Extraction Of Titanium Research Articles

Solvent extraction of titanium(IV) from orthophosphoric acid media using Aliquat-336/kerosene and stripping with nitric acid

Titanium extraction from acidic solutions was investigated using Aliquat-336, considering factors like acid type and concentration for leaching, diluent type for solvent extraction, equilibration time, extractant concentration, phase ratio, and temperature. Kerosene exhibited superior performance as an aliphatic diluent for Aliquat-336 compared to other utilized diluents. The extraction efficiency was inversely proportional to the dielectric constant of the diluents. The quantitative Ti(IV) extraction efficiency from phosphoric acid (6 M H3PO4) leach liquor of ilmenite and rutile achived 98 % at room temperature (298 K) in 10 min after mixing with 0.1 M Aliquat-336 dissolved in kerosene at a phase volume ratio of 1:1 (Aq:Org). The exothermic extraction process occurred spontaneously. The proposed extraction mechanism using Aliquat-336/kerosene involves ion-pair association of the extractant with a Ti(IV) complex, confirmed by FTIR spectroscopy. The Ti(IV) ions were effectively stripped using HNO3 (3 M) with an aqueous:organic phase volume ratio of 1:1 at 25 °C after a contact time of 10 min in each step. The Aliquat-336/kerosene efficiently tested for Ti(IV) recovery from acidic Abu-Ghalaga ilmenite and rutile leachate. The findings indicate that, the phosphate medium is highly efficient in extracting Ti(IV), even with low concentration of Aliquat-336 in kerosene, especially in comparison to the impurities such as Fe, Cr, and Al. The EDX, XRD, and wet chemical analyses of the final product after the hydrolysis of stripped Ti(IV) from samples originating from the Abu-Ghalaga area and rutile samples, confirmed the formation of high-purity TiO2 (predominantly anatase phase). The SEM results showed particles with a regularly spherical structure and uniform size.

Effect and mechanism of calcination on improving the hydration activity of titanium extraction slag

Titanium extraction slag (TES) is a special waste residue in China’s Panxi region. It exhibits low hydration activity because of its high titanium content and carbon- and chlorine-based impurities introduced during production. Thus, TES wastes can only be stored in large quantities. Oil and gas wells’ high-temperature and high-pressure environments contribute to TES hydration. However, its hydration activity should be improved to transform it into a well cementing material. The optimal calcination temperature was 550 ℃. Using NaOH (6 %) as an activator, the compressive strength values of the calcined TES cured for 1 and 14 days reach 19.23 and 34.40 MPa, respectively, 65.49 % and 39.78 % higher than those of untreated TES. These values meet oil and gas well cementing construction requirements. X-ray diffraction, 29Si nuclear magnetic resonance, scanning electron microscopy, and other characterization methods indicate that calcination can reduce the content of the glassy phase in TES. However, it induces impurity removal and reduces the degree of glassy phase polymerization. Thus, TES’s ion leaching and deposition rates, hydration, and compressive strength after calcination improved. Therefore, the method proposed in this study can be successfully used to convert TES into new cementing materials for large-scale applications.

Determining patterns of leaching titanium(IV) from the Irshansky deposit ilmenite

The research object is the ilmenite concentrate from the Irshansky deposit. This study describes an elemental composition of the mineral raw material and confirms its structure using the X-ray diffraction and scanning electron microscopy. Experimental studies have shown that the ilmenite concentrate from the Irshansky deposit has a significant titanium content in terms of titanium dioxide (79 %). Mineral raw materials with such a chemical composition are unique, so there is a need to find alternative methods for its processing. The research demonstrates that the maximum degree of extraction in the process of alkaline leaching of the ilmenite concentrate is achieved under the condition that the average diameter of particles of the mineral raw material should be ≤71 μm. As a result of temperature studies, it has been found that a temperature of 453 K would suffice to obtain potassium titanate at atmospheric pressure. Further temperature increase does not provide for a significant increase in the degree of titanium extraction, and also contributes to the formation of polytitanates of various compositions. The study of the influence of the molar ratio of the starting reagents on the degree of extraction of titanium(IV) from the ilmenite concentrate has showed that the optimal molar ratio between the components corresponds to the stoichiometric one and is 1:2. Increasing the amount of potassium hydroxide in the reaction mixture is impractical as it reduces the yield of potassium titanate, and the final product will have high alkalinity due to excess alkali. The optimal time for alkaline leaching is three hours of continuous heating in a glycerin bath. A further increase in the duration of heating does not lead to an increase in the degree of extraction, which is associated with the diffusion of alkali from the surface of the nucleus into the volume of ilmenite particles due to the formed products of interaction and annihilation of the initial nuclei

