Method for producing high-quality titanium concentrate using ilmenite flotation concentrate

Abstract

The application discloses a method for preparing high-quality titanium concentrate by using ilmenite flotation concentrate, and belongs to the technical field of mineral processing. In order to overcome the problems of low titanium grade, high content of impurities such as CaO, SiO2 and Al2O3, and adsorption of flotation reagents on the surface of minerals in the existing flotation concentrate, the application provides the method for preparing high-quality titanium concentrate by using ilmenite flotation concentrate. The method adopts the working procedure of one-time reagent adding and stirring, two-time reagent adding and stirring, three-time stirring, ultrasonic high-frequency screen grading and table gravity separation, adopts carbonates and water glass as combined reagents, disperses the flotation titanium concentrate, realizes full separation of ilmenite and gangue minerals, obtains high-quality titanium concentrate, significantly reduces the content of CaO, SiO2 and Al2O3 in the high-quality titanium concentrate, is beneficial to the subsequent titanium concentrate processing process, and has low tailing loss rate.

Description

Technical Field

[0001] This invention belongs to the field of mineral processing technology, and specifically relates to a method for preparing high-quality titanium concentrate using ilmenite flotation concentrate. Background Technology

[0002] Titanium is an important and rare strategic metal with a series of superior properties unmatched by other metals, including high specific strength, light weight, corrosion resistance, shape memory, good ductility and biocompatibility, superconductivity, and strong surface decorative properties. It has wide applications in aerospace, petrochemicals, construction, power, medical, and sporting goods, and is often referred to as the "third metal" after iron and aluminum. TiO2 is the best white inorganic pigment and is widely used in coatings, plastics, synthetic fibers, rubber, papermaking, printing inks, and cosmetics. The main industrially valuable titanium-bearing minerals in nature are ilmenite and rutile. Approximately 93.42% of the world's titanium resources (based on TiO2) exist in the form of ilmenite, and my country's titanium resources account for 25% of the world's total. Of this, 93% is distributed in the form of primary ilmenite in the Panxi region's vanadium-titanium magnetite deposits. The effective development and utilization of the Panxi titanium resources is of great significance to my country's national defense, industry, and economic development.

[0003] Since the early 1980s, the Panxi region of my country has been recovering mid-titanium resources from iron tailings of vanadium-titanium magnetite ore beneficiation. The process, initially involving spiral sluice gravity separation, flotation desulfurization, drying, and electrostatic separation, has undergone several innovations to the widely used high-intensity magnetic separation, flotation desulfurization, and flotation titanium separation. Currently, this region produces approximately 80% of my country's domestically produced titanium concentrate. The TiO2 grade of primary ilmenite concentrate produced from vanadium magnetite ore in my country is generally 45%-47%. The low TiO2 grade and high content of CaO, SiO2, and Al2O3 in this concentrate have limited the development of my country's titanium industry chain. This has resulted in my country's titanium dioxide industry primarily relying on the sulfuric acid process and molten salt chlorination, rather than fluidized bed chlorination, thus impacting the competitiveness of my country's titanium industry chain. In practical applications, fluidized bed chlorination typically requires titanium concentrate to contain CaO ≤ 0.15%, Al2O3 ≤ 1.50%, and SiO2 ≤ 1.0%, with particularly stringent requirements for CaO content. Meanwhile, in the process of producing titanium concentrate from vanadium-titanium magnetite ilmenite in my country, flotation reagents are added during flotation desulfurization and titanium beneficiation. These reagents adsorb onto the mineral surface, causing ilmenite to form flocs in the slurry. This is not conducive to using other methods to improve the TiO2 grade of the titanium concentrate in subsequent flotation. Furthermore, increasing the number of flotation stages to reduce CaO is not effective and affects the TiO2 recovery rate of the titanium concentrate.

[0004] CN117483097A discloses a low-grade ilmenite beneficiation process, comprising the following steps: S1: crushing raw ore with TiO2≤10.00wt% and TFe≤20.00wt% and feeding it into a dry ore separator for dry high-intensity magnetic roughing to obtain the desired dry concentrate; S2: screening the dry concentrate after high-pressure roller milling to obtain roller-pressed products; S3: separating the roller-pressed products using a wet magnetic separator to obtain magnetic and non-magnetic products; S4: adding water to the non-magnetic product to obtain a slurry, feeding the slurry into a flotation cell, adding sodium hexametaphosphate for the first stirring and slurry preparation, adding calcium hypochlorite for the second stirring after the first stirring and slurry preparation, and completing the oxidation and activation of ilmenite after the two stirrings; S5: adding titanium concentrate composite collector M and frother to the oxidized and activated slurry and then performing flotation to obtain titanium concentrate after flotation. However, this method still uses flotation technology, and it is still difficult to overcome the problems of impurities such as CaO, SiO2, and Al2O3, as well as the problem of flotation reagents adsorbing on the mineral surface.

