H_2-CO还原钛精粉的热力学及其动力学研究
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摘要
我国钛资源储量丰富，居世界首位，其中四川约占国内的90%，具有独特的资源优势；伴随我国冶金工业机械化、现代化的快速发展，近15年来其产能一直居世界首位，这个以资源和能源消耗为主体的工业，必将直接或间接地产生大量含能气体，即H_2和CO。因此，利用H_2和CO含能气体的还原性，实现钛资源中有价金属高效分离，符合节能减排的绿色冶金发展要求，意义重大。
本文以我国钛资源和含能废气综合利用为目标，采用化学分析、扫描电镜、金相显微镜及X射线等理化手段，系统研究了钛精粉及其预氧化钛精粉在氢气、一氧化碳及其混合气条件下的还原特征及其动力学规律；并初步实现了还原产物中Ti、Fe分离，进行了有益尝试。
为了准确研究100ml·min-1流量还原气体在不同工艺参数条件下，还原产物金属化率的变化关系，本文优化了FeCl3浸出-K_2Cr_2O_7滴定法测定其金属铁含量的方法，其最佳实验参数：取样质量0.1g；FeCl3用量100ml；FeCl3浓度10g·L-1；搅拌时间60min；K_2Cr_2O_7浓度0.01N。该方法标准偏差是0.24%，与前苏联国标结果一致，符合检测要求。
综合考虑金属化率、反应时间等方面因素，钛精粉在H_2-CO条件下的最佳还原工艺参数是：混合气中氢气浓度大于50%、还原温度1150oC、还原时间90min；失重率约12%，金属化率可达87%；还原产物主要由M_3O_5固溶体和金属Fe相组成。在还原过程中，Fe和Ti的相组成主要受温度影响，Fe_2O_3低于600oC，即被还原；高于600oC，FeTiO_3才被还原为金属Fe和TiO_2，并含有TinO_2n-1；1000oC时，出现M_3O_5固溶体，其衍射峰随还原温度的升高而增强。还原温度低于1000oC，如还原气中含有一氧化碳，则还原产物可能存在单质碳或渗碳体相；超过这个温度，其衍射峰极其微弱，甚至消失。
钛精粉在氧化过程中，900oC时重量增加最显著，此时FeTiO_3被氧化为Fe_2Ti_3O_9和部分Fe_2O_3，随后重量逐渐减小，直至1200oC反应开始平衡，最终氧化产物由Fe_2TiO_5和TiO_2相组成。微观形貌分析表明钛精粉在氧化过程中，其内部产生较多不规则孔隙，其为还原气向内部扩散和生成气脱离产物表面提供良好的反应通道和空间，可以提高后续还原速率。氧化过程中产物硫含量随温度的升高而增加，直至1200oC，其脱硫率可达99%。
预氧化处理工艺不但提高了其还原过程的反应速率及还原产物金属化率，而且降低了还原温度。在H_2-CO条件下，还原产物金属化率可达93%以上，与未预氧化钛精粉的还原相比，其增加了6%。最佳还原工艺条件是混合气中氢气浓度大于50%、还原温度1100oC、还原时间80min。最终还原产物相组成与原精粉还原产物相同，即由M_3O_5固溶体和金属Fe相组成，但该固溶体中Fe含量相对较低；研究发现氢气与一氧化碳相比，预氧化处理对于提高反应速率而言，一氧化碳还原的效果显著，随其浓度的升高而增加。
本文采用扩散和界面化学反应模型研究了钛精粉及其预氧化产物的还原动力学。结果表明其还原过程符合未反应核模型，由于钛精粉的氧化作用，其还原机理不同。还原温度低于950oC，钛精粉及其预氧化钛精粉在Fe~(3+)还原为Fe~(2+)的过程中，分别受扩散和界面化学模型控制，高于此温度受扩散与界面化学反应混合控制；950-1200oC，Fe~(2+)还原为Fe时，其模型与Fe~(3+)还原为Fe~(2+)相同，其表观活化能介于59~74kJ·mol-1和48-68kJ·mol-1，随氢气浓度的增加而减小，当氢气浓度大于50%时，活化能数值比较接近，但就其总体而言，预氧化钛精粉还原的表观活化能低于原钛精粉的还原。
相组成、宏观与微观形貌分析表明预氧化钛精粉在还原过程中，除单质Fe外，Fe_2TiO_5依次被还原为FeTiO_3、TiO_2及TinO_2n-1；且混合气氧分压对数ln(PO2/Pθ)介于-14~-16之间，也证明了其相转变；最后TiO_2、TinO2n-1与Mg、Mn等氧化物固溶为M3O5固溶体。以Mn、Al为主形成的固溶体不规则地分布在颗粒边缘，阻碍还原气向反应物内部扩散及气相生成物脱离还原产物；Mg、Ti与少量Fe等元素形成的固溶体则较均匀地分布于整个颗粒，结构致密；两固溶体相均能有效降低反应物活度，减小其还原度，是金属化率降低和后期反应减速的主要原因。此外，以Ca、Si为主的元素与微量Fe等元素形成粘结相，使每个颗粒相互连接而形成一个整体。
最后本文推导出1100oC，氢气浓度大于50%时，预氧化钛精粉还原产物金属化率的预报模型，其表达式如下：
y3.1094.279t6.40610~2t23.202104t3100m Y
该预报模型较好地吻合了本文实验数据，可以定量预1测001100oC时，不同氢气/一氧化碳混合气、不同反应时间条件下预氧化钛精粉还原产物金属化率。
There exists the abundant mineral resource of titanium in China, more than90%of which deposited in province Sichuan of the country, is the richest in titaniumresource in the world. With the rapid development of mechanization andmodernization of metallurgical industry, the output, which is mainly made byconsuming of energy and resources, is biggest in the world so that it must producemuch metallurgical waste gas containing energy of hydrogen and carbon monoxide.Therefore, titanium resources and waste gas energy owned dominant positionobviously in our country. Therefore, efficient separation of multivalent metal intitamium resource is carried out by using reduction of H2and CO, which is in accordwith development of freen metallurgical requriments with saving energy andreducing pollutant smission. It is of great significance to study the above in theoryand practice.
