氯盐体系提取红土矿中镍钴的工艺及基础研究
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摘要
为有效提取红土矿中镍钴资源,避免现有工艺技术中所存在的问题,本论文提出以氯化物为提取介质,分别采用常压盐酸浸出、氯化焙烧、氯化离析-磁选等工艺提取红土矿中的镍钴,并研究了矿相重构对红土矿中镍、钴等元素提取行为的影响机理。
在热力学理论分析的基础上,对常压盐酸浸出红土矿中镍、钴等有价金属进行工艺研究。结果表明,矿料粒度为-0.15 mm,初始酸浓度8 mol/L,浸出温度353 K,固液比S／L=1：4,搅拌速度300 r/min,反应时间2 h,镍、钴、锰、铁、镁的浸出率分别达到93.94%、60.5%、94%、56%、94%。由于在红土矿矿相中,几乎所有的镍和大部分的钻存在铁矿物的矿相中,因此铁的浸出与镍的浸出具有很好的相关性；而钴由于有相当一部分存在于硅酸盐中,因此,钴的浸出率较低并且与铁浸出的相关性较差。动力学实验研究结果表明镍、钴、锰浸出过程动力学符合未反应收缩核模型,属于固膜扩散控制,镍、钴、锰浸出活化能分别为11.56 kJ/mol、11.26 kJ/mol、10.77 kJ/mol。矿石中各主要矿相溶解的优先顺序为：针铁矿矿相>利蛇纹石矿相>磁铁矿矿相≥赤铁矿矿相。
根据热力学计算,氯化焙烧可以选择性的提取红土矿中的镍、钴,并实现有价金属与杂质金属的分离。实验表明,低温通入氯化氢气体进行氯化焙烧可以有效提取镍钴并抑制铁的浸出,其最佳工艺为：矿物粒度为-0.074 mm,焙烧温度300℃,氯化氢气体流速不小于80 mL·min-1,焙烧时间不少于30 min,镍浸出率可达80.6%,钴浸出率为60%,镍铁比相对原矿提高了约15倍,镍镁比相对原矿提高了约8倍。中温氯盐焙烧实验表明,加入固体氯化剂进行焙烧同样可以有效提取镍钴,并抑制杂质铁的浸出,其最佳工艺条件为：矿物粒度为-0.074 mm,以氯化钠和六水氯化镁复配盐作为氯化剂(质量比0.4),其加入量为矿料的18%,焙烧温度900℃,焙烧时间1.5 h,镍浸出率可达85%,钴浸出率为60%,镍铁比相对原矿提高了约20倍,镍镁比相对原矿提高了约15倍。动力学实验结果表明镍、钴的氯化反应属于未反应收缩核模型,镍和钴的氯化反应表观活化能分别为16.469 kJ/mol和32.792 kJ/mol。氯化机理研究结果表明以氯化钠和六水氯化镁复配盐作为氯化剂(质量比0.4)氯化效果最好是由于复配盐具有更低的共熔点温度,可以使氯化剂在较低温度熔化渗入矿料内部,并且能够在较宽温度范围内产生氯化氢气体,避免了集中释放而无法有效氯化有价金属。
氯化离析实验结果表明,选择合适氯化剂、控制还原剂用量及反应温度,主要发生镍的离析反应。通过磁场强度实验发现,在湿式磁选中,先用强磁场再用弱磁场对离析后的碚砂磁选,可以得到品位符合要求的镍钴富集物。氯化离析-磁选工艺相关条件实验结果表明：以-0.074mm矿料为原料,以NaCl+MgCl2·6H2O(质量比0.4)为氯化剂,用量为6%,以粒度为-0.2 mm烟煤作为还原剂,用量为2%,离析温度1000℃,离析时间90 min,磁场强度(先用强磁场为3000 Gs,再用弱磁场1000 Gs)进行氯化离析-磁选实验,得到磁选镍精矿。其工艺指标为镍品位5.79%,镍回收率87.69%,钴品位0.187%,钴回收率69.02%。
对红土矿在不同温度下进行活化焙烧使其发生矿相重构,实验发现矿相中原有的自由水和键合水被分解掉,以及部分矿相的晶型如FeO(OH)在300℃和Mg3[Si2O5(OH)4]在610℃发生脱水反应,导致矿物原有结构的崩塌,比表面积和孔隙增加。当预焙烧温度提高到700℃、800℃时,小颗粒重新团聚成大颗粒,导致比表面积减小,并且发生无定型硅酸镁矿相重构结晶形成镁橄榄石(Mg2SiO4)和顽辉石(MgSiO3)。对比不同温度下预焙烧料和原矿在常压盐酸浸出、氯化焙烧以及氯化离析-磁选实验中镍、钴等浸出率的不同,发现在300℃FeO(OH)的脱水反应使原来存在于铁矿相中的镍钴更多的暴露于反应界面,提高镍、钴在常压盐酸浸出中浸出率的同时抑制铁的浸出,而在610℃发生的Mg3[Si2O5(OH)4]脱水反应使整个矿物达到最大的比表面积,该温度下预焙烧料有利于增加低温通入氯化氢气体焙烧实验中气固反应界面,提高了镍钴浸出率。而中温氯盐焙烧以及氯化离析-磁选实验中氯化剂产生氯化作用的时间较长,导致矿相在未氯化前即开始转变,因此在300℃和610℃下预焙烧未对镍钴的提取产生显著的积极作用。由于在700℃和800℃预焙烧会导致无定型硅酸镁重新结晶,在形成镁橄榄石过程中镍、钴会变得不稳定而进入到硅酸镁盐形成(Mg,Ni)3SiO2并且重结晶形成橄榄石型,不利于其被提取,因此,在此两个温度下预焙烧不利于常压盐酸浸出、氯化焙烧和氯化离析-磁选等过程镍钴的提取。
