A method for enhancing the recovery of fine-grained titanium ore
By oxidizing and activating the surface of ilmenite and using modified collectors, combined with multi-dimensional interface-controlled flotation and deep upgrading processes, the problem of low recovery rate of fine-grained titanium ore was solved, achieving efficient and environmentally friendly titanium concentrate preparation.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-11
- Publication Date
- 2026-04-03
AI Technical Summary
Existing technologies are insufficient for the efficient recovery of fine-grained titanium ore, especially -38μm ilmenite, resulting in low titanium resource utilization. Furthermore, conventional methods suffer from problems such as complex reagents, difficult wastewater treatment, and environmental pollution.
By employing an oxidation-activated ilmenite surface and modified collector, a closed-circuit flotation system is formed through pre-enrichment, multi-dimensional interface-controlled flotation, and deep upgrading processes. This system utilizes a high-efficiency activator and a modified unsaturated fatty acid collector, combined with weak magnetic separation and fine-particle film separation, thereby improving the grade and recovery rate of titanium concentrate.
It achieves efficient recovery of fine-grained titanium ore, improves the grade and recovery rate of titanium concentrate, reduces reagent costs and wastewater treatment volume, avoids secondary pollution, and has a flexible and efficient process flow.
Smart Images

Figure CN117463510B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of fine-grained titanium ore beneficiation technology, specifically relating to a method for enhancing the recovery of fine-grained titanium ore. Background Technology
[0002] The main raw materials for titanium extraction are rutile and ilmenite. Rutile is a high-quality raw material for titanium extraction, but natural rutile resources are increasingly depleted, making ilmenite the primary raw material for titanium extraction. my country has ilmenite reserves of 200 million tons, accounting for 28% of global reserves. my country's titanium resources are mainly distributed in Panzhihua-Xichang region of Sichuan, Chengde region of Hebei, and Yunnan. Titanium ore mainly includes rock ore and placer ore. For rock ore resources, the industrial beneficiation process for ilmenite mainly involves weak magnetic separation of iron, followed by a strong magnetic flotation process to separate titanium from the iron tailings. This beneficiation process has good recovery effects for ilmenite with a particle size of +38μm, but it has significant limitations for ilmenite with a particle size of -38μm, making it difficult to efficiently recover and utilize titanium resources. For placer resources, the industrial process uses a “weak magnetic-strong magnetic-spiral chute” separation process. Although it can obtain about 45% titanium concentrate, the recovery rate is generally low. Most of the ilmenite is lost in the tailings, of which more than 50% is of the -38μm particle size.
[0003] To more effectively recover fine-grained titanium ore, patent CN109433406A employs a combined magnetic levitation process, using carboxymethyl cellulose as an inhibitor and a combination of MOH and talc oil as a collector. This involves a roughing, cleaning, and scavenging flotation operation, ultimately yielding a titanium concentrate grade of 44%–47%. However, this process suffers from low titanium dioxide recovery, complex flotation reagents, and difficulty in wastewater treatment. Patent CN110433964A uses a sodium hypochlorite oxidation process to float fine-grained ilmenite. Sodium perchlorate oxidizes ferrous ions on the ilmenite surface to ferric ions, enhancing collector adsorption and ultimately yielding a titanium concentrate grade of 40%–50% with a recovery rate exceeding 87%. However, the sodium hypochlorite used contains a large amount of chloride ions, which can pollute the environment if it enters water bodies. Patent CN114985098A uses microwave roasting to process ilmenite with a working power of 2500-3600W and an irradiation time of more than 10 minutes. After conventional flotation, titanium concentrate with a grade of 49-51% and a recovery rate of 50-70% is obtained. However, the roasting temperature is high and it is easy to generate low-concentration sulfur dioxide pollution.
[0004] Therefore, providing an enhanced flotation method for fine-grained ilmenite that can significantly improve the flotation grade and recovery rate of fine-grained ilmenite is a technical problem that urgently needs to be solved by those skilled in the art. Summary of the Invention
[0005] In view of this, the present invention proposes a method for enhancing the recovery of fine-grained ilmenite and improving the quality of concentrate by oxidizing and activating the surface of ilmenite and modifying the collector. The method of the present invention can effectively prepare qualified titanium concentrate from fine-grained titanium tailings and obtain a high titanium dioxide recovery rate.
