难处理石煤提钒工艺及相关理论研究
摘要
我国石煤资源丰富,石煤提钒具有极大的经济价值。传统的石煤提钒工艺能耗高,温室气体排放量大,环境污染严重。全湿法浸出提钒流程可有效避免温室气体大量排放,减少污染,但目前工艺存在诸如浸出速度低与钒回收率不高等缺陷；另一方面,现有石煤资源的处理难度越来越大。因此,开发高效、低排放石煤提钒技术,特别是开发难处理矿的提钒技术,对环境保护与矿产资源的综合利用意义重大。论文以难处理石煤作为研究对象,主要研究了湿法处理该种矿物的浸出过程动力学、钒的强化浸出工艺以及高铁浸出液的钒富集技术,并将实验室研究成果进行了中试试验。所获得主要的结论如下：
(1)石煤硫酸浸出过程动力学研究表明,石煤的浸出初期受表面化学反应控制,反应活化能为103.26kJ/mol;随着浸出过程的进行,浸出渣表面出现硅氧质浸出残核,硫酸需要穿过硅氧质浸出残核与内部的钒组分继续反应,反应的控制步骤逐渐由表面化学反应控制向固膜扩散控制转变。
(2)采用含氟添加剂与电磁场加热的双效强化措施,可有效提高难处理石煤中钒的浸出；强化浸出的动力学原因是外场与氟化物强化了浸出后期浸出渣表面硅氧质残核中云母相的破坏,使残核中的钒可较容易地转移到溶液中。创造性地设计了一种新型加热浸出装置,该装置加热时可产生交变电磁场,交变电磁场的采用可使钒浸出率提高2%左右。得到了一个合理的难处理石煤矿浸出工艺条件：在外场作用下采用二段逆流工艺浸出,且当每段浸出时间4h、浸出时总耗酸量55%、氟化物添加剂量1.9wt.%、温度95℃以及液固比1：1时,可获得高达83.27%的钒浸出率。但浸出液中含有大量的铁、铝等杂质离子。
(3)研究了沉淀—转溶法从高铁含钒浸出液中回收钒的工艺,结果表明：①碳酸钠直接中和沉淀富集钒工艺存在过滤困难等缺陷；②先通过还原—沉淀法得到含钒约10%的富集渣,后用碳酸钠与氢氧化钠转溶时,钒的回收率分别约为59%与69%。沉淀—转溶法的钒回收率较低。
(4)采用P204萃取工艺,可从高铁浸出液中高效回收钒。当萃取相比Vo：VA=1：1,水相电位-100mV左右,pH 2.2,两相接触时间8 min,4级萃取后,99%以上钒进入有机相；采用浓度1.5mol/L稀硫酸作反萃剂,反萃相比Vo：VA=10：1,接触时间15min,5级反萃时,反萃率可达99%以上；反萃液用氯酸钠氧化后,用氨水将溶液的pH调至1.5左右、并在95℃左右搅拌3h可沉淀出合格的多钒酸铵,沉淀效率为96.5%。当采用离子交换工艺回收沉钒母液中钒时,可进一步提高总的钒回收率。
(5)研究了工艺流程中废水的处理工艺。离子交换尾液与其它含铵废水通过石灰中和—氨吹脱—折点氯化处理后,可达标排放或循环利用；不含铵废水采用简单石灰中和处理后,可达标排放或循环利用。
(6)根据实验室研究结果,确定了一个包括硫酸强化浸出、溶剂萃取、铵盐沉钒以及离子交换回收沉钒母液中钒等工序在内的石煤提钒工业化中试生产流程,硫酸强化浸出中的强化措施主要包括电磁场加热浸出体系以及添加含氟添加剂。中试结果表明,在酸耗18%与强化浸出剂用量1.5%情况下,可获得高于68%的五氧化二钒总回收率,五氧化二钒产品的各项指标均达到GB3283-87冶金98级标准。与传统工艺相比,该湿法流程具有不排放温室气体与总钒回收率高等优点。
Our country is rich in stone coal resources, and consequently vanadium extraction from stone coal is of great economic value. The traditional vanadium extraction processes are of high energy consumption, great greenhouse gases emissions and serious environment pollution. The hydrometallurgical process of vanadium extraction can effectively avoid greenhouse gas emissions and reduce pollution, but at present, the process has its shortcoming, such as small leaching velocity and low recovery. On the other hand, it is increasingly difficult to extract vanadium from stone coal. Therefore, the development of vanadium extraction process with high efficiency and low emission, especially vanadium extraction process from refractory stone coal, are of great significance to environment protection and comprehensive utilization of mineral resources. In this paper, leaching dynamics, strenthening leaching process of refractory stone coal, separation of vanadium from leaching liquid with high iron concentration were studied; and pilot test was conducted on the base of bench experiment. The main experimental results obtained were as follows.