本研究提出了以氯化物为提取介质,分别采用常压盐酸浸出、氯化焙烧和氯化离析-磁选等工艺提取红土矿中镍钴等有价金属,形成三套适应于不同目的需求的镍钴提取技术原型。并且氯化焙烧、氯化离析-磁选工艺可以选择性的提取镍钴并抑制铁、镁的提取,显著降低了药剂的使用量和后续净化过程的处理量。这对储量丰富的红土镍矿资源的开发利用具有重要意义。
To avoid disadvantange of traditional leaching conditions and extract nickel and cobalt more effectively, this paper studied some extraction conditions in chloride medium, such as the atmospheric (acid) leaching, chloridizing roasting and chloridizing segregation. The effect and mechanism of mineral phase reconstruction on the extraction behavior of nickel and cobalt from laterite in these extraction conditions are discussed in detail.
Based on the analysis of thermodynamics, the atmospheric HCl acid leaching conditions are studied. The optimal conditions are that the particle size of laterite is-0.15 mm, initial hydrochloric acid concentration is 8 mol/L, reaction temperature is 353 K, solid/liquid ratio is 1:4, rotation rate is 300 r/min, and the leaching time is 2 h, the results show that the dissolution yields of Ni, Co, Mn, Fe and Mg can be 93.94%, 60.5%,94%,56%and 94%, respectively. Because Ni in the laterite mainly exists in the ferric mineral phase and the leaching of Ni exhibits linear correlation with iron extraction. Due that part of Co exists in silicate, the leaching of Co does not exhibit good linear correlation with iron extraction. The results of kinetics of leaching laterite show that the dissolution rates of Ni, Co and Mn accord with unreacted shrinking core models for solid film control. And the activation energy of Ni, Co and Mn are 11.56 kJ/mol,11.26 kJ/mol and 10.77 kJ/mol. And the dissolution order of different mineral phases in the laterite is that geothite>lizatdite> magnetite≥hematite.