[0005] CN112871460A discloses a dispersion inhibitor suitable for ultrafine-grained ilmenite, comprising hydroxyethylidene diphosphonate, sodium carboxymethyl cellulose, and water glass in a mass ratio of 1:4 to 6:3 to 5. The components of the dispersion inhibitor exhibit a certain synergistic effect, and the combined use of the three components significantly improves the effect compared to using any one component alone or separately. When applied to the flotation separation of ultrafine-grained ilmenite systems, it can disperse slime, activate ilmenite, and assist in suppressing gangue minerals (olivine, pyroxene), achieving good flotation results with relatively small reagent dosages and a simple flotation process, thereby significantly improving the grade and recovery rate of the obtained titanium concentrate. The hydroxyethylidene diphosphonate primarily plays a dispersing role and does not chemically react with the minerals; the sodium carboxymethyl cellulose and water glass suppress gangue minerals, while the sodium carboxymethyl cellulose also disperses ultrafine-grained minerals. However, this dispersion inhibitor is not suitable for further beneficiation of ilmenite flotation concentrate.

[0006] CN117563785A discloses a flotation process for enhanced recovery of ilmenite, comprising the following steps: S1, Ilmenite direct flotation: The ilmenite flotation raw material is prepared into a slurry, and a direct flotation pH adjuster, an ilmenite activator, an ilmenite collector, and a frother are added sequentially. After thorough slurry conditioning, a "roughing and scavenging" direct flotation process is performed. The resulting flotation froth product is the ilmenite rough concentrate, and the product in the scavenging cell is flotation tailings 1; S2, Ilmenite reverse flotation: The ilmenite rough concentrate is fed into the reverse flotation process, and a reverse flotation ilmenite depressant and a gangue collector are added sequentially. After thorough slurry conditioning, a "roughing and scavenging" reverse flotation process is performed. The resulting product in the roughing cell is the final titanium concentrate, and the reverse flotation froth product is tailings 2; wherein, the TiO2 grade in the ilmenite flotation raw material is 16.50~21.5%. The content of gangue minerals in the ilmenite flotation feedstock is 54.00-68.00%, and the gangue minerals include pyroxene, feldspar, and chlorite; in S1, during roughing, the pH adjuster is sodium carbonate, and the pulp pH value is 7.5-8.0; the ilmenite activator is lead nitrate, with a dosage of 300-400 g / t; the ilmenite collector is a hydroxamic acid collector, with a dosage of 1500-2000 g / t; the frother is No. 2 oil, with a dosage of 30-40 g / t; during scavenging, the pH adjuster is sodium carbonate, and the pulp pH value is 7.5-8.0; the ilmenite activator is lead nitrate, with a dosage of 150-200 g / t; the ilmenite collector is a hydroxamic acid collector, with a dosage of 500-700 g / t; the frother is No. 2 oil, with a dosage of 10-20 g / t. However, this method requires changing from an acidic environment to an alkaline environment throughout the process, resulting in high alkali consumption, an inevitable increase in ions in the slurry, high production costs, and difficulty in controlling water circulation. Summary of the Invention

[0007] To overcome the problems of existing technologies and achieve a significant reduction in CaO, SiO2, and Al2O3 in ilmenite flotation concentrate while improving the TiO2 grade of titanium concentrate, this invention compares and selects the optimal reagent combination suitable for removing flocculation precipitates from titanium concentrate. This solves the problem of flocculation in the slurry of titanium concentrate and, through screening and fractional gravity separation, achieves the goal of preparing high-quality titanium concentrate from flotation precipitates.

[0008] This invention provides a method for preparing high-quality titanium concentrate from ilmenite flotation concentrate, comprising the following steps:

[0009] A. Prepare a slurry with a mass concentration of 50% to 60% for ilmenite flotation concentrate. Add the ilmenite flotation concentrate to a mixing tank 1 equipped with circulation holes and baffles at a flow rate of 0.75 to 1.0 kg ilmenite flotation concentrate / min.

