Method for preparing spinel type microcrystalline ceramic by tempering titanium extraction tailings

By mixing titanium extraction tailings with ilmenite slag, ball milling, and then subjecting the mixture to heat treatment and water cooling, spinel-type microcrystalline ceramics with high hardness and resistance to acid and alkali corrosion were prepared. This solved the problem of the difficulty in directionally generating spinel from titanium extraction tailings and realized the efficient resource utilization of metallurgical solid waste.

CN122010415APending Publication Date: 2026-05-12NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
Filing Date
2026-02-24
Publication Date
2026-05-12

AI Technical Summary

Technical Problem

In existing technologies, it is difficult to directionally generate spinel main crystalline phase in titanium extraction tailings, resulting in insufficient mechanical properties and acid and alkali corrosion resistance of microcrystalline ceramics. At the same time, the stockpiling of metallurgical solid waste leads to environmental pollution and resource waste.

Method used

Titanium extraction tailings and ilmenite slag are mixed and then subjected to ball milling, heat treatment and water cooling to promote the directional formation of magnesium aluminum spinel, forming spinel-type microcrystalline ceramics. The high hardness and chemical stability of spinel are utilized to improve the acid and alkali corrosion resistance.

Benefits of technology

The prepared spinel-type microcrystalline ceramics have high hardness and excellent resistance to acid and alkali corrosion, realizing the high-value utilization of metallurgical solid waste and reducing energy consumption and environmental pollution in the preparation process.

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Abstract

The invention relates to the technical field of comprehensive utilization of metallurgical solid waste resources, in particular to a method for preparing spinel type microcrystalline ceramic by tempering titanium extraction tailings. The method comprises the steps that the titanium extraction tailings serve as raw materials, the titanium iron slag serves as a tempering agent, the titanium extraction tailings and the titanium iron slag are mixed to form mixed slag materials, and after the mixed slag materials are subjected to ball milling and drying, ball-milled materials are obtained; and carrying out heat treatment on the ball-milled material, and then carrying out water-cooling treatment to obtain the spinel type microcrystalline ceramic. According to the method, the titanium-iron slag is doped into the titanium extraction tailings for hardening and tempering, so that the content of Al2O3 in a system is effectively increased, directional generation of a spinel phase is promoted, and the spinel type microcrystalline ceramic is endowed with excellent mechanical strength and acid and alkali corrosion resistance by virtue of high hardness and high chemical stability of spinel. According to the method, the metallurgical solid waste is used as the raw material, synergistic high-value utilization of the solid waste is achieved through a simple technological process, the resource utilization rate is remarkably increased, and good environmental and economic benefits are achieved.
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Description

Technical Field

[0001] This invention relates to the field of comprehensive utilization technology of metallurgical solid waste resources, specifically to a method for preparing spinel-type microcrystalline ceramics by conditioning titanium tailings. Background Technology

[0002] Vanadium and titanium have broad application prospects in high-quality steel, high-end aerospace materials, and all-vanadium redox flow batteries. Vanadium-titanium magnetite is the main mineral where vanadium and titanium are found. According to statistics, my country's vanadium-titanium magnetite reserves exceed 24 billion tons, mainly distributed in Chengde, Hebei; Panzhihua, Sichuan; and Hami, Xinjiang.

[0003] After blast furnace smelting, vanadium-titanium magnetite produces vanadium-containing iron in the molten iron and titanium in the slag, forming titanium-containing blast furnace slag. The vanadium-containing iron is then processed through a converter-hydrometallurgical process to extract vanadium, while the titanium-containing blast furnace slag has a low resource utilization rate and is mainly stockpiled. In my country, over 95% of vanadium-titanium magnetite smelting is done via a blast furnace-converter process, with a vanadium recovery rate of only 44% and a titanium recovery rate of less than 20%, resulting in low vanadium and titanium resource utilization, large amounts of solid waste, and high carbon emissions. Against this backdrop, existing technologies propose a hydrogen-based vertical shaft furnace reduction-electric furnace smelting technology for vanadium-titanium ore. The titanium-containing slag obtained from the electric furnace smelting is then processed through beneficiation and smelting to obtain high-titanium and low-titanium materials. The high-titanium material is then treated with carbonization and chlorination to produce titanium tetrachloride, while the low-titanium material is used to prepare ferrotitanium-titanium alloys through aluminothermic reduction. The preparation of titanium tetrachloride generates titanium extraction tailings, while the aluminothermic process for preparing ferrotitanium alloys produces ferrotitanium slag. The stockpiling of these metallurgical tailings not only occupies large amounts of land and pollutes the environment but also represents a serious waste of resources. Therefore, the high-value utilization of titanium extraction tailings is a crucial link in building a waste-free industrial chain for vanadium-titanium new energy.

