云母型含钒石煤活化焙烧提钒工艺及钒转移行为研究
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摘要
钒以其优良的理化和机械性能,在冶金、宇航、化工和新能源等领域应用广泛。含钒石煤作为一种重要的钒矿资源,在我国储量丰富,从石煤中提取钒是获得V2O5的重要途径。云母型含钒石煤是主要的石煤类型,其具有分布广和储量大的特点,其中的钒多数以类质同象形式存在于云母晶格中,结构难以破坏,是一种典型的难处理含钒矿石。目前关于云母型含钒石煤的提钒过程多集中于工艺方面研究,而欠缺相应的机理分析；同时提钒工艺也存在水浸率低、环境污染严重或酸浸过程酸耗量高等问题。
因此,本文以湖北某地云母型含钒石煤为研究对象,通过寻求新型焙烧活化剂,显著降低NaCl用量并提高钒的水浸率；提出云母型含钒石煤活化焙烧-联合浸出工艺路线,降低了酸耗量并提高了钒浸出率；采用离子交换法处理混合浸出溶液,具有操作简单和提高钒回收率的特点。同时,对云母型含钒石煤活化焙烧过程中矿相变化和热力学进行了深入分析,确定钒的转移行为；探讨并研究了联合浸出过程主要元素和矿物的溶解规律,确定联合浸出的作用机理；分析并完善了联合浸出动力学及钒溶液的热力学理论,有效地指导浸出、富集及沉钒作业。
石煤提钒工艺研究表明：该云母型含钒石煤的最佳提钒工艺参数为：在焙烧温度为950℃,时间为60min,添加4%NaCl和8%K2SO4的条件下活化焙烧,焙烧熟样在温度为90℃、液固比为2.5mL/g条件下水浸45min,水浸渣经1%H2SO4在温度为30℃、液固比为2.0mL/g条件下酸浸60min,钒的水浸率为56%,酸浸率为16%,总浸率达72%；水浸液与酸浸液直接合并后,混合浸出溶液经D201树脂离子交换-酸性铵盐沉钒-煅烧脱氨作业,可获得纯度大于99%的V2O5产品,钒的回收率为70.1%。
石煤活化焙烧理论研究表明：云母型含钒石煤添加NaCl和K2SO4活化焙烧,NaCl的主要作用是加速含钒云母的品格结构破坏；K2SO4的主要作用是焙烧过程中其分解产物SO2易与含钒石煤中方解石的分解产物CaO反应生成CaSO4,从而抑制钙长石和酸溶性Ca(VO3)2的生成；另外NaCl与K2SO4的分解产物Na2O和K2O可与V2O5, A12O3、SiO2反应生成钾钠长石及水溶性的KVO3和NaVO3,从而提高钒的水浸率。焙烧热力学分析说明K2SO4分解产物SO2可与CaO反应生成CaSO4,且CaSO4的△GTθ低于钙长石,故此其会抑制钙长石矿物的生成,同时会促进钾钠长石的形成；3CaO·V2O5和Na2O·V2O5的△GTθ相近,说明若云母型含钒石煤中钙含量较高,则在焙烧过程中该两种钒酸盐可同时生成。
联合浸出过程机理分析结果表明：水浸过程是水溶性钒酸盐和其他盐类的溶解过程；水浸渣的酸浸过程包括两个部分,当硫酸浓度在1%～10%时,酸浸过程是酸溶性的钒酸钙等盐类的溶解过程；当硫酸浓度提高至20%时,酸浸过程为V(Ⅳ)氧化物和长石类矿物的化学反应过程。石煤活化焙烧熟样的颗粒形貌较为规则,多以类球体形貌存在；经水浸作业后,水浸渣呈疏松多孔形貌；水浸渣经硫酸浸出后,酸浸渣颗粒粒径明显降低,且颗粒形貌更不规则。
联合浸出动力学研究表明：水浸过程包括两个控制步骤,开始受未反应收缩核模型中的内扩散步骤控制,然后由液膜非稳态扩散模型控制；酸浸过程开始由未反应收缩核的内扩散和化学反应联合控制,建立经验动力学模型为2ln(1-η)/7+[(1-η)-2/7-1]=Kt,然后由液膜非稳态扩散模型控制,各种化学反应趋于稳定。
含钒溶液热力学研究表明：V(Ⅳ)和V(Ⅴ)是浸出溶液中钒的主要存在价态,VO2+和VO2+是其酸性条件下的主要存在形式；碱性条件下V(Ⅳ)会以HV2O5-或V4O92-形成存在,当V(Ⅴ)溶解浓度较低时,其以简单的H2VO4-\HVO42-和VO43-等阴离子形式存在,当V(Ⅴ)溶解浓度较高时,其以复杂的V4O124-、H3V2O7-、 HV6O173-、H2V6O172-和H2V10O284-等形式存在。在硫酸介质中,会有新型含钒物种如VSO4+、VOSO4和VO2SO4-的形成,同时会改变原来各物种的稳定存在区间,提高钒浸出的可能性；其为选取离子交换和酸性铵盐沉钒作为浸出液后续处理工序提供了理论基础和科学依据。
The vanadium has been widely applied in metallurgical industry, astronavigation, chemical industry and new energy due to its special physical, chemical and mechanical properties. As a kind of important vanadium mineral resources, the stone coal is distributed widely in China, so it is an important method of extracting V2O5from stone coal. The stone coal of which the vanadium exists in the muscovite is a typical kind because of its wide distribution and large reserves, where the vanadium