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CN-122010579-A - Periclase-high-entropy spinel composite refractory material and preparation method thereof

CN122010579ACN 122010579 ACN122010579 ACN 122010579ACN-122010579-A

Abstract

The invention particularly relates to a periclase-high-entropy spinel composite refractory material and a preparation method thereof. The preparation method comprises the steps of mixing the multi-component metal chloride, the complexing agent and water according to the mole ratio of the complexing agent to the multi-component metal chloride being 1-3:1, stirring to obtain multi-component metal oxide sol with the concentration of 10-40 wt%, mixing the multi-component metal oxide sol with periclase with the concentration of 60-90 wt% and the multi-component metal oxide sol with the concentration of 10-40 wt% serving as raw materials, drying, adding a binding agent accounting for 1-8 wt% of the raw materials, mixing, pressing and forming, heating to 1400-1600 ℃ at the rate of 5-10 ℃ per min in an air atmosphere, and cooling to room temperature along with a furnace to obtain the periclase-high entropy spinel composite refractory material. The invention has the characteristics of easy control of the process, low cost and high production efficiency, and the prepared periclase-high entropy spinel composite refractory material has good thermal shock resistance, good hydration resistance and excellent mechanical property.

Inventors

  • LIANG FENG
  • XIAO RUI
  • ZHANG SHAOWEI
  • XU WENXIA
  • Hua Hongzhan
  • ZHANG HAIJUN
  • DUAN HONGJUAN

Assignees

  • 武汉科技大学

Dates

Publication Date
20260512
Application Date
20260206

Claims (10)

  1. 1. A preparation method of periclase-high-entropy spinel composite refractory material is characterized by comprising the steps of mixing a complexing agent, a multicomponent metal chloride and water according to the mole ratio of the complexing agent to the multicomponent metal chloride of 1-3:1, stirring to obtain a multicomponent metal oxide sol with the concentration of 10-40 wt%, mixing 60-90 wt% of periclase and 10-40 wt% of multicomponent metal oxide sol with the periclase, drying, adding a binding agent accounting for 1-8 wt% of the raw materials, mixing, pressing and forming, and then heating to 1400-1600 ℃ at the speed of 5-10 ℃ per minute in an air atmosphere, and cooling to room temperature along with a furnace to obtain the periclase-high-entropy spinel composite refractory material.
  2. 2. The preparation method of the periclase-high-entropy spinel composite refractory material according to claim 1 is characterized in that the multi-component metal chloride salt consists of more than five metal chloride salts, wherein the metal chloride salt is one of magnesium chloride, nickel chloride, manganese chloride, ferrous chloride, cobalt chloride, copper chloride, zinc chloride and aluminum chloride, the molar ratio of other metal chloride salts except aluminum chloride in the multi-component metal chloride salt is equal, the molar ratio of aluminum chloride to any one of the other metal chloride salts is 9-14:1, and the purity of the multi-component metal chloride salt is more than or equal to 98wt%.
  3. 3. The method for preparing periclase-high entropy spinel composite refractory according to claim 1, wherein the complexing agent is citric acid or propylene oxide.
  4. 4. The method for preparing periclase-high-entropy spinel composite refractory according to claim 1, wherein the stirring time is 0.5-2 h, and the stirring rotating speed is 500-1000 rpm.
  5. 5. The method for preparing periclase-high-entropy spinel composite refractory according to claim 1, wherein the MgO content of periclase is more than or equal to 98wt%, and the granularity of periclase is less than or equal to 5mm.
  6. 6. The method for preparing periclase-high entropy spinel composite refractory according to claim 1, wherein the binding agent is one of pulp waste liquid, polyvinyl alcohol and phenolic resin.
  7. 7. The method for preparing periclase-high-entropy spinel composite refractory material according to claim 1, wherein the pressure of the compression molding is 100-300 mpa.
  8. 8. The method for preparing periclase-high entropy spinel composite refractory according to claim 1, wherein the drying temperature is 80-110 ℃ and the drying time is 6-12 h.
  9. 9. The method for preparing periclase-high-entropy spinel composite refractory material according to claim 1, wherein the heat preservation time is 2-6 hours.
  10. 10. Periclase-high-entropy spinel composite refractory material, which is characterized in that the periclase-high-entropy spinel composite refractory material is prepared by the preparation method of the periclase-high-entropy spinel composite refractory material according to any one of claims 1-9.

