A flotation method for simultaneously producing medium and high quality titanium concentrates

Abstract

The application discloses a kind of simultaneously producing medium, high-quality titanium concentrate flotation method, belong to vanadium-titanium magnetite titanium resource comprehensive utilization field.The application method uses one roughing→one scavenging→four-stage cleaning→scavenging and the middlings of the first two stages are returned in turn→the middlings of the 3rd and 4th stage cleaning are combined and then separately reselected→the tailings of reselection are returned to roughing flotation process and corresponding reagent system make the ilmenite and gangue minerals in ilmenite flotation feed fully separate, simultaneously produce TiO2 Grade ≥49% and TiO2 Grade ≥47% titanium concentrate, and do not affect the total recovery rate of flotation concentrate TiO2, beneficial to subsequent titanium concentrate processing process, can effectively solve the problem that existing flotation method produces high-grade and medium-grade two titanium concentrate products, which will reduce the TiO2 recovery rate of flotation concentrate.

Description

Technical Field

[0001] This invention belongs to the field of comprehensive utilization technology of vanadium-titanium magnetite titanium resources, and specifically relates to a flotation method for simultaneously producing medium and high quality titanium 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. As of the end of 2018, approximately 93.42% of the world's titanium resources (based on TiO2) existed in the form of ilmenite, and my country's titanium resources account for 25% of the world's total resources. 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 has undergone several innovations, evolving from spiral sluice gravity separation-flotation desulfurization-drying-electrostatic separation to the widely used high-intensity magnetic separation-flotation desulfurization-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 in my country is generally 45%-47%. The low TiO2 grade and high content of CaO, MgO, SiO2, and Al2O3 have limited the development of my country's titanium industry chain, forcing my country's titanium dioxide industry to primarily rely on the sulfuric acid process and molten salt chlorination, rather than chlorine chlorination, thus affecting the competitiveness of my country's titanium industry chain. To improve the TiO2 grade and reduce impurity content of vanadium-titanium magnetite titanium concentrate, representative vanadium-titanium magnetite mining and utilization enterprises have upgraded their titanium concentrate processes to produce titanium concentrate with a TiO2 grade greater than 48%. Currently, the main methods for upgrading titanium concentrate from flotation are either increasing the number of flotation stages and sequentially returning the middlings, or increasing the number of flotation stages and then using the 46%-47% TiO2 grade flotation concentrate to produce two titanium concentrate products with TiO2 grades of 43%-44% and ≥48% TiO2. The result is that increasing the number of flotation stages and sequentially returning the middlings reduces the TiO2 recovery rate of the flotation concentrate; and increasing the number of flotation stages and using the 46%-47% TiO2 grade flotation concentrate to produce two titanium concentrate products with TiO2 grades of 43%-44% and ≥48% TiO2 does not actually reduce the amount of gangue minerals entering subsequent operations. Summary of the Invention

[0004] The technical problem to be solved by the present invention is that the TiO2 recovery rate of the flotation concentrate is reduced when producing high-grade and medium-grade titanium concentrate products by existing flotation methods.

[0005] The technical solution adopted by this invention to solve its technical problem is: a flotation method for simultaneously producing medium and high quality titanium concentrate, comprising the following steps:

[0006] a. After preparing the ilmenite slurry, add reagent A and mix well. Then add reagents B and C at the same time and mix well for roughing to obtain foam 1 and bottom material 1. Add reagents B and C at the same time to bottom material 1 and mix well for scavenging to obtain foam 2 and bottom material 2 tailings. Combine foam 2 with ilmenite and return to step a for roughing.

[0007] b. After preparing foam 1 into a slurry, add reagent A and mix well for fine selection to obtain foam 3 and bottom material 3. Combine bottom material 3 with ilmenite and return to step a for rough selection.

[0008] c. After preparing foam 3 into a slurry, add reagent A and mix well for fine selection two to obtain foam 4 and bottom material 4. Combine bottom material 4 with foam 1 and return to step b for fine selection one.

