攀钢含钛高炉渣中钛组分的分离提取研究
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摘要
攀西地区蕴藏着极其丰富的钒钛磁铁矿资源,是世界著名的钒钛之都。其钒和钛以钒钛磁铁矿的形式赋存于多金属共生矿床中。钒钛磁铁矿中50%左右的钛随经选矿后的铁精矿进入高炉,钛在炼铁过程中几乎全部进入渣相,形成钛含量约20%~26%的高炉渣。现已有大量的高炉渣堆积如山,造成环境污染,资源浪费。经过几十年的科技攻关,其利用问题仍未得到解决。研究高炉渣中有价组分的提取及其利用是迫切的现实问题。
为了有效分离提取含钛高炉渣中的钛组分,本文对空冷和水淬2种含钛高炉渣的化学成分,渣相组成以及渣的微观组构进行了分析研究。结果表明,两种含钛高炉渣化学组成基本相近,渣相组成以及微观组构却差别很大,造成这种大的差异的原因主要是其冷却方式不同所致。为证明这一推论,通过对水淬含钛高炉渣的热处理研究了其相变情况,在1200℃热处理4h的水淬含钛高炉渣与空冷含钛高炉渣的XRD谱图相似,二者的相组成相同,其结晶顺序大致为钙钛矿、镁铝尖晶石、富钛透辉石、攀钛透辉石等。
热力学计算表明,含钛高炉渣中各组分与盐酸的化学反应均能自发进行。
通过试验研究确定对空冷含钛高炉渣采用酸浸-碱反应-酸浸的三步法工艺路线。在酸浸预处理阶段,当反应时间为4h、反应温度为100℃、酸渣比为1、盐酸浓度为6mol/L时,含钛高炉渣中镁、铝、钙的浸出率较高,钛的浸出率较低,可较好的实现钛组分与镁、铝、钙的初步分离。
用氢氧化钠对经酸预处理除去大部分镁铝钙等杂质而钛相对富集的滤渣进行脱硅制备富钛料过程中,优化确定了工艺参数。反应温度为100℃、反应时间为2h、碱渣比为0.5时,所制得以钙钛矿形式存在的富钛料的品位较高,其TiO2含量接近80%。同时,反应滤液中硅组分为主的滤出物通过盐酸处理得到了回收。用盐酸对所制备的富钛料进行再除杂处理发现,富钛料中少量透辉石和尖晶石等杂质除去的同时,钙钛矿被酸溶的速率也加快。
Panzhihua and Xichang area is the world-famous Vanadium and Titanium Capital for the enrichment of V-Ti magnetite resources. The Vanadium and Ttitanium resources hosted in the polymetallic paragentic mineral deposits in the form of V-Ti magnetite. About 50% titanium in the V-Ti magnetite enter into the concentrate iron ore during the Mineral Separation, after the blast-furnace slag is smelted, which nearly all enter into the Ti-bearing blast furnace slag containing 20～26%TiO2. At present, a large number of slags have been piled up resulting in environmental pollution and resources waste. Although decades of researches and efforts, the utilization of the slags has not been given. Therefore, it is an urgent practical problem to study the extraction and utilization of valuable components from the blast-furnace slags.
In order to extract the titanium components from the blast furnace slag effectively, the chemical composition, phase composition and microstructure of air-cooled and water-quenched blast furnace slags are analyzed and investigated. The results show that the two kinds of slags have similar chemical compositions. However, there are big differences in the phase compositions and microstructures between the two kinds of slags, which should be caused by the different cooling ways after the slags are ejected from the slag hole. To prove this deduction, the phase transformation of water-quenched blast furnace slag by heat treatment process was investigated. XRD analysis shows that the phase compositions are the same between the air-cooled blast furnace slag and the water-quenched one which is heated at 1200℃for 4h, and the crystallization order is about that perovskite, spinel, Ti-rich diopside and Titatic pyroxene.
The Thermodynamic calculation indicates that the various components in blast furnace slag can react with hydrochloric acid spontaneously.
By the experimental research, the three-step process route of acid-alkali-acid leaching reaction is adopted to deal with the air-cooled blast furnace slag. The pretreated experiment on the Ti-bearing blast furnace slag cooled in air by the Hydrochloric acid reveals that under the conditions of reaction time keeps for 4 hours, reaction temperature keeps at 100℃, the Hydrochloric acid concentration is 6mol/L, acid/slag mass ratio keeps at 1, a higher leaching rate of magnesium, aluminum, calcium and a lower leaching rate of titanium of blast furnace slag can be obtained as well as the preparatory selective impurity is achieved.
In the above acid leaching residue, most of magnesium, alumina and calcium are removed off, and the titanium components are relatively enriched. In order to obtain Ti-rich slag, the residue then is treated by alkali leaching process to remove silicon, and the process parameters is optimized. In the process of removing silicon from the residue by alkali, where the most of magnesium, alumina and calcium are removed off, and the titanium components are relatively enriched. It is found that when the reaction temperature keeps at 100℃, reaction time keeps for 2h, alkali/slag mass ratio keeps at 0.5, the obtained Ti-enriched slag mainly occurs in the form of perovskite, which contains about 80% TiO2. In the meanwhile, the silicon components in the filtrate have been recovered by hydrochloric acid treatment process. To study the further enrichment of titanium components, the Ti-enriched slag is purified by the hydrochloric acid . The result shows that part of the diopside and spinel in slag can be removed off in the acid leaching process, at the same time, the perovskite is also participating the reaction.