Electrochemical reduction processes and extraction of titanium with different valence states in molten CaO-CaF2 slags

Titanium is an excellent structural and functional material. At present, the production of titanium has long process cycle, high energy consumption, serious pollution and other characteristics, so the development of low-cost titanium production methods has extremely far-reaching significance. In this work, the electrochemical reduction process of Ti(IV) and Ti(II) in the CaF2-CaO melt were investigated by cyclic voltammetry and square wave voltammetry measurements at 1740 K, respectively. In the CaF2-CaO-5 wt% TiO2 melt, Ti(IV) ions were reduced to Ti by one step. One measure was taken to lower the valence state of Ti ions: Ti(IV) ions in the melt was changed to Ti(II) by adding Ti0. Ti(IV) ions were reduced in two steps: in the CaF2-CaO-5 wt% TiO2-Ti0 melt, Ti(IV) → Ti(II) and Ti(II) → Ti, respectively, and in the CaF2-CaO-5 wt% TiO, the Ti(II) ions were reduced in a single step: Ti(II) → Ti. It was found that both migration and mass transfer affected the reduction processes. In contrast to the Ti(IV) reduction to Ti process, the Ti(II) reduction to Ti process showed a higher diffusion rate. Electrolytes and electrodes were analyzed after titanium electrodeposition by XRD. It was found that there were no metal titanium was detected in the electrolyte placed close to the cathode after electrodeposition. It believed that the formed metallic Ti reacted with dissolved O2- in the melt to form TiO. The reduction process of Ti(IV) on the iron electrode was investigated, the metal Ti was reduced by alloying process, the oxidation of Ti was hindered, there was a dense structure layer of CaTiO3 outside the reduced metal Ti that prevented the ions transfer and affected the Ti(IV) ions migration process, which might be the main factor that the Ti(IV) reduction process was controlled by migration. The lower valence state of Ti in the melt promoted the formation of Ca2TiO4, which increased the ion migration rate and decreased the mass transfer rate. It was suggested that titanium or titanium alloys may be prepared by reducing the valence of Ti(IV) in minerals and altering the melt composition. It is feasible to prepare titanium and titanium alloys by MOE short process using ore as raw material.

Efficient preparation of metallic titanium from lower valence titanium chloride slurry by electrochemical reduction in molten salts

Short extraction of metallic titanium by the electrochemical reduction process in molten salt has attracted increasing interest due to its many advantages. The electrolysis of high-purity titanium to produce lower valence titanium chlorides has so far been industrialized as balancing agents but large-scale production is still challenging due to the high cost of raw materials and easy deterioration. Herein, metallic titanium was extracted from lower valence titanium chlorides (LTCs) slurries by electrochemical reduction in molten salts. The results of LTC slurries at 260 ºC for 48 h revealed the formation of red-violet α- and γ- TiCl3 with an Al content below 0.09 wt%, which gradually reduced to form metallic titanium in molten salt electrolytes. Porous metallic Ti powders were obtained from TiCl3 by electrochemical reduction in KCl-LiCl-MgCl2 molten salt at 400 °C. The reaction at the anode area was accompanied by TiCl4 gas overflow, and continuous electrolysis of metallic titanium was achieved by supplementing the consumed TiCl3. Overall, the proposed electrolysis process looks promising for large-scale applications due to its simple electrolysis equipment, relatively stable electrolyte components, and good product quality, thereby worth further future investigation.