Sulfuric acid leaching dynamics research showed that the leaching process was controlled by surface chemical reaction in the early stage, and activation energy was 103.26 kJ/mol. With the leaching process going on, siliceous residues appeared on the surface of stone coal particles. Sulfuric acid need diffuse through siliceous residues to react with internal vanadium compound, and the controling step of the reaction gradually transformed from surface chemical reaction controlled to solid membrane diffusion controlled.
Electromagnetic field and additive were used to strengthen vanadium leaching. Research results showed that they can effectively strengthen vanadium leaching from refractory stone coal. The reason of electromagnetic field and additive strengthening vanadium leaching was that they can strengthen the destory of micas in siliceous residues, and vanadium in the micas was easier to be transferred to the solution. A new kind of heating device was designed, this device can generate alternating electromagnetic field when heating, the alternating electromagnetic field enabled vanadium leaching efficiency increase by 2% or so. The economic and reasonable leaching condition was:two stages countercurrent leaching process used, leaching time of each stage 4h, total consumption of acid 55%, fluoride addition 1.9%, temperature 95℃, liquid-solid ratio 1:1, vanadium leaching efficiency can reach 83.27%. The leachate contained lots of impurities, such as iron and aluminum.
Precipitating-dis solving method was used to purify vanadium leaching solution with high iron concentration. Results showed that:①enriching effect of direct precipitation with sodium carbonated was poor, and the filtration was slow.②precipitation containing 10%vanadium can obtained when reducing-precipitating method used. Leaching efficiency were about 59% and 69% respectively when the precipitate dissolved by sodium carbonated and sodium hydroxide. In a word, vanadium recovery was low when precipitating-dissolving method used.
Solvent extraction with P204 can efficiently seperate vanadium from iron containing leaching solution. When phase ratio Vo:VA＝1:1, solution electric potential about -100mV, pH 2.2, phase contact time 8 min,99% of vanadium entered organic phase after 4 stage extraction. When 1.5 mol/L sulphuric acid used as the stripping agent, phase ratio Vo: VA= 10:1, contact time 15min, stripping ratio reached 99% after 5 stages. The stripped solution was oxidized by sodium chlorate, adjusted pH value with ammonia solution to 1.5, and agitated at 95℃for 3h, ammonium polyvanadate can precipitate, and precipitating ratio was 96.5%. Ion exchange process was used to recover vanadium from the mother liquid after vanadium precipitation, which can increase vanadium recovery.
Treatment technology of wastewater generated in the process was studied. The ion exchange raffinate and other waste water containing ammonium can meet the discharge standard or be recyled after neutralization with lime, ammonia stripping and fold point-chlorodizing. While waste water not containing ammonium can meet the discharge standard or be recyled after neutralization with lime.