mostly presents in the form of Ⅴ(Ⅲ) and V(IV) embedded in the crystal lattice of aluminosilicate minerals. This lattice structure is very hard to be broken down, leading to high difficulty for the extraction of vanadium from the stone coals. At present, the relevant technology researches mainly focus on the process of vanadium extraction from stone coal, but not the corresponding mechanism analysis. Furthermore, the low water leaching rate of vanadium, environment pollution and high acid consumption of leaching process are existed in the process.
Therefore, this kind of stone coal collected from Hubei was used as the research object in this article. The adding amount of sodium chloride could significantly reduce and the water leaching rate of vanadium could increase by using new roasting activators. The process of activating roasting-cooperating leaching-concentration and precipitation of vanadium was investigated in order to decrease the acid consumption and increase the leaching rate of vanadium. The operation was simple and the vanadium recovery might improve with the method of ion exchange for processing the mixed leaching solution. Furthermore, the mechanism between stone coal and additives and the transfer rule of vanadium during the roasting process were confirmed with detailed analysis of phase change and thermodynamics. The mechanism of cooperating leaching was determined by exploring and studying the dissolved law of main elements and minerals. The related leaching kinetics and thermodynamics of vanadium were investigated and improved to effectively guide the process of leaching, enrichment and precipitation.
The results of vanadium extraction technology show that the water and acid leaching rate of vanadium were56%and16%, furthermore, the total leaching rate of vanadium was more than72%under the conditions of roasting with adding4% sodium chloride and8%potassium sulfate for60min at950℃, and then leaching with water for45min at90℃with the solid-liquid ratio of2.5mL/g. The water residue was leached by using1%H2SO4for60min at30℃with the solid-liquid ratio of2.0mL/g. The vanadium recovery rate could reach70.1%and the purity of V2O5production was more than99%with the ion exchange using D201resin and vanadium precipitation using acid ammonium salt for the mixed leaching solution.
