High-efficiency beneficiation method for complex and refractory titanium placer

Abstract

This invention discloses a highly efficient beneficiation method for complex and refractory titanium sand ore. First, precise classification and desliming are performed to eliminate the influence of coarse particles and slime on the beneficiation system, obtaining three particle sizes of feed material. Then, wet fine beneficiation is carried out separately, with gravity separation discarding waste to improve the grade of valuable metals and the system's processing capacity. Grading and gravity separation improve the grade of titanium dioxide and zirconium dioxide in the wet rough concentrate. Precise interface control of flotation achieves efficient recovery of fine zirconium and titanium particles, improving the overall recovery rate of titanium dioxide and zirconium dioxide throughout the process. Subsequently, the wet rough concentrates of different particle sizes are dewatered and dried to obtain dry rough concentrates. Finally, dry electrostatic separation is performed separately. Through organic synergy of equipment, zircon and rutile electrostatic separation tailings of the same particle size are alternately returned to the corresponding dry separation operation, eliminating alternating wet and dry separation and repeated dewatering and drying. This yields high-quality rutile and zircon concentrates while reducing system energy consumption, achieving highly efficient beneficiation of complex and refractory titanium sand ore.

Description

Technical Field

[0001] This invention relates to the field of mineral processing technology, and more specifically to an efficient beneficiation method for complex and difficult-to-process titanium sand ore. Background Technology

[0002] Rutile is an important metallic mineral and a raw material for refining titanium. Due to its high hiding power, high weather resistance, and high gloss, it is increasingly favored by the coatings industry as a high-performance white pigment. The welding materials market remains the main consumer of rutile, currently experiencing a supply shortage. Rutile deposits mainly include eclogite-type, gneiss-type, acidic tuff hydrothermal alteration-type, and coastal placer-type deposits. Primary rutile deposits account for 86% of the resource reserves, while rutile placer deposits account for only 14%.

[0003] With the continuous development of high-quality primary rutile resources, existing rutile resources are severely weathered and contain large amounts of primary slime. The production process also generates a large amount of secondary slime, and the rutile obtained after beneficiation and enrichment cannot meet the demand for downstream high-grade titanium products and materials. To meet market demand, attention has turned to rutile placer deposits and imported titanium placer deposits. Rutile placer deposits typically co-occur with minerals such as ilmenite, zircon, monazite, garnet, and quartz. Existing beneficiation processes mainly include magnetic separation, gravity separation, drying, and electrostatic separation, ultimately producing various rutile products that meet market demand.

[0004] However, for complex and difficult-to-process titanium sand deposits that have been developed in large quantities in recent years, such as altered marine sand deposits, the main valuable components are leucoxene, iron-bearing rutile, ilmenite, zircon, monazite, etc. Due to the different degrees of alteration, large variations in mud content, and uneven particle size, the existing rutile beneficiation process has low production efficiency, high operating costs, and may even fail to produce high-quality titanium zirconium products.

[0005] For example, Chinese patent ZL202210723982.1 discloses a beneficiation process and its application for fine-grained complex zirconium-titanium ore, which develops a combined technology of magnetic separation, spiral sluice, shaking table, and spherical vibrating concentrator to achieve effective separation of various components. However, the spherical vibrating concentrator has limited recovery capacity for fine-grained titanium-zirconium minerals. Another example is Chinese patent CN202111147548.5, which discloses a method and system for separating and purifying rutile rough concentrate, increasing the TiO2 grade in rutile rough concentrate from about 46% to over 87%. However, the technology requires roasting, with roasting temperatures as high as 900-1100℃, resulting in high costs. Yet another example is Chinese patent ZL201910060984.5, which discloses a rough sand beneficiation process that uses magnetic separation, reduction roasting, and electrostatic separation to achieve comprehensive utilization of titanium rough ore. However, the reduction roasting temperature is as high as 800-900℃, resulting in high energy consumption.

[0006] Therefore, providing an efficient beneficiation method for complex and difficult-to-process titanium sand ore is a problem that urgently needs to be solved by those skilled in the art. Summary of the Invention

[0007] In view of this, the present invention provides an efficient beneficiation method for complex and difficult-to-process titanium sand ore. It addresses the challenges of complex and difficult-to-process titanium sand ore, such as complex mineral composition, multiple types of titanium components, uneven particle size, large variation in mud content, and similar surface physicochemical properties. It can accurately classify, finely sort, and separate dry and wet beneficiations of complex and difficult-to-process titanium sand ore, and obtain high-quality titanium zirconium products with high recovery rate, while saving energy consumption and production costs.

[0008] To achieve the above objectives, the present invention adopts the following technical solution:

[0009] A method for efficient beneficiation of complex and difficult-to-process titanium sand ore includes the following sequential steps:

[0010] 1) Precise grading:

[0011] The complex and difficult-to-process titanium sand ore is first screened to remove large pieces of waste rock and wood chips. Then, the ore that passes through the screen is passed through a classifying screen to obtain three particle size products: +0.15mm, -0.15mm to +0.05mm, and -0.05mm. The -0.05mm particle size product is further classified by a hydrocyclone to obtain two particle size products: -0.05mm to +0.01mm and -0.01mm. The -0.01mm particle size product is sludge, which is directly sent to a settling tank for deep dewatering and then stored.

[0012] 2) Wet sorting:

[0013] I: The +0.15mm particle size product is slurryed and then passed through a diaphragm jig for waste removal to obtain waste concentrate and tailings, with a waste removal rate as high as 40-55%; the waste concentrate is then subjected to strong magnetic separation operation I to obtain titanium concentrate I and magnetic tailings I; after the magnetic tailings I is concentrated, it is subjected to gravity separation operation I to obtain wet zircon rough concentrate I, wet gold rough concentrate I and wet tailings I;

[0014] II: The -0.15mm to +0.05mm particle size product is slurried and then subjected to strong magnetic separation operation II to obtain titanium concentrate II and magnetic tailings II; after the magnetic tailings II are concentrated, they are subjected to gravity separation operation II to obtain wet zircon rough concentrate II, wet alumina rough concentrate II and wet tailings II.

