A mineral recovery method of high-phosphorus vanadium-titanium magnetite tailings

Abstract

The application discloses a mineral recovery method of high-phosphorus vanadium-titanium magnetite tailings, and relates to the technical field of vanadium-titanium magnetite beneficiation. The application obtains coarse-grained concentrate and fine-grained concentrate through cyclone classification, interference bed separation and fine screen classification after one-stage strong magnetic roughing, and the coarse-grained concentrate is subjected to multiple spiral chute gravity separation to obtain gravity separation middlings, which can be returned to the existing titanium ore grinding operation section of the beneficiation plant to recover the coarse-grained titanium ore in the tailings; the fine-grained concentrate is concentrated and subjected to two-stage strong magnetic separation to obtain second strong magnetic concentrate, which is used as the flotation raw material to realize flotation desulfurization, flotation dephosphorization and flotation of titanium ore, and the fine-grained titanium ore in the tailings can be recovered; the high-phosphorus vanadium-titanium magnetite tailings are subjected to multiple ways of strong magnetic separation, spiral chute gravity separation, flotation desulfurization and flotation dephosphorization to remove associated minerals and gangue minerals multiple times, the loss rate of valuable elements is controlled, the ore processing capacity of the whole process is reduced, and the production efficiency is improved; the flotation desulfurization and the flotation dephosphorization are both under neutral conditions, and the PH value is adjusted for sulfur flotation and phosphorus flotation, the amount of adjusting agent in the flotation process is greatly reduced, the negative influence on the titanium flotation process is reduced, and high-quality titanium concentrate can be obtained.

Description

Technical Field

[0001] This invention relates to the field of vanadium-titanium magnetite beneficiation technology, and in particular to a mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings. Background Technology

[0002] my country's total reserves of vanadium-titanium magnetite ore exceed 20.1 billion tons, mainly distributed in the Panxi region of Sichuan, Chengde region of Hebei, Chaoyang region of Liaoning, and Hami region of Xinjiang. Among them, the Panxi region of Sichuan accounts for 75.95% of the national reserves of vanadium-titanium magnetite ore, 95.61% of TiO2, and 97.14% of V2O5, making it an important large-scale energy resource base in my country.

[0003] Currently, the conventional beneficiation process for vanadium-titanium magnetite in the Panxi region is the "step grinding and beneficiation-magnetic separation for iron-flotation for titanium" process, which can achieve efficient development and utilization of vanadium-titanium magnetite. Although step grinding and beneficiation can minimize grinding time, over-grinding is still unavoidable, resulting in a large amount of fine ilmenite mixed in with the tailings of high-phosphorus vanadium-titanium magnetite. In this type of beneficiation process, the fine ilmenite minerals in the tailings cannot be recovered and utilized, which to some extent causes a waste of resources.

[0004] Furthermore, the intergranular spaces between anatase aggregates are filled with a large amount of extremely fine calcite or sphene. These fine-grained gangues, such as calcite or sphene, have a relatively high density and a particle size of less than five micrometers. With current beneficiation processes, fine grinding and liberation are difficult, and calcite or sphene can easily enter the titanium ore with it, which is not conducive to the flotation recovery of ilmenite and leads to a reduction in the quality of the titanium ore after flotation.

[0005] In addition, the phosphorus content of vanadium-titanium magnetite in the mining area is currently increasing. With the current mineral recovery process, sulfur and phosphate minerals are not fully recovered and remain in the titanium beneficiation tailings, which increases the difficulty of recovering titanium ore from flotation and exacerbates the loss of titanium ore resources. Therefore, it is necessary to explore a suitable mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings to improve the recovery rate of titanium ore in the tailings. Summary of the Invention

[0006] The purpose of this invention is to address the problems of unrecoverable fine ilmenite in high-phosphorus vanadium-titanium magnetite tailings, reduced titanium ore quality due to the presence of small-particle-size impurities, and difficulty in recovering flotation titanium ore due to insufficient recovery of iron-sulfur-phosphate ore. This invention provides a mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings, comprising the following steps:

[0007] S1: After a strong magnetic roughing process, the high-phosphorus vanadium-titanium magnetite tailings are used to obtain strong magnetic rough concentrate and first strong magnetic tailings; the strong magnetic rough concentrate is then subjected to hydrocyclone classification and interference bed separation to obtain underflow ore and overflow ore.

[0008] S2: The overflow ore is finely screened and classified to obtain oversize ore and undersize ore;

[0009] S3: The undersize ore is concentrated and then subjected to two-stage strong magnetic cleaning to obtain fine-grained concentrate and a second strong magnetic tailings; the fine-grained concentrate is concentrated to form flotation feedstock; the TiO2 grade of the second strong magnetic tailings is less than 3.31%; the TiO2 grade of the flotation feedstock is greater than 15%.

[0010] The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings described in this invention, compared to the traditional beneficiation process which only involves a first-stage strong magnetic separation and a second-stage strong magnetic separation combined with fine screening, allows for the separation of the rough concentrate into larger-particle underflow ore and smaller-particle overflow ore after the first-stage strong magnetic roughing. The smaller-particle overflow ore is then further separated by fine screening to obtain smaller and more uniform underflow ore. This smaller and more uniform underflow ore is then subjected to a second-stage strong magnetic separation to obtain a fine-particle concentrate. Finally, the fine concentrate is further separated in step S3. After concentration, it is used as flotation feedstock for titanium ore flotation, thereby recovering the fine-grained titanium ore portion from the high-phosphorus vanadium-titanium magnetite tailings. This results in a flotation feedstock pulp concentration of 45% and a TiO2 grade of 18.53%, with the titanium dioxide grade in the fine-grained concentrate exceeding 15%, thus improving resource recovery efficiency. Furthermore, after hydrocyclone classification and interference bed separation, the coarse gangue that has not been finely ground and liberated is separated into the underflow and will not follow the fine-grained concentrate into the titanium flotation process, thus not affecting the quality of the flotation titanium ore and improving the beneficiation quality of the selected titanium ore.