The results of mechanism analysis on roasting activation show that the main effect of NaCl was to accelerate damaging lattice structure of muscovite. The microcline and anhydrite appeared due to the reaction of SO2and CaO, and then the reaction of Na2O, K2O and V2O5, Al2O3, SiO2during roasting process with using K2SO4, which restrained and decreased the generation of anorthite and increased the water-soluble vanadate compound to enhance the water leaching rate of vanadium. The analysis of roasting thermodynamic shows that the SO2decomposed from K2SO4could react with CaO to generate CaSO4, the△GTθ of which was lower than calcium feldspar; therefore it would inhibit the generation of calcium feldspar and promote the formation of sodium potassium feldspar. The similar AGTθ of3CaO-V2O5and Na2O·V2O5suggests that the two kinds of vanadate could be generated together in the roasting process with high content of calcium in stone coal.
The results of mechanism analysis on the leaching process show that the water leaching process of vanadium included the dissolved process of water-soluble vanadate and others. The dissolved process of acid-soluble vanadate and others could take place by aicd leaching with1%-10%H2SO4. The Ⅴ(Ⅳ) could dissolve and several kinds of feldspar might be destroyed with20%H2SO4. The particle morphology of roasted sample was regular and existed in sphere shape. The water leaching slag was porous morphology. The particle morphology of acid leaching slag was more irregular and the particle size was obviously decreased.
The results of kinetics on cooperating leaching show that the control step about water leaching kinetics of roasted stone coal was divided into two stages, internal diffusion control and liquid film unsteady control. The acid leaching process was mainly affected by joint control of the chemical reaction and internal diffusion. Furthermore, the leaching kinetics for21n(1-x)/7+[(1-x)-7-1]=Kt was established. And then it was controlled by liquid membrane unsteady diffusion model, meanwhile, the chemical reactions were basically completed and stable.
The thermodynamics of vanadium solution indicate that Ⅴ(Ⅳ) and V(V) were the main existence valence vanadium in leaching solution. VO2+and VO2+were the main forms under acidic condition, but Ⅴ(Ⅳ) would form HV2O5-and V4O92-under alkaline conditions. When the concentration of dissolved V(V) was low, the simple forms such as H2VO4-, HVO42-and VO43-could appear. While the concentration of dissolved V(V) was high, the complex forms such as V4O124-, H3V2O7-, H2V6O172-and H2V10O284-would generate. In sulfuric acid medium, the new vanadium species such as VSO4+, VOSO4and VO2SO4-could form, which would change the original stability range of the species, so the possibility of vanadium leaching was improved. The thermodynamics provided the theoretical foundation and scientific basis for ion exchange and vanadium precipitation with ammonium saltammonium under acid medium as the subsequent process of leaching solution.
