A method for preparing a titanium-rich material using ilmenite
Patent Information
- Application Number
- CN202310500913.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-04
- Publication Date
- 2026-10-20
- Estimated Expiration
- 2043-05-04
AI Technical Summary
[0011]本发明提供的利用钛铁矿制备富钛料的方法,对低品位钛铁矿还原后进行盐酸酸解、过滤滤渣、水解析出等工艺,能够制备得到钛品位高于85%的富钛料,制备得到的高品质的富钛料用于氯化法钛白及海绵钛的生产;该方法流程简单、可适用范围广、易于工业化生产。
Abstract
Description
Technical Field
[0001] This invention relates to the field of metallurgy, and more specifically, to a method for preparing titanium-rich materials using ilmenite. Background Technology
[0002] Titanium dioxide, also known as titanium dioxide, is an important white pigment widely used in plastics, papermaking, printing inks, synthetic fibers, rubber, cosmetics, and other fields. Its production methods are mainly the sulfuric acid process and the chloride process. The sulfuric acid process is one of the main processes for producing titanium dioxide worldwide. It involves acid hydrolysis, hydrolysis, water washing, bleaching, salt treatment, and calcination of primary ilmenite or high-titanium slag to ultimately obtain titanium dioxide. The chloride process, on the other hand, requires higher quality titanium-rich raw materials. Due to process and equipment requirements, the raw materials must contain at least 85% titanium and have a low impurity content.
[0003] Titanium-rich materials are produced by enriching titanium in ilmenite to increase its titanium grade, thus meeting the requirements of titanium dioxide production via the chloride process. Traditional industrial methods for preparing titanium-rich materials generally fall into two categories: pyrometallurgical titanium slag extraction and hydrometallurgical rutile extraction. Electric furnace titanium slag extraction uses high-temperature electric arc heating to separate ilmenite from titanium, resulting in high-grade titanium-rich materials. Rutile extraction typically involves leaching iron from ilmenite using dilute sulfuric acid or hydrochloric acid, thereby increasing the titanium grade in the leaching residue and producing high-quality titanium-rich materials. Both processes primarily focus on iron removal and do not reduce the content of other elements. Therefore, the production process requires stringent control over the content of other impurities and the titanium grade of the ilmenite raw material, necessitating the use of ilmenite with low calcium and magnesium content and high titanium grade.
[0004] With the increasing demand for titanium dioxide year by year, the consumption of high-quality titanium ore is enormous annually, making the comprehensive utilization of low-grade titanium resources imperative. The development and use of low-grade titanium resources is not only an important supplement to the raw materials for titanium dioxide production but also a way to fully utilize titanium resources. As a high-quality resource containing both high-grade iron and low-grade titanium, the comprehensive and rational utilization of low-grade ilmenite is of great significance for fully exploring the value of ilmenite concentrate and supplementing the raw materials for titanium dioxide production.
[0005] In view of this, the present invention is hereby proposed. Summary of the Invention
[0006] One aspect of the present invention relates to a method for preparing titanium-rich materials using ilmenite, comprising the following steps:
[0007] (a) The ilmenite and the first reducing agent are mixed and then subjected to a reduction reaction to obtain a reduction product; the reduction product is subjected to magnetic separation to obtain reduced ilmenite;
[0008] (b) The reduced ilmenite is acid-hydrolyzed to obtain an acid-hydrolyzed titanium solution; after removing insoluble substances from the acid-hydrolyzed titanium solution, it is hydrolyzed.
[0009] The method for preparing titanium-rich materials using ilmenite can produce high-quality titanium-rich materials from low-grade ilmenite, and the prepared titanium-rich materials can be used as raw materials for the production of titanium dioxide by the chloride process.
[0010] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0011] The present invention provides a method for preparing titanium-rich materials from ilmenite. After reducing low-grade ilmenite, the method involves hydrochloric acid acidolysis, filtration of filter residue, and hydrolysis to obtain titanium-rich materials with a titanium content higher than 85%. The high-quality titanium-rich materials obtained can be used in the production of titanium dioxide and sponge titanium by the chloride process. The method is simple, has a wide range of applications, and is easy to industrialize.
[0012] The method for preparing titanium-rich materials using ilmenite provided by this invention can remove calcium and magnesium impurities while removing iron, making it suitable for low-grade ilmenite with high impurity content and expanding the raw material range for titanium-rich materials.