Effect of ZrO2 on the phase relations for CaO-SiO2-TiO2 system related to efficient extraction of titanium from titania-bearing slag

The selective crystallization and phase separation process has been regarded as a promising process for the recycling of titanium from titania-bearing furnace slag, however, the composition modification mechanism still remains unclear due to the lack of fundamental thermodynamic data. In the present work, the influence of ZrO2 addition on the equilibrium phase relations and the 1400 °C isotherm for CaO-SiO2-TiO2 system were experimentally determined by using the high temperature equilibration-quenching technique, and Scanning Electron Microscopy-Energy Dispersive X-ray Spectrometry, and X-ray diffraction analysis. The equilibrium solid phases of rutile (TiO2), perovskite (CaTiO3), and tridymite (SiO2) are determined to be coexisting with the liquid phase. In addition, comparisons of present results with thermodynamic calculation by FactSage show significant discrepancies. The present work is important for enriching the thermodynamic database of titania-bearing slag oxide systems as well as optimizing the selective crystallization and phase separation process.

Value-added recycling of iron and titanium from bauxite residue (Red Mud) via a flux-free smelting separation process

With enriched iron and titanium elements, red mud produced by the lime-free Bayer process showing high recycling value. This work proposed a pre-reduction and flux-free smelting process to recycle Fe/Ti resources from this red mud. Considering the extraction of titanium from smelting slag, classical calcareous flux was abandoned to avoid the formation of refractory perovskite. Instead, the FeO generated by pre-reduction of red mud itself was creatively applied to regulate the subsequent smelting separation. The full melting temperature of slag can be reduced from > 1700℃ to 1450℃-1550℃, as the FeO content in slag reached 10-20 wt%. The transition from rutile to ferrouspseudobrookite contributed to this change. Since the pre-reduced sample was smelted at 1600℃ for 60 min, 93.60 wt% of the iron element in red mud can be recycled in the form of iron nugget with grade of 99.6 wt%. Titanium in red mud can be recycled as Ti-rich slag, with TiO2 content of 55.91 wt%, for titanium dioxide production. The FeO in slag also suppressed the side reactions (i.e., carbonization of titanium and iron, reduction of silicon) in smelting process, which improved slag fluidity and iron nugget purity. This technique also provides a new approach for the utilization of V-bearing titanomagnetite, ilmenite, and other similar resources.

Synergetic recovery of rutile and preparation of iron phosphate from titanium-extraction tailings by a co-leaching process

This study presents a compelling, eco-friendly methodology for extracting valuable materials from titanium extraction tailing (TET) discharged from the reduction rust process. The process efficiently separates titanium and iron by utilizing a co-leaching technique with sulfuric and phosphoric acids. This method results in a high-grade titanium dioxide (TiO2) with a purity of 61.57 % and an iron leaching rate surpassing 96 % under the optimal conditions of the liquid-to-solid ratio of 4:1, a leaching temperature of 70 °C, and a specific phosphoric acid to iron molar ratio is 1.1. The subsequent refinement phase involves adjusting the pH to 2.0 using ammonia, coupled with controlled precipitation temperature and ageing time, leading to the production of battery-grade iron phosphate (FePO4) with a purity of 98.82 %, in line with the stringent HG/T4701-2014 standards. The material's phase analysis and morphological characterization confirm its high crystallinity and minimal impurity levels. Moreover, the co-leaching approach facilitates magnetite dissolution, effectively enriching the rutile content in the leach residue and concurrently minimizing the formation of ammonium sulfate salts, thereby enhancing the purity of the iron phosphate. These technological advancements contribute to resource recovery research and offer new avenues for industrial material production, laying a solid foundation for sustainable industrial applications.