[0011] Preferably, in the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention, the particle size control value for fine screening is selected as 0.045 mm.

[0012] As a preferred embodiment of the present invention, by selecting a particle size control value of 0.045 mm for the fine screening, the undersize ore with a particle size ≤ 0.045 mm obtained after fine screening is concentrated, subjected to two-stage strong magnetic concentrating, and then further concentrated to obtain minerals with a pulp concentration of 45% and a TiO2 grade of 18.50% as flotation raw materials. The titanium dioxide grade in the fine concentrate is greater than 15%, and the fine-grained titanium ore in the high-phosphorus vanadium-titanium magnetite tailings is recovered with a high recovery rate, further improving the resource recovery rate. Meanwhile, the oversize ore with a particle size ≥ 0.045 mm will not enter the flotation of titanium along with the fine concentrate, thus not affecting the quality of the titanium ore after flotation, thereby further improving the beneficiation quality of the selected titanium ore.

[0013] Preferably, in the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention, the magnetic field strength of the first-stage strong magnetic field is 10000GS, and the magnetic field strength of the second-stage strong magnetic field is 5000GS.

[0014] As a preferred embodiment of the present invention, a strong magnetic field is applied before hydrocyclone classification, interference bed separation, and fine screening. This not only achieves primary magnetic separation of high-phosphorus vanadium-titanium magnetite tailings, but also, given the specific nature of the material used in the present invention (high-phosphorus vanadium-titanium magnetite), the magnetic field strength of the first strong magnetic field is selected as 10000GS, which improves the efficiency of magnetic separation. A second strong magnetic field is then applied after hydrocyclone classification, interference bed separation, and fine screening. The magnetic field strength of the second strong magnetic field is preferably 5000GS, and this is combined with the overflow ore after fine screening for secondary magnetic separation. Since the smaller gaps in the media box are more conducive to improving the concentrate grade in the strong magnetic separation stage, unclassified strong magnetic coarse concentrate is prone to clogging the media box when entering the strong magnetic separation operation, leading to a poor strong magnetic separation process. Therefore, by adjusting the magnetic field strength of the strong magnetic field in two stages and coordinating it with the sequence of hydrocyclone classification, interference bed separation, and fine screening, a balance is achieved between the classification particle size and the strong magnetic operation in terms of recovery rate and operating efficiency, further optimizing the recovery rate and production efficiency.

[0015] Preferably, the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention, wherein step S1 specifically includes the following steps:

[0016] S11: The strong magnetic coarse concentrate is classified by a hydrocyclone into a first underflow ore and a first overflow ore;

[0017] S12: The first bottom flow ore is separated by interference bed separation to obtain the second bottom flow ore and the second overflow ore.

[0018] As a preferred embodiment of the present invention, the coarse concentrate after the first stage of strong magnetic separation is classified by hydrocyclone classification, separating it into a first underflow ore with a larger particle size and a first overflow ore with a smaller particle size. The first underflow ore with a larger particle size is then separated into a second underflow ore with a larger particle size and higher density through a disturbance bed. This classification followed by separation fully considers the properties of the titanium mineral body filled with fine gangue. Since coarse concentrate with a smaller density but larger particle size would reduce the efficiency of fine screening and easily clog the medium box of the second stage of strong magnetic separation if it enters the fine screening, this method avoids the coarse concentrate that was separated before classification entering the second stage of strong magnetic separation and clogging the medium box, making the fine screening and second stage of strong magnetic separation operations smoother and improving the mineral processing efficiency. On the other hand, the uniform fine minerals entering the second stage of strong magnetic separation reduce the amount of strong magnetic separation required, which can reduce electricity consumption and improve production efficiency.

[0019] Preferably, in the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention, step S3 further includes the following step:

[0020] S31: The underflow ore and the overflow ore are jointly subjected to at least one roughing process through a spiral chute to obtain gravity concentrate and gravity tailings;

[0021] S32: The gravity concentrate is recovered through at least three superimposed spiral sluices to obtain gravity concentrate; the TiO2 grade of the gravity concentrate is greater than 25%; after the recovered gravity concentrate is ground, it is put back into the titanium beneficiation process of the concentrator to start beneficiation.

[0022] S33: The gravity separation coarse tailings are recovered by at least one scavenging in a spiral chute to obtain gravity separation tailings; the TiO2 grade of the gravity separation tailings is less than 2.00%.

[0023] In a preferred embodiment of the present invention, the fine gangue that has not been finely ground and dissociated is sorted into the underflow, where it can be combined with the oversize ore for spiral sluice gravity separation to obtain gravity concentrate and gravity tailings. With the help of S1 and S2, there are fewer fine particles in the underflow, which is more conducive to the subsequent spiral sluice separation and pre-enrichment of coarse ilmenite particles, so that the titanium dioxide grade of the gravity concentrate is greater than 25%. After the gravity concentrate is ground, it is subjected to the titanium beneficiation process in the beneficiation plant, so that the larger particles of ore in the tailings are ground and separated again, so that the titanium ore contained in the gravity concentrate can be recovered as much as possible, and the TiO2 grade of the gravity tailings is lower than 2.00%. The reduction of the titanium ore grade in the gravity tailings indicates that the titanium ore has been further recovered, thereby further improving the final titanium ore grade.

[0024] Preferably, the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention further includes step S4: flotation desulfurization of the flotation raw material, specifically including the following steps:

[0025] S42: Add 600g / t of sulfuric acid to the first sulfur ore and perform one refining process to obtain minerals including the second and third sulfur ores;

[0026] S43: After adding 300g / t sulfuric acid to the second sulfur ore and performing a second cleaning, the resulting first middlings are returned to the first cleaning, and the resulting concentrate is added to 200g / t sulfuric acid for a third cleaning. The minerals obtained from the third cleaning include cobalt-sulfur concentrate and second middlings. The second middlings are returned to the second cleaning. The sulfur-cobalt concentrate has a sulfur grade of 30.79%.