On the basis of thermodynamic analysis, Ni and Co can be extracted selectively from laterite ore through chloridizing roasting, and impurities extraction can be suppressed. Experimental results show that low temperature chloridizing roasting by hydrogen chloride gas can effectively extract the nickel and cobalt and inhibit the iron extraction. The optimal conditions are as follows:mineral particle size is-0.074 mm, the roasting temperature is 300℃, hydrogen chloride gas flow rate is not less than 80 mL·min-1, the roasting time is not less than 30 min, nickel leaching rate is up to about 80.6% and cobalt leaching rate is about 60%. Ni/Fe molar ratio is about 15 times than that of raw ore, and Ni/Mg molar ratio is about 8 times than that of raw ore. The chloridizing roasting experiments in the intermediate temperature show that nickel and cobalt can be extracted effectively with solid chlorinating agent used and the leaching of iron can be inhibited. The optimum conditions are that mineral particle size is-0.074 mm, the mixture of NaCl and MgCl2·6H2O is chlorinating agent (mass ratio 0.4), the addition of chlorinating agent are 18% of the ore, the roasting temperature is 900℃, the roasting time is 1.5 h, the leaching rate of nickel is up to about 85% and the leaching rate of cobalt is about 60%. The Ni/Fe ratio is about 20 times than that of raw ore, the Ni/Mg ratio is 15 times than that of raw ore. Kinetic experiments show that the chloride reaction of nickel and cobalt belongs to the unreacted shrinking core model. The chloride reaction apparent activation energy of nickel and cobalt are 16.469 kJ/mol and 32.792 kJ/mol, respectively. The mixture of NaCl and MgCl2·6H2O (mass ratio 0.4) used as chloride reagent has eutectic point and can melt at relative low temperature, it favours the uniform mixing and permeation into the ore. And the chloride reagent can produce hydrogen chloride gas in a wide range temperature which avoids the release of excess hydrogen chloride gas.
Results show that chloridizing segregation of nickel is the main reaction with control of reductant dosage, chlorinating agent dosage and reaction temperature. Through a series of experiments of magnetic field strength, the desired concentrate of nickel and cobalt can be obtained through two times magnetic separation with different magnetic field strength which are 3000 Gs of the first time and 1000 Gs of the second time. The optimum conditions of chloridizing segregation and magnetic separation are that mineral particle size is-0.074 mm, the mixture of NaCl and MgCl2·6H2O is chlorinating agent (mass ratio 0.4), the addition of chlorinating agent are 6% of the ore, the particle size of bituminous coal reductant is-0.2 mm, the reductant dosage is 2% of the ore, reaction temperature is 1000℃, reaction time is 90 min, and magnetic field strength are 3000 Gs of the first time and 1000 Gs of the second time, the grade of nickel and cobalt can be 5.78% and 0.187% respectively and the extraction of nickel and cobalt could reach 87.69% and 69.02% respectively.
The roasting of laterite ores under atmospheric pressure at different temperatures can lead to the release of free water and bound water, dehydroxylation of goethite at 300℃and lizardite at 610℃respectively, which can lead to the change and reconstruction of the structure of original mineral and more fine pores and scraps on the surface of ore roasted can be found. As roasting temperature increases to 700℃and even 800℃, some fine particles reunite together which lead the decrease of specific surface area, and the amorphous magnesium silicate phase appears to have recrystallised as forsterite (Mg2Si04) and enstatite (MgSiO3). Compared with difference of leaching rate of nickel and cobalt between raw ore and roasted ore in atmospheric (acid) leaching, chloridizing roasting and chloridizing segregation, it can be seen that ore roasted at 300℃can make more nickel is exposed to the reaction interface which benefit the leaching of nickel and cobalt, at the same time, the leaching of iron is suppressed. And raw ore is roasted at 610℃, the main mineral lizardite (Mg3Si2(OH)4O5) begins to discompose and leads to mineral structure destroyed, the specific surface area attains the maximum, which benefit gas-solid reaction in the low temperature chloridizing roasting by hydrogen chloride gas and increase the leaching rate of nickel and cobalt. There is no significant effect on the extraction of nickel and cobalt through pre-roasting at 300℃and 610℃in chloridizing roasting at intermediate temperature and chloridizing segregation because the mineral phase have reconstructed before chloridizing reaction. When roasting temperature increases to 700℃and 800℃, it lead to the incorporation of nickel into the magnesium silicate phase (Mg,Ni)3Si02 followed by recrystallisation into the forsterite phase which appears to be detrimental to the nickel recovery. Thereafter, pre-roasting at 700℃and 800℃do not benefit for nickel recovery in the atmospheric (acid) leaching, chloridizing roasting and chloridizing segregation.