[0004] The vanadium-titanium ore hydrogen-based vertical shaft furnace reduction-electric furnace melting technology produces titanium extraction tailings with the main chemical composition of CaO, Al2O3, SiO2, MgO, and TiO2. These tailings can be recycled to prepare cement mortar admixtures, concrete admixtures, and microcrystalline ceramics. Microcrystalline ceramics, also known as glass ceramics, are a type of microcrystalline material containing a large amount of microcrystalline phase and a small amount of glass phase, obtained through heat treatment. Currently, the main methods for preparing microcrystalline ceramics include integral crystallization, melting, and direct sintering. Among these, the crystalline phases of microcrystalline ceramics prepared using titanium extraction tailings as raw material are mainly calcium magnesium feldspar, perovskite, and diopside. The resulting microcrystalline ceramics have low hardness and poor resistance to acid and alkali corrosion. Furthermore, the preparation of microcrystalline ceramics using titanium extraction tailings often employs sintering, a process of heating, melting, cooling, and then heating again for sintering, resulting in high energy consumption. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a method for preparing spinel-type microcrystalline ceramics by tempering titanium extraction tailings. This invention uses titanium extraction tailings as raw material and ilmenite slag as a tempering agent. The mixture of titanium extraction tailings and ilmenite slag is sequentially subjected to ball milling, heat treatment (high-temperature melting-directional crystallization), and water cooling to obtain spinel-type microcrystalline ceramics. By incorporating ilmenite slag into the titanium extraction tailings for tempering, this invention effectively increases the Al2O3 content of the system, promoting the directional formation of the spinel phase. Furthermore, leveraging the high hardness and chemical stability of spinel itself, the microcrystalline ceramics possess excellent mechanical strength and resistance to acid and alkali corrosion. This not only overcomes the problems of existing technologies, such as the difficulty in directionally forming the spinel main crystalline phase from titanium extraction tailings and insufficient mechanical and corrosion resistance of the products, but also solves the problems of environmental pollution and resource waste caused by metallurgical solid waste stockpiling and the inability to achieve synergistic high-value utilization of multi-source solid waste.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows: The first objective of this invention is to provide a method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings, comprising the following steps: S1. Using titanium extraction tailings as raw material and titanium-iron slag with high Al2O3 content as conditioning agent, the titanium extraction tailings and titanium-iron slag are mixed to form a mixed slag material. The mixed slag material is ball-milled and dried to obtain the ball-milled material.

[0007] S2. The ball-milled material is heat-treated by first melting it at a high temperature, then cooling it down to allow the magnesium aluminum spinel to grow in a directional manner. Subsequently, it is rapidly cooled by water cooling to fix the magnesium aluminum spinel phase structure and form a glass phase, thus obtaining spinel-type microcrystalline ceramics.

[0008] Preferably, in the mixed slag material, the mass percentage of titanium extraction tailings is 80wt.%~95wt.% and the mass percentage of ilmenite slag is 5wt.%~20wt.% to promote the formation of magnesium aluminum spinel.

[0009] Preferably, in the mixed slag, the mass percentage of titanium extraction tailings is 90 wt.% and the mass percentage of ilmenite slag is 10 wt.%.

[0010] Preferably, the heat treatment process is as follows: first, the temperature is raised to 1500℃ to melt the ball-milled material, ensuring uniform composition, and then held at 1500℃ for 0.5h~2h; then, the temperature is lowered to 1100℃~1400℃ at a cooling rate of 1℃ / s~5℃ / s, and held at 1100℃~1400℃ for 0.5h~2h to allow the magnesium aluminum spinel to grow in a directional manner, ensuring that the high-melting-point magnesium aluminum spinel is fully precipitated.

[0011] Preferably, the ball milling conditions are as follows: using a planetary ball mill, mixing at 25°C and 500 r / min for at least 4 hours.

[0012] Preferably, the drying conditions are: drying at 60℃~105℃ for at least 8 hours.

[0013] Preferably, the particle size of both titanium extraction tailings and ilmenite slag is less than 200 mesh.