[0015] III: The -0.05mm to +0.01mm particle size product is subjected to strong magnetic separation operation III to obtain titanium concentrate III and magnetic tailings III; the magnetic tailings III are concentrated and then subjected to flotation operation I to obtain flotation operation I froth product and flotation operation I tailings slurry; the flotation operation I tailings slurry is subjected to flotation operation II to obtain flotation operation II froth product and flotation operation II tailings slurry; the froth product of flotation operation I is wet zircon concentrate III, the froth product of flotation operation II is wet rutile concentrate III, and the tailings slurry of flotation operation II is wet tailings III;

[0016] 3) Dehydration and drying:

[0017] Wet zircon rough concentrate I, wet zircon rough concentrate II, wet rutile rough concentrate I, wet rutile rough concentrate II, wet zircon concentrate III, and wet rutile concentrate III were dehydrated using a vacuum filter to obtain six dehydrated products, all with a moisture content of 4-12%. The four dehydrated zircon rough concentrates I, II, I, and II were then dried in a dryer at a temperature of 200-300℃ for 60-120 minutes to finally obtain dry zircon rough concentrate I, dry zircon rough concentrate II, dry rutile rough concentrate I, and dry rutile rough concentrate II.

[0018] 4) Dry separation and purification:

[0019] Dry zircon rough concentrate I and dry rutile rough concentrate I were subjected to electrostatic separation, with the electrostatic separation operations consisting of high-pressure drum electrostatic separation and arc plate electrostatic separation. After electrostatic separation, both yielded conductive and non-conductive mineral products. Dry rutile rough concentrate II and dry zircon rough concentrate II were also subjected to electrostatic separation, with the electrostatic separation operations consisting of high-pressure drum electrostatic separation and screen plate electrostatic separation. Similarly, both yielded conductive and non-conductive mineral products.

[0020] Furthermore, in step 1), the main chemical composition of the complex and refractory titanium sand ore is TiO2: 28%–36%, ZrO2: 5%–8%; the grading sieve is double-layered, with the upper sieve aperture size being 0.15 mm and the lower sieve aperture size being 0.05 mm. The operating yield of the +0.15 mm particle size product is 10–20%, of which TiO2: 12%–19% and ZrO2: 0.5%–1.0%; the operating yield of the -0.15 mm to +0.05 mm particle size product is 60–70%, of which TiO2: 32%–38% and ZrO2: 4%–7%; and the operating yield of the -0.05 mm particle size product is 10–25%, of which TiO2: 40%–48% and ZrO2: 8%–16%.

[0021] Furthermore, in step 1), the feed concentration of the hydrocyclone is 15-25%, the pressure is 0.1-0.25 MPa, the number of classifications is 3-4, and after desliming, a product with a particle size of -0.05 mm to +0.01 mm and a slime with a particle size of -0.01 mm are obtained, wherein the yield of slime with a particle size of -0.01 mm is 30-40%.

[0022] Furthermore, in step 2), the diaphragm jig performs 2 to 3 separations, with a stroke of 2 to 20 mm and a stroke rate of 200 to 350 times / minute; in the strong magnetic separation operation I, the magnetic field strength is 0.8 to 1.2 T, and the diameter of the rod medium is 4 to 5 mm; in the gravity separation operation I, a coarse sand shaking table is used, and the separation number is 4 to 6.

[0023] Furthermore, in step 2), the magnetic field strength of the strong magnetic separation operation II is 0.8 to 1.2 T, and the diameter of the rod medium is 3 to 4 mm; the gravity separation operation II equipment uses a spiral chute and a fine sand shaking table or all fine sand shaking tables, and the separation number is 4 to 7 times.

[0024] Furthermore, in the strong magnetic separation operation III, the magnetic field strength is 1.0–1.4T, and the diameter of the rod medium is 1–3mm; in the flotation operation I, one or a combination of sodium carbonate and sodium hydroxide is used to adjust the pH to 6.5–8.0, and the depressant is one or a combination of water glass and light metal sulfate, at a dosage of 500–900g / t. The collector is an unsaturated or saturated fatty acid salt with 10–20 carbon atoms, at a dosage of 300–600g / t; in the flotation operation II, sodium carbonate and sodium hydroxide are used... One or two of the following reagents are used to adjust the pH to 8.1–9.5. The inhibitor is one or two of alkali metal phosphates and sodium silicate, with a dosage of 300–500 g / t. The activator is lead nitrate, with a dosage of 400–800 g / t. The collector is a carboxylic acid derivative with 7–9 carbon atoms, with a dosage of 500–1000 g / t. Both flotation operation I and flotation operation II include 1–2 roughing stages, 1–2 scavenging stages, and 2–4 cleaning stages. Among them, the cleaning stage can be heated flotation at a temperature of 50–80℃.

[0025] Furthermore, in step 2), the TiO2 content in titanium concentrate I, titanium concentrate II, and titanium concentrate III on a dry basis is 45%–55%, and the total recovery rate of titanium dioxide is 15%–20%.

[0026] Furthermore, in step 3), the dehydrated wet zircon concentrate III has a ZrO2 content of ≥63% on a dry basis and a ZrO2 recovery rate of 25-35%; the dehydrated wet rutile concentrate III has a TiO2 content of ≥80% on a dry basis and a TiO2 recovery rate of 10-15%; the dry zircon rough concentrate I and dry zircon rough concentrate II have a ZrO2 content of 45%-55% and a TiO2 content of 10%-15% on a dry basis; and the dry rutile rough concentrate I and dry rutile rough concentrate II have a TiO2 content of 55%-70% and a ZrO2 content of 5%-10% on a dry basis.

[0027] Furthermore, in step 4), for dry zircon rough concentrate I and dry zircon rough concentrate II feeds, the resulting conductive mineral products are electrostatic tailings I and electrostatic tailings II, respectively, and the resulting non-conductive mineral products are zircon concentrate I and zircon concentrate II, respectively; for dry rutile rough concentrate I and dry rutile rough concentrate II feeds, the resulting conductive mineral products are rutile concentrate I and rutile concentrate II, respectively, and the resulting non-conductive mineral products are electrostatic tailings III and electrostatic tailings IV; for any dry rough concentrate feed, the feed heating temperature is 45–85℃, the high-pressure drum electrostatic separation operating voltage is 5–60KV, the rotation speed is 20–180r / min, and the separation frequency is 3–6 times; the arc plate electrostatic separation operating voltage is 5–50KV, and the arc plate electrostatic separation operation frequency is 6–10 times; the sieve plate electrostatic separation operating voltage is 5–50KV, and the sieve plate electrostatic separation operation frequency is 6–8 times.