[0010] B. Add reagent A to the mixing tank 1 at a flow rate of 7.5 mL / min to 30 mL / min to mix reagent A with the ilmenite flotation concentrate slurry.

[0011] C. The slurry in mixing tank 1 flows by gravity into mixing tank 2, which has circulation holes and baffles;

[0012] D. Add reagent B to mixing tank 2 at a flow rate of 2.25 mL / min to 5 mL / min to mix reagent B and slurry evenly.

[0013] E. The slurry in mixing tank 2 flows by gravity into mixing tank 3, which has circulation holes and baffles, to further mix the slurry.

[0014] F. The slurry in mixing tank 3 flows by gravity into the pump, and then is pumped to an ultrasonic 3-layer vibrating screen. The upper screen mesh size is 0.15mm, the middle screen mesh size is 0.074mm, and the lower screen mesh size is 0.038mm, resulting in three particle sizes: +0.15mm, -0.15+0.074mm, and -0.074mm+0.038mm.

[0015] G. The +0.15mm and -0.15 +0.074mm particle sizes are fed into the Yunnan Tin Ore Slime Shaking Table, and the -0.074mm +0.038mm particle size is fed into the Yunnan Tin Micro-Fine Slime Shaking Table for gravity separation. The shaking table gravity separation process consists of one stage of roughing and three stages of scavenging. The roughing concentrate is used as high-quality titanium concentrate, and the scavenging concentrate is combined with the -0.038mm particle size material to form medium-grade titanium concentrate. The tailings are combined into total tailings.

[0016] The reagent A is an aqueous solution of sodium carbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate with a mass concentration of 5% to 15%; the reagent B is an aqueous solution of water glass with a modulus of 2.0 to 3.2 with a mass concentration of 5% to 15%.

[0017] In the above method, step A, the ilmenite flotation concentrate contains the following components by mass percentage: C 0.063%, TFe 34.23%, SiO2 2.50%, CaO 0.83%, MgO 4.93%, Al2O3 0.98%, TiO2 47.64%, S 0.109%, Co 0.011%, Ni 0.001%, Cu 0.009%, Na2O 0.125%, K2O 0.037%, As 0.003%, and P < 0.01%.

[0018] In the above method, in step A, the ilmenite flotation concentrate contains 93.75 wt% ilmenite, 1.50 wt% labradorite, 1.42 wt% amphibole, 1.05 wt% pyroxene, 0.86 wt% sphene, 0.75 wt% titanomagnetite, 0.20 wt% olivine, and 0.19 wt% pyrrhotite.

[0019] In the above method, the rotation speed of the mixing tank 1 is controlled to be 1000-1500 rad / min.

[0020] In the above method, the rotation speed of the mixing tank 2 is controlled to be 1000-1500 rad / min.

[0021] In the above method, the rotation speed of the mixing tank 3 is controlled to be 1000-1500 rad / min.

[0022] In the above method, in step G, the high-quality titanium concentrate obtained has the following composition: TiO2 ≥ 50 wt%, SiO2 ≤ 1 wt%, CaO ≤ 0.15 wt%, Al2O3 ≤ 0.4 wt%, S ≤ 0.05 wt%, C ≤ 0.03 wt%, with the balance being iron and unavoidable impurities.

[0023] In the above method, in step G, the composition of the medium-quality titanium concentrate obtained is TiO2 ≥ 47wt%, SiO2 ≤ 2.5wt%, CaO ≤ 0.8wt%, Al2O3 ≤ 1.0wt%, S ≤ 0.20wt%, with the balance being iron and unavoidable impurities.

[0024] In the above method, in step G, the tailings obtained contain TiO2 ≤ 6.0 wt%.

