从含钒钢渣中富集钒的研究
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摘要
转炉钢渣是钢铁工业“三废”之一,我国转炉钢渣利用率仅50%,与发达国家差距较大。普通钢渣经处理可作冶金原料、水泥、路基材料等建筑用料和磷肥。攀钢转炉渣含V_2O_5为1~3%,比含钒煤矸石中的钒含量(V_2O_5 1%左右)还高,如果直接以处理普通转炉渣的方式处理,将造成很大的资源浪费。由于该渣含较高的CaO,使其中的钒难以回收利用。虽然从钒渣中提钒的工艺比较成熟,但由于钠盐及酸的耗量大,其工艺并不适合于含V_2O_5低,含CaO高的钢渣。因此需要开发新的工艺来提取低钒钢渣中的含钒组分并有效利用提钒后剩余的其它成分。
本文研究了钒在钢渣中的分布和用碳热还原法提取含钒钢渣中钒的可行性,以及不同渣成分、碱度、CaF_2的添加量、温度、恒温时间等因素对还原过程的影响,另外从理论上分析了分离含钒铁合金中钒磷的可行性。
钒在钢渣中的分布受钒含量和钢渣成分的影响。本实验用的原始钢渣,钒主要存在于石灰固溶体和Ca_3SiO_5中;含3.4%V_2O_5的合成渣,钒氧化物主要存在于Ca_3SiO_5相中;含6.0%V_2O_5的合成渣,钒氧化物主要存在于CaV_2O_6-Ca_2P_2O_7固溶体相中,其中V_2O_5含量高达30%;当V_2O_5含量大于6.0%时,钒则主要存在于钙钛钒氧化物相中。
将不同成分的含钒转炉渣配加石墨粉后在1873K恒温60min,得到了金属相和渣相。当R = 0.91,Al_2O_3含量为22.6%时,钒、磷在铁-渣之间的分配比分别为45、26;当R= 0.34,Al2O3含量为11.6%时,钒、磷在铁-渣之间的分配比分别为15、48;当碱度为1左右时,适当提高渣中Al_2O_3含量可以增大钒在铁-渣之间的分配比。碱度对还原的影响较大, R=1.5时钒的回收率最高,达到91.6%,随碱度的增大回收率逐渐降低,R=3时达到最低为73.9%,当R>3时回收率随碱度增加而增加。随着渣中CaF_2添加量的增加,钒、锰、磷在铁-渣之间的分配比逐渐增大,当添加量为3%时分配比达到最大,但到4%时分配比减小。
随着温度升高,钒、锰、磷在铁-渣之间的分配比逐渐增大。
还原后的渣进行XRD分析表明其主要物相是Ca_2SiO_4、Ca_3SiO_5、硅铝酸钙和铝酸钙,可以作为硅酸盐工业的原料和冶金工业的添加剂加以利用。
还原所得金属进行XRD分析表明:钒主要以Fe_2SiV形式存在,磷以FeP_4、FeSi_4P_4形式存在,锰以Fe_2MnSi形式存在,铁除了以上述几种形式存在外,另外还以Fe_3C、C-Fe-Si以及Fe形式存在。可以通过(CaO+MgO)-FeO-SiO_2渣系对含钒铁合金进行氧化精炼或利用钠化焙烧对含钒铁合金中的钒磷进行分离。通过以上的研究可知,利用碳热还原法提取含钒钢渣中的钒是可行的。
Converter slag is the one of three industrial wastes. Utilization ratio of steel slag is only 50% in China, Which is less than that of developed countries. Usually steel slag is used as metallurgical materials, cement, roadbed materials, construction materials and phosphate fertilizer. Converter slags of Pangang contains 1~3% of V_2O_5. It is higher than that of vanadium-stone coal (containing about 1% V_2O_5). Valuable vanadium resource will be wasted if the converter slags is disposed directly as ordinary steel slags. It is difficult to reclaim vanadium from the slag because its higher CaO content. Techniques of extracting vanadium from steel slags is very perfect, but it is not fit for containing high CaO and low V_2O_5 slag due to very large consumption of sodium salts and acid. So it is necessary to explore novel technics to recovery vanadium from the steel slags and make use of the other remained ingredients effectivly.
This paper mainly investigated distribution of the vanadium-oxide in the as–received V-bearing converter slag and different ingredients, basicity, CaF_2, temperature, time of constant temprature effecting on distribution ratio of vanadium, phosphorus and manganese between ferroalloy and slags. The aim to prove feasibility of extracting vanadium from Panzhihua converter slags by using of carbon thermal reduction process and separating vanadium and phosphous from the obtained V-bearing ferroalloy.
The vanadium-oxide in the as–received V-bearing converter slag is distributed both in the lime solid solution and the tricalcium silicate; in the synthetic slag the vanadium-oxide was found mainly in the tricalcium silicate for the slag containing 3.4% V_2O_5, but for the slag containing 6.0% V_2O_5 the vanadium-oxide was found in the form of CaV2O6-Ca2P2O7 solid solution in which the V_2O_5 content is as high as 30%.
The slag is mixed with additive and melt at 1873K in a graphite crucible. After keeping 1 hour vanadium distribution ratios is 45 and 15, phosphorus distribution ratios is 26 and 48 between ferroalloy and slags when the slags containing Al2O3 for 22.6%, R=0.91 and the slags containing Al2O3 for 11.6%, R=0.34 respectively. More Al2O3 can enhance vanadium distribution ratio when the slags basicity is about 1. Basicity has an great effect on reducing process. Vanadium recovery rate was highest (91.6%) at R = 1.5, and it decreased to 73.9% at R = 3.0, then increased with the increasing of basicity. The distribution ratios of vanadium, phosphorus and manganese increase gradually with increasing CaF_2 percentage. The distribution ratios is the highest at 3% CaF_2, but it decreased at 4% CaF_2. The distribution ratios increase with temperature and reaction time. XRD analysis confirmed that the main phases of the remained slag after reduction were Ca2SiO4、Ca3SiO5、aluminous calcium silicate and aluminate calcium respectively. It can be used as high quality cement materials or metallurgical fluxes.