[0006] To achieve the above objectives, the present invention adopts the following technical solution:
[0007] A method for enhancing the recovery of fine-grained titanium ore, characterized by comprising the following steps:
[0008] (1) Pre-enrichment: The fine-grained titanium ore slurry is concentrated to a slurry mass concentration of 20% to 25%, and then pre-enriched by strong magnetic separation to obtain titanium rough concentrate and tailings I;
[0009] (2) Preparation of modified collector: The high-efficiency activator and unsaturated fatty acid are mixed in an ultrasonic reactor at a mass ratio of 0.5 to 2.5:10, and then placed in an organic reagent reactor and reacted at 40 to 80°C for 1 to 6 hours to obtain the modified unsaturated fatty acid collector.
[0010] (3) Desulfurization: Sulfuric acid, butyl xanthate and 2% sulfuric acid were added sequentially to the titanium crude concentrate slurry obtained in step (1). # The oil is reacted for 1-5 minutes and then subjected to flotation desulfurization to obtain sulfur concentrate and desulfurized tailings.
[0011] (4) Multi-dimensional interface controlled flotation: gangue mineral inhibitor, high-efficiency activator and modified unsaturated fatty acid collector are added to the desulfurized tailings obtained in step (3) in sequence. After each reagent is added, it acts for 3 to 5 minutes. Then, roughing, 2 to 4 scavenging and 1 to 3 cleaning are carried out in sequence to obtain flotation concentrate.
[0012] (5) Deep quality improvement: The flotation concentrate obtained in step (4) is subjected to weak magnetic separation to remove iron, resulting in weak magnetic separation concentrate and weak magnetic separation tailings. The weak magnetic separation tailings are separated using a fine-particle flow film separator to obtain fine-particle flow film separation concentrate and tailings. The tailings are returned to the flotation operation in step (4).
[0013] Furthermore, the strong magnetic separation pre-enrichment in step (1) includes roughing 1 to 2 times, scavenging 1 to 3 times, and cleaning 1 to 3 times, and the middlings in the separation process are returned to the feed operation with a similar titanium dioxide content, forming a closed-loop system.
[0014] Furthermore, the diameter of the coarse selection bar medium is 1-2 mm;
[0015] The diameter of the scanning bar medium is 1-2 mm;
[0016] The magnetic induction intensity of the pre-enriched high-intensity magnetic separation is 1.0T to 1.5T, and the magnetic induction intensity of the scavenging operation is 0.05 to 0.2T higher than that of the coarse separation.
[0017] The selected rod has a medium diameter of 1-3 mm and a magnetic induction intensity of 0.5 T-1.0 T.
[0018] The beneficial effects of adopting the above-mentioned further solutions are as follows: the present invention achieves efficient pre-enrichment of fine-grained ilmenite through precise configuration of strong magnetic separation equipment and control of magnetic separation process structure.
[0019] Furthermore, the titanium dioxide grade in the titanium concentrate described in step (1) is 18% to 25%, and the recovery rate is 65% to 75%.
[0020] The fine-grained titanium ore slurry is the overflow of the thickening equipment in the titanium rock beneficiation process or the tailings in the titanium sand beneficiation process; the TiO2 grade in the fine-grained titanium ore is 3-12%, and the -38μm particle size reaches more than 50%.
[0021] Furthermore, the highly efficient activator in step (2) is a compound containing sulfate and having oxidizing properties; the unsaturated fatty acid has 12 to 20 carbon atoms;
[0022] The beneficial effects of adopting the above-mentioned further solutions are as follows: the highly efficient activator used in this invention can be used as a modifier for unsaturated fatty acid collectors, and it can also be used as a highly efficient activator for ilmenite flotation; and the unsaturated fatty acids not only have the ability to collect ilmenite, but also have the ability to flocculate fine-grained ilmenite.
[0023] The ultrasonic reactor has a power of 100W to 300W and a frequency of 30kHz to 100kHz; the ultrasonic reaction mixing time is 10min to 60min.
[0024] Furthermore, in step (3), sulfuric acid is added to adjust the pH of the titanium crude concentrate slurry to 4-6;
[0025] The dosage of the benzoin is 200g / t to 500g / t;
[0026] The 2 # The oil usage is 20g / t to 50g / t.