[0013] The method for preparing titanium-rich materials using ilmenite provided by this invention produces amorphous anatase titanium dioxide with a rutile content of ≤0.5%. It has higher chlorination reactivity and is more suitable for the production of titanium dioxide and sponge titanium by the chlorination process than common wet-process rutile titanium-rich materials.
[0014] The method for preparing titanium-rich materials using ilmenite provided by this invention allows the dilute hydrochloric acid generated as a waste byproduct to be concentrated and reused, while ferrous chloride solid can be used as a water purification agent and raw material for other chemical products, thereby enhancing the overall economic value and conforming to the concepts of green production and recycling. Detailed Implementation
[0015] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. However, those skilled in the art will understand that the embodiments described below are some embodiments of the present invention, but not all embodiments, and are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. 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. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.
[0016] One aspect of the present invention relates to a method for preparing titanium-rich materials using ilmenite, comprising the following steps:
[0017] (a) The ilmenite and the first reducing agent are mixed and then subjected to a reduction reaction to obtain a reduction product; the reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash;
[0018] (b) The reduced ilmenite is acid-hydrolyzed to obtain an acid-hydrolyzed titanium solution; after removing insoluble substances from the acid-hydrolyzed titanium solution, it is hydrolyzed.
[0019] The method for preparing titanium-rich materials using ilmenite can produce high-quality titanium-rich materials from low-grade ilmenite, and the prepared titanium-rich materials can be used as raw materials for the production of titanium dioxide by the chloride process.
[0020] The method for preparing titanium-rich materials using ilmenite can remove calcium and magnesium impurities while removing iron, making it suitable for low-grade ilmenite with high impurity content and expanding the raw material range for titanium-rich materials.
[0021] The method for preparing titanium-rich materials using ilmenite produces amorphous anatase titanium dioxide, which has higher chlorination reactivity and is more suitable for the production of titanium dioxide and sponge titanium than common wet-process rutile titanium-rich materials.
[0022] Low-grade ilmenite can be treated by removing iron and other impurities through reduction, acidolysis, and hydrolysis to obtain high-quality titanium-rich materials. The theoretical basis for this is as follows:
[0023] Fe + 2HCl = FeCl2;
[0024] FeO·TiO2+4HCl=FeCl2+TiOCl2+2H2O;
[0025] Fe2O3·TiO2+8HCl=2FeCl3+TiOCl2+4H2O;
[0026] MgO·TiO2+4HCl=MgCl2+TiOCl2+2H2O;
[0027] CaO·TiO2+4HCl=CaCl2+TiOCl2+2H2O;
[0028] TiOCl2 + H2O = TiO2↓ + 2HCl.
[0029] Reduction can significantly reduce the amount of iron oxides in low-grade ilmenite, improving acidolysis efficiency and capacity. The acidolysis and hydrolysis of titanium dioxide remove most of the iron and other calcium and magnesium impurities, thus obtaining high-quality titanium-rich materials.
[0030] Preferably, the grade of the ilmenite is 10% to 25%.
[0031] Preferably, the temperature of the reduction reaction is 900–1000°C (e.g., 900°C, 910°C, 920°C, 930°C, 940°C, 950°C, 960°C, 970°C, 980°C, 990°C, or 1000°C).
[0032] Preferably, the reduction reaction takes 12 to 18 hours (e.g., 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, or 18 hours).
[0033] Preferably, the reducing agent is 60% to 80% of the mass of the ilmenite (e.g., 60%, 63%, 65%, 68%, 70%, 73%, 75%, 78% or 80%).
[0034] Preferably, the reduction equipment used for the reduction reaction is a common coal-based reduction equipment with controllable reduction time, including but not limited to vertical shaft furnaces, tunnel kilns, and reduction furnaces.
[0035] Preferably, the acid hydrolysis temperature is 65-85°C (e.g., 65°C, 68°C, 70°C, 73°C, 75°C, 78°C, 80°C, 83°C or 85°C).
[0036] Preferably, the acid hydrolysis time is 3 to 6 hours (e.g., 3 hours, 4 hours, 5 hours or 6 hours).
[0037] Preferably, the liquid-to-solid ratio of the acid hydrolysis is 5-10 kg:1 kg (e.g., 5 kg:1 kg, 6 kg:1 kg, 7 kg:1 kg, 8 kg:1 kg, 9 kg:1 kg or 10 kg:1 kg).