因此,本文以湖北某地云母型含钒石煤为研究对象,通过寻求新型焙烧活化剂,显著降低NaCl用量并提高钒的水浸率；提出云母型含钒石煤活化焙烧-联合浸出工艺路线,降低了酸耗量并提高了钒浸出率；采用离子交换法处理混合浸出溶液,具有操作简单和提高钒回收率的特点。同时,对云母型含钒石煤活化焙烧过程中矿相变化和热力学进行了深入分析,确定钒的转移行为；探讨并研究了联合浸出过程主要元素和矿物的溶解规律,确定联合浸出的作用机理；分析并完善了联合浸出动力学及钒溶液的热力学理论,有效地指导浸出、富集及沉钒作业。
石煤提钒工艺研究表明：该云母型含钒石煤的最佳提钒工艺参数为：在焙烧温度为950℃,时间为60min,添加4%NaCl和8%K2SO4的条件下活化焙烧,焙烧熟样在温度为90℃、液固比为2.5mL/g条件下水浸45min,水浸渣经1%H2SO4在温度为30℃、液固比为2.0mL/g条件下酸浸60min,钒的水浸率为56%,酸浸率为16%,总浸率达72%；水浸液与酸浸液直接合并后,混合浸出溶液经D201树脂离子交换-酸性铵盐沉钒-煅烧脱氨作业,可获得纯度大于99%的V2O5产品,钒的回收率为70.1%。
石煤活化焙烧理论研究表明：云母型含钒石煤添加NaCl和K2SO4活化焙烧,NaCl的主要作用是加速含钒云母的品格结构破坏；K2SO4的主要作用是焙烧过程中其分解产物SO2易与含钒石煤中方解石的分解产物CaO反应生成CaSO4,从而抑制钙长石和酸溶性Ca(VO3)2的生成；另外NaCl与K2SO4的分解产物Na2O和K2O可与V2O5, A12O3、SiO2反应生成钾钠长石及水溶性的KVO3和NaVO3,从而提高钒的水浸率。焙烧热力学分析说明K2SO4分解产物SO2可与CaO反应生成CaSO4,且CaSO4的△GTθ低于钙长石,故此其会抑制钙长石矿物的生成,同时会促进钾钠长石的形成；3CaO·V2O5和Na2O·V2O5的△GTθ相近,说明若云母型含钒石煤中钙含量较高,则在焙烧过程中该两种钒酸盐可同时生成。
联合浸出过程机理分析结果表明：水浸过程是水溶性钒酸盐和其他盐类的溶解过程；水浸渣的酸浸过程包括两个部分,当硫酸浓度在1%～10%时,酸浸过程是酸溶性的钒酸钙等盐类的溶解过程；当硫酸浓度提高至20%时,酸浸过程为V(Ⅳ)氧化物和长石类矿物的化学反应过程。石煤活化焙烧熟样的颗粒形貌较为规则,多以类球体形貌存在；经水浸作业后,水浸渣呈疏松多孔形貌；水浸渣经硫酸浸出后,酸浸渣颗粒粒径明显降低,且颗粒形貌更不规则。
联合浸出动力学研究表明：水浸过程包括两个控制步骤,开始受未反应收缩核模型中的内扩散步骤控制,然后由液膜非稳态扩散模型控制；酸浸过程开始由未反应收缩核的内扩散和化学反应联合控制,建立经验动力学模型为2ln(1-η)/7+[(1-η)-2/7-1]=Kt,然后由液膜非稳态扩散模型控制,各种化学反应趋于稳定。
含钒溶液热力学研究表明：V(Ⅳ)和V(Ⅴ)是浸出溶液中钒的主要存在价态,VO2+和VO2+是其酸性条件下的主要存在形式；碱性条件下V(Ⅳ)会以HV2O5-或V4O92-形成存在,当V(Ⅴ)溶解浓度较低时,其以简单的H2VO4-\HVO42-和VO43-等阴离子形式存在,当V(Ⅴ)溶解浓度较高时,其以复杂的V4O124-、H3V2O7-、 HV6O173-、H2V6O172-和H2V10O284-等形式存在。在硫酸介质中,会有新型含钒物种如VSO4+、VOSO4和VO2SO4-的形成,同时会改变原来各物种的稳定存在区间,提高钒浸出的可能性；其为选取离子交换和酸性铵盐沉钒作为浸出液后续处理工序提供了理论基础和科学依据。
The vanadium has been widely applied in metallurgical industry, astronavigation, chemical industry and new energy due to its special physical, chemical and mechanical properties. As a kind of important vanadium mineral resources, the stone coal is distributed widely in China, so it is an important method of extracting V2O5from stone coal. The stone coal of which the vanadium exists in the muscovite is a typical kind because of its wide distribution and large reserves, where the vanadium mostly presents in the form of Ⅴ(Ⅲ) and V(IV) embedded in the crystal lattice of aluminosilicate minerals. This lattice structure is very hard to be broken down, leading to high difficulty for the extraction of vanadium from the stone coals. At present, the relevant technology researches mainly focus on the process of vanadium extraction from stone coal, but not the corresponding mechanism analysis. Furthermore, the low water leaching rate of vanadium, environment pollution and high acid consumption of leaching process are existed in the process.