Study of the leaching process for dust chamber sublimates followed by the extraction of niobium and zirconium into solution

The material composition of the sublimates from dust chambers in titanium chlorinators has been studied by chemical, X-ray and microprobe analysis methods. Studies of the phase composition of dust chamber sublimates have shown that the object consists of aqueous and anhydrous chloride phases to a greater extent. Two forms of niobium present, such as oxychloride and oxide niobium were found. The presence of zirconium in sublimates has a chloride and oxychloride nature. Experiments for the aqueous leaching of dust chamber sublimates were conducted to determine the optimal process conditions: S:L ratio = 1:8, leaching time = 1 hour, temperature = 25℃. Studies were conducted to choose an acidic reagent for cake leaching followed by the conversion of niobium and zirconium into a solution. A solution consisting of HF+H2SO4 was selected as an acidic reagent for cake leaching. Optimal conditions for the extraction of niobium and zirconium into solution were established, such as 25% [18M HF] +75% [7M H2SO4], S:L ratio = 1:3, temperature = 90 °C, duration of the leaching process = 120 minutes. Under these leaching conditions, the extraction of niobium, zirconium, and titanium into solution was 94.06%, 84.95% and 32.35%, respectively. The elemental and phase composition of the residue from acid leaching of cake were determined.

Study on the high temperature hydration characteristics of titanium extraction slag cementing fluid

Titanium extraction slag (TES) is the residual tailings of high titanium blast furnace slag after secondary titanium extraction, mainly composed of silicoaluminate glass body and crystal impurities such as FeO and TiC. The special chemical composition makes the activity of TES lower than that of granulated blast furnace slag (GBFS), resulting in a large amount of accumulation and causing serious resource waste and environmental pollution. This article preliminarily explores the feasibility of using TES in oil and gas well cementing engineering with reference to underground temperature curing TES. The optimal compressive strength was obtained at a curing temperature of 70 ℃, with a 3 d strength of 15.78 MPa, which not only meets the requirements of cementing engineering but also exceeds the strength of GBFS under the same conditions. At the same time, based on the composition and structural changes of hydration products cured at 70 ℃ for 3 and 28 d, and analyzes the hydration mechanism of TES at high temperatures. The results showed that under the influence of strong alkali activation and CaCO3 nucleation, TES rapidly hydrated and almost completely hydrated at 3 d. As hydration progresses, C-A-S-H crosslinks with each other and gradually transforms into a more dense and thermally stable crystal form (Foshagite), allowing for continuous improvement in compressive strength within 28 d. In summary, TES has high activity at high temperatures, and the strength of the solidified body meets the requirements of cementing, making it suitable as a cementing material for well cementing.

Phase Reduction and Thermodynamic Analysis of Ilmenite Ore by Carbothermal-Iodination using Different Carbon Reductants

The present study is on the combination of carbothermal reduction and iodination reaction (carboiodination) process for the phase reduction of ilmenite ore (FeTiO3). The aim is to understand the phase reduction and thermodynamic reaction analysis of ilmenite ore by a combined method of carbothermal-iodination using different carbon reductants (graphite and palm char). Graphite was used as a standard carbon reductant while palm char as a renewable carbon reductant was prepared via the pyrolysis technique. Ilmenite was mixed with carbon reductants and then first reduced by using a carbothermal reduction process at 1550℃. Then, the reduced samples were further investigated with iodination reaction in different temperature ranges of 900-1000 °C using a vertical tube furnace with mixed argon and iodine gas (0.2 L/min). The proximate and ultimate analyses of carbon reductants were analysed by CHON analyser and their microstructure by using SEM, while XRF and XRD were used for analyzing the chemical compositions and the phase reductions of raw ilmenite ore and reduced samples, respectively. The thermodynamics of possible reactions during carbothermal-iodination reactions were calculated by HSC Chemistry 6.0 software. By comparing graphite and palm char, palm char had an amorphous structure, with porous and high carbon content showing high potential for usage as a reductant in titanium extraction from ilmenite ore. The phases of ilmenite ore were ilmenite, rutile, and anatase transformed into rutile, pseudobrookite, and titanium oxide detected by XRD. Further reduction was performed by palm char where more rutile (TiO2) and titanium oxide (Ti3O5) developed from the iodination reaction at the highest temperature compared to graphite due to better properties and amorphous structure. The rutile and titanium oxide were found as stable phases from the thermodynamic analysis and confirmed with XRD. From the findings, the combination of carbothermal-iodination of ilmenite ore was possible and promising for rutile (TiO2) production in mineral extractions.