[0028] Furthermore, in step 4), the dry zircon concentrate I and dry zircon concentrate II have ZrO2 ≥ 63% on a dry basis and a total ZrO2 recovery rate of 50-60%, and the dry rutile concentrate I and dry rutile concentrate II have TiO2 ≥ 80% on a dry basis and a total TiO2 recovery rate of 55-65%.

[0029] Therefore, this invention provides a highly efficient beneficiation method for complex and difficult-to-process titanium sand ore. Compared with existing titanium sand ore beneficiation methods, the advantages of this invention are:

[0030] 1) After the graded materials are processed through magnetic separation-gravity separation-drying-electrostatic separation and magnetic separation-flotation processes, various high-quality titanium zirconium products are obtained in one go. At the same time, the flotation is precisely controlled, which improves the recovery rate of fine-particle titanium zirconium minerals and realizes the green and efficient recovery of complex and difficult-to-process titanium sand ore.

[0031] 2) The combination of vibrating screen and hydrocyclone for grading enables precise grading and desliming of complex and difficult-to-process titanium sand ore at the source, which greatly improves the adaptability of subsequent gravity separation and electrostatic separation equipment to materials, enhances the separation effect of heavy minerals and light minerals, and conductive minerals and non-conductive minerals, and eliminates the screening operation in the electrostatic separation process, reducing dust pollution.

[0032] 3) By adopting gravity separation and waste disposal, the feed grade of the coarse-grained separation system is improved, and the processing capacity is enhanced. Furthermore, through the fine control of the entire grading-separation process and the deep collaboration of the separation equipment, the tailings of the electrostatic separation are directly returned to the dry separation operation of the corresponding material, avoiding the dry material from re-entering the wet separation-dewatering-drying process, thus realizing the low-carbon separation of complex and difficult-to-process titanium sand ore. Attached Figure Description

[0033] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0034] Figure 1 The attached figure is a process flow diagram of an efficient beneficiation method for complex and difficult-to-process titanium sand ore provided by the present invention. Detailed Implementation

[0035] 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.

[0036] Example 1

[0037] This embodiment is a refractory titanium sand ore of the leucoxene type, whose main mineral composition is leucoxene, iron-bearing rutile, ilmenite, anatase, zircon, quartz, etc., and its main chemical composition is: TiO2: 34.64%, ZrO2: 5.72%, Fe: 6.43%, SiO2: 35.24%, Al2O3: 8.44%.

[0038] like Figure 1 As shown, this embodiment discloses a high-efficiency beneficiation method for complex and difficult-to-process titanium sand ore, including the following sequential steps:

[0039] 1) Precise grading:

[0040] The complex and difficult-to-process titanium sand ore is first passed through a slag-removing screen with a 2mm aperture to remove large pieces of waste rock and wood shavings. The slurry passing through the slag-removing screen is then classified by a vibrating screen to obtain: +0.15mm particle size product, yield 12.5%, of which TiO2: 15.57% and ZrO2: 0.82%; -0.15mm to +0.05mm particle size product, yield 68.25%, of which TiO2: 33.97% and ZrO2: 5.47%; -0.05mm particle size product... The product yielded 19.25%, with TiO2 at 45.32% and ZrO2 at 9.98%. The -0.05mm particle size product was further deslimed using a hydrocyclone. The hydrocyclone feed concentration was controlled at 16%, the pressure at 0.15 MPa, and the classification was performed three times to obtain -0.05mm to +0.01mm particle size grit and -0.01mm particle size slime. The -0.01mm particle size slime yield was 32%. After dewatering, it was stockpiled or sold, while the grit was used as raw material for subsequent flotation.

[0041] 2) Wet sorting:

[0042] I: The +0.15mm particle size product is slurryed and then fed into a diaphragm jig for waste removal. The diaphragm jig has a stroke of 10mm and a stroke rate of 250 strokes / min, with two separations to obtain waste concentrate and tailings. The waste removal rate is 46%, and the tailings are sold as building materials. The waste concentrate is then fed into strong magnetic separation operation I, which uses a single separation process. The magnetic field strength is controlled at 1.0T and the rod medium diameter is 4mm to obtain titanium concentrate I and magnetic tailings I. The magnetic tailings I are further concentrated and then fed into gravity separation operation I. The entire gravity separation operation I uses a coarse sand shaking table and is separated four times to obtain wet zircon rough concentrate I, wet gold rough concentrate I, and wet tailings I.

[0043] II: The -0.15mm to +0.05mm particle size product is slurryed and then enters the high-intensity magnetic separation operation II, which adopts one roughing and one cleaning separation, controlling the magnetic field strength at 1.1T and the rod medium diameter at 3mm, to obtain titanium concentrate II and magnetic separation tailings II; After the magnetic separation tailings II are concentrated, they enter the gravity separation operation II. The entire process of gravity separation operation II adopts a combination of spiral chute and fine sand shaking table. The spiral chute is separated 3 times and the fine sand shaking table is separated 2 times, for a total of 5 times, to obtain wet zircon rough concentrate II, wet alumina rough concentrate II and wet tailings II;

[0044] III: The -0.05mm to +0.01mm particle size is fed into the high-intensity magnetic separation operation III, employing a roughing and cleaning process. The magnetic field strength is controlled at 1.3T, and the rod medium diameter is 2mm, yielding titanium concentrate III and magnetic tailings III. After concentrating the magnetic tailings III, it enters the flotation operation I. The flotation process consists of one roughing, two cleaning, and two scavenging stages. Sodium carbonate is used to adjust the pH to 7.5, the depressant is 650g / t water glass, the collector is 350g / t saturated alkanoate with 18 carbon atoms, and the cleaning temperature is 60℃, yielding wet zircon concentrate III and flotation tailings pulp. This is then continued into flotation operation II, which employs a one-roughing, two-cleaning, and two-scavenging process. The flotation reagent regime is as follows: pH 8.4, alkali metal phosphate dosage of 445g / t, lead nitrate dosage of 550g / t, and collector dosage of 650g / t C6H5C. (OH) =NOH carboxylic acid derivatives, with a selection temperature of 70℃, yielded wet rutile concentrate III and wet tailings III;