In conclusion, the present processes proposed for nickel and cobalt extraction from laterite in chloride medium have been studied comprehensively in this paper. Three kinds of technology prototype are established for different target products. And the nickel and cobalt can be extracted selectively through chloridizing roasting and chloridizing segregation-magnetic separation which can decrease the addition of reagent and disposal in subsequent purification process. It is particularly significant in the exploitation of rich reserves of laterite.
在热力学理论分析的基础上,对常压盐酸浸出红土矿中镍、钴等有价金属进行工艺研究。结果表明,矿料粒度为-0.15 mm,初始酸浓度8 mol/L,浸出温度353 K,固液比S／L=1：4,搅拌速度300 r/min,反应时间2 h,镍、钴、锰、铁、镁的浸出率分别达到93.94%、60.5%、94%、56%、94%。由于在红土矿矿相中,几乎所有的镍和大部分的钻存在铁矿物的矿相中,因此铁的浸出与镍的浸出具有很好的相关性；而钴由于有相当一部分存在于硅酸盐中,因此,钴的浸出率较低并且与铁浸出的相关性较差。动力学实验研究结果表明镍、钴、锰浸出过程动力学符合未反应收缩核模型,属于固膜扩散控制,镍、钴、锰浸出活化能分别为11.56 kJ/mol、11.26 kJ/mol、10.77 kJ/mol。矿石中各主要矿相溶解的优先顺序为：针铁矿矿相>利蛇纹石矿相>磁铁矿矿相≥赤铁矿矿相。
根据热力学计算,氯化焙烧可以选择性的提取红土矿中的镍、钴,并实现有价金属与杂质金属的分离。实验表明,低温通入氯化氢气体进行氯化焙烧可以有效提取镍钴并抑制铁的浸出,其最佳工艺为：矿物粒度为-0.074 mm,焙烧温度300℃,氯化氢气体流速不小于80 mL·min-1,焙烧时间不少于30 min,镍浸出率可达80.6%,钴浸出率为60%,镍铁比相对原矿提高了约15倍,镍镁比相对原矿提高了约8倍。中温氯盐焙烧实验表明,加入固体氯化剂进行焙烧同样可以有效提取镍钴,并抑制杂质铁的浸出,其最佳工艺条件为：矿物粒度为-0.074 mm,以氯化钠和六水氯化镁复配盐作为氯化剂(质量比0.4),其加入量为矿料的18%,焙烧温度900℃,焙烧时间1.5 h,镍浸出率可达85%,钴浸出率为60%,镍铁比相对原矿提高了约20倍,镍镁比相对原矿提高了约15倍。动力学实验结果表明镍、钴的氯化反应属于未反应收缩核模型,镍和钴的氯化反应表观活化能分别为16.469 kJ/mol和32.792 kJ/mol。氯化机理研究结果表明以氯化钠和六水氯化镁复配盐作为氯化剂(质量比0.4)氯化效果最好是由于复配盐具有更低的共熔点温度,可以使氯化剂在较低温度熔化渗入矿料内部,并且能够在较宽温度范围内产生氯化氢气体,避免了集中释放而无法有效氯化有价金属。
氯化离析实验结果表明,选择合适氯化剂、控制还原剂用量及反应温度,主要发生镍的离析反应。通过磁场强度实验发现,在湿式磁选中,先用强磁场再用弱磁场对离析后的碚砂磁选,可以得到品位符合要求的镍钴富集物。氯化离析-磁选工艺相关条件实验结果表明：以-0.074mm矿料为原料,以NaCl+MgCl2·6H2O(质量比0.4)为氯化剂,用量为6%,以粒度为-0.2 mm烟煤作为还原剂,用量为2%,离析温度1000℃,离析时间90 min,磁场强度(先用强磁场为3000 Gs,再用弱磁场1000 Gs)进行氯化离析-磁选实验,得到磁选镍精矿。其工艺指标为镍品位5.79%,镍回收率87.69%,钴品位0.187%,钴回收率69.02%。
