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Method for cracking treatment of organic silicon waste residue slurry

A pyrolysis treatment and organosilicon technology, applied in the fields of organic chemistry, chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, etc., can solve the problems of easy spontaneous combustion, increased waste disposal costs, slow hydrolysis, etc.

Active Publication Date: 2012-03-07
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the disadvantages of this method are: the contact between the slurry and the hydrolysis medium is not sufficient, the hydrolysis rate is relatively slow, and the obtained hydrolyzate is in a viscous state, which is difficult to separate from the system; in addition, this method requires the organosilicon monomer in the slurry In the molecule, there are no less than 3 chlorine groups connected to each silicon atom, but most of the monomers in the slurry do not meet its requirements, so this method cannot be used to treat most of the slurry; and in the hydrolysis process Adding mineral oil will increase the cost of waste disposal and increase new sources of pollution, which does not meet environmental protection requirements
The disadvantage is that hydrogen chloride, one of the reaction products, is neutralized by the alkali in the hydrolysis medium to become a salt, which wastes a part of resources; in addition, the reduced copper contained in the solid hydrolyzate is heated, exposed to sunlight for a long time or piled up. Prone to spontaneous combustion, an important safety hazard
The main disadvantage of this process is that the liquid phase of the slurry is completely hydrolyzed, resulting in waste

Method used

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  • Method for cracking treatment of organic silicon waste residue slurry
  • Method for cracking treatment of organic silicon waste residue slurry
  • Method for cracking treatment of organic silicon waste residue slurry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The raw material slurry is a liquid-solid mixture with a solid content of 20%, and the same quality of high boilers (high boiling point residues in organosilicon monomers with a minimum boiling point of 70° C.) is added to form a cracking raw material liquid. Take 500 grams of raw material liquid and add it to a 1L reaction kettle, and add 15 grams of tributylamine at the same time. The temperature was raised to 80° C., and the raw material liquid was added dropwise, and HCl gas was introduced. The product is condensed and collected by the overhead condenser. The reaction was carried out for 28 hours, and the temperature of the reactor finally rose to 147°C. The conversion rate was 70.04%. The gas chromatography analysis results of the products are shown in Table 1. (the product contains some boiling point less than MeHSiCl 2 components, the content is about 1.0%)

[0016] Table 1 Product Gas Chromatography Analysis

[0017]

Embodiment 2

[0019] The raw material slag is a liquid-solid mixture with a solid content of 20%, and twice the mass fraction of high boilers is added to form a cracking raw material liquid. Take 500 grams of raw material liquid and add it to a 1L reaction kettle, and add 15 grams of tributylamine at the same time. The temperature was raised to 80° C., and the raw material liquid was added dropwise, and HCl gas was introduced. The product is condensed and collected by the overhead condenser. The reaction was carried out for 42 hours, and the temperature of the reactor finally rose to 156°C. The conversion rate was 74.18%. The product gas chromatography analysis results are shown in Table 2. (the product contains some boiling point less than MeHSiCl 2 components, the content is about 1.0%)

[0020] Table 2 Product Gas Chromatography Analysis

[0021]

Embodiment 3

[0023] The raw material slurry is a liquid-solid mixture with a solid content of 20%, and 50% by mass of high boilers are added to form a cracking raw material liquid. Take 500 grams of raw material liquid and add it to a 1L reaction kettle, and add 15 grams of tributylamine at the same time. The temperature was raised to 80° C., and the raw material liquid was added dropwise, and HCl gas was introduced. The product is condensed and collected by the overhead condenser. The reaction was carried out for 17 hours, and the temperature of the reactor finally rose to 146°C. The conversion rate was 67.08%. The product gas chromatography analysis results are shown in Table 3. (the product contains some boiling point less than MeHSiCl 2 components, the content is about 1.0%)

[0024] Table 3 Product Gas Chromatography Analysis

[0025]

[0026] The hydrolysis recovery method of the unlysed matter is not described in detail.

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Abstract

The invention relates to method for the cracking treatment of waste residues slurry produced in a synthesis process of an organic silicone monomer. The comehtod comprises: adding a high-boiling material of the same mass into a organic silicon waste residue slurry liquid and solid mixture containing 20 percent of solid to prepare a cracking feed solution, wherein a catalyst is tri-n-butylamine andthe cracking reaction temperature is 80 to 160 DEG C; and introducing HCl gas, wherein the ratio of the feed speeds of the hydrogen chloride and the raw material mixed liquid is 1:1.05-1:1.12. The method has the advantages that: the residue slurry containing 20 percent of solid is used in combination with the high-boiling material, so a monosilane product can be separated directly in a cracking process; the conversion rate is over 70 percent; the selectivity of dimethyldichlorosilane is over 35 percent; the selectivity of methylsilane is over 40 percent; and the slurry residue obtained after cracking having certain liquidity and can be further treated.

Description

technical field [0001] The invention relates to a method for cracking and treating waste residue slurry formed during the synthesis of organic silicon monomers. Background technique [0002] The waste slurry generated during the synthesis of organosilicon monomer accounts for about 3% of the monomer output. The device with an annual output of 50,000 tons will produce 1,500 tons of waste slurry, resulting in a large amount of chlorine loss. The liquid composition of organic silicon waste slurry has a boiling point greater than 75°C (mainly disilane, disiloxane, silylane, etc.), and there are suspended silicon powder, copper, tin and other metals, which are easy to burn and form when exposed to air. Acid mist. If the stacking method is used for processing, the pollution will be serious and there will be potential safety hazards. However, there is still a blank in domestic waste slurry treatment technology. At present, only the backlog is blocked or the copper is simply reco...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 叶青王皖林赵岩涛崔华张姝
Owner PETROCHINA CO LTD
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