[0045] 3) Dehydration and drying:

[0046] Wet zircon rough concentrate I and II, wet rutile rough concentrate I and II, wet rutile rough concentrate III and wet zircon concentrate III, titanium concentrate I, titanium concentrate II and titanium concentrate III are respectively fed into a vacuum filter for dehydration to obtain dehydrated products. In this embodiment, a belt vacuum filter is used. The four materials, zircon rough concentrate I, zircon rough concentrate II, rutile rough concentrate I and rutile rough concentrate II, are then respectively fed into a dryer for drying at a temperature of 250°C for 80 minutes. In this embodiment, a three-cylinder dryer is used to finally obtain dry zircon rough concentrate I (dry basis ZrO2: 51.2%, TiO2: 12.3%), dry zircon rough concentrate II, and titanium concentrate III. Concentrate II (dry basis ZrO2: 52.6%, TiO2: 11.7%), dry rutile concentrate I (TiO2: 62.4%, ZrO2: 7.9%), and dry rutile concentrate II (TiO2: 65.1%, ZrO2: 9.2%); dehydrated zircon concentrate III and rutile concentrate III are sold directly without drying, with zircon concentrate III containing 64.5% ZrO2 and a ZrO2 recovery rate of 26.7% on a dry basis, and rutile concentrate III containing 90.2% TiO2 and a TiO2 recovery rate of 13.4% on a dry basis; dehydrated titanium concentrate I, titanium concentrate II, and titanium concentrate III are combined as titanium concentrate, with a dry basis TiO2 content of 52.7% and a TiO2 recovery rate of 16.4%;

[0047] 4) Dry separation and purification:

[0048] Part 1: Dry zircon rough concentrate I and dry rutile rough concentrate I are heated to 70℃ and fed into high-pressure drum electrostatic separation operation I and high-pressure drum electrostatic separation operation II, respectively. Each operation is separated 4 times. The voltage of the first high-pressure drum electrostatic separation operation is 26KV and the rotation speed is 150r / min. The voltage of the subsequent separation operations increases or decreases by 2KV depending on the separation purpose. The resulting concentrates are high-pressure drum electrostatic separation operation I, high-pressure drum electrostatic separation operation II, electrostatic tailings I, and electrostatic tailings III. The concentrates from high-pressure drum electrostatic separation operation I and high-pressure drum electrostatic separation operation II are fed into arc plate electrostatic separation operation I and arc plate electrostatic separation operation II, respectively, and separated 6 times. The voltage of the first electrostatic separation operation is 22KV. The voltage of the subsequent separation operations increases or decreases by 1KV depending on the separation purpose. The resulting tailings from the arc plate electrostatic separation operation are returned to the upper arc plate electrostatic separation operation, finally obtaining zircon concentrate I and rutile concentrate I. The tailings from electrostatic separation operation I are fed into high-pressure drum electrostatic separation operation II, and the tailings from electrostatic separation operation III are fed into high-pressure drum electrostatic separation operation I.

[0049] II: Dry zircon rough concentrate II and dry rutile rough concentrate II are heated to 75℃ and fed into high-pressure drum electrostatic separation processes III and IV, respectively. Each process is repeated 5 times. The voltage for the first high-pressure drum electrostatic separation is 30KV, and the rotation speed is 170r / min. For subsequent processes, the voltage is increased or decreased by 2KV depending on the separation objective. This yields concentrates from high-pressure drum electrostatic separation processes III and IV, as well as tailings from processes II and IV, respectively. The concentrates from processes III and IV then enter screen plate electrostatic separation processes I and II, respectively, and are separated 6 and 7 times, respectively. The voltage for the first electrostatic separation was 25 kV. For subsequent separations, the voltage increased or decreased by 1 kV depending on the separation objective. The tailings from the electrostatic separation were returned to the next stage, ultimately yielding zircon concentrate II and rutile concentrate II. Tailings II entered high-pressure drum electrostatic separation operation IV, and tailings IV entered high-pressure drum electrostatic separation operation III. The resulting zircon concentrate I had a ZrO2 content of 64.5% and zircon concentrate II had a ZrO2 content of 65.5%, with a total recovery rate of 55.8%. The resulting rutile concentrate I had a TiO2 content of 83.6% and rutile concentrate II had a TiO2 content of 90.7%, with a total recovery rate of 58.3%.

[0050] Example 2:

[0051] This embodiment is a refractory titanium sand ore of the leucoxene type, whose main mineral composition is leucoxene, iron-bearing rutile, ilmenite, zircon, quartz, etc., and the main chemical composition is: TiO2: 31.78%, ZrO2: 7.42%, Fe: 7.55%, SiO2: 33.48%, Al2O3: 10.57%.

[0052] like Figure 1 As shown, this embodiment discloses a high-efficiency beneficiation method for complex and difficult-to-process titanium sand ore, including the following sequential steps:

[0053] 1) Precise grading:

[0054] The complex and difficult-to-process titanium sand ore is first passed through a slag-removing screen with a 1.5mm aperture to remove large pieces of waste rock, wood shavings, and domestic waste. The slurry passing through the slag-removing screen is then classified by a vibrating screen to obtain: +0.15mm particle size product, with a yield of 15.6%, containing 13.25% TiO2 and 0.68% ZrO2; -0.15mm to +0.05mm particle size product, with a yield of 64.78%, containing 32.12% TiO2 and 6.84% ZrO2; -0.05mm particle size product... The particle size product had a yield of 19.62%, of which TiO2 accounted for 43.15% and ZrO2 for 9.82%. The -0.05mm particle size was further deslimed using a hydrocyclone. The feed concentration of the hydrocyclone was controlled at 18%, the pressure at 0.20 MPa, and the number of classifications was 4, to obtain -0.05mm to +0.01mm particle size grit and -0.01mm particle size slime. The yield of -0.01mm particle size slime was 35%. After deep dewatering, it was stockpiled or sold, and the grit was used as raw material for subsequent flotation.