[0009] d. After preparing foam 4 into a slurry, add reagent D and mix well for fine selection 3 to obtain foam 5 and bottom material 5;

[0010] e. After preparing foam 5 into a slurry, add reagent D and mix well for fine selection 4 to obtain foam 6 titanium concentrate 1 and bottom material 6;

[0011] f. Clarify and combine the bottom material 5 and bottom material 6 to prepare a slurry. Then, add reagents B and C simultaneously and mix well for middlings re-selection and roughing to obtain froth 7 and bottom material 7. Combine bottom material 7 with ilmenite and return to step a for roughing.

[0012] g. After preparing foam 7 into a slurry, add reagent D and mix well for middlings re-selection and flotation to obtain foam 8, titanium concentrate 2 and bottom material 8. After clarifying bottom material 8, combine it with bottom material 5 and bottom material 6 and return to step f for middlings re-selection and roughing.

[0013] In the above method for producing high-quality ilmenite flotation concentrate, reagent A is industrial concentrated sulfuric acid, prepared as a 10% aqueous solution at room temperature; reagent B is ilmenite flotation collector-MOH, prepared as a 5% aqueous solution by heating to 60-70℃; reagent C is ilmenite flotation collector-U-Titanium 2#, prepared as a 5% aqueous solution by heating to 60-70℃; and reagent D is acidified water glass, prepared at a weight ratio of water glass with a modulus of 3.2: industrial concentrated sulfuric acid: water = 2:2:96.

[0014] In step a above, the solid content of the slurry is 40-45 wt%; the dosage of reagent A is 2000-2400 g / t ilmenite; during roughing, the dosage of reagent B is 1000-1400 g / t ilmenite dry basis and the dosage of reagent C is 500-700 g / t ilmenite dry basis; during scavenging, the dosage of reagent B is 200-300 g / t ilmenite dry basis and the dosage of reagent C is 100-200 g / t ilmenite dry basis.

[0015] In step b above, the solid content of the slurry is 50-55 wt%; the dosage of reagent A is 200-400 g / t ilmenite.

[0016] In step c above, the solid content of the slurry is 45-50 wt%; the dosage of reagent A is 100-200 g / t ilmenite.

[0017] In step d above, the solid content of the slurry is 40-45 wt%; the dosage of reagent D is 100-200 g / t ilmenite dry basis.

[0018] In step e above, the solid content of the slurry is 40-45 wt%; the dosage of reagent D is 50-100 g / t ilmenite dry basis.

[0019] In step f above, the solid content of the slurry is 35-40 wt%; the dosage of reagent B is 200-400 g / t ilmenite dry basis, and the dosage of reagent C is 100-200 g / t ilmenite dry basis.

[0020] In step g above, the solid content of the slurry is 30-35 wt%; the dosage of reagent D is 30-50 g / t ilmenite dry basis.

[0021] In the above-mentioned methods for producing high-quality ilmenite flotation concentrate, the flotation process parameters must meet at least one of the following requirements;

[0022] In steps a to g, the impeller speed is 1590 to 1992 r / min, and the scraper speed is 18 to 22 r / min;

[0023] In step a, the inflation rate is 1.4–1.6 L / min;

[0024] In step a, the time for scraping bubbles during roughing is 10-15 minutes, and the time for scraping bubbles during scavenging is 5-7 minutes;

[0025] In steps b to g, the inflation rate is 0.5 to 1.0 L / min;

[0026] In steps b to e, the scraping time is 7 to 9 minutes;

[0027] In steps f to g, the time for scraping the foam is 5 to 7 minutes.

[0028] The beneficial effects of this invention are as follows: the flotation process and corresponding reagent system, which adopts a first-stage roughing → first-stage scavenging → four-stage cleaning → sequential return of middlings from the scavenging and first two cleaning stages → merging the middlings from the third and fourth cleaning stages and then separately re-selecting them → returning the re-selected tailings to the roughing stage, fully separates ilmenite from gangue minerals in the ilmenite flotation feed, resulting in high-quality titanium concentrate 1 (TiO2 50.35%, SiO2 0.87%, CaO 0.12%, MgO 4.09%, Al2O3 0.27%) and medium-quality titanium concentrate 2 (TiO2 47.38%, SiO2 1.96%, CaO 0.54%, MgO 4.94%, Al2O3 0.87%, S 0.12%), with the flotation tailings containing 3.64% TiO2 and the total TiO2 recovery rate of the titanium concentrate being 89.07%. High-quality titanium concentrate was obtained, as well as ilmenite flotation concentrate with a quality not much different from that before upgrading, laying the foundation for the further economic utilization of ilmenite flotation concentrate.