[0027] The beneficial effect of adopting the above-mentioned further scheme is that the xanthate flotation method can preferentially float iron sulfide minerals, but it is difficult to float ilmenite, which makes the titanium concentrate produced by subsequent flotation with modified unsaturated fatty acid collectors of higher grade.
[0028] Furthermore, in step (3) of the present invention, titanium crude concentrate with sulfur content <0.1% does not need to be desulfurized. It is only necessary to adjust the pH of the titanium crude concentrate slurry to 4-6 with sulfuric acid before it can enter the ilmenite flotation step.
[0029] Furthermore, in step (4), the dosage of the gangue mineral inhibitor is 300 g / t to 600 g / t, the dosage of the high-efficiency activator is 300 g / t to 800 g / t, and the dosage of the modified unsaturated fatty acid collector is 600 g / t to 1200 g / t.
[0030] Furthermore, the gangue mineral inhibitor mentioned in step (4) is acidified water glass and / or sodium hexametaphosphate;
[0031] The highly efficient activator is a compound containing sulfate and possessing oxidizing properties.
[0032] The beneficial effects of adopting the above-mentioned further scheme are as follows: by organically synergistically inhibiting gangue minerals, enhancing the surface activation of target minerals, and modifying flotation collectors, a multi-dimensional interface-controlled flotation system is established to achieve enhanced recovery of fine-grained titanium ore.
[0033] In step (4) of this invention, A is used to represent the highly efficient activator, and its reaction principle with the ilmenite surface is shown in equations (1) to (4).
[0034]
[0035]
[0036]
[0037]
[0038] The reaction mechanism of modification with unsaturated fatty acid collectors is as follows:
[0039]
[0040] Furthermore, in step (4), the middlings in the flotation process are returned to the feed operation with a titanium dioxide content equivalent to form a closed-loop flotation system;
[0041] In the flotation process, the amount of reagents used in the cleaning and scavenging operations is reduced by 1 / 10 to 1 / 2 respectively compared to the previous stage operation.
[0042] Furthermore, the magnetic field strength of the weak magnetic separation operation in step (5) is 0.1 to 0.4 T.
[0043] Furthermore, the fine-particle flow film separator mentioned in step (5) is a spherical vibrating rotary mineral separator or a grooved shaking table;
[0044] The spherical vibrating rotary mineral separator has a vibration frequency of 25-40Hz and a rotation frequency of 5-15Hz.
[0045] The grooving shaking machine has a stroke of 8-15 mm and a stroke rate of 240-280 strokes / minute.
[0046] The beneficial effects of adopting the above-mentioned further scheme are as follows: weak magnetic separation can effectively separate titanium-containing magnetite from flotation concentrate, while improving the grade of titanium dioxide in titanium concentrate; fine-particle flow film separator further separates gangue minerals entrained in the product, thus ensuring the preparation of high-quality titanium concentrate.
[0047] In step (5) of this invention, the weak magnetic separation concentrate is a titanium-containing magnetite concentrate, wherein TiO2: 15-25% and Fe: 40-55%;
[0048] The fine-particle film separation concentrate is the final titanium concentrate, wherein the titanium dioxide grade is 43-48% and the operating recovery rate is 80-90%.
[0049] For flotation concentrates with TiO2 > 44%, only weak magnetic separation is needed to remove iron; fine-particle film separation is no longer required.
[0050] The beneficial effects of this invention are as follows:
[0051] (1) The high-efficiency activator developed in this invention can not only be used as a surface activator for ilmenite flotation, selectively oxidizing transition metal ions with unstable valence states but not oxidizing the active sites in gangue, which are mostly non-transition metal ions such as calcium and magnesium, but also as a modifier for unsaturated fatty acids, obtaining a modified collector with good dispersibility and low temperature resistance. It has the advantages of being easy to use, not generating secondary pollution and having low reagent cost.
[0052] (2) The high-efficiency activator oxidizes the ferrous ions on the surface of ilmenite, thereby increasing the content of ferric ions and enhancing the adsorption active sites of the collector on the surface of ilmenite, forming more hydrophobic ferric ion unsaturated fatty acid compounds. On the other hand, it modifies the conventional unsaturated fatty acid collector into unsaturated fatty acid molecular recombinants or multifunctional fatty acids, increasing the adsorption capacity of polar groups while increasing the hydrophobic capacity of nonpolar groups. Under the synergistic effect of these factors, the flotation of fine-grained ilmenite is enhanced, thereby improving the grade and recovery rate of flotation concentrate.