[0014] Preferably, the spinel-type microcrystalline ceramic has a Vickers hardness of 770Hv~810Hv, an acid corrosion weight loss rate (3 vol.% hydrochloric acid, 72h) of less than 18 wt.%, and an alkali corrosion weight loss rate (30 g / L KOH, 72h) of less than 4 wt.%.

[0015] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention provides a method for preparing spinel-type microcrystalline ceramics by conditioning titanium extraction tailings. Using titanium extraction tailings as raw material and ilmenite slag as a conditioning agent, the titanium extraction tailings and ilmenite slag are mixed to form a mixed slag material. The mixed slag material is ball-milled and dried to obtain ball-milled material. The ball-milled material is then heat-treated. First, at high temperature, the ball-milled material is melted through ion diffusion and migration. Then, it is cooled to allow crystallization, resulting in the directional growth of magnesium aluminate spinel. Subsequently, it is rapidly cooled by water cooling to fix the magnesium aluminate spinel phase structure and form a glassy phase, thus obtaining spinel-type microcrystalline ceramics. This invention utilizes ilmenite slag to condition and modify titanium extraction tailings. By increasing the Al2O3 content in the titanium extraction tailings, the high-melting-point spinel phase is preferentially generated at high temperatures, while inhibiting the precipitation of crystals such as feldspar and perovskite. Finally, water cooling is used to obtain spinel-type microcrystalline ceramics. The spinel-type microcrystalline ceramics prepared by this invention have spinel phase as the main crystalline phase, and have high hardness, excellent acid and alkali corrosion resistance and low preparation cost, which are significantly better than unconditioned titanium extraction tailings microcrystalline ceramics.

[0016] 2. This invention adopts a short-process technology of "one-time melting-controllable crystallization-water cooling", which eliminates the re-sintering step in the traditional microcrystalline ceramic preparation. It also uses titanium tailings and titanium-iron slag, two metallurgical solid wastes, as raw materials to achieve synergistic utilization, effectively solving the problems of low resource utilization rate of solid waste and low added value of products. Attached Figure Description

[0017] Figure 1 These are physical images of the spinel-type microcrystalline ceramics prepared according to the present invention, wherein a is the spinel-type microcrystalline ceramic prepared in Example 1, and b is the spinel-type microcrystalline ceramic prepared in Example 4.

[0018] Figure 2These are phase analysis diagrams of the spinel-type microcrystalline ceramics prepared according to the present invention, wherein (a) is the phase analysis diagram of the spinel-type microcrystalline ceramics prepared in Example 1, (b) is the phase analysis diagram of the spinel-type microcrystalline ceramics prepared in Example 2, (c) is the phase analysis diagram of the spinel-type microcrystalline ceramics prepared in Example 3, and (d) is the phase analysis diagram of the spinel-type microcrystalline ceramics prepared in Example 4. Detailed Implementation

[0019] The technical solution of the present invention will be clearly and completely described below with reference to the data in the embodiments of the present invention. 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 of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0020] It should be noted that the technical terms used in this invention are for the purpose of describing specific embodiments only and are not intended to limit the scope of protection of this invention. Unless otherwise specified, all raw materials, reagents, instruments and equipment used in the following embodiments of this invention can be purchased on the market or prepared by existing methods. The chemical composition and content of titanium extraction tailings and ilmenite slag are shown in Tables 1 and 2.

[0021] Table 1 shows the chemical composition (wt.%) of titanium extraction tailings. Table 2 shows the chemical composition (wt.%) of the ilmenite slag. Although the ilmenite slag has a low MgO content, the titanium extraction tailings contain sufficient MgO. After mixing, the stoichiometric ratio of magnesium aluminum spinel is satisfied. The ilmenite slag mainly provides Al2O3 to increase the aluminum content of the system.

[0022] This invention utilizes titanium extraction tailings and ilmenite slag to synergistically prepare spinel-type microcrystalline ceramics, which can fully utilize both titanium extraction tailings and ilmenite slag, achieving their high-value utilization and providing good environmental and economic benefits.