[0029] This method modifies the conventional ilmenite flotation process by adding two stages of flotation cleaning and tailings concentration followed by separate flotation and tailings return to the original process, based on the existing one-stage roughing, two-stage cleaning, and two-stage scavenging ilmenite flotation process. This not only produces titanium concentrate with a TiO2 grade ≥49%, but also titanium concentrate with a TiO2 grade ≥47%, without affecting the overall TiO2 recovery rate of the flotation concentrate. This benefits subsequent titanium concentrate processing, has significant economic benefits, and has great potential for widespread application. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the process flow according to an embodiment of the present invention. Detailed Implementation

[0031] The technical solution of the present invention can be specifically described as follows: Figure 1 The process flow described above uses reagent dosages in g / t, which represent the dosage per unit weight of the raw ore. Reagent A is the weight of ilmenite, while reagents B, C, and D are the dry weights of ilmenite. The technical solution and effects of this invention will be further illustrated below with practical examples.

[0032] The main physicochemical properties of the ore described in this example are as follows: The ilmenite flotation sample contains fixed amounts of TFe 22.25%, SiO2 23.41%, CaO 7.83%, MgO 9.42%, Al2O3 5.88%, TiO2 20.85%, S 0.14%, and Co 0.011%; the sample contains ilmenite 27.32%, titanomagnetite 1.37%, diopside 34.58%, amphibole 18.10%, olivine 5.79%, labradorite 5.63%, anorthite 1.93%, pyroxene 1.59%, chlorite 1.41%, sphene 1.02%, and other minerals in small amounts.

[0033] The example is a small-scale laboratory flotation closed-circuit test, and the raw material is ilmenite flotation feed from the on-site production process.

[0034] A flotation method for simultaneously producing medium- and high-quality titanium concentrate is described in the following experimental procedure:

[0035] 1) Prepare a 10% dilute sulfuric acid solution using tap water as reagent A; prepare a 5% aqueous solution of ilmenite flotation collector MOH (purchased from Hubei Jingjiang Mineral Processing Reagent Co., Ltd.) using 60℃ hot water as reagent B; prepare a 5% aqueous solution of ilmenite flotation collector YouTi 2# (purchased from Guanghan Jinxin Technology Co., Ltd.) using 60℃ hot water as reagent C; prepare reagent D by mixing water glass (modulus 3.2) with industrial concentrated sulfuric acid and water in a weight ratio of 2:2:96.

[0036] 2) Weigh 4000g of ilmenite flotation feed and place it in the flotation cell of XFD type 8L flotation machine 1. Add water to adjust the slurry to the scale line of the flotation cell. Turn on the flotation machine stirring device and adjust the impeller speed to 1992r / min. Add 80mL of reagent A and continue stirring for 3min. At the same time, add 80mL and 40mL of reagents B and C respectively and continue stirring for 3min. Adjust the scraper speed to 20r / min. Open the air valve to control the air volume to 1.5L / min. Turn on the scraper device and scrape the foam for 12min. During the process, add flushing water to maintain the liquid level of the flotation cell. After the time is completed, turn off the air and scraper devices. The products are foam 1 and bottom material 1.

[0037] 3) Add 24 mL and 12 mL of reagents B and C to the flotation cell of flotation machine 1, stir for 3 min, open the aeration valve to control the aeration rate to 1.5 L / min, turn on the scraper device, scrape the foam for 6 min, and turn off the aeration and scraper device. The products are foam 2 and bottom material 2. Bottom material 2 is tailings.