[0027] S44: Add 100g / t of sulfuric acid to the third sulfur ore and scavenging it. The resulting minerals are returned to the primary beneficiation process and used to form floating sulfur tailings.

[0028] As a preferred embodiment of the present invention, the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings, through a flotation desulfurization process, can obtain a sulfur-cobalt concentrate with an S grade of 30.79% and an S recovery rate of 83.04%, which can be sold as a product to generate economic benefits. Furthermore, the S grades in the generated sulfur tailings and phosphorus feedstock are 0.139% and 0.053%, respectively, indicating that the combined effect of S1-S3 classification is good for sulfur recovery and separation, further reducing the S content in the sulfur tailings and phosphorus feedstock, and to a certain extent eliminating the negative impact of associated sulfur elements on subsequent titanium resource recovery, while recovering a high-grade sulfur-cobalt concentrate. Both are carried out under neutral conditions and after roughing, the pH value is adjusted for sulfur and phosphorus refining, which significantly reduces the amount of conditioning agent used in the flotation process and reduces the negative impact on the titanium flotation process, promoting the acquisition of high-quality titanium concentrate.

[0029] Phosphorus is a harmful impurity in titanium concentrate, and the industry generally requires the phosphorus content in titanium concentrate to be below 0.05%. For ordinary low-phosphorus vanadium-titanium magnetite, the phosphorus content in titanium concentrate can be reduced by adding inhibitors; however, when the phosphorus content in the flotation feed is greater than 0.3%, such as the 1% phosphorus content in the high-phosphorus vanadium-titanium magnetite tailings of this invention, it affects the acquisition of titanium concentrate products with higher titanium ore grades; therefore, a further improvement to the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of this invention involves flotation dephosphorization of the flotation feed after flotation desulfurization, specifically including the following steps:

[0030] S45: The flotation dephosphorization test was carried out on the flotation raw material, 200 g / t of collector was added and roughing was performed once. The minerals obtained included first phosphate rock and flotation titanium raw material. The collector is a composite reagent composed of oxidized paraffin soap and MES in a ratio of 9:1. The MES is sodium methyl ester sulfonate of fatty acids, which is an anionic collector. The TiO2 grade in the flotation titanium raw material is 18.53%.

[0031] S46: The first phosphate ore is recycled at least once to obtain phosphorus-containing tailings; the recycled second phosphate ore is returned to S45 for roughing again.

[0032] As a preferred embodiment of the present invention, after obtaining phosphorus feedstock through flotation desulfurization, further flotation dephosphorization of the phosphorus feedstock yields phosphorus-containing tailings with a phosphorus grade of 6.60% and a phosphorus recovery rate of 60.56%. This not only recovers phosphorus tailings but also further enriches them to obtain qualified phosphorus concentrate products, improving the recovery rate of phosphorus ore in high-phosphorus vanadium-titanium magnetite tailings, thereby increasing economic benefits. Furthermore, by combining flotation titanium feedstock obtained after S1-S3, flotation desulfurization, and flotation dephosphorization, the influence of sulfur and phosphorus ore on the flotation titanium ore is eliminated, increasing the titanium ore grade in the flotation titanium feedstock to 18.53%. This facilitates titanium recovery during the flotation titanium beneficiation stage, reduces the difficulty of flotation titanium beneficiation, and further achieves efficient separation and recovery of titanium ore. All processes are carried out under neutral conditions, and after roughing, the pH value is adjusted for sulfur flotation and phosphorus flotation beneficiation, significantly reducing the amount of conditioning agent used in the flotation process and minimizing the negative impact on the flotation titanium beneficiation process, thus promoting the acquisition of high-quality titanium concentrate.

[0033] Preferably, the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention involves flotation of titanium ore after flotation dephosphorization of the titanium raw material, specifically including the following steps:

[0034] S47: Select titanium raw materials for flotation titanium beneficiation test, add 1500g / t sulfuric acid, 1000g / t inhibitor, 2500g / t collector and 300g / t diesel oil and roughing once to obtain the first titanium concentrate and the first titanium tailings.

[0035] The first titanium concentrate is added with 1200g / t of sulfuric acid and 500g / t of collector and then subjected to a first cleaning process to obtain the second titanium concentrate and the first titanium middlings. The first titanium middlings is returned to the roughing process for further separation.

[0036] After adding 800 g / t of sulfuric acid and 300 g / t of collector to the second titanium concentrate and performing a second cleaning process, the third titanium concentrate and the second titanium middlings are obtained. The second titanium middlings are returned to the first cleaning process for further separation.

[0037] The third titanium concentrate is treated with 400 g / t sulfuric acid and 200 g / t collector, and after three cleaning processes, the fourth titanium concentrate and the third titanium middlings are obtained. The third titanium middlings are returned to the second cleaning process for further separation.

[0038] 400 g / t of sulfuric acid was added to the fourth titanium concentrate and it was cleaned four times to obtain titanium concentrate and fourth titanium middlings. The fourth titanium middlings was returned to the third cleaning process for further separation.

[0039] After adding 300 g / t of sulfuric acid and 200 g / t of collector to the first titanium tailings and scavenging, the fifth titanium middlings and flotation tailings are obtained. The fifth titanium middlings are returned to the roughing process for further separation. The TiO2 grade of the titanium concentrate reaches 47.50%, and the TiO2 grade of the flotation tailings is less than 2.50%.

[0040] In a preferred embodiment of the present invention, the titanium ore is sequentially subjected to hydrocyclone classification, interference bed separation, and fine screening for desulfurization and dephosphorization, or sequentially subjected to hydrocyclone classification, interference bed separation, fine screening, spiral sluice gravity separation, desulfurization, and dephosphorization. This increases the recovery and utilization of finer-grained titanium ore. Alternatively, the tailings, which are denser than fine-grained gangue such as calcite or sphene, are further recovered after classification and re-grinding. Furthermore, the influence of sulfur and phosphate ores on the flotation of titanium ore is eliminated, thereby increasing the grade of titanium concentrate from flotation to 47.50%, increasing the titanium ore recovery rate to 91.46%, and reducing the TiO2 grade in the flotation tailings to only 2.46%.

