Preparation of sodium molybdate from molybdenum concentrate by microwave roasting and alkali leaching

The preparation process of sodium molybdate has the disadvantages of high energy consumption,low thermal efficiency,and high raw material requirement of molybdenum trioxide,in order to realize the green and efficient development of molybdenum concentrate resources,this paper proposes a new process for efficient recovery of molybdenum from molybdenum concentrate and preparation of sodium molybdate by microwave-enhanced roasting and alkali leaching.Thermodynamic analysis indicated the feasibility of oxidation roasting of molybdenum concentrate.The effects of roasting temperature,holding time,and power-to-mass ratio on the oxidation product and leaching product sodium molybdate (Na_(2)MoO_(4)·2H_(2)O) were investigated.Under the optimal process conditions:roasting temperature of 700℃,holding time of 110 min,and power-to-mass ratio of 110 W/g,the molybdenum state of existence was converted from MoS_(2) to Mo O3.The process of preparing sodium molybdate by alkali leaching of molybdenum calcine was investigated,the optimal leaching conditions include a solution concentration of 2.5 mol/L,a liquid-to-solid ratio of 2 mL/g,a leaching temperature of 60℃,and leaching solution termination at pH 8.The optimum conditions result in a leaching rate of sodium molybdate of 96.24%.Meanwhile,the content of sodium molybdate reaches 94.08wt%after leaching and removing impurities.Iron and aluminum impurities can be effectively separated by adjusting the pH of the leaching solution with sodium carbonate solution.This research avoids the shortcomings of the traditional process and utilizes the advantages of microwave metallurgy to prepare high-quality sodium molybdate,which provides a new idea for the highvalue utilization of molybdenum concentrate.

Oxidation roasting of molybdenite concentrate

In order to investigate the oxidation roasting of molybdenite concentrate in pure oxygen atmosphere, experiments at 673, 723, 773, 873 and 973 K were carried out. The phase transitions and morphology evolutions of the samples obtained at different temperatures after reacting for different time were analyzed by X-ray diffraction（XRD） and scanning electron microscopy（SEM）. The results showed that molybdenite concentrate was oxidized directly to Mo O3 in pure oxygen atmosphere. There were remarkable changes of the morphologies of products with the increase of the roasting temperature. It was also found that sintering phenomenon occurred during the roasting process in pure oxygen when the temperature was above 873 K. The composition of sintered sample was mainly comprised of Mo O3 and some unreacted Mo S2.

Removal of magnesium and calcium from electric furnace titanium slag by H_3PO_4 oxidation roasting-leaching process

H3PO4 oxidation roasting followed by HCl acid leaching was proposed to remove magnesium and calcium from electric furnace titanium slag containing 3.12% MgO and 0.86% CaO. XRF, XRD and SEM techniques were used to characterize the composition, mineral phase component and microstructure of the titanium slag. The H3PO4 oxidation thermodynamic, mineral phase transformation, microstructure, element distribution in titanium slag during H3PO4 oxidation process and leaching process were investigated. The thermodynamic analysis indicated that H3PO4 could promote the decomposition of MgTi2O5 and CaSiO3. The results indicated that H3PO4 could effectively promote the transformation of titanium-bearing mineral to rutile and enrich the impurities in MxTi（3-x）O5 into phosphate which could be removed by acid leaching process. Under the studied conditions, the leaching rates of magnesium and calcium reached 94.68% and 87.19%, respectively. The acid leached slag containing 0.19% MgO and 0.13% CaO（mass fraction） was obtained.

Molybdenite-limestone oxidizing roasting followed by calcine leaching with ammonium carbonate solution

Oxidizing roasting of molybdenite with lime can significantly reduce SO2pollution compared with the traditional roastingwithout lime.However,the calcine is subsequently leached by sulfuric acid,resulting in serious equipment corrosion and abundantnon-recyclable CaSO4slag.In this work,a novel process,in which the molybdenite was roasted with CaCO3followed by(NH4)2CO3solution leaching,was proposed to improve the art of lime roasting-sulfuric acid leaching.Oxidizing roasting of molybdenite withCaCO3was investigated through thermodynamic calculation,thermogravimetric analysis and roasting experiments.The results showthat the products of the oxidizing reaction of MoS2in the presence of CaCO3and O2are CaSO4,CaMoO4and CO2at573-1000K.The MoS2conversion rate achieves approximately99%and the sulfur-retained rate attains approximately95%with aCaCO3-to-MoS2molar ratio of3.6at500°C for1h by adding5%mineralizer A(mass fraction).The leaching results show that theleaching rate of Mo reaches98.2%at85°C for7h with a(NH4)2CO3concentration of600g/L and a liquid-solid ratio of10mL/g.The results presented are potential to develop a novel cleaner technique for ammonium molybdate production.