Description

Periclase-high-entropy spinel composite refractory material and preparation method thereof Technical Field The invention belongs to the technical field of periclase composite refractory materials. In particular to a periclase-high entropy spinel composite refractory material and a preparation method thereof. Background Periclase (MgO) has a melting point as high as 2800 ℃, has the advantages of excellent high-temperature performance, stable chemical property and strong alkaline slag corrosion resistance, and is a core composition phase of magnesia refractory materials. The magnesia refractory material has good high temperature resistance and slag invasion resistance, so that the magnesia refractory material is widely applied to the fields of ferrous metallurgy, cement rotary kilns, glass, lime kilns and the like. However, periclase at normal temperature to 1000 ℃ has an average thermal expansion coefficient of about 13.5X10 -6/°C, has higher thermal expansion rate, causes stress concentration and poorer thermal shock resistance, is easy to react with water at normal temperature, generates hydration phenomenon, generates magnesium hydroxide [ Mg (OH) 2 ], causes volume expansion and structural damage of the material, and seriously affects the performance and service life of the refractory material. Accordingly, those skilled in the art have studied to improve the thermal shock resistance, hydration resistance and mechanical properties of magnesia refractories: A kind of magnesium manganese spinel refractory material and its preparation method and application "(CN 118754611A) technology," a kind of cement kiln used magnesium iron spinel brick and its preparation method "(CN 118754614A) technology and" a kind of low aluminum magnesium composite unburned brick and its preparation method "(CN 111302769A) technology, the above-mentioned three technologies adopt to add or in situ produce magnesium aluminate spinel, manganese aluminate spinel, zinc aluminate spinel or iron aluminate spinel to prepare the magnesium refractory material into magnesia (periclase), however spinel raw materials are low in activity, difficult to sinter, it is difficult to realize sintering densification of the magnesium refractory material to add spinel directly, the mechanical property of finished products is poor, and the generation of spinel produced in situ causes about 8% volume expansion, easy to cause the material structural damage. The technology prepares a magnesia refractory material by adding magnesia-alumina spinel, silicon carbide, titanium dioxide powder and boron oxide powder, but the unfired technology determines that the magnesia refractory material has inherent control difficulties in links such as raw material treatment, mixed forming, binder adaptation and the like, and borosilicate glass phase is easy to form under high temperature conditions, so that the high temperature mechanical property and thermal shock resistance of the material are reduced. A process for preparing the hydrophobic refractory material (CN 116730728B) difficult to hydrate includes such steps as mixing organic coupling agent, inorganic micro-nano powder and organic solventThe inorganic composite modified solution is uniformly coated on the alkaline refractory material to form super-hydrophobic organic on the surface thereofThe inorganic composite protective layer has higher cost of modified solution, is not friendly to the environment due to the use of an organic coupling agent and a solvent, is difficult to form a continuous protective layer with magnesium oxide and/or calcium oxide by a small amount of inorganic micro-nano powder, is not beneficial to the improvement of high-temperature hydration resistance of the material, and has lower production efficiency due to refined coating operation and high rework rate. Disclosure of Invention The invention aims to overcome the defects of the existing materials and provide a preparation method of periclase-high entropy spinel composite refractory material which is easy to control in process, low in cost and high in production efficiency. In order to achieve the above purpose, the invention adopts the following technical scheme: Mixing the multi-component metal chloride, the complexing agent and water according to the mole ratio of the complexing agent to the multi-component metal chloride of 1-3:1, stirring to obtain multi-component metal oxide sol with the concentration of 10-40 wt%, mixing the multi-component metal oxide sol with periclase with the concentration of 60-90 wt% and the multi-component metal oxide sol with the concentration of 10-40 wt% serving as raw materials, drying, adding a binding agent accounting for 1-8 wt% of the raw materials, mixing, pressing and forming, heating to 1400-1600 ℃ at the rate of 5-10 ℃ per min in an air atmosphere, and cooling to room temperature along with a furnace to obtain the periclase-high entropy spinel composite refractory material. The multi-component me