[0055] 2) Wet sorting:

[0056] I: The +0.15mm particle size product is slurryed and fed into a diaphragm jig for waste removal. The diaphragm jig has a stroke of 15mm and a stroke rate of 280 times / min, with 3 separations to obtain waste concentrate and tailings. The waste removal rate is 51%, and the tailings are sold as building materials. The waste concentrate is then fed into high-intensity magnetic separation operation I, which uses a roughing and cleaning process. The magnetic field strength is controlled at 1.1T and the rod medium diameter is 3.5mm to obtain titanium concentrate I and magnetic tailings I. The magnetic tailings I are further concentrated and then fed into gravity separation operation I. The entire gravity separation operation I uses a coarse sand shaking table and is separated 5 times to obtain wet zircon rough concentrate I, wet gold rough concentrate I, and wet tailings I.

[0057] II: The -0.15mm to +0.05mm particle size product is slurryed and then enters the high-intensity magnetic separation operation II, which adopts one roughing and one cleaning separation, controlling the magnetic field strength at 1.0T and the rod medium diameter at 3.0mm, to obtain titanium concentrate II and magnetic separation tailings II; After the magnetic separation tailings II are concentrated, they enter the gravity separation operation II. The entire process of gravity separation operation II adopts a combination of spiral chute and fine sand shaking table. The spiral chute is separated twice and the fine sand shaking table is separated four times, for a total of six times, to obtain wet zircon rough concentrate II, wet alumina rough concentrate II and wet tailings II;

[0058] III: The -0.05mm to +0.01mm particle size product is fed into the high-intensity magnetic separation operation III, which employs a roughing, cleaning, and scavenging process. The magnetic field strength is controlled at 1.35T, and the rod medium diameter is 1.5mm, to obtain titanium concentrate III and magnetic separation tailings III. After concentration, the magnetic separation tailings III are fed into flotation operation I. The flotation process consists of a roughing, cleaning, and scavenging process. Sodium hydroxide is used to adjust the pH to 7.9, and the depressant is a combination of water glass and light metal aluminate at a dosage of 820g / t. The collector dosage is 350g / t. Unsaturated olefins with 18 carbon atoms are treated at 50℃ to obtain wet zircon concentrate III and flotation tailings slurry. Flotation operation II is then carried out. The process adopts two roughing, two cleaning, and two scavenging steps. The flotation reagent system is as follows: pH value is 8.3, the combined inhibitor of alkali metal phosphate and sodium silicate is 430 g / t, lead nitrate is 580 g / t, and the collector is 650 g / t. A carboxylic acid derivative with the molecular formula C7H7NO3 is treated at 65℃ to obtain wet rutile concentrate III and wet tailings III.

[0059] 3) Dehydration and drying:

[0060] Wet zircon rough concentrate I, wet zircon rough concentrate II, wet rutile rough concentrate I, wet rutile rough concentrate II, wet rutile rough concentrate III, wet zircon concentrate III, titanium concentrate I, titanium concentrate II, and titanium concentrate III are respectively fed into a vacuum filter for dehydration to obtain dehydrated products. In this embodiment, a belt vacuum filter is used. The four materials after dehydration, zircon rough concentrate I, zircon rough concentrate II, rutile rough concentrate I, and rutile rough concentrate II, are respectively fed into a dryer for drying at a drying temperature of 220°C for 90 minutes. In this embodiment, a three-cylinder dryer is used to finally obtain dry zircon rough concentrate I (dry basis ZrO2: 53.2%, TiO2: 10.5%) and dry zircon rough concentrate II. Concentrate II (dry basis ZrO2: 54.1%, TiO2: 11.4%), dry rutile concentrate I (TiO2: 58.7%, ZrO2: 8.6%), and dry rutile concentrate II (TiO2: 61.3%, ZrO2: 9.7%); dehydrated zircon concentrate III and rutile concentrate III are sold directly without drying, with zircon concentrate III containing 65.5% ZrO2 on a dry basis and a ZrO2 recovery rate of 31.2%, and rutile concentrate III containing 86.8% TiO2 on a dry basis and a TiO2 recovery rate of 12.5%; dehydrated titanium concentrate I, titanium concentrate II, and titanium concentrate III are combined as titanium concentrate, with a dry basis TiO2 content of 47.8% and a TiO2 recovery rate of 15.3%;

[0061] 4) Dry separation and purification:

[0062] Part 1: Dry zircon rough concentrate I and dry rutile rough concentrate I are heated to 65℃ and fed into high-pressure drum electrostatic separation operation I and high-pressure drum electrostatic separation operation II, respectively. Each operation is separated 5 times. The voltage of the first high-pressure drum electrostatic separation operation is 28KV and the rotation speed is 160r / min. The voltage of the subsequent separation operations increases or decreases by 1KV depending on the separation purpose. This yields high-pressure drum electrostatic separation operation I concentrate, high-pressure drum electrostatic separation operation II concentrate, electrostatic separation tailings I and electrostatic separation tailings III, respectively. The high-pressure drum electrostatic separation operation I concentrate and high-pressure drum electrostatic separation operation II concentrate are fed into arc plate electrostatic separation operation I and arc plate electrostatic separation operation II, respectively. Each operation is separated 7 times. The voltage of the first electrostatic separation operation is 24KV. The voltage of the subsequent separation operations increases or decreases by 1.5KV depending on the separation purpose. The resulting arc plate electrostatic separation tailings are returned to the upper arc plate electrostatic separation stage, finally yielding zircon concentrate I and rutile concentrate I. Electrostatic separation tailings I are fed into high-pressure drum electrostatic separation operation II, and electrostatic separation tailings III are fed into high-pressure drum electrostatic separation operation I.