[0023] To enable those skilled in the art to more clearly understand the technical solution of the present invention, the following will provide a detailed description in conjunction with specific embodiments: Example 1 A method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings includes the following steps: S1. Add ilmenite slag to the titanium extraction tailings to obtain a mixed slag material, such that the mass percentage of titanium extraction tailings in the mixed slag material is 90 wt.% and the mass percentage of ilmenite slag is 10 wt.%. Use a planetary ball mill to ball mill the mixed slag material at 25℃ and 500 r / min for 4 hours, and then dry it at 105℃ for 8 hours to obtain the ball-milled material.

[0024] S2. The ball-milled material is loaded into an alumina crucible and placed in an electric resistance furnace for heat treatment. The temperature of the electric resistance furnace is raised from 25°C to 1500°C at a heating rate of 5°C / s. After the temperature reaches 1500°C, it is held for 2 hours. After the holding period, the furnace temperature is lowered to 1300°C at a cooling rate of 3°C / s and held at 1300°C for 2 hours to obtain slag.

[0025] S3. The slag is water-cooled at 25°C for 5 minutes to obtain spinel-type microcrystalline ceramics, as shown in the picture. Figure 1 As shown in 'a'.

[0026] X-ray diffraction analysis was performed on the spinel-type microcrystalline ceramics prepared in Example 1, and the results are as follows: Figure 2 As shown. By Figure 2 It was found that the phase composition of the spinel-type microcrystalline ceramic prepared in Example 1 consisted of a spinel phase and a glass phase.

[0027] The hardness of the spinel-type microcrystalline ceramic prepared in Example 1 was analyzed using a Vickers hardness tester, and its Vickers hardness was found to be 800.59 Hv.

[0028] At 25°C, the spinel-type microcrystalline ceramic prepared in Example 1 was immersed in 3 vol.% hydrochloric acid for 72 h and subjected to acid corrosion resistance test. The results showed that the weight loss rate of the spinel-type microcrystalline ceramic prepared in Example 1 was 13.36 wt.%.

[0029] At 25°C, the spinel-type microcrystalline ceramic prepared in Example 1 was immersed in a 30 g / L KOH solution for 72 h and subjected to an alkali corrosion resistance test. The results showed that the weight loss rate of the spinel-type microcrystalline ceramic prepared in Example 1 was 0.54 wt.%.

[0030] Example 2 A method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings includes the following steps: S1. Add ilmenite slag to the titanium extraction tailings to obtain a mixed slag material, such that the mass percentage of titanium extraction tailings in the mixed slag material is 95 wt.% and the mass percentage of ilmenite slag is 5 wt.%. Use a planetary ball mill to ball mill the mixed slag material at 25℃ and 500 r / min for 4 hours, and then dry it at 105℃ for 8 hours to obtain the ball-milled material.

[0031] S2. The ball-milled material is loaded into an alumina crucible, and the alumina crucible is placed in an electric resistance furnace for heat treatment. The temperature of the electric resistance furnace is raised from 25℃ to 1500℃ at a heating rate of 2℃ / s. After the temperature reaches 1500℃, it is held for 1 hour. After the holding period, the furnace temperature is lowered to 1200℃ at a cooling rate of 2℃ / s, and held at 1200℃ for 1 hour to obtain slag.

[0032] S3. The slag is water-cooled at 35°C for 10 minutes to obtain spinel-type microcrystalline ceramics.

[0033] X-ray diffraction analysis was performed on the spinel-type microcrystalline ceramics prepared in Example 2, and the results are as follows: Figure 2 As shown. By Figure 2 It was found that the phase composition of the spinel-type microcrystalline ceramic prepared in Example 2 consisted of spinel phase, perovskite phase and glass phase, with spinel and glass phase being the main components.

[0034] The hardness of the spinel-type microcrystalline ceramics prepared in Example 2 was analyzed using a Vickers hardness tester, and it was found that the Vickers hardness of the spinel-type microcrystalline ceramics prepared in Example 2 was 788.83 Hv.

[0035] At 25°C, the spinel-type microcrystalline ceramics prepared in Example 2 were immersed in 3 vol.% hydrochloric acid for 72 h and subjected to acid corrosion resistance test. It was found that the weight loss rate of the spinel-type microcrystalline ceramics prepared in Example 2 was 17.82 wt.%.

[0036] At 25°C, the spinel-type microcrystalline ceramics prepared in Example 2 were immersed in a 30 g / L KOH solution for 72 h and subjected to an alkali corrosion resistance test. The weight loss rate of the spinel-type microcrystalline ceramics prepared in Example 2 was found to be 3.51 wt.%.