[0025] The effects achieved by implementing this invention patent are:

[0026] This invention employs a method of one-time reagent addition and stirring, two-time reagent addition and stirring, three-time stirring, ultrasonic high-frequency screening and classification, and shaking table to disperse the flotation titanium concentrate, thereby achieving full separation of ilmenite and gangue minerals. The resulting high-quality and medium-quality titanium concentrates have tailings containing very little TiO2, with a tailings loss rate of only 0.29%. This significantly reduces CaO, SiO2, and Al2O3 in the high-quality titanium concentrate, facilitating subsequent titanium concentrate processing. The invention obtains high-quality titanium concentrate and lays the foundation for further economic utilization of ilmenite flotation concentrate, demonstrating significant economic benefits. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the process flow of Embodiment 1 of the present invention. Detailed Implementation

[0028] Specifically, a method for preparing high-quality titanium concentrate from ilmenite flotation concentrate includes the following steps:

[0029] A. Prepare a slurry with a mass concentration of 50% to 60% for ilmenite flotation concentrate. Add the ilmenite flotation concentrate to a mixing tank 1 equipped with circulation holes and baffles at a flow rate of 0.75 to 1.0 kg ilmenite flotation concentrate / min.

[0030] B. Add reagent A to the mixing tank 1 at a flow rate of 7.5 mL / min to 30 mL / min to mix reagent A with the ilmenite flotation concentrate slurry.

[0031] C. The slurry in mixing tank 1 flows by gravity into mixing tank 2, which has circulation holes and baffles;

[0032] D. Add reagent B to mixing tank 2 at a flow rate of 2.25 mL / min to 5 mL / min to mix reagent B and slurry evenly.

[0033] E. The slurry in mixing tank 2 flows by gravity into mixing tank 3, which has circulation holes and baffles, to further mix the slurry.

[0034] F. The slurry in mixing tank 3 flows by gravity into the pump, and then is pumped to an ultrasonic 3-layer vibrating screen. The upper screen mesh size is 0.15mm, the middle screen mesh size is 0.074mm, and the lower screen mesh size is 0.038mm, resulting in three particle sizes: +0.15mm, -0.15+0.074mm, and -0.074mm+0.038mm.

[0035] G. The +0.15mm and -0.15 +0.074mm particle sizes are fed into the Yunnan Tin Ore Slime Shaking Table, and the -0.074mm +0.038mm particle size is fed into the Yunnan Tin Micro-Fine Slime Shaking Table for gravity separation. The shaking table gravity separation process consists of one stage of roughing and three stages of scavenging. The roughing concentrate is used as high-quality titanium concentrate, and the scavenging concentrate is combined with the -0.038mm particle size material to form medium-grade titanium concentrate. The tailings are combined into total tailings.

[0036] The reagent A is an aqueous solution of sodium carbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate with a mass concentration of 5% to 15%; the reagent B is an aqueous solution of water glass with a modulus of 2.0 to 3.2 with a mass concentration of 5% to 15%.

[0037] The main mineral in ilmenite flotation concentrate is ilmenite, whose chemical molecular formula is FeTiO3. Theoretically, the TiO2 content is 52.66% and the FeO content is 47.34%, but in actual mineralization, Mg... 2+ Ca 2+ Mn 4+ and Mn 2+ Will with Fe2+ Isomorphous formation of zeolite, perovskite, and ruthenium zeolite occurs, resulting in high calcium, magnesium, and manganese content, especially calcium and magnesium, in the titanium concentrate produced from vanadium-titanium magnetite in the Panxi region. At the same time, during the crushing, grinding, and beneficiation processes, 100% liberation between mineral particles is impossible. Ilmenite particles inevitably co-occur with ilmenite, pyrrhotite, pyroxene, olivine, feldspar, chlorite, amphibole, and MgO spinel, resulting in high levels of impurities such as SiO2, Al2O3, CaO, and MgO in the ilmenite flotation concentrate.

[0038] In this invention, the ilmenite flotation concentrate raw material can be obtained by conventional flotation processes in the field, through vanadium-titanium magnetite ore mined from mines. The general preparation process of ilmenite flotation concentrate is as follows: Vanadium-titanium magnetite ore (particle size 350-1000mm, TFe grade 15%-30%, TiO2 grade 5%-12%) mined from the mine is crushed to 0-12mm in three stages and closed circuit, followed by three stages of grinding and three stages of weak magnetic grinding and magnetic separation to obtain vanadium-titanium magnetite concentrate and iron tailings (TFe grade 9%-13%, TiO2 grade 4%-10%). The iron tailings are then subjected to weak magnetic iron removal, strong magnetic pre-enrichment of ilmenite, strong magnetic titanium rough concentrate flotation desulfurization, and desulfurized titanium rough concentrate flotation to obtain ilmenite flotation concentrate slurry. The ilmenite flotation concentrate slurry is then concentrated, filtered, and dried to obtain ilmenite flotation concentrate (TiO2 grade usually ≥46.5%). Based on this process, as in step A of embodiment 1 of the present invention, the ilmenite flotation concentrate slurry from the ilmenite flotation concentrate preparation process can actually be directly used, and its concentration can be adjusted to the concentration required by the present invention.

