A kind of regeneration method of waste silicon carbide-silicon nitride refractory brick and its application

A waste silicon carbide and silicon nitride technology, applied in the production of bulk chemicals, carbon preparation/purification, ammonium fluoride, etc., can solve the problems of large water consumption, lack of recycling technology, high energy consumption, etc.

Active Publication Date: 2020-05-26
长沙紫宸科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are a series of technical defects in this method: first, it takes too long and the processing capacity is limited, and the water immersion time reaches 2 to 3 days at a time, and multiple rounds of water immersion, block selection, and water immersion are required; , objectively consumes a lot of water, because the fluoride salt it contains is only slightly soluble in water, and the maximum solubility of sodium fluoride in pure water is only 3.6-5g / 100mL water; pollution, and the cyanide in it has not been safely treated; fourth, the process is complicated; fifth, the energy consumption of the treatment is high, and it needs to be ground into powder with super hardness silicon carbide emery material, and the general grinding body is not competent The grinding function of this superhard material needs to be dried and calcined in a high-temperature electric furnace at 1700-1900°C; Sixth, the product has high content of impurities such as fluorine and aluminum and low value, and calcination in a high-temperature electric furnace at 1700-1900°C is not enough Volatile most of the impurities in it, but it will decompose the silicon carbide and silicon nitride in it, even the highly stable silicon nitride will sublimate and decompose at the melting point of 1900°C
[0006] Although the current SiC-Si 3 N 4 Refractory bricks are expensive, SiC, Si 3 N 4 The market value of the material is high, but due to the lack of effective recycling technology at home and abroad, a large number of waste silicon carbide-silicon nitride refractory bricks in the electrolytic aluminum industry are discarded, landfilled or stockpiled, or sent to high-temperature kilns as waste. Oxidation treatment, only part of the large waste silicon carbide-silicon nitride refractory bricks are used to replace genuine refractory bricks as refractory and wear-resistant materials for industrial kilns, and a small amount is directly crushed to replace genuine abrasives and mixed into the market

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1( approach 1)

[0065] The used waste SiC-Si of the embodiment of the present invention 3 N 4 The refractory brick is taken from the electrolytic cell of an aluminum factory, and its main chemical composition is: SiC 68.46%, Si 3 N 4 19.78%, Al 2 o 3 1.34%, Fe 2 o 3 0.37%, Na 2 O 3.97%, F 4.13%, f-Si0.32%, C 1.73%, cyanide 0.12%; the soaking solution is commercially available sodium hydroxide, sodium hypochlorite (available chlorine content 13%), surfactant sulfamic acid An aqueous solution made of sodium containing 1.0% sodium hypochlorite, 15% sodium hydroxide and 0.35% surfactant in terms of available chlorine.

[0066] Using the impact crushing method, first 10kg waste SiC-Si 3 N 4 The refractory bricks are broken into granular materials with a particle size of less than 5mm, placed in a macerating tank with a stirring device, adding 25kg of macerating solution, stirring and macerating at 80°C for 1.2h to obtain an oxidized macerating slurry, and adding Diluted with 20kg of wa...

Embodiment 2( approach 1)

[0070]The used waste SiC-Si of the embodiment of the present invention 3 N 4 Refractory brick and soaking solution are the same as embodiment 1.

[0071] Put 1 kg of waste silicon carbide-silicon nitride refractory bricks and 6 kg of refractory solution in an impact crusher, crush and retort in the refractory solution at 30°C for 0.5 hours to obtain oxidized refractory slurry, stand still, and separate Suspended carbon slurry and sedimentation slurry are filtered and separated to obtain filter residue and carbon respectively, and the filter residue is washed and dried to a moisture content of 0.6% to obtain a silicon carbide-silicon nitride composite powder.

[0072] After testing, the main chemical components of the obtained silicon carbide-silicon nitride composite powder are: SiC 74.97%, Si 3 N 4 24.23%, Al 2 o 3 0.17%, Fe 2 o 3 0.06%, Na 2 O 0.08%, F 0.08%, f-Si 0.00%, C 0.05%, cyanide was not detected.

[0073] Combine the carbon slurry and the filtrate filtered...

Embodiment 3( approach 1)

[0075] The used waste SiC-Si of the embodiment of the present invention 3 N 4 Refractory brick and soaking solution are the same as embodiment 1.

[0076] Use the impact crushing method to crush 10kg of waste silicon carbide-silicon nitride refractory bricks into granular materials with a particle size of less than 5mm. After macerating for 2 hours, the oxidative maceration slurry was obtained, left to stand, separated into suspended carbon slurry and sedimentation slurry, and then separated by filtration to obtain filter residue and carbon respectively, and the filter residue was washed with 0.50mol / L dilute hydrochloric acid, Dry to a moisture content of 0.8% to obtain a silicon carbide-silicon nitride composite powder.

[0077] After testing, the main chemical components of the obtained silicon carbide-silicon nitride composite powder are: SiC 75.31%, Si 3 N 4 23.90%, Al 2 o 3 0.11%, Fe 2 o 3 0.06%, Na 2 O 0.08%, F0.07%, f-Si 0.00%, C0.09%, cyanide was not detect...

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Abstract

The invention discloses a regeneration method of waste silicon carbide-silicon nitride refractory brick and applications thereof. The method comprises following schemes: (1) grinding waste silicon carbide-silicon nitride refractory bricks, adding a retting solution, carrying out retting, allowing the solution to stand still, filtering the solution, washing, and drying; (2) after grinding, adding ammonium chloride, heating, keeping the temperature, extracting the slag by water, washing by water, and drying; (3) after grinding, adding ammonium chloride and water, heating, keeping the temperature, filtering, soaking dry slag in water, filtering, washing by water, and drying; (4) after grinding, adding ammonium chloride, adopting supercritical ammonia-ethanol-methanol extraction, and carrying out separation; and (5) after grinding, adding ammonium chloride, adopting supercritical carbon dioxide extraction, performing separation, extracting silicon carbide-silicon nitride by water, filtering, washing by water, and drying. The product is used to produce refractory bricks. The content of SiC and Si3N4 in regenerated powder is high. The reaction conditions are mild and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a regeneration method and its application, in particular to a regeneration method of waste silicon carbide-silicon nitride refractory bricks and its application. Background technique [0002] At present, the aluminum smelting enterprises of electrolytic aluminum in my country have built a production capacity of 43.698 million tons, and the operating production capacity has reached 36.739 million tons. The electrolysis temperature of the large-scale aluminum electrolytic prebaking tank is between 950 and 970 ° C, and about 50 kg of cryolite, aluminum fluoride, magnesium fluoride and other electrolytes are consumed for each ton of aluminum produced. Due to thermal effects, chemical effects, mechanical erosion, Due to the molten salt reaction and chemical reaction caused by the action of electricity, the penetration of sodium and electrolyte, etc., the cathode carbon block in the aluminum electrolytic cell will be damaged after a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/66C01C1/16C01B32/05
CPCC01C1/162C04B35/66Y02P20/54
Inventor 尹小林
Owner 长沙紫宸科技开发有限公司
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