[0038] 4) Place foam 1 in the flotation cell of XFD type 3.0L flotation machine 2, add water to adjust the slurry to the scale line of the flotation cell, turn on the flotation machine stirring device, adjust the impeller speed to 1790r / min, add 8mL of reagent A, continue stirring for 3min, adjust the scraper speed to 20r / min, open the air valve to control the air volume to 1.0L / min, turn on the scraper device, scrape the foam for 9min, add flushing water during the process to maintain the liquid level of the flotation cell, turn off the air and scraper device after the time is completed, the product is foam 3 and cell bottom material 3;

[0039] 5) Place foam 3 in the flotation cell of XFD type 3.0L flotation machine 3, add water to adjust the slurry to the scale line of the flotation cell, turn on the flotation machine stirring device, adjust the impeller speed to 1790r / min, add 6 mL of reagent A, continue stirring for 3min, adjust the scraper speed to 20r / min, open the air valve to control the air volume to 1.0L / min, turn on the scraper device, scrape the foam for 8min, add flushing water during the process to maintain the liquid level of the flotation cell, turn off the air and scraper device after the time is completed, the product is foam 4 and bottom material 4;

[0040] 6) After combining the bottom material 4 and foam 1, place them in the flotation cell of the XFD type 3.0L flotation machine 2, and repeat step 3) to form a closed loop;

[0041] 7) Place foam 4 in the flotation cell of XFD type 3.0L flotation machine 4, add water to adjust the slurry to the scale line of the flotation cell, turn on the flotation machine stirring device, adjust the impeller speed to 1590r / min, add reagent D 32mL, continue stirring for 3min, adjust the scraper speed to 18r / min, open the air valve to control the air volume to 1.0L / min, turn on the scraper device, scrape the foam for 8min, add flushing water during the process to maintain the liquid level of the flotation cell, and turn off the air and scraper device after the time is completed. The products are foam 5 and bottom material 5.

[0042] 8) Place foam 5 in the flotation cell of XFDⅣ type 3L flotation machine 5, add water to adjust the slurry to the scale line of the flotation cell, turn on the flotation machine stirring device, adjust the impeller speed to 1590 r / min, add reagent D16 mL, continue stirring for 3 min, adjust the scraper speed to 18 r / min, open the air valve to control the air volume to 1.0 L / min, turn on the scraper device, scrape the foam for 8 min, add flushing water during the process to maintain the liquid level of the flotation cell, turn off the air and scraper device after the time is completed, the product is foam 6 and cell bottom 6, foam 6 is titanium concentrate 1;

[0043] 9) After clarification, add bottom material 5, bottom material 6, and bottom material 8 to the flotation cell of XFD type 1.5L flotation machine 6, and add water to adjust the slurry to the scale line of the flotation cell. Turn on the flotation machine stirring device, adjust the impeller speed to 1590r / min, and add 24mL and 12mL of reagents B and C respectively. Continue stirring for 3min, adjust the scraper speed to 18r / min, open the air valve to control the air volume to 0.5L / min, turn on the scraper device, and scrape the foam for 6min. During the process, add flushing water to maintain the liquid level of the flotation cell. After the time is completed, turn off the air and scraper devices. The products are foam 7 and bottom material 7.

[0044] 10) Place foam 7 in the flotation cell of XFD type 1.5L flotation machine 5, add water to adjust the slurry to the scale line of the flotation cell, turn on the flotation machine stirring device, adjust the impeller speed to 1590r / min, add reagent D 8mL, continue stirring for 3min, adjust the scraper speed to 18r / min, open the air valve to control the air volume to 0.5L / min, turn on the scraper device, scrape the foam for 6min, add flushing water during the process to maintain the liquid level of the flotation cell, turn off the air and scraper device after the time is completed, the product is foam 8 and cell bottom material 8, foam 8 is titanium concentrate 2;

[0045] 11) Weigh 4000g of ilmenite flotation feed and combine it with the flotation foam 2 (extracted in 2), the bottom material 3 (extracted in 3), and the bottom material 7 (extracted in 8) in the flotation cell of the XFD 8.0L flotation machine 1. Continue the steps in 1) to form a closed loop, and perform the above steps 2)-10) in sequence for a total of 6 loops to obtain 6 groups of titanium concentrate 1, titanium concentrate 2, and tailings. After filtration, weighing, sample preparation, and analysis, the test results of the last three groups of samples were selected after the closed loop test was determined to be in equilibrium for balance calculation. The results are shown in Table 1.

