CN-122010415-A - Method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium extraction tailings

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 ceramics by quenching and tempering titanium extraction tailings. The method comprises the steps of taking titanium extraction tailings as a raw material, taking titanium iron slag as a hardening and tempering agent, mixing the titanium extraction tailings and the ferrotitanium slag to form mixed slag, ball milling the mixed slag, drying to obtain ball milling materials, performing heat treatment on the ball milling materials, and performing water cooling treatment to obtain spinel type microcrystalline ceramics. According to the invention, the titanium slag is doped into the titanium extraction tailings for tempering, so that the content of the system Al 2 O 3 is effectively improved, the spinel phase is promoted to be directionally generated, and the spinel type microcrystalline ceramic is endowed with excellent mechanical strength and acid and alkali corrosion resistance by virtue of the high hardness and high chemical stability of the spinel. The invention takes metallurgical solid waste as a raw material, realizes the synergistic high-value utilization of the solid waste through a concise process flow, obviously improves the utilization rate of resources and has good environmental and economic benefits.

Inventors

• LIU BAO
• LI JUNGUO
• ZHU WU
• ZENG YANAN
• WANG YAJUN
• WANG YITONG
• ZHANG XI

Assignees

• 华北理工大学

Dates

Publication Date

20260512

Application Date

20260224

Claims (8)

1. 1. The method for preparing spinel type microcrystalline ceramics by quenching and tempering the titanium extraction tailings is characterized by comprising the following steps of: mixing the titanium extraction tailings with ferrotitanium slag serving as a hardening and tempering agent to form mixed slag, ball-milling the mixed slag, and drying to obtain a ball-milled material; And (3) carrying out heat treatment on the ball-milling material, melting the ball-milling material at a high temperature, cooling and crystallizing to enable the magnesia-alumina spinel to grow directionally, and carrying out water cooling treatment and rapid cooling to fix a magnesia-alumina spinel phase structure and form a glass phase to obtain the spinel type microcrystalline ceramic.
2. 2. The method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium extraction tailings according to claim 1, wherein the mass percentage of the titanium extraction tailings in the mixed slag is 80-95 wt.% and the mass percentage of the titanium iron slag is 5-20 wt.%.
3. 3. The method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium-extracted tailings according to claim 1, wherein the mixed slag comprises 90wt.% titanium-extracted tailings and 10wt.% titanium-iron tailings.
4. 4. The method for preparing spinel-type microcrystalline ceramic by quenching and tempering titanium extraction tailings according to claim 1, wherein the heat treatment is carried out by heating to 1500 ℃, preserving heat for 0.5-2 h at 1500 ℃, cooling to 1100-1400 ℃ at a cooling rate of 1-5 ℃ per second, and preserving heat for 0.5-2 h at 1100-1400 ℃.
5. 5. The method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium extraction tailings according to claim 1, wherein the ball milling condition is that a planetary ball mill is adopted, and mixing is carried out for at least 4 hours under the conditions of 25 ℃ and 500 r/min.
6. 6. The method for preparing spinel-type microcrystalline ceramic by quenching and tempering titanium extraction tailings according to claim 1, wherein the water cooling treatment condition is that cooling is carried out for 5 min-10 min at 25 ℃ to 45 ℃.
7. 7. The method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium extraction tailings according to claim 1, wherein the drying condition is that the spinel type microcrystalline ceramics are dried for at least 8 hours at 60-105 ℃.
8. 8. The method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium-extracted tailings according to claim 1, wherein the grain sizes of the titanium-extracted tailings and the titanium-iron slag are less than 200 meshes.

Description

Method for preparing spinel type microcrystalline ceramics by quenching and tempering titanium extraction tailings Technical Field 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 ceramics by quenching and tempering titanium extraction tailings. Background The vanadium and the titanium have wide application prospects in the fields of high-quality steel, high-end aviation materials, all-vanadium redox flow batteries and the like. Vanadium titano-magnetite is the main occurring mineral of vanadium and titanium, and the reserve of vanadium titano-magnetite in China is more than 240 hundred million tons according to statistics, and the vanadium titano-magnetite is mainly distributed in regions such as Hebei Maillard, sichuan Panzhihua and Xinjiang Hami. After the vanadium titano-magnetite is smelted by a blast furnace, vanadium element enters molten iron to generate vanadium-containing molten iron, and titanium element enters slag to generate titanium-containing blast furnace slag. Vanadium products are obtained by extracting vanadium from vanadium-containing molten iron through a converter-wet method, and the recycling utilization rate of titanium-containing blast furnace slag is low, and the method mainly comprises piling. The vanadium titano-magnetite smelting of more than 95% of China is a blast furnace-converter process, the vanadium recovery rate is only 44%, the titanium recovery rate is less than 20%, and the problems of low vanadium and titanium resource utilization rate, large solid waste and high carbon emission exist. Under the background, the prior art proposes a technical scheme of vanadium-titanium ore hydrogen-based shaft furnace reduction-electric furnace melting, titanium-containing slag obtained by electric furnace melting is subjected to dressing and smelting cooperative treatment to obtain high-titanium materials and low-titanium materials, the high-titanium materials are subjected to carbonization-chlorination treatment to prepare titanium tetrachloride, and the low-titanium materials are subjected to aluminothermic reduction to prepare ferrotitanium. Titanium extraction tailings are generated in the preparation process of titanium tetrachloride, titanium iron slag is generated in the preparation process of ferrotitanium alloy by an aluminothermic method, and the stockpiling of metallurgical tailings not only occupies a large amount of land and pollutes the environment, but also is a serious waste of resources. Therefore, the high-value utilization of the titanium extraction tailings is an important link for realizing the construction of the vanadium-titanium new energy waste-free industrial chain. The main chemical components of the titanium extraction tailings generated by the technical scheme of the reduction of the vanadium-titanium ore hydrogen-based shaft furnace and the electric furnace melting are CaO, al 2O3、SiO2, mgO and TiO 2, and the cement mortar admixture, the concrete admixture and the microcrystalline ceramics can be recycled and prepared. Microcrystalline ceramics, also known as glass ceramics, are a class of microcrystalline materials obtained by heat treatment that contain a large amount of microcrystalline phases and a small amount of glass phases. At present, the preparation method of the microcrystalline ceramics mainly comprises an integral crystallization method, a melting method and a direct sintering method. The crystalline phase of the microcrystalline ceramic prepared by taking the titanium extraction tailings as the raw material is mainly perovskite, perovskite and diopside, and the prepared microcrystalline ceramic has low hardness and poor acid and alkali corrosion resistance. In addition, the sintering method is mostly adopted for preparing the microcrystalline ceramics by adopting the titanium extraction tailings, so that the preparation method is a preparation flow of heating melting, cooling and then heating sintering, and the microcrystalline ceramics has higher preparation energy consumption. Disclosure of Invention Aiming at the defects existing in the prior art, the invention provides a method for preparing spinel-type microcrystalline ceramics by quenching and tempering extracted titanium tailings, which takes extracted titanium tailings as raw materials and titanium iron slag as a quenching and tempering agent, and (3) sequentially performing ball milling, heat treatment (high-temperature melting-directional crystallization) and water cooling treatment on the mixed slag of the titanium extraction tailings and the titanium iron slag to obtain the spinel type microcrystalline ceramic. According to the invention, by doping titanium iron slag into the titanium extraction tailings for tempering, the content of a system Al 2O3 is effectively improved, the spinel phase is promoted to be directionally generated, and the spine