Therefore, this kind of stone coal collected from Hubei was used as the research object in this article. The adding amount of sodium chloride could significantly reduce and the water leaching rate of vanadium could increase by using new roasting activators. The process of activating roasting-cooperating leaching-concentration and precipitation of vanadium was investigated in order to decrease the acid consumption and increase the leaching rate of vanadium. The operation was simple and the vanadium recovery might improve with the method of ion exchange for processing the mixed leaching solution. Furthermore, the mechanism between stone coal and additives and the transfer rule of vanadium during the roasting process were confirmed with detailed analysis of phase change and thermodynamics. The mechanism of cooperating leaching was determined by exploring and studying the dissolved law of main elements and minerals. The related leaching kinetics and thermodynamics of vanadium were investigated and improved to effectively guide the process of leaching, enrichment and precipitation.
The results of vanadium extraction technology show that the water and acid leaching rate of vanadium were56%and16%, furthermore, the total leaching rate of vanadium was more than72%under the conditions of roasting with adding4% sodium chloride and8%potassium sulfate for60min at950℃, and then leaching with water for45min at90℃with the solid-liquid ratio of2.5mL/g. The water residue was leached by using1%H2SO4for60min at30℃with the solid-liquid ratio of2.0mL/g. The vanadium recovery rate could reach70.1%and the purity of V2O5production was more than99%with the ion exchange using D201resin and vanadium precipitation using acid ammonium salt for the mixed leaching solution.
The results of mechanism analysis on roasting activation show that the main effect of NaCl was to accelerate damaging lattice structure of muscovite. The microcline and anhydrite appeared due to the reaction of SO2and CaO, and then the reaction of Na2O, K2O and V2O5, Al2O3, SiO2during roasting process with using K2SO4, which restrained and decreased the generation of anorthite and increased the water-soluble vanadate compound to enhance the water leaching rate of vanadium. The analysis of roasting thermodynamic shows that the SO2decomposed from K2SO4could react with CaO to generate CaSO4, the△GTθ of which was lower than calcium feldspar; therefore it would inhibit the generation of calcium feldspar and promote the formation of sodium potassium feldspar. The similar AGTθ of3CaO-V2O5and Na2O·V2O5suggests that the two kinds of vanadate could be generated together in the roasting process with high content of calcium in stone coal.
The results of mechanism analysis on the leaching process show that the water leaching process of vanadium included the dissolved process of water-soluble vanadate and others. The dissolved process of acid-soluble vanadate and others could take place by aicd leaching with1%-10%H2SO4. The Ⅴ(Ⅳ) could dissolve and several kinds of feldspar might be destroyed with20%H2SO4. The particle morphology of roasted sample was regular and existed in sphere shape. The water leaching slag was porous morphology. The particle morphology of acid leaching slag was more irregular and the particle size was obviously decreased.
The results of kinetics on cooperating leaching show that the control step about water leaching kinetics of roasted stone coal was divided into two stages, internal diffusion control and liquid film unsteady control. The acid leaching process was mainly affected by joint control of the chemical reaction and internal diffusion. Furthermore, the leaching kinetics for21n(1-x)/7+[(1-x)-7-1]=Kt was established. And then it was controlled by liquid membrane unsteady diffusion model, meanwhile, the chemical reactions were basically completed and stable.
The thermodynamics of vanadium solution indicate that Ⅴ(Ⅳ) and V(V) were the main existence valence vanadium in leaching solution. VO2+and VO2+were the main forms under acidic condition, but Ⅴ(Ⅳ) would form HV2O5-and V4O92-under alkaline conditions. When the concentration of dissolved V(V) was low, the simple forms such as H2VO4-, HVO42-and VO43-could appear. While the concentration of dissolved V(V) was high, the complex forms such as V4O124-, H3V2O7-, H2V6O172-and H2V10O284-would generate. In sulfuric acid medium, the new vanadium species such as VSO4+, VOSO4and VO2SO4-could form, which would change the original stability range of the species, so the possibility of vanadium leaching was improved. The thermodynamics provided the theoretical foundation and scientific basis for ion exchange and vanadium precipitation with ammonium saltammonium under acid medium as the subsequent process of leaching solution.
引文
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