Aiming at comprehensive utilization of titanium resources and metallurgicalwaste gas, reduction characteristics and kinetics were studied in the atmosphere ofhydrogen, carbon monoxide or their mixture gas by using chemical analysis,scanning electron microscopy, optical microscopy and X-ray diffraction and so on.We successed preliminarily in separating of titanium and iron from reductionproducts of preoxidation ilmenite concentrate. Several significative tries were donein the experimental process.
In order to investigate metallization rate of reduction products reduced bydifferent gas of100ml·min-1, the method of measuring the metal iron concentrationwas optimized by FeCl3dissolution-K_2Cr_2O_7titrmetric method. The optimal processparameters were as follows: the sample quality of0.1g, the composition andconcentration of FeCl_3of100ml and10g·L~(-1), the electromagnetic stirring time of60min, K_2Cr_2O_7concentration of0.01N. The method, standard error of which was0.24%, was consistant with national standard of early Russian and satisfied with chemical analysis.
Considering the factors of metallization rate and reaction time and so on, theoptimal reduction process parameters were obtained. As follows: hydrogenconcentration of more than50%in mixture gas, reduction temperature of1150oC,reduction time of90min. The weight loss and metallization rate can reach12%and87%respectively. The final reduction product phases contained mainly Fe and M_3O_5solid solution. Influence of reaction temperature on composition of Fe and Ti phasein the reduction process. Fe_2O_3was only reduced below600oC and FeTiO_3wasgradually reduced to Fe, TiO_2and TinO_2n-1. The intensities for M_3O_5solid solutionappeared at1000oC increased gradually with adding of reduction temperature. Thephase of carbon and ferric carbide could occur in the reduction products if reductiongas contained carbon monoxide below1000oC, or the intensities of diffractions wereweak and could disappear above1000oC.
FeTiO_3phases, weight increment of which reached maximum, were oxidized toFe_2Ti_3O_9and Fe_2O_3at900oC in the oxidation process, and then weight changedecreased gradually until oxidation products were mainly composed of Fe2TiO5andTiO2at1200oC. Microstructure evolution indicated that a lot of internal porositiesappeared in the oxidation process could provide reaction path and space forreduction gas diffusion from outside into intior and productive gas separation fromreduction products, which could raise reaction velocity. Sulphur concentrationproducts decreased with increasing of reaction temperature in the processing ofoxidation and desulphurization ratio could reach99%at1200oC.
