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Carbothermal Reduction and Nitridation of Ilmenite Concentrates and Chlorination of the Reduced Samples

Sep 13, 2010

By S. S. Yu

In this paper, the producing process of using V2O3 as raw material to obtain vanadium nitride was analyzed through the means of thermodynamic. The analysis shows that conversion follows the principle of reduction step by step in the conversion process of V2O3. The temperature of the reaction system has prominent influence on the nitrogen content of products, and the reaction is very sensitive to temperature. As raising temperature, the fine grain structure of the nitrides is more evident, and the grain size of nitrides increases. At 1703K, the nitrogen content of the products tended to be constant after soaking over 3 hours.

Jan 1, 2014

Carbothermal Reduction of Ilmenite Concentrates and Synthetic Rutile in Different Gas Atmospheres

Sep 13, 2010

By Run Huang, Xuewei Lv, Lei Lei, Guibao Qiu, Chenguang Bai

"The TiO2-rich slag and pig iron can be produced from ilmenite concentrate by the electric furnace process. In this study, ilmenite concentrate was reduced in a vertical furnace equipped with a weighting data acquisition system. The effects of reducing agent (carbon) amount on the iron reduction were studied. The phase transformation, morphology and chemical compositions of reduced samples were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS), respectively. It was found that the reductive degree of ilmenite concentrate increased with the increase of reducing time. The phases of reduced samples were mostly iron, rutile, Ti3O5 and Fe2TiO5. The mass loss percentage increased with increasing the carbon amount from 8% to 12%. When the carbon amount exceeded 12%, the mass loss percentage decreased with the increasing of carbon amount.IntroductionIlmenite and rutile are the main raw materials for producing titania pigment and titanium metal. With the development of the titanium industry, huge amounts of titanium resources are needed. As sources of high-grade titania mineral decrease worldwide, more attention should be paid to the processes involving low grade mineral such as ilmenite ore. In ilmenite, MgO and CaO are the gangue parts. Therefore, the ilmenite refining becomes more and more popular. In the previous studies, the methods of ilmenite refining are electric furnace smelting, direct acid leaching, selective chlorination and thermal reduction [1]. Electric furnace smelting method is widely used in the titanium industry, however, which consumes a great deal of energies and has a high CO2 emission. Its essence is to remove iron oxides and obtain a high titania slag. So the thermal reduction of ilmenite concentrate is an important step in titanium industry, which can decrease carbon reagent consumption and save energy.Over the past several decades, many studies have been carried out on the mechanism and kinetics of the reduction of different ilmenite ores, which are as follows: The carbothermal reduction of Panzhihua ilmenite initiated at about 860 oC. In the temperatures ranging from 900 oC to 1400 oC, the reaction rate was changed like a shape of “M”. That was to say that the reaction rate increased with the growth of temperature at first, then decreased, afterward increased again and at last the reaction was arrested [2]. The Mohammad A.R group [3, 4] showed that the carbothermal reduction of primary ilmenite concentrate was faster in hydrogen and initiated at a lower reduced temperature than in argon and helium. The reduction in argon and helium had about the same rate and extent. Titanium oxycarbide started at 1000°C in hydrogen. The conversion of primary ilmenite concentrate to metallic iron and titanium oxycarbide at 1200 °C was completed in 300 minutes. Monoxide as the reductant to reduce ilmenite had been studied intensively by a few research groups [5, 6]. The rate and the degree of reduction depended on the formation of a metallic shell of iron which inhibited the transfer of CO to the reaction zones; titanium had a strong effect on the mechanism and rate of reduction of iron oxides. Wang and Yuan [7] studied the reductive kinetics of the reaction between a natural ilmenite and carbon. At temperature below 1100°C, chemical reaction was the rate controlling step, at 1100 to 1250°C mixed controlling was rate controlling step, above 1250°C diffusion through the product layer controlled the reaction. Zhang [8] investigated the reduction of natural, sintered and preoxidized ilmenite concentrates in hydrogen methane mixtures. Preoxidation and sintering of ilmenite concentrates changed their phase composition and caused a sharp decrease in specific surface area of raw materials and an increase in carburization temperature. Sintering also increased the metallization temperature of iron."