[0038] Preferably, the acid used for acid hydrolysis includes: first hydrochloric acid.
[0039] Preferably, the mass concentration of the first hydrochloric acid is 30% to 35% (e.g., 30%, 31%, 32%, 33%, 34% or 35%).
[0040] Preferably, the hydrolysis specifically includes:
[0041] The acid-hydrolyzed titanium solution, after being heated to remove insoluble substances, is heated to 100–110°C (e.g., 100°C, 102°C, 104°C, 106°C, 108°C, or 110°C). Distilled water at 80–90°C (e.g., 80°C, 82°C, 84°C, 86°C, 88°C, or 90°C) is then added to carry out the hydrolysis. The hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 3–5 g / L (e.g., 3 g / L, 4 g / L, or 5 g / L). The hydrolysis of TiOCl2 in the titanium solution is unique compared to the hydrolysis of other ions. Its hydrolysis does not occur at a fixed pH value; dilution or heating will cause hydrolysis and the precipitation of TiO2. Other impurity elements in the titanium solution, such as iron, calcium, and magnesium, do not undergo hydrolysis during dilution and heating, resulting in a lower impurity content in the hydrolyzed TiO2.
[0042] Preferably, the hydrolysis temperature is 100–110°C (e.g., 100°C, 102°C, 104°C, 106°C, 108°C, or 110°C). The hydrolysis temperature needs to be maintained at 100–110°C. If the temperature drops after adding distilled water, an external heating method can be used to maintain the hydrolysis temperature.
[0043] Preferably, the hydrolysis time is 2 to 3 hours (e.g., 2 hours, 2.2 hours, 2.4 hours, 2.6 hours, 2.8 hours or 3 hours).
[0044] Preferably, the magnetic field strength of the magnetic separator is 2000-3000 GS (e.g., 2000 GS, 2100 GS, 2200 GS, 2300 GS, 2400 GS, 2500 GS, 2600 GS, 2700 GS, 2800 GS, 2900 GS or 3000 GS).
[0045] Preferably, the first reducing agent includes a carbon-based reducing agent.
[0046] Preferably, the first reducing agent includes at least one of bituminous coal, anthracite, or metallurgical coke.
[0047] Preferably, the hydrolysis process further includes sedimentation, washing, solid-liquid separation, and drying.
[0048] Preferably, a second reducing agent is added to the liquid after solid-liquid separation, followed by evaporation and crystallization to obtain a second hydrochloric acid and ferrous chloride; the second hydrochloric acid is concentrated and used for acid hydrolysis.
[0049] The method for preparing titanium-rich materials using ilmenite provided by this invention allows the dilute hydrochloric acid generated as a waste byproduct to be concentrated and reused, while ferrous chloride solid can be used as a water purification agent and raw material for other chemical products, thereby enhancing the overall economic value and conforming to the concepts of green production and recycling.
[0050] Preferably, after adding the second reducing agent, the Ti in the liquid after solid-liquid separation 3+ The concentration is 0.5–1.5 g / L.
[0051] Preferably, the second reducing agent comprises: reduced iron powder.
[0052] Preferably, the temperature of the water wash is 35-45°C (e.g., 35°C, 36°C, 37°C, 38°C, 39°C, 40°C, 41°C, 42°C, 43°C, 44°C or 45°C).
[0053] Preferably, the drying temperature is 150–200°C (e.g., 150°C, 155°C, 160°C, 165°C, 170°C, 175°C, 180°C, 185°C, 190°C, 195°C, or 200°C).
[0054] The embodiments of the present invention will now be described in detail with reference to specific examples and comparative examples.
[0055] The ilmenite used in the following embodiments and comparative examples of the present invention is a vanadium-titanium magnetite from the Panzhihua-Xichang region, whose main components are as follows (mass fraction): titanium dioxide 11.87%, total iron content 56.30%, silicon dioxide 4.40%, magnesium oxide 5.46%, and the remaining metallic impurities are sodium, calcium, chromium and manganese, etc.
[0056] Example 1
[0057] The method for preparing titanium-rich materials using ilmenite provided in this embodiment includes the following steps:
[0058] (1) Low-grade ilmenite and bituminous coal are added to a reduction device to carry out a reduction reaction to obtain a reduction product; the temperature of the reduction reaction is 950℃, the time of the reduction reaction is 15h, and the reducing agent is 70% of the mass of the ilmenite.