Preoxidation treatment not only raised the reduction speed and metallizationrate of products but also decreased reaction temperature in the reduction process.Metallization rate of reduction products could reach93%and was more6%than thatfrom ilmenite concentrate by H_2-CO. The optimal reduction process parameters wereas follows: hydrogen concentration of more than50%, reaction temperature of1100oC, reduction time of80min. The final reduction product, same as that of ilmenite concentrate, consisted of iron and M3O5solid solution with less Feconcentration. The preoxidation ilmenite concentrates were reduced more quickly bycarbon monoxide than by hydrogen and the speed increased with increasing ofcarbon monoxide concentration.
The reduction kinetics of ilmenite concentrates and preoxidation products wereinvestigated by diffusion and chemical reaction model. The results shew thatreduction process satisfied unreacted ores model and reaction mechanism wasdifferent owing to oxidation of ilmenite concentrates. The reaction of Fe~(3+) Fe~(2+)inthe reduction of ilmenite concentrates and preoxidation products was controlled bydiffusion and chemical reaction model respectively below950oC, or by bothdiffusion and chemical reaction. The reaction mechanism of Fe~(3+) Fe~(2+)was same asthe above from950oC to1200oC, but the apparent activation energy of them wasfrom59to74kJ·mol-1and48to68kJ·mol-1, and decreased with the increasing ofhydrogen concentration in mixture. In general, the energy was more in the reductionof ilmenite concentrates than preoxidation products in the constant atmosphere.
The analysis of phase, macrograph and microstructure indicated that Fe2TiO5was reduced gradually to FeTiO_3, TiO_2and TinO2n-1, which was proved by oxygenpartial press with ln(PO2/Pθ) from-14to-16, then TiO_2, TinO2n-1and MgO, MnOand so on formed M_3O_5solid solution. The solid solutions, which consisted mainlyof Mn and Al and so on, appeared on outer rims or the cracks; this could inhibitdiffusing of reduction gas from outerside into intior and separating of product gasfrom the reduced samples. The solid solutions of Mg, Ti and less Fe phasesoccurred in all of particle so that the structure was dense. The formation of bothsolid solutions could decrease the activity and reduction degree of the reactant,which was main season of decreasing the metallization rate and reaction speed.Besides, the binding phases, which were informed from Ca, Si, O and less Febetween the volids of different particles, made the reduction products form thetense structure.
Forecasting model of metallization rate of preoxidation ilmenite concentrate is deduced in hydrogen of above50%at1100℃. The model is shown as following:
The forecasting model is fit with the experimental datas of the paper. It can forecast quantitatively the metallization rate of preoxidation ilmenite concentrate under the condition of different hydrogen and carbon monoxide concentration and reaction time at1100℃.
本文以我国钛资源和含能废气综合利用为目标，采用化学分析、扫描电镜、金相显微镜及X射线等理化手段，系统研究了钛精粉及其预氧化钛精粉在氢气、一氧化碳及其混合气条件下的还原特征及其动力学规律；并初步实现了还原产物中Ti、Fe分离，进行了有益尝试。
为了准确研究100ml·min-1流量还原气体在不同工艺参数条件下，还原产物金属化率的变化关系，本文优化了FeCl3浸出-K_2Cr_2O_7滴定法测定其金属铁含量的方法，其最佳实验参数：取样质量0.1g；FeCl3用量100ml；FeCl3浓度10g·L-1；搅拌时间60min；K_2Cr_2O_7浓度0.01N。该方法标准偏差是0.24%，与前苏联国标结果一致，符合检测要求。