[0041] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0042] 1. This invention, after a first stage of strong magnetic roughing, further classifies the rough concentrate using hydrocyclones and interference bed separation, separating the large-particle underflow ore and the small-particle overflow ore. The small-particle overflow ore is then further classified by fine screening to obtain small and uniform underflow ore. The small and uniform underflow ore is then subjected to a second stage of strong magnetic refining to obtain a fine-particle concentrate. In step S3, the fine-particle concentrate is concentrated and used as flotation feedstock, thereby recovering the fine-particle titanium ore from the tailings of high-phosphorus vanadium-titanium magnetite. This results in a flotation feedstock pulp concentration of 45% and a TiO2 grade of 18.53%, with a titanium dioxide grade greater than 15% in the fine concentrate, thus improving resource recovery efficiency.

[0043] 2. After hydrocyclone classification and interference bed separation, the coarse gangue that has not been finely ground and separated is separated into the underflow and will not follow the fine concentrate into the flotation of titanium, thus not affecting the quality of the titanium ore after flotation, thereby improving the beneficiation quality of the selected titanium ore. Attached Figure Description

[0044] Figure 1 This is a schematic flowchart of the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings according to the present invention.

[0045] Figure 2 This is a schematic diagram of the flotation desulfurization process described in this invention;

[0046] Figure 3 This is a schematic diagram of the flotation dephosphorization process described in this invention;

[0047] Figure 4 This is a schematic diagram of the flotation process for titanium selection according to the present invention. Detailed Implementation

[0048] The present invention will now be described in detail with reference to the accompanying drawings.

[0049] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0050] It should be noted that the high-phosphorus vanadium-titanium magnetite tailings described in this invention come from the beneficiation plant of Chongqing Iron & Steel Xichang Mining Co., Ltd. Before the mineral recovery of this invention, the TiO2 grade of the high-phosphorus vanadium-titanium magnetite tailings was 5.06%, the S grade was 0.33%, and the P content was 1%.

[0051] Example 1

[0052] This embodiment provides a mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings, referencing... Figure 1 The process shown includes the following steps:

[0053] S1: After a strong magnetic roughing process, the high-phosphorus vanadium-titanium magnetite tailings are converted into strong magnetic rough concentrate and first strong magnetic tailings. The strong magnetic rough concentrate is then classified by hydrocyclone and separated by interfering bed to obtain underflow ore and overflow ore. The particle size of the underflow ore is larger than that of the overflow ore.

[0054] S2: The overflow ore is finely screened and classified to obtain oversize ore and undersize ore, with the particle size of the oversize ore being larger than that of the undersize ore.

[0055] S3: After the undersize ore is concentrated, it undergoes two-stage strong magnetic cleaning to obtain fine-grained concentrate and a second strong magnetic tailings; the fine-grained concentrate is concentrated to form flotation feedstock; the TiO2 grade of the second strong magnetic tailings is less than 3.31%; the TiO2 grade of the flotation feedstock is greater than 15%.

[0056] Specifically, the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings described in this embodiment can recover titanium ore or other minerals from graded fine-grained ore. After step S1, the vanadium-titanium magnetite tailings are roughed by strong magnetic separation to obtain strong magnetic rough concentrate, and the first strong magnetic tailings are discarded. The strong magnetic rough concentrate is then graded and separated by hydrocyclones and interference beds respectively.

[0057] In this embodiment, the magnetic field strength is selected according to the actual mineral processing needs. The magnetic field strength of the first stage magnetic field can be selected from 8000GS to 12000GS, and the magnetic field strength of the second stage strong magnetic field can be selected from 4000Gs to 8000Gs. Preferably, the magnetic field strength of the first stage strong magnetic field is 10000GS, and the magnetic field strength of the second stage strong magnetic field is 5000GS. With the control of the cyclone grading particle size and the fine screen grading particle size, the concentration of the concentrated underflow of the undersize ore can be obtained as 30%, the concentration of the concentrated underflow after the second stage strong magnetic field is 45%, and the TiO2 grade of the concentrate after the second stage strong magnetic field is greater than 15%.

[0058] For details, please refer to Figure 1 The process flow shown controls the particle size of hydrocyclone classification and interference bed separation within the range of -0.15mm to +0.075mm. For example, overflow ore with a particle size ≤0.075mm enters fine screening for classification, followed by concentration and two-stage strong magnetic separation; or overflow ore with a particle size ≤0.15mm enters fine screening for classification, followed by concentration and two-stage strong magnetic separation to form flotation raw materials. More specifically, the preferred value for fine screening is 0.045mm. This allows for the acquisition of minerals with a pulp concentration of 45% and a TiO2 grade of 18.53% as flotation raw materials. The titanium dioxide grade in the fine-grained concentrate is greater than 15%, and the TiO2 grade in the second strong magnetic tailings after fine screening is less than 3.31%. The test results are shown in Table 1.

[0059] Table 1: Test Results of Example 1

[0060] Flotation raw materials 13.65 18.53 49.99 coarse concentrate 9.47 10.63 19.89 Second Strong Magnetic Tailings 11.83 3.31 7.76 First strong magnetic tailings 65.02 1.74 22.36 total 100.00 5.06 100.00

[0061] It should be noted that the hydrocyclone classification principle is as follows: under external pressure, the mixture enters the hydrocyclone tangentially, obtaining an external swirling flow; particles with higher density, heavier weight, and larger particle size are ultimately discharged from the underflow port, while components with lower density, lighter weight, and smaller particle size move towards the central axis, forming an internal swirling flow that is discharged through the overflow port, thus achieving separation of two phases with different densities. It should also be noted that the interference bed convection separation principle is as follows: using the feed well of the tangential slurry feed equipment, an upward turbulent water flow is formed through the turbulence plate. Particles with higher density will sink to the bottom of the bed, forming an underflow; while particles with lower density will float on the upper layer, forming an overflow.