[0053] (3) The developed fine-grained titanium ore “pre-enrichment-multi-dimensional interface-controlled flotation-deep upgrading” technology can not only obtain high-quality titanium concentrate and titanium-containing magnetite, but also has flexible process implementation, low cost, small wastewater treatment volume and no secondary pollution. Attached Figure Description
[0054] Figure 1This is a flow chart of the enhanced recovery process of fine-grained titanium ore according to the present invention.
[0055] Figure 2 This is a flowchart illustrating the preparation process of the modified collector of the present invention.
[0056] Figure 3 This is a flow chart of the titanium rough concentrate desulfurization tailings flotation process of the present invention. Detailed Implementation
[0057] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0058] Example 1: Yunnan titanium sand ore gravity separation tailings
[0059] An experimental study was conducted on the tailings from a titanium sand mine in Yunnan Province. The study revealed that the main target mineral in the tailings was ilmenite, with feldspar and pyroxene as the main gangue minerals. The TiO2 grade in the valuable metal compounds was 3.85%, the sulfur content of the impurity element was 0.07%, and the -38μm particle size accounted for 60.42%. The specific implementation methods are as follows:
[0060] (1) Pre-enrichment:
[0061] The tailings slurry of fine-grained titanium sand ore is concentrated to a slurry concentration of 21%, and then subjected to a high-gradient magnetic separation process consisting of a rougher, a cleaner, and a scavenger. The rougher is controlled with a magnetic induction intensity of 1.3T and a rod media diameter of 2mm; the scavenger is controlled with a magnetic induction intensity of 1.35T and a rod media diameter of 1.5mm; and the cleaner is controlled with a magnetic induction intensity of 0.6T and a rod media diameter of 2.5mm. The middlings are sequentially returned to the previous stage to form a closed-loop system, resulting in a titanium rough concentrate with a titanium dioxide grade of 18.9% and an operation recovery rate of 72.5%.
[0062] (2) Preparation of modified collector:
[0063] Potassium persulfate and a fatty acid containing double bonds with 18 carbon atoms were mixed uniformly in an ultrasonic reactor at a mass ratio of 1.5:10. The ultrasonic reactor had a power of 100W and a frequency of 45kHz. After mixing for 20 minutes, the mixture was transferred to an organic reagent reactor and heated at 70℃ for 4 hours to obtain a modified fatty acid collector.
[0064] (3) Desulfurization:
[0065] Sulfuric acid was added to the titanium crude concentrate slurry obtained in step (1) to adjust the pH to 4.5, eliminating the need for flotation desulfurization.
[0066] (4) Multi-dimensional interface control of flotation:
[0067] In the slurry prepared in step (3), acidified water glass was added at 500 g / t for 3 min, followed by the addition of a high-efficiency activator at 700 g / t for 5 min, and then a modified fatty acid collector at 820 g / t for 3 min before roughing. Then, scavenging operations I and II, and cleaning operations I and II were performed. The reagent dosage for scavenging operation I was reduced by 1 / 2 compared to roughing operation, the reagent dosage for scavenging operation II was reduced by 1 / 2 compared to scavenging operation I, the reagent dosage for cleaning operation I was reduced by 1 / 4 compared to roughing operation, and the reagent dosage for cleaning operation II was reduced by 1 / 8 compared to cleaning operation I. The middlings were returned to the previous stage of beneficiation in sequence to form a closed-circuit flotation, obtaining flotation concentrate and tailings II. The titanium dioxide grade in the flotation concentrate was 39.50%, and the recovery rate was 81.4%.
[0068] (5) Deep quality improvement
[0069] The flotation concentrate obtained in step (4) was subjected to weak magnetic separation to remove iron. The magnetic field strength of the weak magnetic separation operation was 0.25T, resulting in titanium-bearing magnetite concentrate and weak magnetic separation tailings. The titanium-bearing magnetite concentrate contained TiO2: 22.5% and Fe: 43.5%. The weak magnetic separation tailings were then separated using a grooved shaking table with a stroke of 9mm and a stroke rate of 270 times / min, resulting in titanium concentrate and grooved shaking table tailings. The titanium concentrate contained 46.47% titanium dioxide, with an operation recovery rate of 86.6%. The tailings were returned to the flotation operation in step (4).