[0039] In this embodiment of the invention, the ilmenite flotation concentrate used contains the following components by mass percentage: C 0.063%, TFe 34.23%, SiO2 2.50%, CaO 0.83%, MgO 4.93%, Al2O3 0.98%, TiO2 47.64%, S 0.109%, Co 0.011%, Ni 0.001%, Cu 0.009%, Na2O 0.125%, K2O 0.037%, As 0.003%, and P < 0.01%. The ilmenite flotation concentrate contains 93.75 wt% ilmenite, 1.50 wt% labradorite, 1.42 wt% amphibole, 1.05 wt% pyroxene, 0.86 wt% sphene, 0.75 wt% titanomagnetite, 0.20 wt% olivine, and 0.19 wt% pyrrhotite. However, the method of the present invention is not limited to the ilmenite flotation concentrate of the embodiment.

[0040] This invention involves a continuous process, controlling the flow rates of the ilmenite flotation concentrate slurry, reagent A, and reagent B to achieve precise material proportions. In step A, the flow rate of the ilmenite flotation concentrate is controlled at 0.75–1.0 kg / min, and the flow rate of reagent A is controlled at 7.5 mL / min–30 mL / min, resulting in a carbonate dosage of 1000–3000 g carbonate / t ilmenite flotation concentrate. The carbonate not only acts as a pH adjuster, allowing the collector to dissolve in the slurry solution in an ionic state, but more importantly, it also functions as a dispersant and competitive adsorbent on the surface of ilmenite particles, reducing CO3 in the solution. 2- Fe on the surface of ilmenite 2+ and Ti 4+ Ions undergo chemical reactions to generate water-insoluble and hydrophilic FeCO3 and Ti(CO3)2 and their complexes.

[0041] Simultaneously, in step D, the flow rate of reagent B is controlled at 2.25 mL / min to 5 mL / min, thereby ensuring that the amount of water glass used is 300 to 500 g water glass per t of ilmenite flotation concentrate. This invention uses a Na₂SiO₃ aqueous solution, utilizing SiO₃... 2- The special dispersion properties of SiO3 in aqueous solution 2- The principle of competitive adsorption between mineral particles and collector ions.

[0042] The addition of reagent A and reagent B can be achieved by using a stainless steel container with a valve, as described in this embodiment of the invention, to control their flow rate; or by using a stainless steel container with a stainless steel tube to add reagent A and a stainless steel container with a latex tube to add reagent B.

[0043] Furthermore, the mixing tanks 1 to 3 used in this invention are all equipped with circulation holes and baffles, thereby ensuring thorough mixing of the slurry and reagents to achieve the de-removal effect and guarantee the continuous and stable operation of the process. The rotation speed of mixing tank 1 is controlled at 1000–1500 rad / min to ensure uniform dispersion of the ilmenite flotation concentrate slurry and its uniform mixing with reagent A; the rotation speed of mixing tank 2 is controlled at 1000–1500 rad / min to ensure uniform mixing of the slurry and reagent B; and the rotation speed of mixing tank 3 is controlled at 1000–1500 rad / min to appropriately extend the processing time and further homogenize the slurry.