[0062] It should be noted that the classification principle of the interference bed separator is as follows: Water is pumped into the distributor at the bottom of the separator at a predetermined pressure and flow rate from the feed well of the tangential feeder. The water is evenly distributed to the bottom of the separator via a turbulence plate, forming an upward turbulent water flow. The descending material encounters the rising water flow, forming an interference layer, also known as a fluidized bed. The particles in the feed undergo disturbed settling motion within the separator. Due to differences in particle density, the settling velocities vary, providing a basis for separation. When a steady state is reached, particles with a density higher than the average density of the interference bed will enter the settling stream and be discharged through the bottom discharge port, while particles with a density lower than the average density of the interference bed will be discharged through the top overflow port.

[0063] Specifically, in this embodiment, S1 includes the following steps: S11: The rough concentrate is classified by a hydrocyclone into a first underflow ore and a first overflow ore, the particle size of the first underflow ore being larger than that of the first overflow ore; S12: The first underflow ore is separated by a disturbing bed to obtain a second underflow ore and a second overflow ore, the density of the second underflow ore being larger than that of the second overflow ore.

[0064] It should be noted that the terms "coarse" and "fine" in the coarse or fine concentrates of this invention are relative terms and are defined only for the convenience of differentiation. They can be selected based on the particle size control value and are not defined as coarse or fine in a general sense.

[0065] The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings described in this embodiment improves the TiO2 grade in the flotation feedstock. This allows for the subsequent titanium beneficiation using conventional flotation methods, thereby increasing the final titanium ore recovery rate.

[0066] Comparative Example 1

[0067] Comparative Example 1 used high-phosphorus vanadium-titanium magnetite tailings with a TiO2 grade of 5.06%, an S grade of 0.33%, and a P content of 1%. The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 only used fine screening after a first-stage strong magnetic roughing, without hydrocyclone classification and interference bed separation. Other parameters, such as magnetic field strength and the selection of fine screening particle size control values, can be set under the same conditions as in Example 1. Specifically, in Comparative Example 1, the high-phosphorus vanadium-titanium magnetite tailings were subjected to a first-stage strong magnetic roughing to obtain a rough concentrate, and the first strong magnetic tailings were discarded. Then, the rough concentrate was subjected to fine screening for coarse and fine classification, with the classification particle size controlled at 0.045 mm. The portion with a particle size smaller than 0.045 mm entered a thickening-second-stage strong magnetic separation-thickening process to obtain a slurry with a concentration of 45% as flotation feedstock. The test results are shown in Table 2.

[0068] Table 2: Results of Comparative Example 1

[0069] Flotation raw materials 11.68 16.39 37.83 coarse concentrate 14.37 12.15 34.51 Second Strong Magnetic Tailings 8.00 3.86 6.10 First strong magnetic tailings 65.95 1.65 21.56 total 100.00 5.06 100.00

[0070] Comparing Table 2 and Table 1, it can be seen that the titanium tailings from the strong magnetic separation of vanadium-titanium magnetite were not subjected to hydrocyclone classification and interference bed separation after the first stage of strong magnetic separation. Only after fine screening and coarse-fine classification, the TiO2 grade of the flotation feedstock decreased to 16.39%, and the TiO2 recovery rate dropped significantly to only 37.83%. Meanwhile, the TiO2 grade in the second strong magnetic tailings was higher than that in Example 1, indicating that the separation effect of Comparative Example 1 was weaker than that of Example 1. Furthermore, the applicant found that during the experiment, the classification efficiency of Comparative Example 1 was only 50% of that of Example 1.

[0071] Example 2

[0072] Based on Example 1, further improvements were made to the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings, with reference to... Figure 1 The process flow shown includes the following step S3:

[0073] S31: The bottom flow ore and the oversize ore are jointly roughed by a spiral chute at least once to obtain gravity concentrate and gravity tailings.

[0074] S32: The gravity concentrate is recovered through at least three superimposed spiral sluices to obtain gravity ore; the TiO2 grade of the gravity ore is greater than 25%; after the recovered gravity ore is ground, it is put back into the titanium beneficiation process of the concentrator to start beneficiation.

[0075] S33: Gravity separation coarse tailings are recovered by at least one scavenging in a spiral chute to obtain gravity separation tailings; the TiO2 grade of the gravity separation tailings is less than 2.00%.

[0076] For details, please refer to Figure 1 As shown, based on Example 1, through the S1-S2 process steps, after the rough concentrate after a strong magnetic field is classified by hydrocyclone classification, interference bed separation and fine screening, not only is a fine concentrate with a smaller particle size finally obtained as flotation raw material, but also underflow ore and overflow ore with a larger particle size than the underflow ore are obtained. For example, underflow ore with a particle size greater than 0.15 mm or greater than 0.075 mm and overflow ore with a particle size greater than 0.045 mm are obtained. After being roughed at least once by spiral chute, they are then subjected to at least three superimposed cleaning processes and at least one scavenging process to recover titanium ore from the rough concentrate and obtain gravity concentrate and gravity tailings.

[0077] In this embodiment, the test conditions in steps S1-S2 are set to the test conditions selected in the embodiment, such as magnetic field strength and classification particle size settings, using the optional range provided in embodiment 1. The test results are shown in Table 3. Through the combination of S3 and S1-S2, and then through spiral sluice gravity separation, the TiO2 grade of the gravity-separated ore is 28.53%, which can be returned to the original process of the beneficiation plant. The TiO2 grade of the gravity-separated tailings is 1.56%, indicating that the spiral sluice gravity separation further increases the recovery of titanium ore, reduces the titanium ore grade in the tailings, and further recovers and utilizes titanium resources.