Jan 1, 2011

By Sutham Niyomwas

Synthesis of alumina-mullite-silicon carbide composite (Al2O3-Al6Si2O13-SiCw) was obtained in situ by carbothermal reduction of a mixture of kaolin and two different silica sources. The carbothermal reduction was carried out in a horizontal tube furnace under flow of argon gas. The standard Gibbs energy minimization method was used to calculate the equilibrium composition of the reacting species. The synthesized products were mixtures of alumina, mullite and silicon carbide in the form of whiskers. The effects of adding two different silica sources of rice husk ash and silica powder to the mixture of kaolin and activated carbon were investigated. XRD and SEM analyses indicate complete reaction of precursors to yield Al2O3- Al6Si2O13-SiC as product powders, with the SiC having whisker morphology.

Jan 1, 2006

By S. Ganguly, R. Kononov

Carbothermal reduction of manganese oxides and manganese ores in the solid state was studied in hydrogen, helium and argon at different temperatures, ore compositions and carbon to manganese oxide ratios. Wesselsore (South Africa) and two grades of the Groote Eylandt ore (Australia) with different level of impurities were examined. Ores were characterised by XRD, X-ray fluorescence, optical microscopy and scanning electronmicroscopy. Isothermal and temperature programmed carbothermal reduction experiments were conducted in a fixed bed reactor in a vertical tube furnace, with on-line monitoring of gas composition by the CO-CO2 infrared sensor. The reduced samples were characterised by XRD, SEM and LECO analyses. Extent of reduction was calculated using data on the off-gas composition, and LECO carbon and oxygen contents in the reduced sample. Manganese oxides in the ore were reduced to a-Mn and carbides Mn23C6 and Mn7C3 depending on the carbon to ore ratio. The reduction rate of manganese ores in hydrogen was higher than in helium and argon. Key words: Manganese, Carbothermal Reduction, Hydrogen, Argon, Carbon Monoxide, Helium, Kinetics.

Jan 1, 2007

By F. Awotwe-Appiah, P. Koshy, A. Y. Fosu, J. Dankwah, J. R. Dankwah

Ghana currently exports its bauxite raw without any value addition. Gradual depletion of high grade bauxite (with high alumina content) and the emergence of low grade bauxite (with high iron oxide content) calls for novel and inexpensive ways to recover alumina from these low grade ores. Bauxite users have indicated their willingness to pay 10% to 50% higher for a corresponding reduction in impurities by a similar amount. This project therefore investigates the carbothermal upgrading of the Ghana Awaso bauxite using waste polypropylene as reductant in a locally designed gas-fired furnace. Composite pellets of low grade bauxite sample (assaying 45% Al2O3) containing pulverised waste polypropylene were formed, oven dried, placed in fireclay crucible and fired for 30 minutes. The magnetic fraction after reduction was separated by a Low Intensity Magnet and weighed. It was observed that up to 97% of the iron oxides (occurring as hematite and goethite) could be separated into the magnetic fraction as magnetite leaving a nonmagnetic fraction with over 98% Al2O3 as opposed to the 45% Al2O3 in the as-received bauxite sample. This research direction provides yet another simple but effective way for simultaneously upgrading low grade bauxite and recycling waste polypropylene, whilst at the same time decreasing the amount of waste material generated as red mud after the Bayer process.