对红土矿在不同温度下进行活化焙烧使其发生矿相重构,实验发现矿相中原有的自由水和键合水被分解掉,以及部分矿相的晶型如FeO(OH)在300℃和Mg3[Si2O5(OH)4]在610℃发生脱水反应,导致矿物原有结构的崩塌,比表面积和孔隙增加。当预焙烧温度提高到700℃、800℃时,小颗粒重新团聚成大颗粒,导致比表面积减小,并且发生无定型硅酸镁矿相重构结晶形成镁橄榄石(Mg2SiO4)和顽辉石(MgSiO3)。对比不同温度下预焙烧料和原矿在常压盐酸浸出、氯化焙烧以及氯化离析-磁选实验中镍、钴等浸出率的不同,发现在300℃FeO(OH)的脱水反应使原来存在于铁矿相中的镍钴更多的暴露于反应界面,提高镍、钴在常压盐酸浸出中浸出率的同时抑制铁的浸出,而在610℃发生的Mg3[Si2O5(OH)4]脱水反应使整个矿物达到最大的比表面积,该温度下预焙烧料有利于增加低温通入氯化氢气体焙烧实验中气固反应界面,提高了镍钴浸出率。而中温氯盐焙烧以及氯化离析-磁选实验中氯化剂产生氯化作用的时间较长,导致矿相在未氯化前即开始转变,因此在300℃和610℃下预焙烧未对镍钴的提取产生显著的积极作用。由于在700℃和800℃预焙烧会导致无定型硅酸镁重新结晶,在形成镁橄榄石过程中镍、钴会变得不稳定而进入到硅酸镁盐形成(Mg,Ni)3SiO2并且重结晶形成橄榄石型,不利于其被提取,因此,在此两个温度下预焙烧不利于常压盐酸浸出、氯化焙烧和氯化离析-磁选等过程镍钴的提取。
本研究提出了以氯化物为提取介质,分别采用常压盐酸浸出、氯化焙烧和氯化离析-磁选等工艺提取红土矿中镍钴等有价金属,形成三套适应于不同目的需求的镍钴提取技术原型。并且氯化焙烧、氯化离析-磁选工艺可以选择性的提取镍钴并抑制铁、镁的提取,显著降低了药剂的使用量和后续净化过程的处理量。这对储量丰富的红土镍矿资源的开发利用具有重要意义。
To avoid disadvantange of traditional leaching conditions and extract nickel and cobalt more effectively, this paper studied some extraction conditions in chloride medium, such as the atmospheric (acid) leaching, chloridizing roasting and chloridizing segregation. The effect and mechanism of mineral phase reconstruction on the extraction behavior of nickel and cobalt from laterite in these extraction conditions are discussed in detail.
Based on the analysis of thermodynamics, the atmospheric HCl acid leaching conditions are studied. The optimal conditions are that the particle size of laterite is-0.15 mm, initial hydrochloric acid concentration is 8 mol/L, reaction temperature is 353 K, solid/liquid ratio is 1:4, rotation rate is 300 r/min, and the leaching time is 2 h, the results show that the dissolution yields of Ni, Co, Mn, Fe and Mg can be 93.94%, 60.5%,94%,56%and 94%, respectively. Because Ni in the laterite mainly exists in the ferric mineral phase and the leaching of Ni exhibits linear correlation with iron extraction. Due that part of Co exists in silicate, the leaching of Co does not exhibit good linear correlation with iron extraction. The results of kinetics of leaching laterite show that the dissolution rates of Ni, Co and Mn accord with unreacted shrinking core models for solid film control. And the activation energy of Ni, Co and Mn are 11.56 kJ/mol,11.26 kJ/mol and 10.77 kJ/mol. And the dissolution order of different mineral phases in the laterite is that geothite>lizatdite> magnetite≥hematite.