[0070] A comparative example was set up according to the scheme of Example 1. The difference between the comparative example and Example 1 is that no high-efficiency activator was added, but an unmodified fatty acid collector with 18 carbon atoms containing double bonds was added, resulting in a flotation concentrate with a TiO2 grade of 38.41% and an operating recovery rate of 69.2%. Alternatively, a high-efficiency activator and an unmodified fatty acid with 18 carbon atoms containing double bonds were added, resulting in a flotation concentrate with a TiO2 grade of 39.32% and an operating recovery rate of 77.52%. Comparing the three methods, it was found that the addition of a high-efficiency activator to activate ilmenite and a modified collector resulted in the highest titanium dioxide grade and recovery rate of the ilmenite concentrate, as shown in Table 1.
[0071] Table 1
[0072]
[0073] Example 2: Fine-grained titanium ore from an ilmenite beneficiation plant in Sichuan
[0074] An experimental study was conducted on the overflow of a sloping plate thickener at a titanium ore beneficiation plant in Sichuan Province. The study revealed that the main target minerals in the tailings were titanomagnetite and ilmenite, with the main gangue minerals being pyroxene, amphibole, chlorite, and serpentine. The TiO2 grade in the valuable metal compounds was 10.78%, the sulfur content was approximately 0.7%, and the -38μm particle size accounted for over 82.14%. The specific implementation method is as follows:
[0075] (1) Pre-enrichment:
[0076] The overflow from the inclined plate thickener is concentrated to a pulp concentration of 25%. Then, it undergoes a high-gradient magnetic separation process consisting of a rougher, a cleaner, and a scavenger. The magnetic induction intensity of the rougher is controlled at 1.35T and the rod medium diameter is 1.5mm; the magnetic induction intensity of the scavenger is controlled at 1.45T and the rod medium diameter is 1mm; and the magnetic induction intensity of the cleaner is controlled at 0.7T and the rod medium diameter is 2.0mm. The middlings are sequentially returned to the previous stage to form a closed-loop system, resulting in a titanium rough concentrate with a titanium dioxide grade of 24.32% and an operation recovery rate of 78.6%.
[0077] (2) Preparation of modified collector:
[0078] Ammonium persulfate and a triple-bonded fatty acid with 18 carbon atoms were mixed uniformly in an ultrasonic reactor at a mass ratio of 1.8:10. The ultrasonic reactor had a power of 120W and a frequency of 55kHz. After mixing for 18 minutes, the mixture was transferred to an organic reagent reactor and heated at 65°C for 4.5 hours to obtain a modified fatty acid collector.
[0079] (3) Desulfurization:
[0080] In step (1), sulfuric acid was added sequentially to adjust the pH to 5.0 and reacted for 1 min, followed by the addition of butyl xanthate at 350 g / t for 3 min, and then 2 g / t of butyl xanthate was added at 30 g / t. # The oil was applied for 1 minute, followed by flotation desulfurization to obtain sulfur concentrate and desulfurized tailings.
[0081] (4) Multi-dimensional interface control of flotation:
[0082] In step (3), a combined collector is added to the slurry at a rate of 450 g / t for 3 min. The combined collector is obtained by combining acidified water glass and sodium hexametaphosphate in a mass ratio of 1:1. A high-efficiency activator is added at a rate of 760 g / t for 4 min, and a modified collector is added at a rate of 950 g / t for 3 min. Then, scavenging operations I and II, and cleaning operations I and II are carried out. The reagent dosage for scavenging operation I is reduced by 1 / 2 compared to the roughing operation, the reagent dosage for scavenging operation II is reduced by 1 / 2 compared to scavenging operation I, the reagent dosage for cleaning operation I is reduced by 1 / 5 compared to the roughing operation, and the reagent dosage for cleaning operation II is reduced by 1 / 7 compared to cleaning operation I. The middlings are returned to the previous stage of beneficiation in sequence to form a closed-circuit flotation, and flotation concentrate and tailings II are obtained. The titanium dioxide grade in the flotation concentrate is 45.85%, and the recovery rate is 84.67%.