Jan 1, 2015

By Dinabandhu Ghosh

The stability diagram of the ternary system Ti-C-O is drawn in the present work for four temperatures, 1473 K, 1573 K, 1673 K and 1873 K, showing the stability fields of TiC, Ti, TiO, Ti2O3 and TiO2. An analysis of the system reveals that it is not possible to produce Ti in a carbon-saturated system; instead, the stable product is TiC. However, Ti can be an equilibrium product in a carbon-unsaturated system at prohibitively low values of pCO and pCO2; for example, at 1873 K, these limiting values are: pCO = 10-6.76 atm and pCO2 = 10-13.36 atm, which, when exceeded, produce TiC and TiO respectively. The magnesiothermic reduction is examined through the stability diagram (log pO2 vs. 1/T) of the system Ti-Mg-O, drawn for a number of pMg values, presenting the pairwise stability fields such as Mg(l) + Ti(s), Mg(v) + Ti(s), MgO(s) + Ti(s), etc. The diagram shows that magnesium reduction of TiO to Ti is possible only at T < 1641 K with pMg = 1 atm and only at T < 1569 K with pMg = 0.5 atm. An experimental scheme for Mg vapor reduction of TiO2 is proposed in which an argon stream is passed over a Mg(liquid) evaporator at temperature T1 (say, 1234 K); the resulting Ar-Mg mixture at 1 atm is subsequently flown over a bed of TiO2 at temperature T2. A thermodynamic analysis establishes that complete reduction to Ti is possible and that the best results are obtained when T1 = T2.

Jan 1, 2006

By W. K. Connor, O&apos

The Bureau of Mines has conducted beneficiation, carbothermic reduction, and leaching tests of Mn oxide ores as part of its evaluation of the Mn and Co resources of the West- Central Arkansas District. The major Mn oxides in the ore include cryptomelane, psilomelane, pyrolusite, and lithiophorite. Cobalt is contained within the Mn oxides. Nonbeneficiated ore was reduced at 800&apos; C with coal and leached in ammonium sulfate and ammonium carbonate leach liquors. Ore concentrates were calcined at 600" C prior to reduction under the same conditions as the raw ore. Head analyses reported up to 21 ptt Mn and 0.11 pct Co. Extractions of 70 to 90 pct Mn and 40 to 60 pct Co were achieved.

Jan 1, 1992

By Wei Li

Carbothermic reduction kinetics of ilmenite concentrates catalyzed by sodium chloride and the microwaveabsorbing characteristics of the resulting reductive products were investigated; the reduction degree of the reaction was deduced to be . Results show that the activation energy is 112.03 kJ/ mol when NaCl is used as catalyst, lowering to 23.11 kJ/mol for the final stage activation energy using sodium silicate as a catalyst. There is a sharp change in the reduction rate constant at temperature ranges of 1,223 K - 1,273 K and 1,373 K - 1,423 K. Microwave-absorbing characteristics of reductive products were measured by the method of microwave cavity perturbation. It was found that microwave-absorbing characteristics of reductive products obtained at temperatures of 850° C, 1,100° C and 1,150° C show sharp changes. Through X-ray diffraction (XRD) characterization, it was found that the formation of Fe occurs at a temperature of 900° C during the reduction process of ilmenite concentrate. The decrease of FeTiO3 content results in the decrease of microwave-absorbing characteristics, while the increase of Fe content gives rise to the increase of microwaveabsorbing characteristics. The decreasing trend is larger than the increasing trend, which is the main reason for the sharp changes in the microwave-absorbing characteristics of reductive products at the temperature range of 850° C to 900° C. When the decreasing trend is smaller than the increasing trend, it becomes the main reason for the sharp changes in microwave-absorbing characteristics of reductive products at the temperature range of 1,100° C to 1,150° C. Kinetics results show that sodium chloride can catalyze the carbothermic reduction of ilmenite, and microwave-absorbing characteristic investigations indicate that microwave heating can be used in the carbothermic reduction of ilmenite.

By V. A. Leão, V. S. Coimbra, V. A. A. Oliveira, R. F. M. de Souza, G. M. de Lima

A willemite concentrate consisting mainly of willemite (55.3%) and dolomite (15.6%) was reduced in a tube furnace with charcoal as reductant. The effects of temperature and varying reductant additions on zinc extraction were studied. A zinc recovery of 86% was achieved with 20% reductant in the charge at 1100°C. During reduction, the calcium oxide generated through calcination of the dolomite promoted decomposition of the willemite, thus lowering the temperature at which reduction took place. The presence of CaO improved the zinc recovery at all temperatures studied. The best zinc recovery (93%) was obtained in the presence of 5% CaO, 20% charcoal reductant, and at a temperature of 1100°C. The results show that the willemite concentrate studied has great potential to be used as a raw material for the Waelz process.

