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Continuous Preparation Process of Methyl Silicone Resin

A technology of methyl silicone resin and preparation process, applied in the field of continuous preparation technology of methyl silicone resin, can solve the problems of low production efficiency, poor mass transfer and heat transfer effect, large production energy consumption and the like

Active Publication Date: 2018-06-29
TANGSHAN SANYOU SILICON IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high viscosity of the material and the poor mass and heat transfer effect, the average reaction time of the polycondensation process is 4 to 10 hours. If the polycondensation reaction time is too long, the production efficiency is low and the production energy consumption is large. It is meaningful to develop a reaction device that is more suitable for the polycondensation process. major

Method used

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  • Continuous Preparation Process of Methyl Silicone Resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A continuous preparation process of methyl silicone resin, carried out as follows:

[0034] Feed according to the following raw material ratio:

[0035] Methyltrichlorosilane: 100kg / h; Dimethyldichlorosilane: 22 kg / h; Xylene: 260kg / h.

[0036] Washing dilute acid water: 400 kg / h; ethanol: 20kg / h.

[0037] a. Hydrolysis

[0038] Methyltrichlorosilane, dimethyldichlorosilane, and xylene are mixed at a ratio of 5:1:13, and after being initially mixed in a static mixer 11, they enter the tubular hydrolysis reactor 12, where they are washed with dilute acid water and ethanol at a ratio of 20: The ratio of 1 enters the tubular hydrolysis reactor 12, and the washing dilute acid water is dilute hydrochloric acid with a mass concentration of 0.8% (the washing water after the first-level washing in the washing process of the previous kettle material can also be used). The hydrolysis temperature of the material is controlled at 15°C in the hydrolysis system. After the feeding i...

Embodiment 2

[0052] A continuous preparation process of methyl silicone resin, carried out as follows:

[0053] Feed according to the following raw material ratio:

[0054] Methyltrichlorosilane: 90kg / h; Dimethyldichlorosilane: 32 kg / h; Xylene: 250kg / h.

[0055] Washing dilute acid water: 400 kg / h; ethanol: 10kg / h.

[0056] a. Hydrolysis

[0057] Methyltrichlorosilane, dimethyldichlorosilane, and xylene are mixed at a ratio of 3:1:8, initially mixed in a static mixer 11, and then entered into a tubular hydrolysis reactor 12, and washed with dilute acid water and ethanol at a ratio of 40: The ratio of 1 enters the tubular hydrolysis reactor 12, and the dilute acid water for washing is dilute hydrochloric acid with a mass concentration of 0.9% (the washing water after the first-level washing in the washing process of the material in the previous kettle can also be used). The hydrolysis temperature of the material is controlled at 20°C in the hydrolysis system. After the feeding is complet...

Embodiment 3

[0071] A continuous preparation process of methyl silicone resin, carried out as follows:

[0072] Feed according to the following raw material ratio:

[0073] Methyltrichlorosilane: 85kg / h; Dimethyldichlorosilane: 35 kg / h; Xylene: 240kg / h.

[0074] Washing dilute acid water: 400 kg / h; ethanol: 8kg / h.

[0075] a. Hydrolysis

[0076] Methyltrichlorosilane, dimethyldichlorosilane, and xylene are mixed in a ratio of 2.5:1:7, and then enter the tubular hydrolysis reactor 12 after being initially mixed in a static mixer 11, and washed with dilute acid water and ethanol at a ratio of 50: The ratio of 1 enters the tubular hydrolysis reactor 12, and the dilute acid water for washing is dilute hydrochloric acid with a mass concentration of 0.9% (the washing water after the first-level washing in the washing process of the material in the previous kettle can also be used). The hydrolysis temperature of the material is controlled at 25°C in the hydrolysis system. After the feeding is ...

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Abstract

The invention relates to a production process of silicone resin, in particular to a continuous preparation process of methyl silicone resin. The process of the present invention is carried out according to the following steps: hydrolysis: methyltrichlorosilane, dimethyldichlorosilane, and benzene-based solvents are mixed according to the mass ratio and then enter the tubular hydrolysis reactor, and the dilute acid water and alkyl alcohol are washed according to the mass ratio Enter the reactor to react together; washing: the hydrolyzate is washed to neutral after three or more stages; concentration: continuous concentration under vacuum; polycondensation: when the effective content of siloxane reaches 50% to 60% of the volume of the kettle , add catalyst, blow inert gas for polycondensation reaction. Beneficial effects of the present invention: the present invention has no waste water discharge, solves the problems of large amount of washing acid water discharge, contains a lot of organic matter, and difficult to handle waste water, improves the product yield, injects inert gas into the polycondensation process, and shortens the de-lowering time , while avoiding product yellowing. The reaction conditions of the system are stable, and the product performance is more excellent.

Description

technical field [0001] The invention relates to a production process of silicone resin, in particular to a continuous preparation process of methyl silicone resin. Background technique [0002] According to different raw materials, the preparation of silicone resin is mainly divided into two routes: alkoxysilane as raw material and chlorosilane as raw material. Due to the low cost of using chlorosilane monomers to produce silicone resins, mainstream products at home and abroad are still produced using chlorosilanes as raw materials. Mixed chlorosilane monomers are hydrolyzed under the protection of benzene-based solvents to prepare methyl silicone resin. In the traditional intermittent hydrolysis process, a large amount of water is required to be washed many times to make the hydrolyzate neutral. The production of 1 ton of silicone resin produces about 10-15 tons of washing wastewater, which not only pollutes the environment, but also reduces the product yield. Benzene-bas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06C08G77/04
Inventor 孙长江任海涛刘秋艳王春英李献起
Owner TANGSHAN SANYOU SILICON IND
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