New insights into the mechanisms of TiB[formula omitted](001) thermal oxidation combining molecular dynamics and density functional theory calculations

Using reactive force field molecular dynamics and Density Functional Theory, this study unravels the early stages of TiB2 oxidation. Overall, it is found that the TiB2 boron sheets hinder the oxidation until a temperature of 800 K is reached, above which a complex sequence of chemical mechanisms leads to the formation of a titanium oxide at the top surface and agglomeration of pure boron underneath, preventing further TiO2 growth below 900 K. It is demonstrated that titanium oxidation is possible after the softening and distortion of boron sheets due to oxygen adsorbate presence; mostly BO radicals, no B2O3-like structure is formed. The local distortions of boron aromatic rings allow oxygen insertion into the subsurface, which is followed by titanium extraction and migration towards the outer surface in contact with the molecular oxygen atmosphere. Mechanistic details of these complex extraction–oxidation processes and their relation to cooperative oxygen atoms and molecules are detailed in terms of pathways and corresponding energetics. Interestingly different reaction stages are identified, that do not exceed 2 eV activation. The proposed hierarchical scenario of oxidation of titanium and boron in TiB2 might benefit to the general understanding of metal diboride oxidation.

REDUCTION ROASTING OF ROUGH TITANIUM-MAGNETITE CONCENTRATE OF THE GREMYAKHA-VYRMES DEPOSIT WITH THE PRODUCTION OF TITANIUM-VANADIUM SLAG AND GRANULAR METAL

The studies results on the reduction firing of rough titanium-magnetite concentrate of the Gremyakha-Vyrmes deposit are presented. The reduction firing of the briquetted charge was carried out on a coal substrate to obtain granular metal and titanium-vanadium slag suitable for subsequent hydrometallurgical processing with the extraction of titanium and vanadium. Studies on reducing roasting were carried out in the temperature range of 1450-1500 °C at different costs of a solid reducing agent — coke. The coke content influence in the mixture and the reduction temperature on the composition of the resulting titanium-vanadium slag has been studied. As a result of solid-phase reduction of rough titanium-magnetite concentrate, optimal conditions for obtaining titanium-vanadium slag suitable for further processing have been established.

A novel method for efficient recovery of ilmenite by high gradient magnetic separation coupling with magnetic fluid

Ilmenite is the main raw material for titanium extraction. The vanadium titanium magnetite deposit in Panzhihua has abundant ilmenite resources. A flowsheet combining high gradient magnetic separation (HGMS) and flotation was applied to recover the ilmenite, which had defects of high production cost due to high flotation regent consumption, low ilmenite utilization rate of 20% as ultrafine minerals were directly discharged into tailings, as well as bring a series of environmental problems. In this study, a novel method termed high gradient magnetic separation coupling with magnetic fluid (HGMSCMF) was developed to recovery ilmenite in Panzhihua. Paramagnetic MnCl2 solutions were introduced to eliminate competing capture between ilmenite and titanaugite particles and improve selectivity. Under equivalent TiO2 recovery, TiO2 grade of magnetic products increased significantly with MnCl2 concentration. Pulsating flow could further strengthen the improvement effect of selectivity by magnetic fluids. For the first time, qualified ilmenite concentrate (TiO2 grade > 46%) with TiO2 recovery equal to that in industrial production was obtained only through HGMSCMF (without using flotation) with one roughing and three cleaning processes under the optimal conditions of MnCl2 concentration 40%, applied induction 0.6 T and pulsating frequency 400 r/min. HGMSCMF presents great potential in solving tough problems being faced in processing weakly magnetic minerals. Follow-up studies will focus on recycling and reuse of magnetic fluids for realizing industrial application of HGMSCMF in recovering ilmenite or other refractory weakly magnetic minerals.