[0063] II: Dry zircon rough concentrate II and dry rutile rough concentrate II are heated to 80℃ and fed into high-pressure drum electrostatic separation operation III and high-pressure drum electrostatic separation operation IV, respectively. Each operation is separated 6 times. The voltage for the first high-pressure drum electrostatic separation operation is 32KV, and the rotation speed is 155r / min. For subsequent operations, the voltage is increased or decreased by 1KV depending on the separation objective. This yields high-pressure drum electrostatic separation operation III concentrate, high-pressure drum electrostatic separation operation IV concentrate, and electrostatic separation tailings II and IV, respectively. The high-pressure drum electrostatic separation operation III concentrate and high-pressure drum electrostatic separation operation IV concentrate are then fed into screen plate electrostatic separation operation I and screen plate electrostatic separation operation II, respectively, and separated 7 and 8 times, respectively. The voltage for the first electrostatic separation was 24KV. For subsequent separations, the voltage increased or decreased by 1KV depending on the separation objective. The tailings from the electrostatic separation were returned to the next stage, ultimately yielding zircon concentrate II and rutile concentrate II. Tailings II entered high-pressure drum electrostatic separation operation IV, and then entered high-pressure drum electrostatic separation operation III. The resulting zircon concentrate I contained 65.7% ZrO2, and concentrate II contained 66.1% ZrO2, with a combined recovery rate of 57.1%. The resulting rutile concentrate I contained 82.3% TiO2, and concentrate II contained 84.5% TiO2, with a combined recovery rate of 57.2%.

[0064] Example 3:

[0065] This example is an altered, refractory titanium sand ore, whose main mineral composition is leucoxene, iron-bearing rutile, ilmenite, brookite, zircon, quartz, etc., and its main chemical composition is: TiO2: 29.77%, ZrO2: 6.84%, Fe: 9.12%, SiO2: 34.88%, Al2O3: 9.85%.

[0066] like Figure 1 As shown, this embodiment discloses a high-efficiency beneficiation method for complex and difficult-to-process titanium sand ore, including the following sequential steps:

[0067] 1) Precise grading:

[0068] The complex and difficult-to-process titanium sand ore is first passed through a slag-removing screen with a 2.5mm aperture to remove large pieces of waste rock, wood shavings, and domestic waste. The slurry passing through the slag-removing screen is then classified by a vibrating screen to obtain: +0.15mm particle size product, with a yield of 18.5%, containing 12.17% TiO2 and 0.97% ZrO2; -0.15mm to +0.05mm particle size product, with a yield of 68.89%, containing 32.01% TiO2 and 7.75% ZrO2; -0.05mm particle size... The product yield was 12.61%, with TiO2 at 40.52% and ZrO2 at 8.31%. The -0.05mm particle size was further deslimed using a hydrocyclone. The hydrocyclone feed concentration was controlled at 20%, the pressure at 0.18 MPa, and the classification was performed 4 times to obtain -0.05mm to +0.01mm particle size grit and -0.01mm particle size slime. The -0.01mm particle size slime yield was 38.5%. After deep dewatering, it was stockpiled or sold, while the grit was used as raw material for subsequent flotation.

[0069] 2) Wet sorting:

[0070] I: The +0.15mm particle size product is slurryed and fed into a diaphragm jig for waste removal. The diaphragm jig has a stroke of 11mm and a stroke rate of 224 times / min, with 3 separations to obtain waste concentrate and tailings. The waste removal rate is 53%, and the tailings are sold as building materials. The waste concentrate is then fed into strong magnetic separation operation I, using a one-roughing-one-cleaning-one-sweeping process. The magnetic field strength is controlled at 0.95T and the rod medium diameter is 3.5mm to obtain titanium concentrate I and magnetic tailings I. After further concentration of magnetic tailings I, it is fed into gravity separation operation I. The entire gravity separation operation I uses a coarse sand shaking table and is separated 6 times to obtain wet zircon rough concentrate I, wet gold rough concentrate I, and wet tailings I.

[0071] II: The -0.15mm to +0.05mm particle size product is slurryed and then fed into the high-intensity magnetic separation operation II. A one-coarse-one-sweep process is adopted, and the coarsening magnetic field strength is controlled at 1.3T and the rod medium diameter is 3.5mm to obtain titanium concentrate II and magnetic separation tailings II. After the magnetic separation tailings II are concentrated, they are fed into gravity separation operation II. The entire gravity separation operation II adopts a combination of spiral chute and fine sand shaking table. The spiral chute is separated twice and the fine sand shaking table is separated four times, for a total of six times, to obtain wet zircon rough concentrate II, wet alumina rough concentrate II and wet tailings II.

[0072] III: The -0.05mm to +0.01mm particle size product is fed into the high-intensity magnetic separation operation III, which employs a roughing, cleaning, and scavenging process. The magnetic field strength is controlled at 1.4T, and the rod medium diameter is 1.0mm, yielding titanium concentrate III and magnetic separation tailings III. After concentration, the magnetic separation tailings III are fed into flotation operation I. The flotation process consists of two roughing, two scavenging, and three cleaning processes, using a combination of sodium carbonate and sodium hydroxide as modifiers to adjust the pH to 8.0. The depressant is 890g / t of light metal aluminate, and the collector is 58g / t. Saturated fatty acid salts with 10-18 carbon atoms were processed at a temperature of 75℃ to obtain wet zircon concentrate III and flotation tailings slurry. Flotation operation II was then carried out. The process adopted two roughing, two cleaning, and two scavenging operations. The flotation reagent system was as follows: pH value 9.0, sodium silicate 365g / t, lead nitrate 492g / t, and collector 800g / t of carboxylic acid derivatives with the molecular formula C8H17NO2. The processing temperature was 82℃ to obtain wet rutile concentrate III and wet tailings III.

[0073] 3) Dehydration and drying:

[0074] Wet zircon rough concentrate I, wet zircon rough concentrate II, wet rutile rough concentrate I, wet rutile rough concentrate II, wet rutile rough concentrate III, wet zircon concentrate III, titanium concentrate I, titanium concentrate II, and III are respectively fed into a vacuum filter for dehydration to obtain dehydrated products. In this embodiment, a belt vacuum filter is used. The four materials, zircon rough concentrate I, zircon rough concentrate II, and rutile rough concentrate I and II, are then respectively fed into a dryer for drying at a temperature of 265°C for 130 minutes. In this embodiment, a three-cylinder dryer is used to finally obtain dry zircon rough concentrate I (dry basis ZrO2: 48.7%, TiO2: 12.6%) and dry zircon rough concentrate II (… The dry-basis ZrO2 content is 51.9%, TiO2 content is 12.2%, and the dry-basis rutile concentrate I (TiO2 content is 56.9%, ZrO2 content is 7.8%) and the dry-basis rutile concentrate II (TiO2 content is 58.3%, ZrO2 content is 7.7%) are produced. The dehydrated zircon concentrate III and rutile concentrate III are not dried and are sold directly. The dry-basis ZrO2 content of zircon concentrate III is 64.1% and the ZrO2 recovery rate is 26.3%. The dry-basis TiO2 content of rutile concentrate III is 83.9% and the TiO2 recovery rate is 13.6%. The dehydrated titanium concentrate I, titanium concentrate II and titanium concentrate III are combined as titanium concentrate. The dry-basis TiO2 content is 46.3% and the TiO2 recovery rate is 16.4%.