[0083] (5) Deep quality improvement
[0084] The flotation concentrate obtained in step (4) was subjected to weak magnetic separation to remove iron. The magnetic field strength of the weak magnetic separation operation was 0.20T, and titanium-containing magnetite concentrate and weak magnetic separation tailings were obtained. The titanium-containing magnetite concentrate had TiO2 of 22.45% and Fe of 48.55%, and the weak magnetic separation tailings, which is the final titanium concentrate, had TiO2 of 47.68%. The recovery rate of the operation was 88.95%.
[0085] A comparative example was set up according to the scheme of Example 2. The difference between the comparative example and Example 2 is that no high-efficiency activator was added. Instead, an unmodified collector with 18 carbon atoms containing triple bonds was added for comparative experiments, resulting in a flotation concentrate with a TiO2 grade of 44.78% and an operating recovery rate of 72.5%. Alternatively, a high-efficiency activator and an unmodified collector with 18 carbon atoms containing triple bonds were added, resulting in a flotation concentrate with a TiO2 grade of 46.32% and an operating recovery rate of 75.76%. Comparing the three methods, it was found that the addition of a high-efficiency activator to activate ilmenite and a modified collector resulted in the highest titanium dioxide grade and recovery rate in the ilmenite concentrate, as shown in Table 2.
[0086] Table 2
[0087]
[0088] Example 3: Fine-grained titanium ore from an ilmenite beneficiation plant in northern China
[0089] An experimental study was conducted on the overflow of a sloping plate thickener in a northern ilmenite beneficiation plant. The study revealed that the main target minerals in the tailings were titanomagnetite and ilmenite, with plagioclase and pyroxene as the main gangue minerals. The TiO2 grade in the valuable metal compounds was 8.35%, the sulfur content was approximately 0.07%, and the -38μm particle size accounted for 86.34%. The specific implementation method is as follows:
[0090] (1) Pre-enrichment:
[0091] The overflow from the inclined plate thickener is concentrated to a pulp concentration of 24%. Then, it undergoes a high-gradient magnetic separation process with one rougher, one cleaner, and two scavengers. The magnetic induction intensity of the rougher is controlled at 1.25T and the rod medium diameter is 2.5mm, the magnetic induction intensity of the scavenger is 1.4T and the rod medium diameter is 1.5mm, and the magnetic induction intensity of the cleaner is 0.55T and the rod medium diameter is 2.5mm. The middlings are sequentially returned to the previous stage to form a closed-loop system, resulting in a titanium rough concentrate with a titanium dioxide grade of 21.46% and an operation recovery rate of 73.89%.
[0092] (2) Preparation of modified collector:
[0093] Sodium persulfate and a fatty acid with two double bonds and 18 carbon atoms were mixed uniformly in an ultrasonic reactor at a mass ratio of 2.1:10. The ultrasonic reactor had a power of 145W and a frequency of 58kHz. After mixing for 40 minutes, the mixture was transferred to an organic reagent reactor and heated at 72℃ for 4.3 hours to obtain a modified fatty acid collector.
[0094] (3) Desulfurization:
[0095] Sulfuric acid was added to the titanium crude concentrate slurry obtained in step (1) to adjust the pH to 4.5.
[0096] (4) Multi-dimensional interface control of flotation:
[0097] In the slurry prepared in step (3), acidified water glass was added at 560 g / t for 3 min, a high-efficiency activator at 755 g / t for 4 min, and a modified collector at 1020 g / t for 3 min. Then, scavenging I and scavenging II operations and cleaning I and cleaning II operations were carried out. The reagent dosage for scavenging I was reduced by 1 / 2 compared to the roughing operation, the reagent dosage for scavenging II was reduced by 1 / 2 compared to scavenging I, the reagent dosage for cleaning I was reduced by 1 / 6 compared to the roughing operation, and the reagent dosage for cleaning II was reduced by 1 / 8 compared to cleaning I. The middlings were returned to the previous stage of beneficiation in sequence to form a closed-circuit flotation, obtaining flotation concentrate and tailings II. The titanium dioxide grade in the flotation concentrate was 44.77%, and the recovery rate was 81.39%.
[0098] (5) Deep quality improvement
[0099] The flotation concentrate obtained in step (4) was subjected to weak magnetic separation to remove iron. The magnetic field strength of the weak magnetic separation operation was 0.35T, and titanium-containing magnetite concentrate and weak magnetic separation tailings were obtained. The titanium-containing magnetite concentrate had TiO2 of 23.76% and Fe of 51.36%, and the weak magnetic separation tailings, which is the final titanium concentrate, had TiO2 of 46.12%. The recovery rate of the operation was 86.37%.