[0059] (2) The reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash; the magnetic field strength of the magnetic separation is 2500GS;
[0060] (3) Reduced ilmenite and 33% hydrochloric acid are added to an acidolysis device for acidolysis to obtain acidolysis titanium liquid; the acidolysis temperature is 75℃, the acidolysis time is 5h, and the liquid-solid ratio of the acidolysis is 7.5:1;
[0061] (4) Filter the acid-hydrolyzed titanium solution to remove insoluble substances;
[0062] (5) The acid-hydrolyzed titanium solution after removing insoluble substances is heated to 105°C, and distilled water at 85°C is added to carry out the hydrolysis. The hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 4 g / L. The hydrolysis temperature is 105°C and the hydrolysis time is 2.5 h.
[0063] (6) High-quality titanium-rich material can be obtained by settling, washing, filtering and drying the hydrolysis products.
[0064] (7) Adding reduced iron powder to the solution after solid-liquid separation and evaporating and crystallizing yields ferrous chloride solid and a second hydrochloric acid. The second hydrochloric acid, after concentration, can be returned to step (3) for acid hydrolysis. After adding the second reducing agent, Ti in the liquid after solid-liquid separation is reduced. 3+ The concentration is 0.5–1.5 g / L.
[0065] Example 2
[0066] The method for preparing titanium-rich materials using ilmenite provided in this embodiment includes the following steps:
[0067] (1) Low-grade ilmenite and anthracite are added to a reduction device to carry out a reduction reaction to obtain a reduction product; the temperature of the reduction reaction is 900℃, the time of the reduction reaction is 12h, and the reducing agent is 60% of the mass of the ilmenite.
[0068] (2) The reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash; the magnetic field strength of the magnetic separation is 2000GS;
[0069] (3) Reduced ilmenite and 30% hydrochloric acid are added to an acidolysis device for acidolysis to obtain acidolysis titanium liquid; the acidolysis temperature is 65℃, the acidolysis time is 3h, and the liquid-solid ratio of the acidolysis is 5:1.
[0070] (4) Filter the acid-hydrolyzed titanium solution to remove insoluble substances;
[0071] (5) The acid-hydrolyzed titanium solution after removing insoluble substances is heated to 100°C, and distilled water at 80°C is added to carry out the hydrolysis. The hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 3 g / L. The hydrolysis temperature is 100°C and the hydrolysis time is 2 h.
[0072] (6) High-quality titanium-rich material can be obtained by settling, washing, filtering and drying the hydrolysis products.
[0073] (7) Adding reduced iron powder to the solution after solid-liquid separation and evaporating and crystallizing yields ferrous chloride solid and a second hydrochloric acid. The second hydrochloric acid, after concentration, can be returned to step (3) for acid hydrolysis. After adding the second reducing agent, Ti in the liquid after solid-liquid separation is reduced. 3+The concentration is 0.5–1.5 g / L.
[0074] Example 3
[0075] The method for preparing titanium-rich materials using ilmenite provided in this embodiment includes the following steps:
[0076] (1) Low-grade ilmenite and metallurgical coke are added to a reduction device to carry out a reduction reaction to obtain a reduction product; the temperature of the reduction reaction is 1000℃, the time of the reduction reaction is 18h, and the reducing agent is 80% of the mass of the ilmenite.
[0077] (2) The reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash; the magnetic field strength of the magnetic separation is 3000GS;
[0078] (3) Reduced ilmenite and 35% hydrochloric acid are added to an acidolysis device for acidolysis to obtain acidolysis titanium liquid; the acidolysis temperature is 85℃, the acidolysis time is 6h, and the liquid-solid ratio of the acidolysis is 10:1.
[0079] (4) Filter the acid-hydrolyzed titanium solution to remove insoluble substances;
[0080] (5) The acid-hydrolyzed titanium solution after removing insoluble substances is heated to 110°C, and distilled water at 90°C is added to carry out the hydrolysis. The hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 5 g / L. The hydrolysis temperature is 110°C and the hydrolysis time is 3 h.
[0081] (6) High-quality titanium-rich material can be obtained by settling, washing, filtering and drying the hydrolysis products.