[0078] Table 3: Test Results of Example 2

[0079]

[0080]

[0081] It should be noted that spiral sluice gravity separation is understood as using the difference in specific gravity of different mineral particles to achieve separation. Although specific gravity is the main basis for separation, the size and shape of the particles also affect their behavior in the spiral sluice. Larger or irregularly shaped particles may settle more easily to form coarse minerals, while smaller or spherical particles may move more easily with the water flow to form fine minerals. Due to gravity, mineral particles with higher density will slide down the slope more quickly to form heavy minerals, while particles with lower density will move more slowly or be discharged with the water flow as light minerals.

[0082] In this embodiment, the coarse and heavy ore particles formed by spiral sluice gravity separation are further refined at least three times to form gravity-separated ore. The fine and light ore particles formed are then scavenged and recovered to form gravity-separated tailings. The lower the TiO2 grade in the gravity-separated tailings, the better the separation effect of the titanium ore using this invention.

[0083] Comparative Example 2

[0084] A spiral gravity separation test was conducted on the coarse concentrate obtained in Comparative Example 1. The process steps and process parameters of S3 in Example 2 were selected. The spiral gravity separation is a traditional process of primary roughing, tertiary cleaning and primary scavenging. The test results are shown in Table 4 below. The TiO2 grade of the gravity concentrate obtained in Comparative Example 2 is lower than that in Example 2, while the TiO2 grade of the gravity tailings is higher than that in Example 2, indicating that the effect of Comparative Example 2 is weaker than that of Example 2.

[0085] Table 4: Experimental Results of Comparative Example 2

[0086]

[0087]

[0088] Example 3

[0089] In this embodiment, based on Embodiment 1, with reference to Figure 2 The process shown in the diagram, specifically step S4, includes the following steps:

[0090] S41: Select flotation feedstock, add 600g / t xanthate and 150g / t frother and perform roughing in one stage. The minerals obtained include flotation phosphate feedstock and first sulfur ore; the sulfur grade of the flotation phosphate feedstock is 0.053%.

[0091] S42: Add 600g / t of sulfuric acid to the first sulfur ore and perform one refining process to obtain minerals including the second and third sulfur ores;

[0092] S43: After adding 300g / t sulfuric acid to the second sulfur ore and performing a second cleaning, the first middlings obtained are returned to the first cleaning, and the obtained concentrate is added with 200g / t sulfuric acid for a third cleaning. The minerals obtained include cobalt-sulfur concentrate and second middlings; the sulfur grade of the cobalt-sulfur concentrate is 30.79%.

[0093] S44: Add 100g / t of sulfuric acid to the third sulfur ore and scavenging it. The resulting minerals are returned to the primary beneficiation process and used to form floating sulfur tailings.

[0094] Specifically, flotation desulfurization test: The flotation raw material obtained in Example 1 was subjected to flotation desulfurization test. The dosage of each reagent was 600 g / t xanthate, 150 g / t frother, and 1200 g / t sulfuric acid. The results of the flotation desulfurization test are shown in Table 5.

[0095] Table 5: Test results of flotation desulfurization using the flotation feedstock of Example 1

[0096] cobalt sulfide concentrate 0.89 30.79 83.04 floating sulfur tailings 4.01 0.139 1.69 Floating phosphorus raw materials 95.10 0.053 15.27 total 100.00 0.33 100.00

[0097] The test results show that, through Figure 2 The flotation desulfurization process shown can obtain a cobalt-sulfur concentrate with an S grade of 30.79% and an S recovery rate of 83.04%, which can be sold as a product to generate economic benefits. The S grades in the generated sulfur tailings and phosphorus feedstock are 0.139% and 0.053%, respectively, indicating that combining the flotation feedstock obtained in Example 1 with the desulfurization test has a good effect on the enrichment and separation of sulfur, and to a certain extent eliminates the negative impact of associated sulfur elements on the subsequent recovery of titanium resources.

[0098] Comparative Example 3

[0099] The flotation feedstock obtained in Comparative Example 1 was subjected to flotation desulfurization tests. The dosages of each reagent were as follows: xanthate 600 g / t, No. 2 oil 150 g / t, and sulfuric acid 1200 g / t. For the specific process, please refer to [reference needed]. Figure 2 The experimental procedure of Example 3 is shown; the difference between Comparative Example 3 and Example 3 is that Comparative Example 3 uses flotation raw materials prepared from Comparative Example 1, while Example 3 uses flotation raw materials prepared from Example 1; Table 6 shows the flotation desulfurization test results of Comparative Example 3 using flotation raw materials prepared from Comparative Example 1.

[0100] Table 6: Results of flotation desulfurization tests using the flotation feedstock of Comparative Example 3 (Comparative Example 1)

[0101] cobalt sulfide concentrate 0.84 30.180 76.82 floating sulfur tailings 5.00 0.249 3.78 Floating phosphorus raw materials 94.16 0.068 19.40 total 100.00 0.330 100.00

[0102] A comparison of Tables 6 and 5 shows that when only fine screening is used in the pre-enrichment process, the S grade in the obtained cobalt-sulfur concentrate decreases to 30.180%, and the S recovery rate decreases to 76.82%; the S grade and recovery rate in the phosphorus feedstock change by 0.249% and 19.40%, respectively, indicating that the combined classification method has a promoting effect on the subsequent flotation effect.

[0103] Example 4

[0104] In Example 4, the flotation raw material from Example 3 and Example 1 was used to obtain the phosphorus flotation raw material after desulfurization, i.e., the phosphorus flotation raw material used was the same as in Example 3. A flotation dephosphorization experiment was then conducted. For details, please refer to [link / reference needed]. Figure 3 As shown, the flotation dephosphorization specifically includes the following steps:

[0105] S45: The flotation dephosphorization test was carried out on the flotation raw material, 200 g / t of collector was added and roughing was performed once. The minerals obtained included first phosphate rock and flotation titanium raw material. The collector is a composite reagent composed of oxidized paraffin soap and MES in a ratio of 9:1. The MES is sodium methyl ester sulfonate of fatty acids, which is a typical anionic collector. The TiO2 grade in the flotation titanium raw material is 18.53%.