[0075] 4) Dry separation and purification:

[0076] Part 1: Dry zircon rough concentrate I and dry rutile rough concentrate I are heated to 78℃ and fed into high-pressure drum electrostatic separation operation I and high-pressure drum electrostatic separation operation II, respectively. Each operation is separated 6 times. The voltage of the first high-pressure drum electrostatic separation operation is 21KV and the rotation speed is 155r / min. The voltage of the subsequent separation operations increases or decreases by 1KV depending on the separation purpose. The resulting concentrates are high-pressure drum electrostatic separation operation I, high-pressure drum electrostatic separation operation II, electrostatic tailings I, and electrostatic tailings III. The concentrates from high-pressure drum electrostatic separation operation I and high-pressure drum electrostatic separation operation II are fed into arc plate electrostatic separation operation I and arc plate electrostatic separation operation II, respectively, and separated 8 times. The voltage of the first electrostatic separation operation is 22KV. The voltage of the subsequent separation operations increases or decreases by 1.2KV depending on the separation purpose. The resulting tailings from the arc plate electrostatic separation operation are returned to the upper arc plate electrostatic separation operation, finally obtaining zircon concentrate I and rutile concentrate I. The tailings from electrostatic separation operation I are fed into high-pressure drum electrostatic separation operation II, and the tailings from electrostatic separation operation III are fed into high-pressure drum electrostatic separation operation I.

[0077] II: Dry zircon rough concentrate II and dry rutile rough concentrate II are heated to 82℃ and fed into high-pressure drum electrostatic separation operation III and IV, respectively. Each operation is separated 4 times. The voltage for the first high-pressure drum electrostatic separation operation is 23KV, and the rotation speed is 138r / min. For subsequent operations, the voltage is increased or decreased by 1KV depending on the separation objective. This yields high-pressure drum electrostatic separation operation III concentrate, high-pressure drum electrostatic separation operation IV concentrate, electrostatic separation tailings II, and electrostatic separation tailings IV, respectively. The high-pressure drum electrostatic separation operation III concentrate and high-pressure drum electrostatic separation operation IV concentrate are then fed into screen plate electrostatic separation operation I and screen plate electrostatic separation operation II, respectively, for 6 and 8 separations. The voltage for the first electrostatic separation was 22KV. For subsequent separations, the voltage increased or decreased by 1.1KV depending on the separation objective. The tailings from the electrostatic separation were returned to the next stage, ultimately yielding zircon concentrate II and rutile concentrate II. Tailings II entered high-pressure drum electrostatic separation operation IV, and then entered high-pressure drum electrostatic separation operation III. The zircon concentrate I yielded ZrO2 of 63.8% and concentrate II yielded ZrO2 of 65.4%, with a combined recovery rate of 54.4%. The rutile concentrate I yielded TiO2 of 81.2% and concentrate II yielded TiO2 of 80.6%, with a combined recovery rate of 58.5%.

[0078] The various embodiments in this specification are described in a progressive or parallel manner. Each embodiment focuses on its differences from other embodiments, and the same or similar parts between the embodiments can be referred to mutually. For the apparatus disclosed in the embodiments, since it corresponds to the method disclosed in the embodiments, the description is relatively simple, and relevant parts can be referred to in the method section.

[0079] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A high-efficiency beneficiation method for complex refractory titanium placer, characterized in that, Includes the following sequential steps: Precise grading: The complex and difficult-to-process titanium sand ore is first screened to remove large pieces of waste rock and wood shavings. Then, the ore that passes through the screen is passed through a classifying screen to obtain three particle size products: +0.15mm, -0.15mm to +0.05mm, and -0.05mm. The -0.05mm particle size product is further classified by a hydrocyclone to obtain two particle size products: -0.05mm to +0.01mm and -0.01mm. The -0.01mm particle size product is sludge, which is directly sent to a settling tank for deep dewatering and then stockpiled. Wet sorting: I: The +0.15mm particle size product is slurryed and then passed through a diaphragm jig for waste removal to obtain waste concentrate and tailings, with a waste removal rate as high as 40-55%; the waste concentrate is then subjected to strong magnetic separation operation I to obtain titanium concentrate I and magnetic tailings I; after the magnetic tailings I is concentrated, it is subjected to gravity separation operation I to obtain wet zircon rough concentrate I, wet gold rough concentrate I and wet tailings I; II: The -0.15mm to +0.05mm particle size product is slurried and then subjected to strong magnetic separation operation II to obtain titanium concentrate II and magnetic tailings II; after the magnetic tailings II are concentrated, they are subjected to gravity separation operation II to obtain wet zircon rough concentrate II, wet alumina rough concentrate II and wet tailings II. III: The -0.05mm to +0.01mm particle size product is subjected to strong magnetic separation operation III to obtain titanium concentrate III and magnetic tailings III; the magnetic tailings III are concentrated and then subjected to flotation operation I to obtain flotation operation I froth product and flotation operation I tailings slurry; the flotation operation I tailings slurry is subjected to flotation operation II to obtain flotation operation II froth product and flotation operation II tailings slurry; the froth product of flotation operation I is wet zircon concentrate III, the froth product of flotation operation II is wet rutile concentrate III, and the tailings slurry of flotation operation II is wet tailings III; Dehydration and drying: Wet zircon rough concentrate I, wet zircon rough concentrate II, wet rutile rough concentrate I, wet rutile rough concentrate II, wet zircon concentrate III, and wet rutile concentrate III were dehydrated using a vacuum filter to obtain six dehydrated products, each with a moisture content of 4-12%. The four dehydrated zircon rough concentrates I, II, I, and II were then dried in a dryer at a temperature of 200-300℃ for 60-120 minutes to finally obtain dry zircon rough concentrate I, dry zircon rough concentrate II, dry rutile rough concentrate I, and dry rutile rough concentrate II. Dry separation and purification: Dry zircon rough concentrate I and dry rutile rough concentrate I were subjected to electrostatic separation, with the electrostatic separation operations consisting of high-pressure drum electrostatic separation and arc plate electrostatic separation. After electrostatic separation, both yielded conductive and non-conductive mineral products. Dry rutile rough concentrate II and dry zircon rough concentrate II were also subjected to electrostatic separation, with the electrostatic separation operations consisting of high-pressure drum electrostatic separation and screen plate electrostatic separation. Similarly, both yielded conductive and non-conductive mineral products.