[0082] (7) Adding reduced iron powder to the solution after solid-liquid separation and evaporating and crystallizing yields ferrous chloride solid and a second hydrochloric acid. The second hydrochloric acid, after concentration, can be returned to step (3) for acid hydrolysis. After adding the second reducing agent, Ti in the liquid after solid-liquid separation is reduced. 3+ The concentration is 0.5–1.5 g / L.
[0083] Example 4
[0084] The method for preparing titanium-rich materials using ilmenite provided in this embodiment includes the following steps:
[0085] (1) Low-grade ilmenite and bituminous coal are added to a reduction device to carry out a reduction reaction to obtain a reduction product; the temperature of the reduction reaction is 930℃, the time of the reduction reaction is 14h, and the reducing agent is 68% of the mass of the ilmenite.
[0086] (2) The reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash; the magnetic field strength of the magnetic separation is 2100GS;
[0087] (3) Reduced ilmenite and 31% hydrochloric acid are added to an acidolysis device for acidolysis to obtain acidolysis titanium liquid; the acidolysis temperature is 70℃, the acidolysis time is 3.5h, and the liquid-solid ratio of the acidolysis is 6:1;
[0088] (4) Filter the acid-hydrolyzed titanium solution to remove insoluble substances;
[0089] (5) The acid-hydrolyzed titanium solution after removing insoluble substances is heated to 103°C, and distilled water at 82°C is added to carry out the hydrolysis. The hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 4 g / L. The hydrolysis temperature is 104°C and the hydrolysis time is 2 h.
[0090] (6) High-quality titanium-rich material can be obtained by settling, washing, filtering and drying the hydrolysis products.
[0091] (7) Adding reduced iron powder to the solution after solid-liquid separation and evaporating and crystallizing yields ferrous chloride solid and a second hydrochloric acid. The second hydrochloric acid, after concentration, can be returned to step (3) for acid hydrolysis. After adding the second reducing agent, Ti in the liquid after solid-liquid separation is reduced. 3+ The concentration is 0.5–1.5 g / L.
[0092] Example 5
[0093] The method for preparing titanium-rich materials using ilmenite provided in this embodiment includes the following steps:
[0094] (1) Low-grade ilmenite and anthracite are added to a reduction device to carry out a reduction reaction to obtain a reduction product; the temperature of the reduction reaction is 980℃, the time of the reduction reaction is 16h, and the reducing agent is 74% of the mass of the ilmenite.
[0095] (2) The reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash; the magnetic field strength of the magnetic separation is 2800GS;
[0096] (3) Reduced ilmenite and hydrochloric acid with a mass concentration of 34% are added to an acidolysis device for acidolysis to obtain acidolysis titanium liquid; the acidolysis temperature is 80℃, the acidolysis time is 6h, and the liquid-solid ratio of the acidolysis is 9:1;
[0097] (4) Filter the acid-hydrolyzed titanium solution to remove insoluble substances;
[0098] (5) The acid-hydrolyzed titanium solution after removing insoluble substances is heated to 108°C, and distilled water at 88°C is added to carry out the hydrolysis. The hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 3 g / L. The hydrolysis temperature is 109°C and the hydrolysis time is 3 h.
[0099] (6) High-quality titanium-rich material can be obtained by settling, washing, filtering and drying the hydrolysis products.
[0100] (7) Adding reduced iron powder to the solution after solid-liquid separation and evaporating and crystallizing yields ferrous chloride solid and a second hydrochloric acid. The second hydrochloric acid, after concentration, can be returned to step (3) for acid hydrolysis. After adding the second reducing agent, Ti in the liquid after solid-liquid separation is reduced. 3+ The concentration is 0.5–1.5 g / L.
[0101] Comparative Example 1
[0102] The method for preparing titanium-rich materials using ilmenite provided in this comparative example differs from Example 1 only in that the reduction time is 10 hours.
[0103] Comparative Example 2
[0104] The method for preparing titanium-rich materials using ilmenite provided in this comparative example differs from Example 1 only in that the acid hydrolysis temperature is 90°C.
[0105] Comparative Example 3
[0106] The method for preparing titanium-rich materials using ilmenite provided in this comparative example includes the following steps:
[0107] (1) Low-grade ilmenite and bituminous coal are added to a reduction device to carry out a reduction reaction to obtain a reduction product; the temperature of the reduction reaction is 1100℃, the time of the reduction reaction is 15h, and the reducing agent is 70% of the mass of the ilmenite.