[0106] S46: The first phosphate ore undergoes at least one fine-refinement and recovery process to obtain phosphorus-containing tailings; the recovered second phosphate ore is returned to S45 for further roughing.

[0107] Specifically, the above process flow is for reference. Figure 3 As shown, based on the completed flotation desulfurization test, a flotation dephosphorization test was conducted: Example 4 used Example 3 as the flotation raw material, and the obtained phosphorus raw material was subjected to a flotation dephosphorization test. The collector was a composite agent composed of oxidized paraffin soap and MES in a ratio of 9:1, and the dosage was 200g / t of the feed material. The results of the flotation dephosphorization test are shown in Table 7.

[0108] Table 7: Results of Flotation Dephosphorization Test in Example 4

[0109] Phosphorus tailings 5.23 6.60 60.56 Floating titanium raw materials 94.77 0.24 39.44 total 100.00 0.57 100.00

[0110] The test results show that, through the flotation dephosphorization test shown in Example 4, phosphorus-containing tailings with a P grade of 6.60% and a P recovery rate of 60.56% can be obtained, and the P grade in the titanium flotation raw material is 0.24%, with good separation effect. Moreover, the phosphorus-containing tailings can be further enriched by flotation to obtain qualified phosphorus concentrate products.

[0111] Comparative Example 4

[0112] Comparative Example 4 uses the same flotation feedstock as Comparative Example 3, specifically the phosphorus feedstock obtained after flotation desulfurization. The phosphorus feedstock used is the same as that used in Comparative Example 3. A flotation dephosphorization test is conducted using a composite reagent composed of oxidized paraffin soap and MES in a 9:1 ratio, at a dosage of 200 g / t. This comparative example uses the flotation dephosphorization feedstock shown in Example 4. Figure 3 The methods and procedures shown are presented, and the experimental results are shown in Table 8. The difference between Comparative Example 4 and Example 4 is that the phosphorus raw material used in Comparative Example 4 was obtained from Comparative Example 3.

[0113] Table 8: Results of Flotation Dephosphorization Test in Comparative Example 4

[0114] Phosphorus tailings 5.15 6.05 54.66 Floating titanium raw materials 94.85 0.27 45.34 Floating phosphorus raw materials 100.00 0.57 100.00

[0115] Comparing Comparative Example 4 with Example 4, it can be seen that under the same reagent system and flotation process conditions, only fine screening can inhibit the flotation dephosphorization process. The phosphorus grade and phosphorus recovery rate in the obtained phosphorus-containing tailings are lower than those in the phosphorus-containing tailings obtained in Example 4, which are 6.05% and 54.66%, respectively. The phosphorus grade in the obtained titanium flotation feedstock increases to 0.27%, which will increase the difficulty of titanium flotation.

[0116] Example 5

[0117] Based on Example 4, the mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings of the present invention involves flotation of titanium ore in the titanium feedstock after flotation dephosphorization. The specific process is as follows: Figure 4 As shown, the flotation of titanium ore specifically includes the following steps:

[0118] S47: Select titanium flotation feedstock for titanium beneficiation tests. Add 1500 g / t sulfuric acid, 1000 g / t inhibitor, 2500 g / t collector, and 300 g / t diesel oil. After a roughing process, obtain the first titanium concentrate and the first titanium tailings. Add 1200 g / t sulfuric acid and 500 g / t collector to the first titanium concentrate and perform a cleaning process, obtaining the second titanium concentrate and the first titanium middlings. The first titanium middlings are returned to the roughing process for further separation. Add 800 g / t sulfuric acid and 300 g / t collector to the second titanium concentrate and perform a second cleaning process, obtaining the third titanium concentrate and the second titanium middlings. The second titanium middlings are returned to the first cleaning process for further separation. Add 4 g / t sulfuric acid and 300 g / t collector to the third titanium concentrate. After three cleaning processes using 00 g / t sulfuric acid and 200 g / t collector, a fourth titanium concentrate and a third titanium middlings are obtained. The third titanium middlings are returned to a second cleaning process for further separation. After four cleaning processes using 400 g / t sulfuric acid, a titanium concentrate and a fourth titanium middlings are obtained. The fourth titanium middlings are returned to a third cleaning process for further separation. After scavenging using 300 g / t sulfuric acid and 200 g / t collector, a fifth titanium middlings and flotation tailings are obtained. The fifth titanium middlings are returned to a rougher for further separation. The TiO2 grade of the titanium concentrate reaches 47.50%. The TiO2 grade of the flotation tailings is less than 6.06%. The experimental results are shown in Table 9.

[0119] Table 9: Results of Titanium Flotation Test in Example 5

[0120] Titanium concentrate 35.68 47.50 91.46 flotation tailings 64.32 2.46 8.54 Floating titanium raw materials 100.00 18.53 100.00

[0121] The test results show that, through Figure 4 The titanium flotation process shown in the figure can be used to conduct titanium beneficiation tests and obtain titanium concentrate with a TiO2 grade of 47.50% and a TiO2 recovery rate of 91.46%. The TiO2 grade in the flotation tailings is only 2.46%, which realizes the efficient separation and recycling of titanium resources.

[0122] Comparative Example 5

[0123] Comparative Example 5: The titanium flotation raw material obtained in Comparative Example 3 was subjected to a titanium flotation test. The process flow is as shown in Example 5. Figure 4 The process and dosage of each reagent are as described in Example 5. Table 10 shows the results of the titanium flotation test in Comparative Example 5. The difference between Comparative Example 5 and Example 5 is that Comparative Example 5 uses flotation raw materials obtained from Comparative Example 4, while Example 5 uses flotation raw materials obtained from Example 4.