本文研究了钒在钢渣中的分布和用碳热还原法提取含钒钢渣中钒的可行性,以及不同渣成分、碱度、CaF_2的添加量、温度、恒温时间等因素对还原过程的影响,另外从理论上分析了分离含钒铁合金中钒磷的可行性。
钒在钢渣中的分布受钒含量和钢渣成分的影响。本实验用的原始钢渣,钒主要存在于石灰固溶体和Ca_3SiO_5中;含3.4%V_2O_5的合成渣,钒氧化物主要存在于Ca_3SiO_5相中;含6.0%V_2O_5的合成渣,钒氧化物主要存在于CaV_2O_6-Ca_2P_2O_7固溶体相中,其中V_2O_5含量高达30%;当V_2O_5含量大于6.0%时,钒则主要存在于钙钛钒氧化物相中。
将不同成分的含钒转炉渣配加石墨粉后在1873K恒温60min,得到了金属相和渣相。当R = 0.91,Al_2O_3含量为22.6%时,钒、磷在铁-渣之间的分配比分别为45、26;当R= 0.34,Al2O3含量为11.6%时,钒、磷在铁-渣之间的分配比分别为15、48;当碱度为1左右时,适当提高渣中Al_2O_3含量可以增大钒在铁-渣之间的分配比。碱度对还原的影响较大, R=1.5时钒的回收率最高,达到91.6%,随碱度的增大回收率逐渐降低,R=3时达到最低为73.9%,当R>3时回收率随碱度增加而增加。随着渣中CaF_2添加量的增加,钒、锰、磷在铁-渣之间的分配比逐渐增大,当添加量为3%时分配比达到最大,但到4%时分配比减小。
随着温度升高,钒、锰、磷在铁-渣之间的分配比逐渐增大。
还原后的渣进行XRD分析表明其主要物相是Ca_2SiO_4、Ca_3SiO_5、硅铝酸钙和铝酸钙,可以作为硅酸盐工业的原料和冶金工业的添加剂加以利用。
还原所得金属进行XRD分析表明:钒主要以Fe_2SiV形式存在,磷以FeP_4、FeSi_4P_4形式存在,锰以Fe_2MnSi形式存在,铁除了以上述几种形式存在外,另外还以Fe_3C、C-Fe-Si以及Fe形式存在。可以通过(CaO+MgO)-FeO-SiO_2渣系对含钒铁合金进行氧化精炼或利用钠化焙烧对含钒铁合金中的钒磷进行分离。通过以上的研究可知,利用碳热还原法提取含钒钢渣中的钒是可行的。
Converter slag is the one of three industrial wastes. Utilization ratio of steel slag is only 50% in China, Which is less than that of developed countries. Usually steel slag is used as metallurgical materials, cement, roadbed materials, construction materials and phosphate fertilizer. Converter slags of Pangang contains 1~3% of V_2O_5. It is higher than that of vanadium-stone coal (containing about 1% V_2O_5). Valuable vanadium resource will be wasted if the converter slags is disposed directly as ordinary steel slags. It is difficult to reclaim vanadium from the slag because its higher CaO content. Techniques of extracting vanadium from steel slags is very perfect, but it is not fit for containing high CaO and low V_2O_5 slag due to very large consumption of sodium salts and acid. So it is necessary to explore novel technics to recovery vanadium from the steel slags and make use of the other remained ingredients effectivly.
This paper mainly investigated distribution of the vanadium-oxide in the as–received V-bearing converter slag and different ingredients, basicity, CaF_2, temperature, time of constant temprature effecting on distribution ratio of vanadium, phosphorus and manganese between ferroalloy and slags. The aim to prove feasibility of extracting vanadium from Panzhihua converter slags by using of carbon thermal reduction process and separating vanadium and phosphous from the obtained V-bearing ferroalloy.
The vanadium-oxide in the as–received V-bearing converter slag is distributed both in the lime solid solution and the tricalcium silicate; in the synthetic slag the vanadium-oxide was found mainly in the tricalcium silicate for the slag containing 3.4% V_2O_5, but for the slag containing 6.0% V_2O_5 the vanadium-oxide was found in the form of CaV2O6-Ca2P2O7 solid solution in which the V_2O_5 content is as high as 30%.
The slag is mixed with additive and melt at 1873K in a graphite crucible. After keeping 1 hour vanadium distribution ratios is 45 and 15, phosphorus distribution ratios is 26 and 48 between ferroalloy and slags when the slags containing Al2O3 for 22.6%, R=0.91 and the slags containing Al2O3 for 11.6%, R=0.34 respectively. More Al2O3 can enhance vanadium distribution ratio when the slags basicity is about 1. Basicity has an great effect on reducing process. Vanadium recovery rate was highest (91.6%) at R = 1.5, and it decreased to 73.9% at R = 3.0, then increased with the increasing of basicity. The distribution ratios of vanadium, phosphorus and manganese increase gradually with increasing CaF_2 percentage. The distribution ratios is the highest at 3% CaF_2, but it decreased at 4% CaF_2. The distribution ratios increase with temperature and reaction time. XRD analysis confirmed that the main phases of the remained slag after reduction were Ca2SiO4、Ca3SiO5、aluminous calcium silicate and aluminate calcium respectively. It can be used as high quality cement materials or metallurgical fluxes.
引文
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