temperature is 60℃, the molar ratio of S to Zn is 0.95:1 and the reaction time is 15 minutes, the precipitation rate of Zn is 93%.The mother liquor after Zn precipitation will be sent to leach Zn again. When the CaO dosage is 1.25 times of the theoretical quantity, temperature is 110℃, NaOH concentration is 5 mol/L, liquid-solid ratio (L/S) is 10:1 and leaching time is 1h, the recovery of Zn remains around 91%, but other elements are not accumulated during the leaching process.
3). Planed the process of Zn alkali extraction from high-silicon hemimorphite. Firstly, extract Zn in alkali solution from high-silicon hemimorphite in a hot ball mill reactor. When the reaction temperature is 130℃, NaOH concentration is 8 mol/L, liquid-solid ratio (L/S) is 8:1 and leaching time is 1h, the recovery of Zn is 95% and the decomposition rate of SiO2 is 64%. Then add the solid Na2S into leaching solution. When the reaction temperature is 60℃, the molar ratio of S to Zn is 0.98:1 and the reaction time is 15 minutes, the precipitation rate of Zn is 95%. After that, add the solid CaO into the mother liquor. When the reaction temperature is 60℃, CaO dosage is 1.5 times of the theoretical quantity and the reaction time is 1 h, the desilication rate is 96% The desilicated mother liquor will be sent to leach Zn again. When the reaction temperature is 130℃, NaOH concentration is 8.5mol/L, liquid-solid ratio (L/S) is 8:1 and leaching time is 1h, the recovery of Zn remains about 93%, but other elements are not accumulated during the leaching process.
(一)通过绘制Zn-Si-H2O系的lgC-pH图,分析了苛性钠处理异极矿的热力学条件,得知,异极矿在碱浸出过程中,锌、硅分别以Zn(OH)42-和H2SiO42-的形式进入溶液。苛性钠处理异极矿的动力学研究表明,浸出过程受化学反应控制,其反应活化能E=45.7 kJ/mol,反应级数n=1.4。
(二)设计了碱法处理低硅型异极矿的工艺流程。首先在热球磨中对低硅型异极矿进行苛性钠浸出,并在浸出的同时加CaO抑制矿物中硅的浸出,在CaO用量为理论用量的1倍、NaOH浓度为4.5mol/L、浸出温度为110℃、L：S=10：1、浸出时间1h的条件下,锌的浸出率可达到93%,而只有7%左右的Si02被浸出。然后在浸出液中添加Na2S固体,使S2-与溶液中的ZnO22-反应生成ZnS沉淀,而Na+将与溶液中的OH-结合生成NaOH,在反应温度为60℃、S／Zn摩尔比为0.95：1、时间为15分钟的条件下,沉锌率为93%,沉锌母液返回再次浸矿,在NaOH浓度为5 mol/L、CaO用量为理论用量的1.25倍、浸出温度为110℃、L：S=10：1、浸出时间1h的条件下,锌的浸出率维持在91%左右,而其它元素在循环浸出过程中不会积累。
(三)设计了碱法处理高硅型异极矿的工艺流程。首先在热球磨中对高硅型异极矿进行苛性钠浸出,在NaOH浓度为8mol/L、浸出温度为130℃、L：S=8：1、浸出时间1h的条件下,锌的浸出率为95%,Si02的浸出率为64%。然后在浸出液中添加Na2S固体,在反应温度为60℃、S／Zn摩尔比为0.98、时间为15分钟的条件下,沉锌率可达到95%。接着在沉锌母液中添加CaO固体,在反应温度为75℃、CaO用量为理论量的1.5倍、时间0.5h的条件下,沉硅率达到96%。沉硅母液返回再次浸矿,在氢氧化钠浓度为8.5mol/L、浸出温度为130℃、L：S=8：1、浸出时间1h的条件下,锌的浸出率维持在93%左右,未发现其它元素在循环浸出过程中积累。
With the increasing shortage of Zinc sulfide ore, Zinc oxide resources are gradually developed and utilized. Aiming at the status that hemimorphite in Zinc oxide mine is difficult to deal with, we proposed a new alkaline process to treat hemimorphite, and carried out systematic conditions and theoretical studies. The specific contents are as follows:
1). Drawed the lgC-pH diagram of Zn-Si-H2O system, and analized the thermodynamic conditions with caustic soda to treat hemimorphite. We can learn that in alkaline leaching process of hemimorphite, Zn and silicon entered into solution with Zn (OH)42- and H2SiO42- respectively. We also studied its dynamics mechanism, and determined its activation energy E= 45.7 kJ/mol, the reaction order n= 1.4, which showed that the leaching process was controlled by chemical reaction.
2). Designed the process flow with Alkaline to treat low-silicon hemimorphite. First of all, extract Zn in alkali solution from low-silicon hemimorphite in a hot ball mill reactor. In order to control the leaching of SiO2, CaO was added into NaOH solution during the leaching process. When CaO dosage is 1 time of the theoretical quantity, temperature is 110℃, NaOH concentration is 4.5 mol/L, liquid-solid ratio (L/S) is 10:1 and leaching time is 1h, the recovery of Zn is 93%, but the decomposition rate of SiO2 is only 7.3%. And then, add the solid Na2S into leaching solution, in which the ion of S2- and ZnO22- will be formed as the precipitation ZnS, and the ion of Na+ will be formed as NaOH combined with OH-. When the reaction temperature is 60℃, the molar ratio of S to Zn is 0.95:1 and the reaction time is 15 minutes, the precipitation rate of Zn is 93%.The mother liquor after Zn precipitation will be sent to leach Zn again. When the CaO dosage is 1.25 times of the theoretical quantity, temperature is 110℃, NaOH concentration is 5 mol/L, liquid-solid ratio (L/S) is 10:1 and leaching time is 1h, the recovery of Zn remains around 91%, but other elements are not accumulated during the leaching process.
3). Planed the process of Zn alkali extraction from high-silicon hemimorphite. Firstly, extract Zn in alkali solution from high-silicon hemimorphite in a hot ball mill reactor. When the reaction temperature is 130℃, NaOH concentration is 8 mol/L, liquid-solid ratio (L/S) is 8:1 and leaching time is 1h, the recovery of Zn is 95% and the decomposition rate of SiO2 is 64%. Then add the solid Na2S into leaching solution. When the reaction temperature is 60℃, the molar ratio of S to Zn is 0.98:1 and the reaction time is 15 minutes, the precipitation rate of Zn is 95%. After that, add the solid CaO into the mother liquor. When the reaction temperature is 60℃, CaO dosage is 1.5 times of the theoretical quantity and the reaction time is 1 h, the desilication rate is 96% The desilicated mother liquor will be sent to leach Zn again. When the reaction temperature is 130℃, NaOH concentration is 8.5mol/L, liquid-solid ratio (L/S) is 8:1 and leaching time is 1h, the recovery of Zn remains about 93%, but other elements are not accumulated during the leaching process.
引文
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