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Solvent-free hydrogen-containing silicone oil and preparation method thereof

A hydrogen-containing silicon and solvent-free technology, applied in the chemical industry, can solve the problems of inconvenient control, difficult handling, high hydrogen content in hydrogen-containing silicone oil, etc., and achieve the effects of easy reaction control, stable product quality, and simple process

Active Publication Date: 2014-02-05
LUZHOU NORTH CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional production method of hydrogen-containing silicone oil is to add methyl dichlorosilane dropwise in water, hydrolyze and deacidify to obtain hydrogen-containing silicone oil. This method is a common method in silicone enterprises, but this method will bring a lot of The oil-containing hydrolysis acid has an acid value of about 20%, which is difficult to handle; and in the hydrolysis process, hydrogen chloride dissolves in water to generate a large amount of heat, which is not only inconvenient to control the reaction but also brings safety hazards, so the traditional production The process brings unstable factors to normal production and safety and environmental protection
[0004] Use the method of back-dropping to produce hydrogen-containing silicone oil, that is, the method of adding water to the monomer dropwise. This method can ensure that hydrogen chloride leaves the system in the form of gas to the greatest extent. Under the condition of anhydrous, the hydrogen content of the obtained hydrogen-containing silicone oil will be higher than that prepared by the traditional method, but this method will bring the problem of inconvenient control, because when the water is added dropwise to the monomer When the monomer is not touched, the temperature will rise sharply due to the incorporation of a large amount of hydrogen chloride, so the hydrolysis of the monomer is likely to be a reaction under an uncontrollable temperature condition

Method used

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  • Solvent-free hydrogen-containing silicone oil and preparation method thereof
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preparation example Construction

[0019] The invention relates to a solvent-free hydrogen-containing silicone oil and a preparation method thereof. The hydrogen-containing silicone oil is added dropwise into methyldichlorosilane with hydrochloric acid, telomerized with an acidic catalyst, capped with a capping agent, and alkaline substance The product obtained after neutralization has good storability, and at the same time, the method of the invention has good controllability and environmental protection.

[0020] A solvent-free hydrogen-containing silicone oil, the raw material of which is composed of the following components by weight: 100 parts of methyldichlorosilane, 1-10 parts of capping agent, 10-70 parts of hydrochloric acid, 1-10 parts of Acidic catalyst, alkaline neutralization; wherein, the capping agent is hexamethyldisiloxane or octamethyltrisiloxane; the mass fraction of hydrochloric acid is 5-36%; the acidic The catalyst is one of concentrated sulfuric acid, concentrated hydrochloric acid, acid ...

Embodiment 1

[0038] Add 10 parts by weight of dilute hydrochloric acid (5wt%) dropwise to 100 parts by weight of methyldichlorosilane at a constant speed, control the temperature at 10°C, and stir vigorously. The hydrogen chloride gas generated enters the absorption device. After the reaction is completed, separate the oil phase. The acidic silicone oil is obtained, and the aqueous hydrochloric acid is recovered and stored for future use. Add 2 parts by weight of hexamethyldisiloxane and 1 part by weight of concentrated sulfuric acid to the acidic silicone oil, raise the temperature and control the temperature at 50±2°C, and react for 2 hours. After completion, add solid sodium carbonate to neutralize to neutrality, filter, and The filtrate was removed for 3 hours at 130±2°C and a vacuum of -0.08MPa to obtain the product. The physical and chemical indicators of the obtained hydrogen-containing silicone oil were hydrogen content of 1.58%, refractive index of 1.3987, and viscosity of 24mm 2 ...

Embodiment 2

[0040] Add 10 parts by weight of dilute hydrochloric acid (20wt%) to 100 parts by weight of methyldichlorosilane dropwise at a constant speed, control the temperature at 10°C, and stir vigorously. The hydrogen chloride gas generated enters the absorption device. After the reaction is completed, the oil phase is separated. The acidic silicone oil is obtained, and the aqueous hydrochloric acid is recovered and stored for future use. Add 2 parts by weight of hexamethyldisiloxane and 1 part by weight of concentrated sulfuric acid to the acidic silicone oil, raise the temperature and control the temperature at 70±2°C, and react for 2 hours. After completion, add solid sodium carbonate to neutralize to neutrality, filter, and The filtrate was removed for 3 hours at 130±2°C and a vacuum of -0.08MPa to obtain the product. The physical and chemical indicators of the obtained hydrogen-containing silicone oil were hydrogen content of 1.61%, refractive index of 1.3962, and viscosity of 27m...

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Abstract

The invention belongs to the field of chemical engineering, and in particular relates to solvent-free hydrogen-containing silicone oil and a preparation method thereof. The solvent-free hydrogen-containing silicone oil disclosed by the invention is composed of the following components in weight ratio: 100 parts of methyldichlorosilane, 1-10 parts of blocking agent, 10-70 parts of hydrochloric acid, 1-10 parts of acid catalyst, and alkaline neutral substance. The hydrogen-containing silicone oil disclosed by the invention is prepared by comprising the following steps of: reacting by dropping hydrochloric acid into methyldichlorosilane, separating, reacting again by adding the blocking agent and the acid catalyst into oil phase, adding the alkaline neutral substance, filtering, removing boiling substances from filtrate, etc. The hydrogen-containing silicone oil prepared by the invention is better in waterproof effect and can be used for waterproof treatment.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a solvent-free hydrogen-containing silicone oil and a preparation method thereof. technical background [0002] Hydrogen-containing silicone oil is one of the most important products in silicone products. Its siloxane main chain contains active hydrogen, which has high activity and can react with many active groups. Its notable feature is good waterproof effect and low-temperature cross-linking Film forming, forming a waterproof layer on the surface of the material, can be used for waterproofing of fabrics, glass, ceramics, paper, leather, metal, and building materials industries, with excellent results. [0003] Hydrogen-containing silicone oil is a product obtained by hydrolysis and neutralization of methyldichlorosilane. The traditional production method of hydrogen-containing silicone oil is to add methyl dichlorosilane dropwise in water, hydrolyze and deacidify ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/12C08G77/06
Inventor 张文博李争鸣唐纹涛唐荣娟张莹徐志远杨文俊
Owner LUZHOU NORTH CHEM IND
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