[0124] Table 10: Results of Titanium Separation by Flotation Test in Comparative Example 5

[0125] Titanium concentrate 30.46 45.83 85.17 flotation tailings 69.54 3.49 14.83 Floating titanium raw materials 100.00 16.39 100.00

[0126] Comparing Comparative Example 5 with Example 5, it can be seen that applying only fine screening during the pre-enrichment process does not improve the TiO2 grade in titanium concentrate, and may even reduce the titanium concentrate grade. It can be seen that the titanium concentrate grade obtained by flotation titanium selection through hydrocyclone classification, interference bed separation and fine screening, spiral sluice gravity separation, desulfurization and dephosphorization processes is increased to 47.50%, thus improving the titanium ore recovery rate.

[0127] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for mineral recovery from high-phosphorus vanadium-titanium magnetite tailings, characterized in that, Includes the following steps: S1: After a strong magnetic roughing process, the high-phosphorus vanadium-titanium magnetite tailings are obtained as strong magnetic rough concentrate and first strong magnetic tailings; the strong magnetic rough concentrate is then subjected to hydrocyclone classification and interference bed separation to obtain second underflow ore and overflow ore; the overflow ore consists of first overflow ore and second overflow ore. The strong magnetic rough concentrate is classified by a hydrocyclone into a first underflow ore and a first overflow ore; The first bottom flow ore is separated by a disturbed bed to obtain the second bottom flow ore and the second overflow ore; S2: The overflow ore is finely screened and classified to obtain oversize ore and undersize ore; S3: The second bottom flow ore and the over-screen ore are jointly roughed by a spiral chute at least once to obtain gravity concentrate and gravity tailings. The gravity concentrate is recovered through at least three superimposed spiral sluices to obtain gravity concentrate; the TiO2 grade of the gravity concentrate is greater than 25%; after grinding, the recovered gravity concentrate is put back into the titanium beneficiation process of the concentrator to start beneficiation. The gravity separation coarse tailings are recovered by at least one scavenging operation using a spiral sluice to obtain gravity separation tailings; the TiO2 grade of the gravity separation tailings is less than 2.00%. The undersize ore is concentrated and then subjected to two-stage strong magnetic separation to obtain fine-grained concentrate and a second strong magnetic tailings; the fine-grained concentrate is concentrated to form flotation feedstock; the TiO2 grade of the second strong magnetic tailings is less than 3.31%; and the TiO2 grade of the flotation feedstock is greater than 15%.

2. The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings according to claim 1, characterized in that, The particle size control value for the fine sieve grading is selected as 0.045 mm.

3. The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings according to claim 1, characterized in that, The magnetic field strength of the first strong magnet is 10000GS, and the magnetic field strength of the second strong magnet is 5000GS.

4. The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings according to claim 1, characterized in that, It also includes step S4: desulfurizing the flotation raw material by flotation, specifically including the following steps: S41: Select the flotation raw material, add 600 g / t of xanthate and 150 g / t of frother, and perform a single roughing process. The obtained minerals include flotation phosphate raw material and first sulfur ore; the sulfur grade of the flotation phosphate raw material is 0.053%. S42: Add 600g / t of sulfuric acid to the first sulfur ore and perform one refining process to obtain minerals including the second and third sulfur ores; S43: After adding 300 g / t sulfuric acid to the second sulfur ore and performing a second cleaning, the resulting first middlings are returned to the first cleaning, and the resulting concentrate is added to 200 g / t sulfuric acid for a third cleaning. The minerals obtained from the three cleanings include cobalt-sulfur concentrate and the second middlings. The second middlings are returned to the second cleaning. The sulfur-cobalt concentrate has a sulfur grade of 30.79%. S44: Add 100g / t of sulfuric acid to the third sulfur ore and scavenging it. The resulting minerals are returned to the primary beneficiation process and used to form floating sulfur tailings.

5. The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings according to claim 4, characterized in that, After flotation desulfurization, the phosphorus feedstock is subjected to flotation dephosphorization, which specifically includes the following steps: S45: The flotation dephosphorization test was conducted on the aforementioned flotation feedstock. 200 g / t of collector was added, and a single roughing process was performed. The obtained minerals included first-grade phosphate rock and flotation titanium feedstock. The collector was a composite reagent composed of oxidized paraffin soap and MES in a 9:1 ratio. The MES was sodium methyl ester sulfonate of fatty acids. The TiO2 grade in the flotation titanium feedstock was 18.53%. S46: The first phosphate ore is recycled at least once to obtain phosphorus-containing tailings; the recycled second phosphate ore is returned to S45 for roughing again.

6. The mineral recovery method for high-phosphorus vanadium-titanium magnetite tailings according to claim 5, characterized in that, After flotation dephosphorization, the titanium feedstock is subjected to flotation titanium ore, which specifically includes the following steps: S47: Select titanium raw materials for flotation titanium beneficiation test, add 1500g / t sulfuric acid, 1000g / t inhibitor, 2500g / t collector and 300g / t diesel oil and roughing once to obtain the first titanium concentrate and the first titanium tailings. The first titanium concentrate is added with 1200g / t of sulfuric acid and 500g / t of collector and then subjected to a first cleaning process to obtain the second titanium concentrate and the first titanium middlings. The first titanium middlings is returned to the roughing process for further separation. After adding 800 g / t of sulfuric acid and 300 g / t of collector to the second titanium concentrate and performing a second cleaning process, the third titanium concentrate and the second titanium middlings are obtained. The second titanium middlings are returned to the first cleaning process for further separation. The third titanium concentrate is treated with 400 g / t sulfuric acid and 200 g / t collector, and after three cleaning processes, the fourth titanium concentrate and the third titanium middlings are obtained. The third titanium middlings are returned to the second cleaning process for further separation. 400 g / t of sulfuric acid was added to the fourth titanium concentrate and it was cleaned four times to obtain titanium concentrate and fourth titanium middlings. The fourth titanium middlings was returned to the third cleaning process for further separation. After adding 300 g / t of sulfuric acid and 200 g / t of collector to the first titanium tailings and scavenging, the fifth titanium middlings and flotation tailings are obtained. The fifth titanium middlings are returned to the roughing process for further separation. The TiO2 grade of the titanium concentrate reaches 47.50%, and the TiO2 grade of the flotation tailings is less than 2.50%.

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