Pilot test was conducted on the base of laboratory experiment. Technics process of the pilot test contained sulfuric acid leaching, solvent extraction, vanadium precipitation with ammonium salt, vanadium recovery with ion exchange process. Vanadium leaching was strengthened with the electromagnetic field and additive. The result showed that when acid consumption 18%, leaching strengthening agent addition 1.5%, total yield of vanadium pentoxide was more than 68%, each index of vanadium pentoxide reached GB3283-87 metallurgy grade 98. Compared with other traditional processes, hydrometallurgical process can reduce environment pollution, especially avoid greenhouse gas emissions.
(1)石煤硫酸浸出过程动力学研究表明,石煤的浸出初期受表面化学反应控制,反应活化能为103.26kJ/mol;随着浸出过程的进行,浸出渣表面出现硅氧质浸出残核,硫酸需要穿过硅氧质浸出残核与内部的钒组分继续反应,反应的控制步骤逐渐由表面化学反应控制向固膜扩散控制转变。
(2)采用含氟添加剂与电磁场加热的双效强化措施,可有效提高难处理石煤中钒的浸出；强化浸出的动力学原因是外场与氟化物强化了浸出后期浸出渣表面硅氧质残核中云母相的破坏,使残核中的钒可较容易地转移到溶液中。创造性地设计了一种新型加热浸出装置,该装置加热时可产生交变电磁场,交变电磁场的采用可使钒浸出率提高2%左右。得到了一个合理的难处理石煤矿浸出工艺条件：在外场作用下采用二段逆流工艺浸出,且当每段浸出时间4h、浸出时总耗酸量55%、氟化物添加剂量1.9wt.%、温度95℃以及液固比1：1时,可获得高达83.27%的钒浸出率。但浸出液中含有大量的铁、铝等杂质离子。
(3)研究了沉淀—转溶法从高铁含钒浸出液中回收钒的工艺,结果表明：①碳酸钠直接中和沉淀富集钒工艺存在过滤困难等缺陷；②先通过还原—沉淀法得到含钒约10%的富集渣,后用碳酸钠与氢氧化钠转溶时,钒的回收率分别约为59%与69%。沉淀—转溶法的钒回收率较低。
(4)采用P204萃取工艺,可从高铁浸出液中高效回收钒。当萃取相比Vo：VA=1：1,水相电位-100mV左右,pH 2.2,两相接触时间8 min,4级萃取后,99%以上钒进入有机相；采用浓度1.5mol/L稀硫酸作反萃剂,反萃相比Vo：VA=10：1,接触时间15min,5级反萃时,反萃率可达99%以上；反萃液用氯酸钠氧化后,用氨水将溶液的pH调至1.5左右、并在95℃左右搅拌3h可沉淀出合格的多钒酸铵,沉淀效率为96.5%。当采用离子交换工艺回收沉钒母液中钒时,可进一步提高总的钒回收率。
(5)研究了工艺流程中废水的处理工艺。离子交换尾液与其它含铵废水通过石灰中和—氨吹脱—折点氯化处理后,可达标排放或循环利用；不含铵废水采用简单石灰中和处理后,可达标排放或循环利用。
(6)根据实验室研究结果,确定了一个包括硫酸强化浸出、溶剂萃取、铵盐沉钒以及离子交换回收沉钒母液中钒等工序在内的石煤提钒工业化中试生产流程,硫酸强化浸出中的强化措施主要包括电磁场加热浸出体系以及添加含氟添加剂。中试结果表明,在酸耗18%与强化浸出剂用量1.5%情况下,可获得高于68%的五氧化二钒总回收率,五氧化二钒产品的各项指标均达到GB3283-87冶金98级标准。与传统工艺相比,该湿法流程具有不排放温室气体与总钒回收率高等优点。
Our country is rich in stone coal resources, and consequently vanadium extraction from stone coal is of great economic value. The traditional vanadium extraction processes are of high energy consumption, great greenhouse gases emissions and serious environment pollution. The hydrometallurgical process of vanadium extraction can effectively avoid greenhouse gas emissions and reduce pollution, but at present, the process has its shortcoming, such as small leaching velocity and low recovery. On the other hand, it is increasingly difficult to extract vanadium from stone coal. Therefore, the development of vanadium extraction process with high efficiency and low emission, especially vanadium extraction process from refractory stone coal, are of great significance to environment protection and comprehensive utilization of mineral resources. In this paper, leaching dynamics, strenthening leaching process of refractory stone coal, separation of vanadium from leaching liquid with high iron concentration were studied; and pilot test was conducted on the base of bench experiment. The main experimental results obtained were as follows.