2. The efficient beneficiation method of complex refractory titanium placer according to claim 1, characterized in that, In step 1), the main chemical composition of the complex and difficult-to-process titanium sand ore is TiO2: 28%~36% and ZrO2: 5%~8%. The grading sieve is double-layered, with the upper sieve aperture size being 0.15mm and the lower sieve aperture size being 0.05mm. The operating yield of the +0.15mm particle size product is 10~20%, of which TiO2: 12%~19% and ZrO2: 0.5%~1.0%; the operating yield of the -0.15mm~+0.05mm particle size product is 60-70%, of which TiO2: 32%~38% and ZrO2: 4%~7%; and the operating yield of the -0.05mm particle size product is 10~25%, of which TiO2: 40%~48% and ZrO2: 8%~16%.

3. The efficient beneficiation method of complex refractory titanium placer according to claim 1 or 2, characterized in that, In step 1), the feed concentration of the hydrocyclone is 15~25%, the pressure is 0.1~0.25MPa, the number of classifications is 3~4, and after desliming, a product with a particle size of -0.05mm~+0.01mm and a slime with a particle size of -0.01mm are obtained, wherein the yield of slime with a particle size of -0.01mm is 30~40%.

4. The efficient beneficiation method of complex refractory titanium placer according to claim 1, characterized in that, In step 2), the diaphragm jig is used for 2-3 separations, with a stroke of 2-20 mm and a stroke rate of 200-350 times / min; in strong magnetic separation operation I, the magnetic field strength is 0.8-1.2T and the diameter of the rod medium is 4-5 mm; in gravity separation operation I, a coarse sand shaking table is used, and the separation is performed 4-6 times.

5. The efficient beneficiation method of complex refractory titanium placer according to claim 1, characterized in that, In step 2), the magnetic field strength of the strong magnetic separation operation II is 0.8~1.2T, and the diameter of the rod medium is 3~4mm; the equipment for gravity separation operation II is a spiral chute and a fine sand shaking table or all fine sand shaking tables, and the separation number is 4~7 times.

6. A method for efficient beneficiation of complex and difficult-to-process titanium sand ore according to claim 1, 4, or 5, characterized in that, In strong magnetic separation operation III, the magnetic field strength is 1.0~1.4T, and the diameter of the rod medium is 1~3mm. In flotation operation I, one or a combination of sodium carbonate and sodium hydroxide is used to adjust the pH to 6.5~8.

0. The depressant is one or a combination of water glass and light metal sulfate, at a dosage of 500~900g / t. The collector is an unsaturated or saturated fatty acid salt with 10~20 carbon atoms, at a dosage of 300~600g / t. In flotation operation II, one or a combination of sodium carbonate and sodium hydroxide is used. One or two combined reagents are used to adjust the pH to 8.1-9.

5. The inhibitor is one or two of alkali metal phosphates and sodium silicate, with a dosage of 300-500 g / t. The activator is lead nitrate, with a dosage of 400-800 g / t. The collector is a carboxylic acid derivative with 7-9 carbon atoms, with a dosage of 500-1000 g / t. Both flotation operation I and flotation operation II include 1-2 roughing stages, 1-2 scavenging stages, and 2-4 cleaning stages. The cleaning stage involves heated flotation at a temperature of 50-80℃.

7. The efficient beneficiation method of complex refractory titanium placer according to claim 1, characterized in that, In step 2), the TiO2 content in titanium concentrate I, titanium concentrate II and titanium concentrate III on a dry basis is 45%~55%, and the total recovery rate of titanium dioxide is 15~20%.

8. The efficient beneficiation method of complex refractory titanium placer according to claim 1, characterized in that, In step 3), the dry basis of dehydrated wet zircon concentrate III contains ZrO2 ≥ 63% and ZrO2 recovery rate 25~35%; the dry basis of dehydrated wet rutile concentrate III contains TiO2 ≥ 80% and TiO2 recovery rate 10~15%; the dry basis of dry zircon rough concentrate I and dry zircon rough concentrate II contains ZrO2 45%~55% and TiO2 10%~15%; the dry basis of dry rutile rough concentrate I and dry rutile rough concentrate II contains TiO2 55%~70% and ZrO2 5%~10%.

9. The efficient beneficiation method of complex refractory titanium placer according to claim 1, characterized in that, In step 4), for dry zircon rough concentrate I and dry zircon rough concentrate II feeds, the conductive mineral products obtained are electrostatic tailings I and electrostatic tailings II, respectively, and the non-conductive mineral products obtained are zircon concentrate I and zircon concentrate II, respectively; for dry rutile rough concentrate I and dry rutile rough concentrate II feeds, the conductive mineral products obtained are rutile concentrate I and rutile concentrate II, respectively, and the non-conductive mineral products obtained are electrostatic tailings III and electrostatic tailings IV; for any dry rough concentrate feed, the feed heating temperature is 45~85℃, the high-pressure drum electrostatic separation operating voltage is 5~60KV, the rotation speed is 20~180r / min, and the separation number is 3~6 times; the arc plate electrostatic separation operating voltage is 5~50KV, and the arc plate electrostatic separation operation number is 6~10 times; the sieve plate electrostatic separation operating voltage is 5~50KV, and the sieve plate electrostatic separation operation number is 6~8 times.

10. The efficient beneficiation method of complex refractory titanium placer ores according to claim 1 or 9, characterized in that, In step 4), ZrO2 ≥ 63% in dry zircon concentrate I and dry zircon concentrate II on a dry basis, with a total ZrO2 recovery rate of 50-60%, and TiO2 ≥ 80% in dry rutile concentrate I and dry rutile concentrate II on a dry basis, with a total TiO2 recovery rate of 55-65%.

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