[0100] A comparative example was set up according to the scheme of Example 3. The difference between the comparative example and Example 3 is that no high-efficiency activator was added. Instead, an unmodified fatty acid collector with 18 carbon atoms and two double bonds was added for comparative experiments, resulting in a flotation concentrate with a TiO2 grade of 41.36% and an operating recovery rate of 73.12%. Alternatively, a high-efficiency activator and an unmodified fatty acid collector with 18 carbon atoms and two double bonds were added, resulting in a flotation concentrate with a TiO2 grade of 44.05% and an operating recovery rate of 77.82%. Comparing the three methods, it was found that the addition of a high-efficiency activator to activate ilmenite and a modified collector resulted in the highest titanium dioxide grade and recovery rate in the ilmenite concentrate, as shown in Table 3.
[0101] Table 3
[0102]
[0103]
[0104] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.
Claims
1. A method for enhancing the recovery of fine-grained titanium ore, characterized in that, Includes the following steps: (1) Pre-enrichment: The overflow from the inclined plate thickener is concentrated to achieve a pulp concentration of 25%. Then, it undergoes a high-gradient magnetic separation process consisting of a rougher, a cleaner, and a scavenger. The magnetic induction intensity of the rougher is controlled at 1.35T and the diameter of the rod medium is 1.5mm. The magnetic induction intensity of the scavenger is controlled at 1.45T and the diameter of the rod medium is 1mm. The magnetic induction intensity of the cleaner is controlled at 0.7T and the diameter of the rod medium is 2.0mm. The middlings are sequentially returned to the previous stage to form a closed-loop system, resulting in titanium rough concentrate. (2) Preparation of modified collector: Ammonium persulfate and a fatty acid with 18 carbon atoms containing triple bonds were mixed uniformly in an ultrasonic reactor at a mass ratio of 1.8:
10. The ultrasonic reactor had a power of 120W and a frequency of 55kHz. After mixing for 18 minutes, the mixture was transferred to an organic reagent reactor and heated at 65℃ for 4.5 hours to obtain a modified fatty acid collector. (3) Desulfurization: In step (1), sulfuric acid was added sequentially to adjust the pH to 5.0 and reacted for 1 min, followed by the addition of butyl xanthate at 350 g / t for 3 min, and then 2 g / t of butyl xanthate was added at 30 g / t. # The oil was applied for 1 minute, followed by flotation desulfurization to obtain sulfur concentrate and desulfurized tailings. (4) Multi-dimensional interface-controlled flotation: In the slurry prepared in step (3), a combined inhibitor is added at 450 g / t for 3 min. The combined inhibitor is obtained by combining acidified water glass and sodium hexametaphosphate in a mass ratio of 1:
1. A high-efficiency activator is added at 760 g / t for 4 min, and a modified collector is added at 950 g / t for 3 min. Then, scavenging I and scavenging II operations and cleaning I and cleaning II operations are carried out. The dosage of reagents for scavenging I is reduced by 1 / 2 compared to the roughing operation, the dosage of reagents for scavenging II is reduced by 1 / 2 compared to scavenging I, the dosage of reagents for cleaning I is reduced by 1 / 5 compared to the roughing operation, and the dosage of reagents for cleaning II is reduced by 1 / 7 compared to cleaning I. The middlings are returned to the previous stage of beneficiation in sequence to form a closed-circuit flotation to obtain flotation concentrate and tailings II. (5) Deep quality improvement The flotation concentrate obtained in step (4) is subjected to weak magnetic separation to remove iron. The magnetic field strength of the weak magnetic separation operation is 0.20T, and titanium-containing magnetite concentrate and weak magnetic separation tailings are obtained.
Citation Information
Patent Citations
Recovering method for ultra-fine-grain ilmenite in inclined plate thickener overflow
CN109433406A
Ilmenite activation flotation method
CN110433964A
Ilmenite concentration process
CN103721841A
Recovery method of ultrafine fine fraction ilmenite in strong magnetic separation tailings
CN109433407A
Mineral separation and recovery process for micro-fine-particle ilmenite
CN114985098A