[0044] In step F of this invention, after classification by a three-layer ultrasonic vibrating screen, four particle sizes are obtained: +0.15mm, -0.15+0.074mm, -0.074mm+0.038mm, and -0.038mm. Among these, the +0.15mm, -0.15+0.074mm, and -0.074mm+0.038mm particle sizes require a further re-selection step. The +0.15mm and -0.15+0.074mm particle sizes were fed into a shaking table for gravity separation. The gravity separation process consisted of one roughing stage and three scavenging stages. The +0.15mm particle size roughing concentrate was used as high-quality titanium concentrate 1, and the -0.15+0.074mm particle size roughing concentrate was used as high-quality titanium concentrate 2. The +0.15mm particle size scavenging concentrate was used as medium-quality titanium concentrate 1, and the -0.15+0.074mm particle size scavenging concentrate was used as medium-quality titanium concentrate 2. The +0.15mm particle size scavenging tailings were used as tailings 1, and the -0.15+0.074mm particle size scavenging tailings were used as tailings 2. The -0.074 to +0.038 mm particle size was fed into a Yunnan Tin Micro-Fine Sludge Shaking Table for gravity separation. The gravity separation process consisted of one stage of roughing and three stages of scavenging. The -0.074 to +0.038 mm particle size roughing concentrate was designated as high-quality titanium concentrate 3, the -0.074 to +0.038 mm particle size scavenging concentrate was designated as medium-quality titanium concentrate 3, and the -0.074 to +0.038 mm particle size scavenging tailings were designated as tailings 3. The -0.038 mm particle size material was designated as medium-quality titanium concentrate 4. High-quality titanium concentrates 1, 2, and 3 were combined into a total high-quality titanium concentrate, medium-quality titanium concentrates 1, 2, and 3, along with the -0.038 mm particle size product, were combined into a total medium-quality titanium concentrate, and scavenging tailings 1, 2, and 3 were combined into a total tailings.

[0045] In step G of this invention, the high-quality titanium concentrate has the following composition: TiO2 ≥ 50 wt%, SiO2 ≤ 1 wt%, CaO ≤ 0.15 wt%, Al2O3 ≤ 0.4 wt%, S ≤ 0.05 wt%, C ≤ 0.03 wt%, with the balance being iron and unavoidable impurities. In step G of this invention, the medium-quality titanium concentrate has the following composition: TiO2 ≥ 47 wt%, SiO2 ≤ 2.5 wt%, CaO ≤ 0.8 wt%, Al2O3 ≤ 1.0 wt%, S ≤ 0.20 wt%, with the balance being iron and unavoidable impurities. In step G of this invention, the tailings contain TiO2 ≤ 6.0 wt%.

[0046] The present invention will be further described in detail below through embodiments, but the scope of protection of the present invention is not limited to the embodiments described herein.

[0047] Experimental Example 1

[0048] Because the surface of ilmenite flotation concentrate particles is adsorbed with flotation collectors, they agglomerate in the pulp and exhibit strong hydrophobicity, making screening and classification impossible. Therefore, this experiment first focuses on reducing the hydrophobicity of the ilmenite flotation concentrate particle surface. The experimental procedure is as follows:

[0049] ① Weigh 100g of ilmenite flotation concentrate sample;

[0050] ② Add the sample to a beaker, add 200 mL of deionized water to adjust the liquid-solid ratio to 2:1, add the additives as required, stir manually with a glass rod until well mixed, and let stand for 10 minutes.

[0051] ③ Filter the treated slurry, and after filtration, rinse the filter cake three times with 150mL of deionized water.

[0052] ④ Place the filtered cake in an oven and dry it at 65℃ until it reaches a constant weight;

[0053] ⑤ Weigh 5g of the treated sample and use a high-pressure tablet press to press the sample into a blocky round cake shape to meet the requirements of the rotating drop interfacial tension meter for measuring the contact angle of the mineral surface;

[0054] ⑥ The contact angle of the pressed sample was measured using a rotating drop interfacial tension meter to determine the change law of hydrophilicity (hydrophobicity) of the ilmenite surface after the agent treatment.

[0055] The results of the additive types and dosages, slurry pH, and sample particle surface contact angle measurements are shown in Table 1.

[0056] Table 1. Test Results of Types of Additives for De-processing Titanium Concentrate in Flotation

[0057] 1 No addition 6.0 125.00 2 CaO: 2.0g 12.5 118.00 3 <![CDATA[Na2CO3:1g;Na2SiO3:1g]]> 11.5 71.68 4 NaOH: 1g 13.0 118.00 5 <![CDATA[NaOH:1g;Na2SiO3:1g]]> 13.0 106.50 6 <![CDATA[NaHCO3:1g;Na2SiO3:1g]]> 11.0 103.54

[0058] As shown in Table 1, the addition of CaO, Na2CO3+Na2SiO3, NaOH, and NaOH+Na2SiO3 can all reduce the hydrophobicity of the surface of flotation titanium concentrate particles. Among them, the reduction in hydrophobicity of the sample particle surface is most obvious when Na2CO3+Na2SiO3 is added.

