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Hydrogen-containing silicone oil and preparation method thereof

A technology containing hydrogen-containing silicon and potassium hydroxide, applied in the field of hydrogen-containing silicone oil and its preparation, can solve the problems of high price and sharp increase in raw material cost, and achieve the effect of low price and good cost advantage

Inactive Publication Date: 2016-01-20
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Its main preparation method is to use tetramethyldisiloxane as the head-sealing agent, use acidic substances such as sulfuric acid and acid resin as the catalyst, and react with dimethylcyclosiloxane. The method is simple, but tetramethyldisiloxane Siloxane is expensive, accounting for more than 15% of the cost of raw materials. When preparing low-viscosity hydrogen silicone oil, the cost of raw materials can even reach more than 40%. Tetramethyldisiloxane makes the cost of raw materials increase sharply

Method used

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  • Hydrogen-containing silicone oil and preparation method thereof
  • Hydrogen-containing silicone oil and preparation method thereof
  • Hydrogen-containing silicone oil and preparation method thereof

Examples

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Effect test

Embodiment 1

[0031] Add 1000g of linear body into the reaction kettle, stir, heat up to 130°C, add 0.025g of potassium hydroxide, keep the temperature at 130°C, vacuumize, check the viscosity online, when the viscosity reaches 10000mPa·s, return to normal pressure, add phosphoric acid 0.03 g, neutralize for 1 hour, then lower the temperature to 80°C, add 30g of methyldiethoxysilane and 10g of triethylamine, stir the reaction for 1 hour, raise the temperature to 140°C, remove the low molecular weight by vacuuming for 2 hours, and obtain the hydrogen-containing Silicone oil, viscosity 984mPa·s, hydrogen content (mass content) 0.0054%.

Embodiment 2

[0033] Add 1000g of linear body into the reaction kettle, stir, raise the temperature to 135°C, add 0.015g of potassium hydroxide, keep the temperature at 135°C, vacuumize, check the viscosity online, when the viscosity reaches 5000mPa·s, return to normal pressure, add silicon base Phosphate (calculated as phosphoric acid) 0.023g was neutralized for 0.8h, then cooled to 70°C, added 35g of methyldiethoxysilane and 20g of dipropylamine, stirred for 3h, heated to 120°C, vacuumed to remove low molecular weight for 4h , to obtain the hydrogen-containing silicone oil with a viscosity of 4930mPa·s and a hydrogen content (mass content) of 0.0066%.

Embodiment 3

[0035] Add 1000g of linear body into the reaction kettle, stir, raise the temperature to 140°C, add 0.008g of potassium hydroxide, keep the temperature at 140°C, vacuumize, check the viscosity online, when the viscosity reaches 650mPa·s, return to normal pressure, add silicon base Phosphate ester (calculated as phosphoric acid) 0.014g was neutralized for 0.5h, then the temperature was lowered to 60°C, 50g of methyldiethoxysilane and 30g of cyclohexanone oxime were added, stirred for 2h, the temperature was raised to 130°C, vacuum removed Molecule 3h, the hydrogen-containing silicone oil is obtained, the viscosity is 4930mPa·s, and the hydrogen content (mass content) is 0.0135%.

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Abstract

The invention belongs to the technical field of polysiloxane synthesis, and particularly relates to hydrogen-containing silicone oil and a preparation method thereof. A molecular formula of the hydrogen-containing silicone oil is as shown in the specification, wherein n is 200-500; and R is CH3 or CH2CH3. The preparation method comprises the following steps: (1) adding a linear body to a reaction kettle, stirring, warming to 130-140 DEG C, and adding potassium hydroxide; (2) carrying out vacuum supply, and detecting the viscosity online, when the appointed viscosity is achieved, restoring into atmospheric pressure and adding phosphoric acid or silicon-based phosphate for neutralization; (3) cooling, adding methyldialkoxysilane and a catalyst, and carrying out stirred reaction; and (4) warming, carrying out vacuum supply and removing low molecules to obtain the hydrogen-containing silicone oil. The hydrogen-containing silicone oil provided by the invention can be used as an addition-type silicone rubber chain extender or is applied to the aspects of synthetic fabric finishing agents and the like; the linear body and the methyldialkoxysilane which is low in cost and easy to prepare are adopted as raw materials, so that the raw material cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of polysiloxane synthesis, and in particular relates to a hydrogen-containing silicone oil and a preparation method thereof. Background technique [0002] Hydrogen-terminated silicone oil is a polysiloxane terminated with silicon hydrogen, which contains highly active silicon-hydrogen bonds and has a wide range of uses. It is the basic raw material for the synthesis of SRS modified silicone oil and can be used as a chain extender for addition-type silicone rubber. , It can also be used for plastic resin modification reactions, etc. [0003] Its main preparation method is to use tetramethyldisiloxane as a head-sealing agent, use acidic substances such as sulfuric acid and acid resin as a catalyst, and react with dimethylcyclosiloxane. The method is simple, but tetramethyldisiloxane Siloxane is expensive, accounting for more than 15% of the cost of raw materials. When preparing low-viscosity hydrogen silicone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/12
Inventor 刘海龙张海磊伊港周续中许栋
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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