[0037] Example 3 A method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings includes the following steps: S1. Add ilmenite slag to the titanium extraction tailings to obtain a mixed slag material, such that the mass percentage of titanium extraction tailings in the mixed slag material is 86 wt.% and the mass percentage of ilmenite slag is 14 wt.%. Use a planetary ball mill to ball mill the mixed slag material at 25℃ and 500 r / min for 4 hours, and then dry it at 105℃ for 8 hours to obtain the ball-milled material.

[0038] S2. The ball-milled material is loaded into an alumina crucible, and the alumina crucible is placed in an electric resistance furnace for heat treatment. The temperature of the electric resistance furnace is raised from 25℃ to 1500℃ at a heating rate of 3℃ / s. After the temperature reaches 1500℃, it is held for 1.5h. After the holding period, the furnace temperature is lowered to 1250℃ at a cooling rate of 5℃ / s and held for 1.5h to obtain slag.

[0039] S3. The slag is water-cooled at 45°C for 5 minutes to obtain spinel-type microcrystalline ceramics.

[0040] X-ray diffraction analysis was performed on the spinel-type microcrystalline ceramics prepared in Example 3, and the results are as follows: Figure 2 As shown. By Figure 2 It was found that the phase composition of the spinel-type microcrystalline ceramic prepared in Example 3 consisted of spinel phase, perovskite phase and glass phase, with spinel and glass phase being the main components.

[0041] The hardness of the spinel-type microcrystalline ceramics prepared in Example 3 was analyzed using a Vickers hardness tester, and it was found that the Vickers hardness of the spinel-type microcrystalline ceramics prepared in Example 3 was 801.26 Hv.

[0042] At 25°C, the spinel-type microcrystalline ceramic prepared in Example 3 was immersed in 3 vol.% hydrochloric acid for 72 h and subjected to acid corrosion resistance test. It was found that the weight loss rate of the spinel-type microcrystalline ceramic prepared in Example 3 was 17.24 wt.%.

[0043] At 25°C, the spinel-type microcrystalline ceramic prepared in Example 3 was immersed in a 30 g / L KOH solution for 72 h and subjected to an alkali corrosion resistance test. The weight loss rate of the spinel-type microcrystalline ceramic prepared in Example 3 was found to be 3.16 wt.%.

[0044] Example 4 A method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings includes the following steps: S1. Add ilmenite slag to the titanium extraction tailings to obtain a mixed slag material, such that the mass percentage of titanium extraction tailings in the mixed slag material is 92 wt.% and the mass percentage of ilmenite slag is 8 wt.%. Use a planetary ball mill to ball mill the mixed slag material at 25℃ and 500 r / min for 4 hours, and then dry it at 105℃ for 8 hours to obtain the ball-milled material.

[0045] S2. The ball-milled material is loaded into an alumina crucible and placed in an electric resistance furnace for heat treatment. The temperature of the electric resistance furnace is raised from 25°C to 1500°C at a heating rate of 5°C / s. After the temperature reaches 1500°C, it is held for 2 hours. After the holding period, the furnace temperature is lowered to 1300°C at a cooling rate of 2°C / s and held for 2 hours to obtain slag.

[0046] S3. The slag is water-cooled at 25°C for 5 minutes to obtain spinel-type microcrystalline ceramics, as shown in the picture. Figure 1 As shown in b in the figure.

[0047] X-ray diffraction analysis was performed on the spinel-type microcrystalline ceramics prepared in Example 4, and the results are as follows: Figure 2 As shown. By Figure 2It was found that the phase composition of the spinel-type microcrystalline ceramic prepared in Example 4 consisted of a spinel phase and a glass phase, with the spinel phase content being lower than that of the spinel-type microcrystalline ceramic prepared in Example 1.

[0048] The hardness of the spinel-type microcrystalline ceramic prepared in Example 4 was analyzed using a Vickers hardness tester, and it was found that the Vickers hardness of the spinel-type microcrystalline ceramic prepared in Example 4 was 773.51 Hv.

[0049] At 25°C, the spinel-type microcrystalline ceramic prepared in Example 4 was immersed in 3 vol.% hydrochloric acid for 72 h and subjected to acid corrosion resistance test. It was found that the weight loss rate of the spinel-type microcrystalline ceramic prepared in Example 4 was 15.27 wt.%.