[0059] Example 1

[0060] The main physicochemical properties of the ore described in this embodiment are:

[0061] The ilmenite flotation concentrate contains 0.063% C, 34.23% TFe, 2.50% SiO2, 0.83% CaO, 4.93% MgO, 0.98% Al2O3, 47.64% TiO2, 0.109% S, 0.011% Co, 0.001% Ni, 0.009% Cu, 0.125% Na2O, 0.037% K2O, 0.003% As, and <0.01% P. In the ilmenite flotation concentrate, ilmenite accounts for 93.75%, labradorite 1.50%, amphibole 1.42%, pyroxene 1.05%, sphene 0.86%, titanomagnetite 0.75%, olivine 0.20%, and pyrrhotite 0.19%.

[0062] This embodiment is a scaled-up, continuous pilot-scale test conducted in the laboratory. The raw material is ilmenite flotation concentrate slurry produced on-site, and the processing capacity is 50 kg of dry ilmenite flotation concentrate / h. The test procedure is as follows:

[0063] 1) Place the prepared 10% Na2CO3 aqueous solution into a 10L stainless steel container 1 equipped with a valve;

[0064] 2) Place the prepared 10% water glass aqueous solution into a 10L stainless steel container 2 equipped with a valve;

[0065] 3) Place the ilmenite flotation concentrate slurry with a mass concentration of 50% to 60% into a 30L volume mixing tank 1, control the slurry flow rate at 0.85L / min (approximately 50kg of dry ilmenite flotation concentrate / h), and adjust the main shaft speed of mixing tank 1 to 1200rad / min.

[0066] 4) Open the valve of stainless steel container 1 to allow the Na2CO3 aqueous solution to flow into the stirring tank 1 by gravity, and adjust the flow rate of the Na2CO3 aqueous solution to 16.7 mL / min (approximately 2000 g Na2CO3 / t ilmenite flotation concentrate);

[0067] 5) The slurry in mixing tank 1 flows into mixing tank 2 by gravity, and the main shaft speed of mixing tank 2 is adjusted to 1200 rad / min;

[0068] 6) Open the valve of stainless steel container 2 to allow the water glass solution to flow into the stirring tank 2 by gravity, and adjust the flow rate of the water glass solution to 3.4 mL / min (approximately 400 g water glass / t ilmenite flotation concentrate);

[0069] 7) The slurry in mixing tank 2 flows into mixing tank 3 by gravity, and the main shaft speed of mixing tank 3 is adjusted to 1200 rad / min;

[0070] 8) The slurry from the mixing tank 3 flows by gravity into the XBSL1 / 4 vertical sand pump and is pumped to the KM-800-4s ultrasonic 3-layer vibrating screen. The upper screen mesh size is 0.15mm, the middle screen mesh size is 0.074mm, and the lower screen mesh size is 0.038mm.

[0071] 9) The +0.15mm and -0.15+0.074mm particle sizes are fed into a 2100×1050 type Yunnan tin ore slime shaking table for gravity separation. The process consists of one stage of roughing and three stages of scavenging. The roughing concentrate is used as high-quality titanium concentrate 1 and high-quality titanium concentrate 2, the scavenging concentrate is used as medium-quality titanium concentrate 1 and medium-quality titanium concentrate 2, and the scavenging tailings are tailings 1 and tailings 2.

[0072] 10) The -0.074+0.038mm particle size is fed into a 2100×1050 type Yunnan Tin Micro-fine Mud Shaking Table for gravity separation. The process consists of one stage of roughing and three stages of scavenging. The roughing concentrate is used as high-quality titanium concentrate 3, the scavenging concentrate is used as medium-quality titanium concentrate 3, and the scavenging tailings are used as tailings 3.

[0073] 11) -0.038mm particle size product as medium-quality titanium concentrate 4;

[0074] 12) Combine high-quality titanium concentrates 1, 2, and 3 into total high-quality titanium concentrate, combine medium-quality titanium concentrates 1, 2, and 3 and the -0.038mm particle size product into total medium-quality titanium concentrate, and combine scavenging tailings 1, 2, and 3 into total tailings.

[0075] Example 1 process flow is as follows Figure 1 As shown in Table 2, the results are as follows.

[0076] Table 2. Experimental Results of Example 1

[0077]

[0078] This invention utilizes the above-mentioned process to produce two types of titanium concentrate products with TiO2 grades of 50.24% and 47.38% from flotation titanium concentrate with a TiO2 grade of 47.64%, without significantly affecting the overall utilization rate of the flotation titanium concentrate (with a TiO2 loss rate of 0.29% in tailings). The titanium concentrate with a TiO2 grade of 50.24% meets the requirements for boiling chlorination in terms of SiO2, CaO, and Al2O3, while the titanium concentrate with a TiO2 grade of 47.38% can be further used for molten salt chlorination.