为了有效分离提取含钛高炉渣中的钛组分,本文对空冷和水淬2种含钛高炉渣的化学成分,渣相组成以及渣的微观组构进行了分析研究。结果表明,两种含钛高炉渣化学组成基本相近,渣相组成以及微观组构却差别很大,造成这种大的差异的原因主要是其冷却方式不同所致。为证明这一推论,通过对水淬含钛高炉渣的热处理研究了其相变情况,在1200℃热处理4h的水淬含钛高炉渣与空冷含钛高炉渣的XRD谱图相似,二者的相组成相同,其结晶顺序大致为钙钛矿、镁铝尖晶石、富钛透辉石、攀钛透辉石等。
热力学计算表明,含钛高炉渣中各组分与盐酸的化学反应均能自发进行。
通过试验研究确定对空冷含钛高炉渣采用酸浸-碱反应-酸浸的三步法工艺路线。在酸浸预处理阶段,当反应时间为4h、反应温度为100℃、酸渣比为1、盐酸浓度为6mol/L时,含钛高炉渣中镁、铝、钙的浸出率较高,钛的浸出率较低,可较好的实现钛组分与镁、铝、钙的初步分离。
用氢氧化钠对经酸预处理除去大部分镁铝钙等杂质而钛相对富集的滤渣进行脱硅制备富钛料过程中,优化确定了工艺参数。反应温度为100℃、反应时间为2h、碱渣比为0.5时,所制得以钙钛矿形式存在的富钛料的品位较高,其TiO2含量接近80%。同时,反应滤液中硅组分为主的滤出物通过盐酸处理得到了回收。用盐酸对所制备的富钛料进行再除杂处理发现,富钛料中少量透辉石和尖晶石等杂质除去的同时,钙钛矿被酸溶的速率也加快。
Panzhihua and Xichang area is the world-famous Vanadium and Titanium Capital for the enrichment of V-Ti magnetite resources. The Vanadium and Ttitanium resources hosted in the polymetallic paragentic mineral deposits in the form of V-Ti magnetite. About 50% titanium in the V-Ti magnetite enter into the concentrate iron ore during the Mineral Separation, after the blast-furnace slag is smelted, which nearly all enter into the Ti-bearing blast furnace slag containing 20～26%TiO2. At present, a large number of slags have been piled up resulting in environmental pollution and resources waste. Although decades of researches and efforts, the utilization of the slags has not been given. Therefore, it is an urgent practical problem to study the extraction and utilization of valuable components from the blast-furnace slags.
In order to extract the titanium components from the blast furnace slag effectively, the chemical composition, phase composition and microstructure of air-cooled and water-quenched blast furnace slags are analyzed and investigated. The results show that the two kinds of slags have similar chemical compositions. However, there are big differences in the phase compositions and microstructures between the two kinds of slags, which should be caused by the different cooling ways after the slags are ejected from the slag hole. To prove this deduction, the phase transformation of water-quenched blast furnace slag by heat treatment process was investigated. XRD analysis shows that the phase compositions are the same between the air-cooled blast furnace slag and the water-quenched one which is heated at 1200℃for 4h, and the crystallization order is about that perovskite, spinel, Ti-rich diopside and Titatic pyroxene.
The Thermodynamic calculation indicates that the various components in blast furnace slag can react with hydrochloric acid spontaneously.
By the experimental research, the three-step process route of acid-alkali-acid leaching reaction is adopted to deal with the air-cooled blast furnace slag. The pretreated experiment on the Ti-bearing blast furnace slag cooled in air by the Hydrochloric acid reveals that under the conditions of reaction time keeps for 4 hours, reaction temperature keeps at 100℃, the Hydrochloric acid concentration is 6mol/L, acid/slag mass ratio keeps at 1, a higher leaching rate of magnesium, aluminum, calcium and a lower leaching rate of titanium of blast furnace slag can be obtained as well as the preparatory selective impurity is achieved.
In the above acid leaching residue, most of magnesium, alumina and calcium are removed off, and the titanium components are relatively enriched. In order to obtain Ti-rich slag, the residue then is treated by alkali leaching process to remove silicon, and the process parameters is optimized. In the process of removing silicon from the residue by alkali, where the most of magnesium, alumina and calcium are removed off, and the titanium components are relatively enriched. It is found that when the reaction temperature keeps at 100℃, reaction time keeps for 2h, alkali/slag mass ratio keeps at 0.5, the obtained Ti-enriched slag mainly occurs in the form of perovskite, which contains about 80% TiO2. In the meanwhile, the silicon components in the filtrate have been recovered by hydrochloric acid treatment process. To study the further enrichment of titanium components, the Ti-enriched slag is purified by the hydrochloric acid . The result shows that part of the diopside and spinel in slag can be removed off in the acid leaching process, at the same time, the perovskite is also participating the reaction.
引文
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[2]刘熙,邱克辉,张其春等.关于钒钛磁铁矿综合利用可持续发展问题的探讨[J].中国矿业大学学报,2001,10(4):21～23.
[3]易小祥,李亚伟,杨大兵.用磁选的方法从含钛高炉渣中回收碳氮化钛[J].钢铁钒钛,2008,29(4):22～25.
[4]吴本羡,孟长春,范章杰等.攀枝花钒钛磁铁矿工艺矿物学[M].四川科学技术出版社,1998.
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