[0050] At 25°C, the spinel-type microcrystalline ceramic prepared in Example 4 was immersed in a 30 g / L KOH solution for 72 h and subjected to an alkali corrosion resistance test. The weight loss rate of the spinel-type microcrystalline ceramic prepared in Example 4 was found to be 0.93 wt.%.

[0051] Comparative Example 1 A method for preparing microcrystalline ceramics by tempering titanium tailings includes the following steps: S1. Microcrystalline ceramics were prepared directly using titanium extraction tailings. A planetary ball mill was used to ball mill the titanium extraction tailings at 25℃ and 500r / min for 4 hours, and then dried at 105℃ for 8 hours to obtain the ball-milled material.

[0052] S2. The ball-milled material is loaded into an alumina crucible and placed in an electric resistance furnace for heat treatment. The temperature of the electric resistance furnace is raised from 25°C to 1500°C at a heating rate of 5°C / s. After the temperature reaches 1500°C, it is held for 2 hours. After the holding period, the furnace temperature is lowered to 1300°C at a cooling rate of 2°C / s and held for 2 hours to obtain slag.

[0053] S3. The slag is water-cooled at 25°C for 5 minutes to obtain microcrystalline ceramics.

[0054] X-ray diffraction analysis of the microcrystalline ceramics prepared in Comparative Example 1 revealed that the phase composition of the microcrystalline ceramics prepared in Comparative Example 1 consisted of albite phase, perovskite phase, pyroxene phase, anorthite phase, glass phase, and a small amount of spinel phase.

[0055] The hardness of the microcrystalline ceramic prepared in Comparative Example 1 was analyzed using a Vickers hardness tester, and it was found that the Vickers hardness of the microcrystalline ceramic prepared in Comparative Example 1 was 702.92 Hv.

[0056] At 25°C, the microcrystalline ceramic prepared in Comparative Example 1 was immersed in 3 vol.% hydrochloric acid for 72 h and subjected to acid corrosion resistance test. The weight loss rate of the microcrystalline ceramic prepared in Comparative Example 1 was found to be 32.82 wt.%.

[0057] At 25℃, the microcrystalline ceramics prepared in Comparative Example 1 were immersed in a 30 g / L KOH solution for 72 h and subjected to alkali corrosion resistance test. It was found that the weight loss rate of the spinel-type microcrystalline ceramics prepared in Comparative Example 1 was 10.27 wt.%.

[0058] It should be noted that when numerical ranges are involved in this invention, it should be understood that both endpoints of each numerical range, as well as any value between the two endpoints, can be selected. Since the steps and methods used are the same as in the embodiments, preferred embodiments are described here to avoid redundancy. Although preferred embodiments of the invention have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of this invention.

Claims

1. A method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings, characterized in that, Includes the following steps: Titanium extraction tailings are used as raw material and ilmenite slag is used as a conditioning agent. The titanium extraction tailings and ilmenite slag are mixed to form a mixed slag material. The mixed slag material is ball-milled and dried to obtain the ball-milled material. The ball-milled material is heat-treated by first melting it at a high temperature, then cooling it down to allow magnesium aluminum spinel to grow in a directional manner. It is then rapidly cooled by water cooling to fix the magnesium aluminum spinel phase structure and form a glassy phase, thus obtaining spinel-type microcrystalline ceramics.

2. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, In the mixed slag, the mass percentage of titanium extraction tailings is 80wt.%~95wt.%, and the mass percentage of ilmenite slag is 5wt.%~20wt.%.

3. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, In the mixed slag, the mass percentage of titanium extraction tailings is 90 wt.% and the mass percentage of ilmenite slag is 10 wt.%.

4. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, The heat treatment process is as follows: first, heat the temperature to 1500℃ and hold it at 1500℃ for 0.5h to 2h; then, cool the temperature to 1100℃ to 1400℃ at a cooling rate of 1℃ / s to 5℃ / s and hold it at 1100℃ to 1400℃ for 0.5h to 2h.

5. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, The ball milling conditions are as follows: using a planetary ball mill, mixing at 25℃ and 500 r / min for at least 4 hours.

6. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, The conditions for water cooling are: cooling at 25℃~45℃ for 5min~10min.

7. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, The drying conditions are: drying at 60℃~105℃ for at least 8 hours.

8. The method for preparing spinel-type microcrystalline ceramics by tempering titanium tailings according to claim 1, characterized in that, The particle size of both titanium extraction tailings and ilmenite slag is less than 200 mesh.