Roasting oxidation behaviors of ReS_2 and MoS_2 in powdery rhenium-bearing, low-grade molybdenum concentrate

The oxidation roasting process of molybdenum concentrate has significant advantages in industrial applications.However,utilization of low-grade mineral has many problems because it is more complex than the standard concentrate.In this study,the oxidation behaviors of powdery rhenium-bearing low-grade molybdenum concentrate were investigated through thermodynamic calculation,roasting experiments,thermogravimetric analysis,and phase analysis.The results obtained show that oxidation of MoS2 begins at 450℃,and MoO3 reacts with metal-oxide forming molybdate at 600℃.Finally,MoO3 can be dissolved in ammonia with a maximum content of approximately 80%.The volatile speed of Re was considerably slower than the oxidation speed of MoS2 because the nonvolatile products ReO2 and ReO3 were generated in reactions among MoS2,SO2,and Re2O7.The final volatilization rate of Re was almost 70%.This study determined the problems related to the roasting of low-grade molybdenum concentrate,which lays the scientific foundations for subsequent enhancement of molybdenum and rhenium extraction.

Thermodynamics of chromite ore oxidative roasting process

To explicate the thermodynamics of the chromite ore lime-free roasting process, the thermodynamics of reactions involved in this process was calculated and the phrases of sinter with different roasting times were studied. The thermodynamics calculation shows that all the standard Gibbs free energy changes of the reactions to form Na2CrO4, Na2O-Fe2O3, Na2O·Al2O3 and Na2O3 SiO2 via chromite ore and Na2CO3 are negative, and the standard Gibbs free energy changes of the reactions between MgO, Fe2O3 and SiO2 released from chromite spinel to form MgO-Fe2O3 and MgO·SiO2 are also negative at the oxidative roasting temperatures （1 173 1 473 K）. The phrase analysis of the sinter in lime-free roasting process shows that Na2O·Fe2O3, Na2O·Al2O3 and Na2O·SiO2 can be formed in the first 20 min, but they decrease in contents and finally disappear with the increase of roasting time. The final phase compositions of the sinter are Na2CrO4, MgO·Fe2O3, MgO·SiO2 and MgO. The results indicate that Na2CrO4 can be formed easily via the reaction ofNa2CO3 with chromite ore. Na2O·Fe2O3, Na2O-Al2O3 and Na2O·SiO2 can be formed as intermediate compounds in the roasting process and they can further react with chromite ore to form Na2CrO4. MgO released from chromite ore may react with iron oxides and silicon oxide to form stable compounds of MgO·Fe2O3 and MgO·SiO2, respectively.

Features and mechanisms of self-sintering of molybdenite during oxidative roasting

Roasting experiments were carried out with pure reagents as raw materials.The self-sintering behaviors of molybdenite(MoS_(2))during oxidation were investigated by thermodynamic calculation,XRD,SEM-EDS and high-temperature in situ analysis.The results indicate that the desulfurization efficiency of MoS_(2) pellet decreases with the increase of roasting temperature from 600 to 700℃,owing to the expansion of sintered area.At the very beginning of roasting,sintered layer can be rapidly formed and cover the pellet surface on the windward side,and meanwhile,MoO_(2)and Mo_(4)O_(11) intensively appear and constitute the sintered layer together with MoO_(3).Moreover,it is proven that MoO_(3)-rich products containing low-valence molybdenum oxides have low melting points,thus easy to be melted during the occurrence of exothermic reaction between MoS_(2) and O_(2),which leads to the sintering of materials.

Recovery of Ferric Oxide from Bayer Red Mud by Reduction Roasting-Magnetic Separation Process

A great amount of red mud generated from alumina production by Bayer process was considered as a low-grade iron ore with a grade of 5wt% to 30wt% iron.We adopted the reduction roastingmagnetic separation process to recover ferric oxide from red mud.The red mud samples were processed by reduction roasting,grinding and magnetic separating respectively.The effects of different parameters on the recovery rate of iron were studied in detail.The optimum techqicalparameters were proposed with 700 ℃roasting for 20 min,as 50wt% carbon and 4wt% additive were added.The experimentalresults indicated that the iron recovery and the grade of totaliron were 91% and 60%,respectively.A novelprocess is applicable to recover ferric oxide from the red mud waste fines.