Extraction of titanium from Ti-doped seaside magnetite concentrate in HCl media

Extraction of titanium from Ti-doped seaside magnetite concentrate in HCl media

Strengthening effect and mechanism of titanium extraction slag on the mechanical property of calcium aluminate cement

In heavy oil recovery, calcium aluminate cement (CAC) is in the working environment of “low-temperature hardening and ultrahigh temperature service.” However, the formation of C3AH6 under low temperatures results in a decrease in strength and reduce the cementing quality. In this study, titanium extraction slag (TES) was used to inhibit CAC strength deterioration. TES, characterized by a high Ti content, presents challenges in terms of utilization and poses significant ecological risks owing to its large accumulation. Cementite hydration with 0%, 20%, 30%, and 40% TES relative to CAC was examined at 30 °C for 28 d. The high C3AH6 content of the pure CAC increased the strength deterioration, pore size, and cementite carbonation. With 20% TES, a dilution effect was observed without strength improvement. Furthermore, 30% TES generated layered double hydroxides and converted C–S–H into C–A–S–H, thereby increasing compressive strength. By-products were generated with 40% TES, which inhibited the strength development while generating C–A–S–H to maintain the compressive strength. Therefore, TES can inhibit the strength decline of CAC, and the byproducts of the LDH structure can improve corrosion resistance.

Extraction of Titanium, Aluminum, and Rare Earth Values from Upgraded Bauxite Residue

Extraction of Titanium, Aluminum, and Rare Earth Values from Upgraded Bauxite Residue

Изучение экстракции титана и ниобия из сернокислых растворов с использованием бинарных экстрагентов

The extraction of titanium and niobium from sulfuric acid solutions obtained after the perovskite concentrate processing has been studied. Extraction has been performed using a number of binary extractants, and distribution data have been estimated. The possibility of separation of titanium and niobium from sulfuric acid solutions has been demonstrated.

Extraction of a perovskite from red mud and its photocatalytic reduction of CO2

The extensive utilization of red mud is an urgent problem for the worldwide alumina plants, and the extraction of titanium from the red mud is especially difficult. The extraction of perovskite from a red mud alkaline leaching slag (by using acid leaching), in addition to its photocatalytic reduction of CO2, have been investigated in the present study. The results showed that the photocatalytic CO2 reduction performance of the extracted perovskite was like that of pure synthesized perovskite After a reaction duration of 4 h, the yields of CO and CH4 reached 10.24 μmol·g−1, 2.85 μmol·g−1, respectively, which were 0.96 times and 0.99 times that of pure perovskite, respectively. This study provides a promising method to use the titanium, as recovered from red mud, and presents a novel idea for using hazardous waste for the photocatalytic reduction of CO2, which is beneficial for the sustainable development of the alumina industry.

Preparation of micro‐crystal stones from molten titanium slag by “one‐step” cooling method

AbstractMedium‐titanium blast furnace slag (MTS) is a major solid waste in the smelting process of vanadium and titanium magnetite. The moderate TiO2 content in MTS makes it unsuitable for titanium extraction and difficult to be used as cement mixing material in large quantities. In this study, the molten MTS was utilized to prepare micro‐crystal stones by a “one‐step” cooling method, and the TiO2 in the slag was used as a nucleating agent. The effects of the cooling process and MTS utilization on the slag structure, crystallization characteristics, and physical properties of the micro‐crystal stones were investigated. The results show that when the utilization of MTS is 100 wt%, the main crystalline phase of the micro‐crystal stones is akermanite, the compressive strength and micro‐hardness are 142.5 MPa and 696.9 kgf·mm−2. When the utilization of MTS is 90 wt%, the main phases of microcrystalline stone are augite and akermanite, and the compressive strength rises to 194.8 MPa. Hence, through proper cooling control, the preparation of micro‐crystal stones with good performance by using molten MTS as raw material will have considerable economic value.