On the basis of thermodynamic analysis, Ni and Co can be extracted selectively from laterite ore through chloridizing roasting, and impurities extraction can be suppressed. Experimental results show that low temperature chloridizing roasting by hydrogen chloride gas can effectively extract the nickel and cobalt and inhibit the iron extraction. The optimal conditions are as follows:mineral particle size is-0.074 mm, the roasting temperature is 300℃, hydrogen chloride gas flow rate is not less than 80 mL·min-1, the roasting time is not less than 30 min, nickel leaching rate is up to about 80.6% and cobalt leaching rate is about 60%. Ni/Fe molar ratio is about 15 times than that of raw ore, and Ni/Mg molar ratio is about 8 times than that of raw ore. The chloridizing roasting experiments in the intermediate temperature show that nickel and cobalt can be extracted effectively with solid chlorinating agent used and the leaching of iron can be inhibited. The optimum conditions are that mineral particle size is-0.074 mm, the mixture of NaCl and MgCl2·6H2O is chlorinating agent (mass ratio 0.4), the addition of chlorinating agent are 18% of the ore, the roasting temperature is 900℃, the roasting time is 1.5 h, the leaching rate of nickel is up to about 85% and the leaching rate of cobalt is about 60%. The Ni/Fe ratio is about 20 times than that of raw ore, the Ni/Mg ratio is 15 times than that of raw ore. Kinetic experiments show that the chloride reaction of nickel and cobalt belongs to the unreacted shrinking core model. The chloride reaction apparent activation energy of nickel and cobalt are 16.469 kJ/mol and 32.792 kJ/mol, respectively. The mixture of NaCl and MgCl2·6H2O (mass ratio 0.4) used as chloride reagent has eutectic point and can melt at relative low temperature, it favours the uniform mixing and permeation into the ore. And the chloride reagent can produce hydrogen chloride gas in a wide range temperature which avoids the release of excess hydrogen chloride gas.
Results show that chloridizing segregation of nickel is the main reaction with control of reductant dosage, chlorinating agent dosage and reaction temperature. Through a series of experiments of magnetic field strength, the desired concentrate of nickel and cobalt can be obtained through two times magnetic separation with different magnetic field strength which are 3000 Gs of the first time and 1000 Gs of the second time. The optimum conditions of chloridizing segregation and magnetic separation are that mineral particle size is-0.074 mm, the mixture of NaCl and MgCl2·6H2O is chlorinating agent (mass ratio 0.4), the addition of chlorinating agent are 6% of the ore, the particle size of bituminous coal reductant is-0.2 mm, the reductant dosage is 2% of the ore, reaction temperature is 1000℃, reaction time is 90 min, and magnetic field strength are 3000 Gs of the first time and 1000 Gs of the second time, the grade of nickel and cobalt can be 5.78% and 0.187% respectively and the extraction of nickel and cobalt could reach 87.69% and 69.02% respectively.
The roasting of laterite ores under atmospheric pressure at different temperatures can lead to the release of free water and bound water, dehydroxylation of goethite at 300℃and lizardite at 610℃respectively, which can lead to the change and reconstruction of the structure of original mineral and more fine pores and scraps on the surface of ore roasted can be found. As roasting temperature increases to 700℃and even 800℃, some fine particles reunite together which lead the decrease of specific surface area, and the amorphous magnesium silicate phase appears to have recrystallised as forsterite (Mg2Si04) and enstatite (MgSiO3). Compared with difference of leaching rate of nickel and cobalt between raw ore and roasted ore in atmospheric (acid) leaching, chloridizing roasting and chloridizing segregation, it can be seen that ore roasted at 300℃can make more nickel is exposed to the reaction interface which benefit the leaching of nickel and cobalt, at the same time, the leaching of iron is suppressed. And raw ore is roasted at 610℃, the main mineral lizardite (Mg3Si2(OH)4O5) begins to discompose and leads to mineral structure destroyed, the specific surface area attains the maximum, which benefit gas-solid reaction in the low temperature chloridizing roasting by hydrogen chloride gas and increase the leaching rate of nickel and cobalt. There is no significant effect on the extraction of nickel and cobalt through pre-roasting at 300℃and 610℃in chloridizing roasting at intermediate temperature and chloridizing segregation because the mineral phase have reconstructed before chloridizing reaction. When roasting temperature increases to 700℃and 800℃, it lead to the incorporation of nickel into the magnesium silicate phase (Mg,Ni)3Si02 followed by recrystallisation into the forsterite phase which appears to be detrimental to the nickel recovery. Thereafter, pre-roasting at 700℃and 800℃do not benefit for nickel recovery in the atmospheric (acid) leaching, chloridizing roasting and chloridizing segregation.
In conclusion, the present processes proposed for nickel and cobalt extraction from laterite in chloride medium have been studied comprehensively in this paper. Three kinds of technology prototype are established for different target products. And the nickel and cobalt can be extracted selectively through chloridizing roasting and chloridizing segregation-magnetic separation which can decrease the addition of reagent and disposal in subsequent purification process. It is particularly significant in the exploitation of rich reserves of laterite.
引文
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