Novel method to prepare sodium chromate from carbon ferrochrome

An oxidizing roasting process of carbon ferrochrome to prepare sodium chromate in the presence of sodium carbonate and air was investigated. The effects of reaction temperature, reaction time, mole ratio of sodium carbonate to carbon ferrochrome were studied, and thermodynamics and kinetics of the reaction were also discussed. It was observed that there was a sudden increase in reaction rate when the temperature rose to a certain value, and the sample with a smaller grain size could start the sudden increase at a lower temperature. The chromium recovery rate increased with the increase of mole ratio of sodium carbonate to carbon ferrochrome, and it reached up to 99.34% when mole ratio of sodium carbonate to carbon ferrochrome increased to 1.2:1. The chromium residue yielded from this method was only about 1/3 of the product. Moreover, the content of Fe in the residue was as high as 60.41%. Therefore, it can be easily recovered to produce sponge iron, realizing complete detoxication and zero-emission of chromium residue.

Valency Study of Vanadium in Stone Coal Ash of Jiangxi Province

Vanadium-bearing stone coal is a new vanadium resource; recovery of V2O5 from the coal has been investigated. It has been found that a satisfactory extraction of V2O5 depends on both the oxidation of V and its reaction with sodium salt. V in the coal ash of Yushan mainly exists in two oxidation states; 98% V (Ⅲ) and 2% V(Ⅳ). The distribution of valency of V shows that organic matter determines V valency at low temperatures, at about 470℃ , V(Ⅲ) is completely oxidized to V (Ⅳ); above 500 ℃, the temperature is the most important factor for the oxidation of V At higher temperatures no more V is oxidized to V(Ⅴ); an equilibrium is established after 92% of V is oxidized to V(Ⅴ). The roles of NaCl in the recovery of V2O5 from the coal ash were discussed. The best conditions for roasting are temperature 750-800℃ for 1 h. under the oxidation-chlorination atmosphere. When the ore : NaCl = 100 :10 by weight, ηroast reaches 85.5%. According to the results, a flowsheet for V2O5 extraction from coal ash has been proposed.

Behavior of phase transformation of Baotou mixed rare earth concentrate during oxidation roasting

Based on the new process named "Combination Method" for metallurgy and separation of Baotou mixed rare earth concentrate(BMREC),the aim of this paper is to clearly elucidate the phase change behavior of BMREC without additives during oxidative roasting at 450-800℃.The results indicate that the bastnaesite in BMREC is decomposed at 450-550℃,the weight loss is about 10.3 wt%,and the activation energy(E) is 144 kJ/mol.The bastnaesite in BMREC is decomposed into rare earth fluoride,rare earth oxides(La_(2)O_(3),Ce_(7)O_(12),Pr_(6)O_(11) and Nd_(2)O_(3)),and CO_(2),particularly,with the increase of roasting temperature,bastnaesite in BMREC is more completely decomposed into LaF_(3),which causes a decrease in leaching rate of La during the HCI leaching process.Additionally,the maximum cerium oxidation efficiency reaches about 60 wt% when the roasting temperature is equal to or above 500℃,and the oxidation reaction rate of cerium increases with the increasing roasting temperature.

Separation chemistry and clean technique of cerium(IV): A review

The separation method of changeable valence RE element of cerium （Ce） was reviewed in this paper. Solvent extraction is the most effective and efficient method to separate Ce（IV） from RE（III）, usually accompanied with fluorine （F） and phosphor （P） from bastnaesite and monazite etc. By roast or wet-air oxidation, Ce（III） of bastnaesite and monazite was oxidized into Ce（IV）, and Cyanex923 and [A336][P507] have been investigated to co-extract and recover Ce（IV）, F and P from H2SO4 leaching liquor, leading to favorable conditions for the subsequent separation of Th（IV） and RE（III）. The interaction of Ce（IV） and F and/or P enhances the roasting, leaching and extraction of Ce（IV） due to increasing of the stability of Ce（IV）, and the formation of CeF3 and CePO4 after reductive stripping will benefit the utilization of F and P. For dealing with RE ores of high-content Ce, the clean process of oxidation roasting and Ce（IV）-F separation for Sichuan bastnaesite highlights the advantages of Ce（IV） based clean technique, which firstly demonstrates the comprehensive utilization of Ce（IV）, Th（IV）, F and RE（III） and prevention of environmental pollution from fountainhead. A preliminary flowsheet of two-step oxidation and extraction of Ce（IV） for Bayan Obo mixed ores was further proposed to process the oxidation and extraction of Ce（IV） in presence of both F and P, indicating the possibility of similar effects with clean process of Sichuan bastnaesite. Ce（IV） separation chemistry and clean technique will open up new realms for light RE resources utilization, meeting“Emission Standards of Pollutants from Rare Earths Industry”promulgated by China’s Ministry of Environment Protection （MOP） in 2011.