Nov 6, 2023

By Derek Caizergues, Hurman Eric

Experiments have been conducted at around 1700°C to determine the possibility of carbothermic reduction of alumina under the presence of a metallic solvent. Total pressure of the system was reduced to around 30kPa and metallic nickel, iron, copper and tin were selected as the solvent. The highest recovery of aluminium was achieved with the nickel solvent followed by iron, copper and tin. This ranking for the first three was also in accord with the extent of negative deviation form ideality in the respective binary solutions of these solvents with aluminium. The tin-aluminium system displays positive deviation form ideality. The rate and extent of reduction was found to be highly dependent on temperature and pressure. The pseudo first order reaction rate was found to be applicable to the process in all the solvents used. Rate constants were calculated and it is also suggested that the reduction was controlled primarily by the chemical reaction rate.

Jan 1, 2003

By Derek Caizergues, Hurman Eric

The principle of carbothermic reduction has been around for many years. In principle it is a simple process, yet with a multitude of problems. The temperature required to affect reduction is in the region of 2200ºC and results in aluminium oxy-carbide formation rather than metallic aluminium. From a thermodynamic point of view, reducing the temperatures of reaction which would suppress oxy-carbide formation would only be possible by lowering the total pressure of the system. A decrease in thermodynamic activity of product aluminium by dissolving it in another phase would also help preventing the formation of oxy-carbides and would also increase the yield of the reduction reaction. Thus experiments have been conducted at around 1700ºC to determine the possibility of carbothermic reduction of alumina under the presence of a metallic solvent. Total pressure of the system was reduced to around 30kPa and metallic nickel, iron, copper and tin were selected as the solvent. The highest recovery of aluminium was achieved with the nickel solvent followed by iron, copper and tin. This ranking for the first three was also in accord with the extent of negative deviation form ideality in the respective binary solutions of these solvents with aluminium. The tin-aluminium system displays positive deviation form ideality. The rate and extent of reduction was found to be highly dependent on temperature and pressure. The pseudo first order reaction rate was found to be applicable to the process in all the solvents used. Rate constants were calculated and it is also suggested that the reduction was controlled primarily by the chemical reaction rate.

Jan 1, 2003

By Animesh Jha

The carbothermic reduction of chalcopyrite has been studied in the temperature range 1073 to 1273K in presence of lime. The role of lime during the reduction process is explained and the phase equilibria leading to the metallisation of copper and iron are discussed. The effect of coal and carbon monoxide on the reduction process have been studied and the rate governing steps are identified. This investigation also cites examples of possible mechanisms of physical separation of metallic Cu from iron during the reduction process.

Jan 1, 1992

By Bing Song, Fei Xi, Xuewei Lv, Kai Zhang

The electric arc furnace process is a common method to produce high TiO2 slag from ilmenite. The pre-reduction process was proposed in recent years in order to reduce electricity consumption. In order to enhance the pre-reduction degree, high energy ball milling was proposed to improve the specific surface area of the ilmenite prior to reduction. In this study, the carbothermic reduction behavior of milled ilmenite concentrate was investigated. It was found that the ball milling method can result in a higher reduction rate and improved metallization of iron. The metallization of iron increased with increasing the time of ball milling. The metallization of iron with milling reached 89.49% when the time of ball milling was 70 min., while the FeO content decreased with 70 min. of milling from 11.84% to 4.76%.

