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Environment-friendly comprehensive recycling method of organic silicon pulp residues

A technology of organosilicon and pulp residue, which is applied in the production of silicon compounds, chemical instruments and methods, and hydrogen, can solve the problems of poor fluidity of waste residue slurry, difficulty in utilization, and small solid particle size, and achieves significant environmental friendliness and Economic significance, reduction of waste disposal pressure, effect of reduction of waste of raw materials

Pending Publication Date: 2022-05-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of waste residue slurry is 20-70%. It is mainly organochlorosilane with high boiling point, which is easy to hydrolyze and will generate a large amount of acid mist when exposed to the air, polluting the environment
The waste slurry has poor fluidity, is not only abrasive and corrosive, and is easy to block pipes and equipment, but also has small solid particle size, large specific surface area, high activity, easy spontaneous combustion, and difficult utilization
[0004] In the production process of organic silicon, a certain amount of organic silicon waste will be produced. Due to the complex composition and easy hydrolysis, the cost of extracting useful components from waste liquid by direct and simple distillation is relatively high.
Some researchers use simple hydrolysis treatment, but a large amount of HCl will be produced during the hydrolysis process, and the hydrolysis conditions are difficult to control
The solid matter produced by hydrolysis has not been fully utilized, so the treatment and recycling of organic silicon waste has always been an urgent issue for the organic silicon industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1: Pretreat the slurry residue:

[0025] Simple sedimentation separation is used to extract the upper layer of high boiling point chlorosilane; or use reduced pressure distillation, 150 °C, the high boiling point chlorosilane is distilled out under reduced pressure; the residue black slag, hydrolyzed treatment, can enter the crushing process.

[0026] The high boiling content of the black slag obtained by the sedimentation separation is controlled at 10%, while the black slag obtained by reduced pressure distillation, the high boiling content is controlled at 5%.

[0027] Step 2: Crush the pretreated black slag.

[0028] Among the widely available mechanical crushing methods, ball milling is the highest priority choice for hydrolyzed slurry slag crushing. In the ball milling process, a certain amount of water is added to the black slag, and the water added is 50% of the dry weight of the black slag. After ball grinding, the mixed crushing slurry slag is obtained. The s...

Embodiment 2

[0037] Step 1: Pretreat the slurry residue:

[0038] Simple sedimentation separation is used to extract the upper high boiling point chlorosilane; or use reduced pressure distillation, at 160 °C, the high boiling point chlorosilane is distilled out under reduced pressure; the residue black slag, hydrolyzed treatment, can enter the crushing process.

[0039] The high boiling content of the black slag obtained by the sedimentation separation is controlled at 20%, while the black residue obtained by reduced pressure distillation, the high boiling content is controlled at 6%.

[0040] Step 2: Crush the pretreated black slag.

[0041] Among the widely available mechanical crushing methods, ball milling is the highest priority choice for hydrolyzed slurry slag crushing. In the ball milling process, a certain amount of water is added to the black slag, and the water is added to 100% of the dry weight of the black slag. After ball grinding, the mixed crushing slurry slag is obtained. The ...

Embodiment 3

[0050] Step 1: Pretreat the slurry residue:

[0051] Simple sedimentation separation is used to extract the upper high boiling point chlorosilane; or use reduced pressure distillation, at 160 °C, the high boiling point chlorosilane is distilled out under reduced pressure; the residue black slag, hydrolyzed treatment, can enter the crushing process.

[0052] The high boiling content of the black slag obtained by the sedimentation separation is controlled at 20%, while the black slag obtained by reduced pressure distillation, the high boiling content is controlled at 6.5%.

[0053] Step 2: Crush the pretreated black slag.

[0054] Among the widely available mechanical crushing methods, ball milling is the highest priority choice for hydrolyzed slurry slag crushing. In the ball milling process, a certain amount of water is added to the black slag, and the water is added to 150% of the dry weight of the black slag. After ball grinding, the mixed crushing slurry slag is obtained. The s...

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Abstract

The invention relates to a green comprehensive recycling method of organic silicon pulp residues. At present, a direct method is the only industrial production method for methyl chlorosilane monomers, and about 2-5% of waste residue slurry is produced as a byproduct in the production process. The harmless treatment of the waste residue slurry is carried out through a series of comprehensive separation and treatment methods. On the basis of a hydrolysis method, efficient pretreatment methods such as sedimentation, reduced pressure distillation, ball milling and pulping are combined, then a series of regeneration comprehensive utilization treatments such as hydrogen extraction, filtration, slag washing and copper extraction are carried out, and efficient harmless treatment of the organic silicon waste slag is achieved. After the residues treated by the method are washed and neutralized by calcium oxide, the residual quantity is only about 10% of the weight of the slurry residues, chlorine radicals and heavy metal residues are avoided, the carbon content is 30-50%, and the residues can be used for building and thermal power fuel and can be reused. Meanwhile, recovery products, namely water glass and copper sulfate, are obtained through comprehensive treatment, raw material waste and waste treatment pressure are reduced, and the method has remarkable environment-friendly significance and economic significance.

Description

Technical field [0001] The present invention relates to the field of silicone waste residue treatment technology, specifically to a green comprehensive recycling method of silicone slurry residue. Background [0002] Silicone materials are a new type of material that cannot be replaced by modern high-tech industries, and more than 90% of the products are derived from methylchlorosilane monomers. At present, the direct method is the only industrial production method of methylchlorosilane monomer, and its production process is a by-product of about 2%-5% of the waste slurry. [0003] In recent years, the production capacity of silicone has been expanding, and the waste slag slurry has seriously restricted the healthy development of the industry, and its resource treatment is imminent. Methyl chlorosilane monomer is formed by the catalytic reaction of silicon powder and chloromethane in the fluidized bed, and the reaction mixture is removed by the cyclone separator to remove most of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B3/02C01B33/021C01G3/10B09B3/45B09B3/40B09B3/70B09B3/35B09B5/00B09B3/00
CPCC01B3/02C01B33/021C01G3/10B09B3/00B09B5/00Y02P10/20
Inventor 张庆华佟哲名李伏琦詹晓力吴旭日
Owner ZHEJIANG UNIV
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