Sulfuric acid leaching dynamics research showed that the leaching process was controlled by surface chemical reaction in the early stage, and activation energy was 103.26 kJ/mol. With the leaching process going on, siliceous residues appeared on the surface of stone coal particles. Sulfuric acid need diffuse through siliceous residues to react with internal vanadium compound, and the controling step of the reaction gradually transformed from surface chemical reaction controlled to solid membrane diffusion controlled.
Electromagnetic field and additive were used to strengthen vanadium leaching. Research results showed that they can effectively strengthen vanadium leaching from refractory stone coal. The reason of electromagnetic field and additive strengthening vanadium leaching was that they can strengthen the destory of micas in siliceous residues, and vanadium in the micas was easier to be transferred to the solution. A new kind of heating device was designed, this device can generate alternating electromagnetic field when heating, the alternating electromagnetic field enabled vanadium leaching efficiency increase by 2% or so. The economic and reasonable leaching condition was:two stages countercurrent leaching process used, leaching time of each stage 4h, total consumption of acid 55%, fluoride addition 1.9%, temperature 95℃, liquid-solid ratio 1:1, vanadium leaching efficiency can reach 83.27%. The leachate contained lots of impurities, such as iron and aluminum.
Precipitating-dis solving method was used to purify vanadium leaching solution with high iron concentration. Results showed that:①enriching effect of direct precipitation with sodium carbonated was poor, and the filtration was slow.②precipitation containing 10%vanadium can obtained when reducing-precipitating method used. Leaching efficiency were about 59% and 69% respectively when the precipitate dissolved by sodium carbonated and sodium hydroxide. In a word, vanadium recovery was low when precipitating-dissolving method used.
Solvent extraction with P204 can efficiently seperate vanadium from iron containing leaching solution. When phase ratio Vo:VA＝1:1, solution electric potential about -100mV, pH 2.2, phase contact time 8 min,99% of vanadium entered organic phase after 4 stage extraction. When 1.5 mol/L sulphuric acid used as the stripping agent, phase ratio Vo: VA= 10:1, contact time 15min, stripping ratio reached 99% after 5 stages. The stripped solution was oxidized by sodium chlorate, adjusted pH value with ammonia solution to 1.5, and agitated at 95℃for 3h, ammonium polyvanadate can precipitate, and precipitating ratio was 96.5%. Ion exchange process was used to recover vanadium from the mother liquid after vanadium precipitation, which can increase vanadium recovery.
Treatment technology of wastewater generated in the process was studied. The ion exchange raffinate and other waste water containing ammonium can meet the discharge standard or be recyled after neutralization with lime, ammonia stripping and fold point-chlorodizing. While waste water not containing ammonium can meet the discharge standard or be recyled after neutralization with lime.
Pilot test was conducted on the base of laboratory experiment. Technics process of the pilot test contained sulfuric acid leaching, solvent extraction, vanadium precipitation with ammonium salt, vanadium recovery with ion exchange process. Vanadium leaching was strengthened with the electromagnetic field and additive. The result showed that when acid consumption 18%, leaching strengthening agent addition 1.5%, total yield of vanadium pentoxide was more than 68%, each index of vanadium pentoxide reached GB3283-87 metallurgy grade 98. Compared with other traditional processes, hydrometallurgical process can reduce environment pollution, especially avoid greenhouse gas emissions.
引文
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