[0108] (2) The reduction product is subjected to magnetic separation to obtain reduced ilmenite and magnetic separation ash; the magnetic field strength of the magnetic separation is 2500GS;
[0109] (3) Reduced ilmenite and 20% dilute sulfuric acid are added to an acid leaching device for acid leaching; the leaching temperature is 90℃, the leaching time is 3h, and the liquid-solid ratio of the acid hydrolysis is 5:1.
[0110] (4) The leachate is filtered to separate solids and liquids, and the solid is dried to obtain rutile.
[0111] Experimental Example
[0112] The titanium grade and impurity content of the titanium-rich materials prepared in each embodiment and comparative example were tested, and the results are shown in Table 1.
[0113] Table 1
[0114] Example 1 89.22 0.58 Example 2 86.04 0.76 Example 3 91.15 0.47 Example 4 87.87 0.65 Example 5 90.48 0.51 Comparative Example 1 82.26 1.03 Comparative Example 2 81.49 3.17 Comparative Example 3 49.19 13.02
[0115] As can be seen from the data in Table 1, the titanium-rich material prepared by the method for preparing titanium-rich material using ilmenite provided by the present invention has a high titanium grade and a low impurity content.
[0116] Although the present invention has been illustrated and described with specific embodiments, it should be understood that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; those skilled in the art should understand that modifications can be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein, without departing from the spirit and scope of the present invention; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention; therefore, this means that all such substitutions and modifications that fall within the scope of the present invention are included in the appended claims.
Claims
1. A method for preparing titanium-rich materials using ilmenite, characterized in that, Includes the following steps: (a) Ilmenite and the first reducing agent are mixed and then subjected to a reduction reaction to obtain the reduction product; The reduction product is subjected to magnetic separation to obtain reduced ilmenite; The reduction reaction is carried out at a temperature of 900~1000℃; The reduction reaction takes 12-18 hours; The first reducing agent is 60% to 80% of the mass of the ilmenite; The grade of the ilmenite is 10%~25%; (b) The reduced ilmenite is acid-hydrolyzed to obtain acid-hydrolyzed titanium solution; After removing insoluble substances from the acid-hydrolyzed titanium solution, the acid-hydrolyzed titanium solution is then hydrolyzed. The acid used in the acid hydrolysis is hydrochloric acid. The mass concentration of the first hydrochloric acid is 30%~35%; The hydrolysis specifically includes: The acid-hydrolyzed titanium solution, after being heated to remove insoluble substances, is heated to 100-110°C. Distilled water at 80-90°C is then added to carry out the hydrolysis. The hydrolysis temperature is 100-110°C, the hydrolysis time is 2-3 hours, and the hydrolysis is terminated when the concentration of tetravalent titanium in the hydrolyzed mixture is 3-5 g / L.
2. The method for preparing titanium-rich materials using ilmenite according to claim 1, characterized in that, The acid hydrolysis temperature is 65~85℃; The acid hydrolysis time is 3-6 hours.
3. The method for preparing titanium-rich materials using ilmenite according to claim 1, characterized in that, The liquid-to-solid ratio of the acid hydrolysis is 5-10 kg: 1 kg.
4. The method for preparing titanium-rich materials using ilmenite according to claim 1, characterized in that, The magnetic field strength of the magnetic separator is 2000~3000GS.
5. The method for preparing titanium-rich materials using ilmenite according to claim 1, characterized in that, The first reducing agent includes carbon-based reducing agents.
6. The method for preparing titanium-rich materials using ilmenite according to claim 1, characterized in that, The first reducing agent is selected from at least one of bituminous coal, anthracite, or metallurgical coke.
7. The method for preparing titanium-rich materials using ilmenite according to claim 1, characterized in that, The hydrolysis process also includes sedimentation, washing, solid-liquid separation, and drying.
8. The method for preparing titanium-rich materials using ilmenite according to claim 7, characterized in that, A second reducing agent is added to the liquid after solid-liquid separation, followed by evaporation and crystallization to obtain second hydrochloric acid and ferrous chloride; the second hydrochloric acid is concentrated and used for acid hydrolysis. After adding the second reducing agent, Ti in the liquid after solid-liquid separation 3+ The concentration is 0.5~1.5 g / L; The second reducing agent includes reduced iron powder.
Citation Information
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