[0046] Table 1. Test Results of Examples

[0047]

Claims

1. A flotation method for simultaneously producing medium- and high-quality titanium concentrate, characterized in that, Includes the following steps: a. After preparing the ilmenite slurry, add reagent A and mix well. Then add reagents B and C at the same time and mix well for roughing to obtain foam 1 and bottom material 1. Add reagents B and C at the same time to bottom material 1 and mix well for scavenging to obtain foam 2 and bottom material 2 tailings. Combine foam 2 with ilmenite and return to step a for roughing. b. After preparing foam 1 into a slurry, add reagent A and mix well for fine selection to obtain foam 3 and bottom material 3. Combine bottom material 3 with ilmenite and return to step a for rough selection. c. After preparing foam 3 into a slurry, add reagent A and mix well for fine selection two to obtain foam 4 and bottom material 4. Combine bottom material 4 with foam 1 and return to step b for fine selection one. d. After preparing foam 4 into a slurry, add reagent D and mix well for fine selection 3 to obtain foam 5 and bottom material 5; e. After preparing foam 5 into a slurry, add reagent D and mix well for fine selection 4 to obtain foam 6 titanium concentrate 1 and bottom material 6; f. Clarify and combine the bottom material 5 and bottom material 6 to prepare a slurry. Then, add reagents B and C simultaneously and mix well for middlings re-selection and roughing to obtain froth 7 and bottom material 7. Combine bottom material 7 with ilmenite and return to step a for roughing. g. After preparing foam 7 into a slurry, add reagent D and mix well for middlings re-selection and flotation to obtain foam 8 titanium concentrate 2 and bottom material 8. After clarifying bottom material 8, combine it with bottom material 5 and bottom material 6 and return to step f for middlings re-selection and roughing. Reagent A is industrial concentrated sulfuric acid, prepared as a 10% aqueous solution at room temperature; Reagent B is ilmenite flotation collector - MOH, prepared as a 5% aqueous solution by heating to 60~70℃; Reagent C is ilmenite flotation collector - YouTi 2#, prepared as a 5% aqueous solution by heating to 60~70℃; Reagent D is acidified water glass, prepared at a volume ratio of water glass with a modulus of 3.2: industrial concentrated sulfuric acid: water = 2:2:

96.

2. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step a, the solid content of the slurry is 40-45 wt%; the dosage of reagent A is 2000-2400 g / t ilmenite; during roughing, the dosage of reagent B is 1000-1400 g / t ilmenite dry basis, and the dosage of reagent C is 500-700 g / t ilmenite dry basis. During scavenging, the dosage of reagent B is 200-300 g / t dry ilmenite, and the dosage of reagent C is 100-200 g / t dry ilmenite.

3. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step b, the solid content of the slurry is 50-55 wt%; the dosage of reagent A is 200-400 g / t ilmenite.

4. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step c, the solid content of the slurry is 45-50 wt%; the dosage of reagent A is 100-200 g / t ilmenite.

5. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step d, the solid content of the slurry is 40-45 wt%; the dosage of reagent D is 100-200 g / t ilmenite dry basis.

6. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step e, the solid content of the slurry is 40-45 wt%; the dosage of reagent D is 50-100 g / t ilmenite dry basis.

7. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step f, the solid content of the slurry is 35-40 wt%; the dosage of reagent B is 200-400 g / t ilmenite dry basis, and the dosage of reagent C is 100-200 g / t ilmenite dry basis.

8. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: In step g, the solid content of the slurry is 30-35 wt%; the dosage of reagent D is 30-50 g / t ilmenite dry basis.

9. The flotation method for simultaneously producing medium- and high-quality titanium concentrate according to claim 1, characterized in that: The flotation process parameters must meet at least one of the following requirements; In steps a~g, the impeller speed is 1590~1992 r / min, and the scraper speed is 18~22 r / min; In step a, the inflation rate is 1.4~1.6 L / min; In step a, the time for scraping bubbles during roughing is 10-15 minutes, and the time for scraping bubbles during scavenging is 5-7 minutes; In steps b to g, the inflation rate is 0.5 to 1.0 L / min; In steps b to e, the foam scraping time is 7 to 9 minutes; In steps f to g, the time for scraping the foam is 5 to 7 minutes.

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