综合考虑金属化率、反应时间等方面因素，钛精粉在H_2-CO条件下的最佳还原工艺参数是：混合气中氢气浓度大于50%、还原温度1150oC、还原时间90min；失重率约12%，金属化率可达87%；还原产物主要由M_3O_5固溶体和金属Fe相组成。在还原过程中，Fe和Ti的相组成主要受温度影响，Fe_2O_3低于600oC，即被还原；高于600oC，FeTiO_3才被还原为金属Fe和TiO_2，并含有TinO_2n-1；1000oC时，出现M_3O_5固溶体，其衍射峰随还原温度的升高而增强。还原温度低于1000oC，如还原气中含有一氧化碳，则还原产物可能存在单质碳或渗碳体相；超过这个温度，其衍射峰极其微弱，甚至消失。
钛精粉在氧化过程中，900oC时重量增加最显著，此时FeTiO_3被氧化为Fe_2Ti_3O_9和部分Fe_2O_3，随后重量逐渐减小，直至1200oC反应开始平衡，最终氧化产物由Fe_2TiO_5和TiO_2相组成。微观形貌分析表明钛精粉在氧化过程中，其内部产生较多不规则孔隙，其为还原气向内部扩散和生成气脱离产物表面提供良好的反应通道和空间，可以提高后续还原速率。氧化过程中产物硫含量随温度的升高而增加，直至1200oC，其脱硫率可达99%。
预氧化处理工艺不但提高了其还原过程的反应速率及还原产物金属化率，而且降低了还原温度。在H_2-CO条件下，还原产物金属化率可达93%以上，与未预氧化钛精粉的还原相比，其增加了6%。最佳还原工艺条件是混合气中氢气浓度大于50%、还原温度1100oC、还原时间80min。最终还原产物相组成与原精粉还原产物相同，即由M_3O_5固溶体和金属Fe相组成，但该固溶体中Fe含量相对较低；研究发现氢气与一氧化碳相比，预氧化处理对于提高反应速率而言，一氧化碳还原的效果显著，随其浓度的升高而增加。
本文采用扩散和界面化学反应模型研究了钛精粉及其预氧化产物的还原动力学。结果表明其还原过程符合未反应核模型，由于钛精粉的氧化作用，其还原机理不同。还原温度低于950oC，钛精粉及其预氧化钛精粉在Fe~(3+)还原为Fe~(2+)的过程中，分别受扩散和界面化学模型控制，高于此温度受扩散与界面化学反应混合控制；950-1200oC，Fe~(2+)还原为Fe时，其模型与Fe~(3+)还原为Fe~(2+)相同，其表观活化能介于59~74kJ·mol-1和48-68kJ·mol-1，随氢气浓度的增加而减小，当氢气浓度大于50%时，活化能数值比较接近，但就其总体而言，预氧化钛精粉还原的表观活化能低于原钛精粉的还原。
相组成、宏观与微观形貌分析表明预氧化钛精粉在还原过程中，除单质Fe外，Fe_2TiO_5依次被还原为FeTiO_3、TiO_2及TinO_2n-1；且混合气氧分压对数ln(PO2/Pθ)介于-14~-16之间，也证明了其相转变；最后TiO_2、TinO2n-1与Mg、Mn等氧化物固溶为M3O5固溶体。以Mn、Al为主形成的固溶体不规则地分布在颗粒边缘，阻碍还原气向反应物内部扩散及气相生成物脱离还原产物；Mg、Ti与少量Fe等元素形成的固溶体则较均匀地分布于整个颗粒，结构致密；两固溶体相均能有效降低反应物活度，减小其还原度，是金属化率降低和后期反应减速的主要原因。此外，以Ca、Si为主的元素与微量Fe等元素形成粘结相，使每个颗粒相互连接而形成一个整体。
最后本文推导出1100oC，氢气浓度大于50%时，预氧化钛精粉还原产物金属化率的预报模型，其表达式如下：
y3.1094.279t6.40610~2t23.202104t3100m Y
该预报模型较好地吻合了本文实验数据，可以定量预1测001100oC时，不同氢气/一氧化碳混合气、不同反应时间条件下预氧化钛精粉还原产物金属化率。
There exists the abundant mineral resource of titanium in China, more than90%of which deposited in province Sichuan of the country, is the richest in titaniumresource in the world. With the rapid development of mechanization andmodernization of metallurgical industry, the output, which is mainly made byconsuming of energy and resources, is biggest in the world so that it must producemuch metallurgical waste gas containing energy of hydrogen and carbon monoxide.Therefore, titanium resources and waste gas energy owned dominant positionobviously in our country. Therefore, efficient separation of multivalent metal intitamium resource is carried out by using reduction of H2and CO, which is in accordwith development of freen metallurgical requriments with saving energy andreducing pollutant smission. It is of great significance to study the above in theoryand practice.
Aiming at comprehensive utilization of titanium resources and metallurgicalwaste gas, reduction characteristics and kinetics were studied in the atmosphere ofhydrogen, carbon monoxide or their mixture gas by using chemical analysis,scanning electron microscopy, optical microscopy and X-ray diffraction and so on.We successed preliminarily in separating of titanium and iron from reductionproducts of preoxidation ilmenite concentrate. Several significative tries were donein the experimental process.
In order to investigate metallization rate of reduction products reduced bydifferent gas of100ml·min-1, the method of measuring the metal iron concentrationwas optimized by FeCl3dissolution-K_2Cr_2O_7titrmetric method. The optimal processparameters were as follows: the sample quality of0.1g, the composition andconcentration of FeCl_3of100ml and10g·L~(-1), the electromagnetic stirring time of60min, K_2Cr_2O_7concentration of0.01N. The method, standard error of which was0.24%, was consistant with national standard of early Russian and satisfied with chemical analysis.