Claims

1. A method for preparing high-quality titanium concentrate from ilmenite flotation concentrate, characterized in that: Includes the following steps: A. Prepare a slurry with a mass concentration of 50% to 60% for ilmenite flotation concentrate. Add the ilmenite flotation concentrate to a mixing tank 1 equipped with circulation holes and baffles at a flow rate of 0.75 to 1.0 kg ilmenite flotation concentrate / min. B. Add reagent A to the mixing tank 1 at a flow rate of 7.5 mL / min to 30 mL / min to mix reagent A with the ilmenite flotation concentrate slurry. C. The slurry in mixing tank 1 flows by gravity into mixing tank 2, which has circulation holes and baffles; D. Add reagent B to mixing tank 2 at a flow rate of 2.25 mL / min to 5 mL / min to mix reagent B and slurry evenly. E. The slurry in mixing tank 2 flows by gravity into mixing tank 3, which has circulation holes and baffles, to further mix the slurry. F. The slurry in mixing tank 3 flows by gravity into the pump, and then is pumped to an ultrasonic 3-layer vibrating screen. The upper screen mesh size is 0.15mm, the middle screen mesh size is 0.074mm, and the lower screen mesh size is 0.038mm, resulting in three particle sizes: +0.15mm, -0.15+0.074mm, and -0.074mm+0.038mm. G. The +0.15mm and -0.15 +0.074mm particle sizes are fed into the Yunnan Tin Ore Slime Shaking Table, and the -0.074mm +0.038mm particle size is fed into the Yunnan Tin Micro-Fine Slime Shaking Table for gravity separation. The shaking table gravity separation process consists of one stage of roughing and three stages of scavenging. The roughing concentrate is used as high-quality titanium concentrate, and the scavenging concentrate is combined with the -0.038mm particle size material to form medium-grade titanium concentrate. The tailings are combined into total tailings. The reagent A is an aqueous solution of sodium carbonate, potassium carbonate, sodium bicarbonate or potassium bicarbonate with a mass concentration of 5% to 15%; the reagent B is an aqueous solution of water glass with a modulus of 2.0 to 3.2 with a mass concentration of 5% to 15%.

2. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: In step A, the ilmenite flotation concentrate contains the following components by mass percentage: C 0.063%, TFe 34.23%, SiO2 2.50%, CaO 0.83%, MgO 4.93%, Al2O3 0.98%, TiO2 47.64%, S 0.109%, Co 0.011%, Ni 0.001%, Cu 0.009%, Na2O 0.125%, K2O 0.037%, As 0.003%, and P < 0.01%.

3. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: In step A, the ilmenite flotation concentrate contains 93.75 wt% ilmenite, 1.50 wt% labradorite, 1.42 wt% amphibole, 1.05 wt% pyroxene, 0.86 wt% sphene, 0.75 wt% titanomagnetite, 0.20 wt% olivine, and 0.19 wt% pyrrhotite.

4. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: Control the rotation speed of mixing tank 1 to 1000-1500 rad / min.

5. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: Control the rotation speed of mixing tank 2 to 1000-1500 rad / min.

6. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: Control the rotation speed of mixing tank 3 to 1000-1500 rad / min.

7. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: In step G, the high-quality titanium concentrate obtained has the following composition: TiO2 ≥ 50 wt%, SiO2 ≤ 1 wt%, CaO ≤ 0.15 wt%, Al2O3 ≤ 0.4 wt%, S ≤ 0.05 wt%, C ≤ 0.03 wt%, with the balance being iron and unavoidable impurities.

8. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to claim 1, characterized in that: In step G, the composition of the medium-quality titanium concentrate obtained is TiO2 ≥ 47 wt%, SiO2 ≤ 2.5 wt%, CaO ≤ 0.8 wt%, Al2O3 ≤ 1.0 wt%, S ≤ 0.20 wt%, with the balance being iron and unavoidable impurities.

9. The method for preparing high-quality titanium concentrate from ilmenite flotation concentrate according to any one of claims 1 to 8, characterized in that: In step G, the tailings obtained contain TiO2 ≤ 6.0 wt%.

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