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Method for splitting dimethyl dichlorosilane hydrolysate

A technology of dimethyldichlorosilane and hydrolyzate, applied in the directions of organic silicon compounds, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of inability to separate products, increase the difficulty of refining, increase production costs, etc. Comprehensive alkalinity enhancement, strong catalytic activity, and the effect of reducing pollution

Active Publication Date: 2014-09-24
九江星成高分子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Most of the catalysts used in existing patents and literature technologies are soluble catalysts, which cannot be separated from the product and generate solid waste such as cracking residue, which increases the difficulty of refining and increases the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 100Kg of strongly basic macroporous anion exchange resin, 40Kg of potassium hydroxide, 2Kg of potassium trimethylsiliconate, [bmim]BF to the 1000L reactor 4 0.3Kg of ionic liquid and 300Kg of ethanol were reacted at 40°C for 10h, filtered and dried to obtain a composite catalyst, which was used for later use.

[0022] (2) Add 100Kg of hydrolyzate, 15Kg of solvent oil, and 4Kg of composite catalyst into the 1000-degree pyrolysis kettle. At a temperature of 120°C, the cracking reaction pressure is 0.07Mpa, the residence time of the hydrolyzate is 1h, and the hydrolyzate is cracked and rearranged to obtain a ring mixture, After washing with water, high boilers and low boilers are removed to obtain pure octamethylcyclotetrasiloxane D4 and mixed cyclosiloxane DMC and other products. The reaction yield and the content of pure octamethylcyclotetrasiloxane D4 in the product are shown in Table 1.

Embodiment 2

[0024] (1) Add 100Kg of strong basic macroporous anion exchange resin, 20Kg of potassium hydroxide, 1Kg of potassium trimethylsiliconate, [bmim]BF to the 1000L reactor 4 0.1Kg of ionic liquid and 200Kg of ethanol were reacted at 30°C for 20h, filtered and dried to obtain a composite catalyst, which was used for later use.

[0025] (2) Add 100Kg of hydrolyzate, 3Kg of solvent oil, and 4Kg of composite catalyst into the 1000-degree pyrolysis kettle, at a temperature of 100°C, the cracking reaction pressure is 0.04Mpa, the residence time of the hydrolyzate is 2h, and the hydrolyzate is cracked and rearranged to obtain a ring mixture, After washing with water, high boilers and low boilers are removed to obtain pure octamethylcyclotetrasiloxane D4 and mixed cyclosiloxane DMC and other products. The reaction yield and the content of pure octamethylcyclotetrasiloxane D4 in the product are shown in Table 1.

Embodiment 3

[0027] (1) Add 100Kg of strong basic macroporous anion exchange resin, 50Kg of potassium hydroxide, 5Kg of potassium trimethylsiliconate, [bmim]BF to the 1000L reactor 4 0.5Kg of ionic liquid and 500Kg of ethanol were reacted at 60°C for 5h, filtered and dried to obtain a composite catalyst, which was used for later use.

[0028] (2) Add 100Kg of hydrolyzate, 30Kg of solvent oil, and 4Kg of composite catalyst into the 1000-degree pyrolysis kettle. At a temperature of 150°C, the cracking reaction pressure is 0.09Mpa, the residence time of the hydrolyzate is 0.5h, and the hydrolyzate is cracked and rearranged to obtain a ring mixture After washing with water, high boilers and low boilers are removed to obtain pure octamethylcyclotetrasiloxane D4 and mixed cyclosiloxane DMC and other products. The reaction yield and the content of pure octamethylcyclotetrasiloxane D4 in the product are shown in Table 1.

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PUM

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Abstract

The invention discloses a method for splitting dimethyl dichlorosilane hydrolysate. The method comprises the following steps: carrying out load reaction onto strong-basicity macroporous anion exchange resin, potassium hydroxide, potassium trimethylsilanolate and [bmim]BF4 ionic liquid to obtain a composite catalyst after the reaction is ended; adding dimethyl dichlorosilane hydrolysate into a splitting kettle to obtain a ring-body mixture by splitting and re-arranging solvent oil, the composite catalyst and the hydrolysate; and washing with water to remove high-boiling point residues and low-boiling point residues to obtain products such as octamethylcyclotetrasiloxane D4, hexamethylcyclotrisiloxane and decamethylcyclopentasiloxane.

Description

technical field [0001] The invention relates to a preparation method of an organosilicon product, in particular to a method for cracking dimethyldichlorosilane hydrolyzate. Background technique [0002] The solvent-based cracking process adds solvent oil as a heat carrier into the cracking reaction kettle, so that the heat transfer of the cracking reaction is uniform, the local overheating phenomenon is eliminated, and the disproportionation reaction is controlled, thereby reducing the residue, reducing the consumption of alkali, improving the yield of the ring body and prolonging the production. cycle. The research on domestic solvent-based pyrolysis of dimethyl hydrolysate began in the 1990s. The Research Institute of PetroChina Jilin Petrochemical Company started the solvent-based cracking process and the ring separation experiment in 1993. The cracking process is to carry out the cracking and rearrangement reaction of dimethyl hydrolyzate under the condition of basic ca...

Claims

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Application Information

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IPC IPC(8): C07F7/21B01J31/26
Inventor 王琪宇董建国
Owner 九江星成高分子材料有限公司
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