Considering the factors of metallization rate and reaction time and so on, theoptimal reduction process parameters were obtained. As follows: hydrogenconcentration of more than50%in mixture gas, reduction temperature of1150oC,reduction time of90min. The weight loss and metallization rate can reach12%and87%respectively. The final reduction product phases contained mainly Fe and M_3O_5solid solution. Influence of reaction temperature on composition of Fe and Ti phasein the reduction process. Fe_2O_3was only reduced below600oC and FeTiO_3wasgradually reduced to Fe, TiO_2and TinO_2n-1. The intensities for M_3O_5solid solutionappeared at1000oC increased gradually with adding of reduction temperature. Thephase of carbon and ferric carbide could occur in the reduction products if reductiongas contained carbon monoxide below1000oC, or the intensities of diffractions wereweak and could disappear above1000oC.
FeTiO_3phases, weight increment of which reached maximum, were oxidized toFe_2Ti_3O_9and Fe_2O_3at900oC in the oxidation process, and then weight changedecreased gradually until oxidation products were mainly composed of Fe2TiO5andTiO2at1200oC. Microstructure evolution indicated that a lot of internal porositiesappeared in the oxidation process could provide reaction path and space forreduction gas diffusion from outside into intior and productive gas separation fromreduction products, which could raise reaction velocity. Sulphur concentrationproducts decreased with increasing of reaction temperature in the processing ofoxidation and desulphurization ratio could reach99%at1200oC.
Preoxidation treatment not only raised the reduction speed and metallizationrate of products but also decreased reaction temperature in the reduction process.Metallization rate of reduction products could reach93%and was more6%than thatfrom ilmenite concentrate by H_2-CO. The optimal reduction process parameters wereas follows: hydrogen concentration of more than50%, reaction temperature of1100oC, reduction time of80min. The final reduction product, same as that of ilmenite concentrate, consisted of iron and M3O5solid solution with less Feconcentration. The preoxidation ilmenite concentrates were reduced more quickly bycarbon monoxide than by hydrogen and the speed increased with increasing ofcarbon monoxide concentration.
The reduction kinetics of ilmenite concentrates and preoxidation products wereinvestigated by diffusion and chemical reaction model. The results shew thatreduction process satisfied unreacted ores model and reaction mechanism wasdifferent owing to oxidation of ilmenite concentrates. The reaction of Fe~(3+) Fe~(2+)inthe reduction of ilmenite concentrates and preoxidation products was controlled bydiffusion and chemical reaction model respectively below950oC, or by bothdiffusion and chemical reaction. The reaction mechanism of Fe~(3+) Fe~(2+)was same asthe above from950oC to1200oC, but the apparent activation energy of them wasfrom59to74kJ·mol-1and48to68kJ·mol-1, and decreased with the increasing ofhydrogen concentration in mixture. In general, the energy was more in the reductionof ilmenite concentrates than preoxidation products in the constant atmosphere.
The analysis of phase, macrograph and microstructure indicated that Fe2TiO5was reduced gradually to FeTiO_3, TiO_2and TinO2n-1, which was proved by oxygenpartial press with ln(PO2/Pθ) from-14to-16, then TiO_2, TinO2n-1and MgO, MnOand so on formed M_3O_5solid solution. The solid solutions, which consisted mainlyof Mn and Al and so on, appeared on outer rims or the cracks; this could inhibitdiffusing of reduction gas from outerside into intior and separating of product gasfrom the reduced samples. The solid solutions of Mg, Ti and less Fe phasesoccurred in all of particle so that the structure was dense. The formation of bothsolid solutions could decrease the activity and reduction degree of the reactant,which was main season of decreasing the metallization rate and reaction speed.Besides, the binding phases, which were informed from Ca, Si, O and less Febetween the volids of different particles, made the reduction products form thetense structure.
Forecasting model of metallization rate of preoxidation ilmenite concentrate is deduced in hydrogen of above50%at1100℃. The model is shown as following:
The forecasting model is fit with the experimental datas of the paper. It can forecast quantitatively the metallization rate of preoxidation ilmenite concentrate under the condition of different hydrogen and carbon monoxide concentration and reaction time at1100℃.
引文
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