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Comprehensive utilization method of etching waste liquid

A technology for etching waste liquid and filtrate, which is applied in the preparation/separation of ammonia, silicon dioxide, alkali metal fluoride, etc., can solve the problems of inability to carry out secondary cascade application, complex components, and pollute the environment, and achieve environmental protection benefits Significant, simple process, no three wastes discharge effect

Pending Publication Date: 2022-04-08
河南省氟基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the domestic BOE market demand is about 20,000 tons. After wet etching, a large amount of waste liquid containing fluorine, silicon, and ammonia nitrogen will be produced. The composition is complex and cannot be used in secondary cascade applications. If it is directly discharged, it will cause serious pollution. environment and waste of resources

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  • Comprehensive utilization method of etching waste liquid
  • Comprehensive utilization method of etching waste liquid
  • Comprehensive utilization method of etching waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] To 100kg of etching waste liquid containing 3% ammonium fluorosilicate, 2.5% ammonium sulfate, 15% ammonium fluoride, 10% ammonium hydrogen fluoride, and the balance is water, add 26.8kg of 17% ammonia water reaction , the reaction temperature was controlled at 40°C, the reaction time was 1h, and the pH at the end of the reaction was 7.5. The obtained reaction solution was filtered to obtain the filtrate (the first filtrate) and the solid (the first solid); the first solid was washed and dried , to obtain 0.99kg of white carbon black.

[0068] To the 121.8kg first filtrate prepared above, add 20.6kg lithium hydroxide, control the reaction temperature to 50°C, stir the reaction for 1h, and filter the obtained reaction product to obtain a filtrate (the second filtrate) and a solid (the second solid ); The second solid matter is washed and dried to obtain 21.1kg lithium fluoride; In the 103kg second filtrate, add 1.3kg white ash and filter after processing, obtain soft wat...

Embodiment 2

[0070] To 100kg of etching waste liquid containing 0.1% ammonium fluorosilicate, 0.1% ammonium sulfate, 10% ammonium fluoride, 3% ammonium hydrogen fluoride, and the balance is water, add 6.5kg mass fraction of 17% ammonia water to react, The reaction temperature was controlled at 50°C, the reaction time was 0.5h, and the pH of the reaction end was 7. The obtained reaction solution was filtered to obtain a filtrate (the first filtrate) and a solid (the first solid); the first solid was washed and dried , to obtain 10 g of white carbon black.

[0071] 10.3kg of aluminum hydroxide was added to the first filtrate of the above 106.3g, the reaction temperature was controlled at 70°C, the reaction was stirred for 0.5h, and the obtained reaction product was filtered to obtain a filtrate (the second filtrate) and a solid (the second solid) With the second solid matter washing, drying, obtain 21.4kg aluminum fluoride; Add 0.06kg white ash to 83.5kg second filtrate and filter after proc...

Embodiment 3

[0073] To 100kg of etching waste liquid containing 5% ammonium fluorosilicate, 5% ammonium sulfate, 25% ammonium fluoride, 15% ammonium bifluoride, and the balance of water, add 26.3kg of 17% ammonia water to react, The reaction temperature was controlled at 30°C, the reaction time was 1.5h, and the end point of the reaction was pH 8. The obtained reaction solution was filtered to obtain a filtrate (the first filtrate) and a solid (the first solid); the first solid was washed and dried , to obtain 1.66kg of white carbon black.

[0074] Add 55.8kg of sodium hydroxide to 120kg of the above-mentioned first filtrate, control the reaction temperature to 40 ° C, stir the reaction for 1.5h, and filter the obtained reaction product to obtain a filtrate (the second filtrate) and a solid (the second solid); The second solid matter is washed and dried to obtain 54.6kg of sodium fluoride; to the second filtrate of 83kg, add 2.55kg of white ash and filter after treatment, the gained soft w...

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Abstract

The invention provides a comprehensive utilization method of etching waste liquid, which comprises the following steps: carrying out first reaction on the etching waste liquid and ammonia water to obtain reaction liquid; filtering the reaction liquid to obtain filtrate and white carbon black; and carrying out a second reaction on the filtrate and a metal compound to obtain the metal fluoride. Compared with the prior art, the method has the advantages that the by-product etching waste liquid in the semiconductor industry is adopted as a raw material, efficient separation and recovery of fluorine and silicon elements and recycling of system ammonia are achieved through ammonolysis, fluorine precipitation and ammonia absorption, and high-purity metal fluoride, by-product high-quality white carbon black and industrial ammonia water are prepared; the comprehensive utilization method of the etching waste liquid provided by the invention is simple in process flow, low in production cost, good in product quality, free of emission of three wastes, and remarkable in economic, social and environment-friendly benefits.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemistry, and in particular relates to a comprehensive utilization method of etching waste liquid. Background technique [0002] Wet etching is an indispensable process in the processing of semiconductors and liquid crystal panels, and requires special electronic chemicals for etching. For fluorine-containing electronic chemicals, due to the extremely strong reactivity and large electronegativity of fluorine atoms, the product performance is more significant by replacing other groups on electronic chemicals with fluorine atoms and fluorine-containing groups. [0003] Electronic grade buffered etchant (BOE) composed of HF and NH 4 F is mixed in different proportions, HF is the main etching solution, NH 4 F is used as a buffer, using NH 4 F fixed [H + ] to maintain a certain etching rate, which is easier to control and better than electronic-grade hydrofluoric acid and ammonium fluoride etchin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04C01D3/02C01C1/02C01B33/18C01F7/50
Inventor 李云峰薛旭金李凌云刘海庆王建萍张明军高胜军席志渊郭海涛
Owner 河南省氟基新材料科技有限公司