Jan 1, 2014

By T Kitajima, T Kawaguchi, T Nakamura

Carbothermic reduction of iron oxide is an attractive mechanism to produce metallic iron, since it can directly utilise coal as both reductant and fuel. To improve energy efficiency and productivity of the metallic iron production based on this mechanism, the combustion bed process packed with the composites of iron oxide and coal powder was experimentally evaluated. The process has a potential of high heat efficiency since it can automatically utilise the heat of reduced materials as that necessary to the subsequent reduction of the composite by a large heat exchange rate between the packed particles and gas flowed across the bed. However, it is hard to perfectly prevent the reoxidation of formed metallic iron in the bed. The present paper reports the effect of coal content, pellet size and so forth on the reduction/metallisation degrees of the samples after the reduction experiment. It also discusses the effect of pretreatment of the composite pellets using CaO bearing materials to suppress the reoxidation of formed metallic iron in the bed.

Jan 1, 2000

By B. L. Chulu

In the carbothermic reduction of lead sulfate to produce lead, the inclusion of soda ash (Na,CO,) in the charge provides for the control of sulfur dioxide in the effluent gas. An important mechanism in the process appears to be the carbothermic reduction of the sodium carbonate whereby sodium gas and carbon monoxide are produced. These intermediates then participate in the reduction of the lead sulfate to produce lead metal and stable sulfur species in the molten slag phase. In addition, there is some evidence that the presence of lead metal in the charge may also serve to increase the lead recovery in the process. These aspects were investigated by conducting laboratory-scale smelting tests with small charges (;3g), at 1173°K(9000C). Recovery did not exceed 74w% and the role of incipient lead metal in the charge could not be clearly assessed.

Jan 1, 1993

By J. J. Moore

The application of plasma technology to process metallurgy is briefly discussed. Experiments involving in-flight reduction of minerals (taconite, chromite, in particular) with a solid-based carbon reductant are described. The resultant metallic and slag product analysis is discussed with respect to thermodynamic and kinetic considerations.

Jan 1, 1985

By Eoghan T. M Doyle

Oxide mixtures of nickel (NiO), cobalt (COO) and chromium (Cr203) were prepared with graphite in stoichiometric amounts and the powder mixtures were compacted to produce cylindrical pellets. The composition of chromium oxide in these mixtures were varied. Pressed pellets were reduced in a flowing stream of argon-4% hydrogen gas (500 ml/min). Both slow and rapid heating methods were adopted to raise the temperature of a pellet during reduction of oxides to form superalloy powder. The reduction temperature was varied between. 1523 and 1623K. The effect of heating rate and niobium oxide addition on the microstructure of the superalloy produced was studied by using ordinary light and scanning electron microscopes. New phases formed as a result of reduction were identified by X-ray powder diffraction technique. The mechanism of reduction of oxides together with the microstructure of NiCrCo alloy are discussed. The thermodynamics of formation of ternary alloy phase is elucidated on the basis of binary phase equilibria and Gibbs free energy of mixing data for the constituent alloy compositions.

Jan 1, 1992

By Fernanda da Silva Machado

Em um mundo de recursos naturais decrescentes, com a intensificação das indústrias automatizadas de todos os tipos (I4) e contínuo aumento da população, é necessário desenvolver melhores caminhos para a geração e distribuição de riquezas. Uma das alternativas para este objetivo é o conceito da Economia Circular. Este artigo apresenta um exemplo focado na intensificação do uso de resíduos de biomassa na produção integrada de aço exclusivamente baseada na combinação de reatores industriais existentes em um layout que favorece o conceito da economia circular. O ferro também é obtido do processamento tradicional de sucata, reprocessamento de resíduos de ferro e óxidos de ferro, como a escória, pequenos óxidos de ferro, reversos metálicos, resíduos da indústria siderúrgica integrada tradicional. Os resíduos de biomassa são provenientes da demolição de casas de madeira, e outros resíduos de biomassa, como limpeza florestal para evitar-se incêndios, resíduos de moinhos, paletes usados e qualquer outra fonte de biomassa. As combinações dos reatores tornaram-se possíveis devido à nova versão do processo de Carbonização Contínua, Carboval, um reator especialmente projetado da tecnologia Lambiotte tradicional, para produzir, de preferência, o carvão vegetal que possui as mesmas características necessárias para alimentar o Mini Alto Forno tradicional a base de carvão.

Oct 30, 2017