Preparation method for phenyl hydrogen-containing silicone oil

A technology of phenyl hydrogen-containing silicone oil and phenyl alkoxysilane, applied in chemical instruments and methods, adhesive additives, polymer adhesive additives, etc. Poor controllability, poor product stability and other problems, to achieve the effect of easy control, simple operation and wide application

Active Publication Date: 2013-04-24
NICHE TECH KAISER SHANTOU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Existing phenyl hydrogen-containing silicone oils are all produced by hydrolysis and polycondensation of hydrochlorosilanes and non-hydrogen-containing chlorosilanes, and the reaction controllability is poor
The composition of the product obtained under different raw material ratios and hydrolysis conditions (i.e. phenyl hydrogen-containing silicone oil) is very different, resulting in poor stability of the product; moreover, the reaction repeatability is poor, even under the same raw material ratio and the same reaction conditions, The resulting product may still vary

Method used

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  • Preparation method for phenyl hydrogen-containing silicone oil
  • Preparation method for phenyl hydrogen-containing silicone oil

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Embodiment 1

[0025] The preparation method of the present embodiment phenyl hydrogen-containing silicone oil comprises the following steps successively:

[0026] (1) Use phenylalkoxysilane and cyclosiloxane as basic reaction monomers, add organic solvent, water and end-capping agent, and carry out hydrolysis polycondensation reaction under the action of acidic catalyst;

[0027] The above-mentioned phenylalkoxysilane is phenyltrimethoxysilane, and its amount is 14.50 g (0.0731 mol). The above-mentioned cyclosiloxane is tetramethyltetrahydrocyclotetrasiloxane, and its usage amount is 10.67 g (0.0443 mol). In phenylalkoxysilane and cyclosiloxane, the ratio of the total moles of phenyl groups to the total moles of Si—H groups is about 0.413:1.

[0028] Above-mentioned organic solvent is toluene, and its consumption is 40.00g. The consumption of organic solvent is about 1.59 times of the total mass of basic reaction monomers.

[0029] The above-mentioned water is deionized water, and its co...

Embodiment 2

[0039] The preparation method of the present embodiment phenyl hydrogen-containing silicone oil comprises the following steps successively:

[0040] (1) Use phenylalkoxysilane and cyclosiloxane as basic reaction monomers, add organic solvent, water and end-capping agent, and carry out hydrolysis polycondensation reaction under the action of acidic catalyst;

[0041] In this step (1), the hydrolysis polycondensation reaction is carried out under stirring, the reaction time of the hydrolysis polycondensation reaction is 10 hours, and the reaction temperature is 100°C.

[0042] The above-mentioned phenylalkoxysilane is phenyltrimethoxysilane, and its amount is 19.80 g (0.0999 mol). The above-mentioned cyclosiloxane is tetramethyltetrahydrocyclotetrasiloxane, and its dosage is 2.60 g (0.0108 mol). In phenylalkoxysilane and cyclosiloxane, the ratio of the total moles of phenyl groups to the total moles of Si—H groups is 2.3125:1.

[0043] Above-mentioned organic solvent is toluene,...

Embodiment 3

[0052] The preparation method of the present embodiment phenyl hydrogen-containing silicone oil comprises the following steps successively:

[0053] (1) Use phenylalkoxysilane and cyclosiloxane as basic reaction monomers, add organic solvent, water and end-capping agent, and carry out hydrolysis polycondensation reaction under the action of acidic catalyst;

[0054] In this step (1), the hydrolysis polycondensation reaction is carried out under stirring, the reaction time of the hydrolysis polycondensation reaction is 14 hours, and the reaction temperature is 20°C.

[0055] The above-mentioned phenylalkoxysilane is phenyltrimethoxysilane, and its amount is 19.80 g (0.0999 mol). The above-mentioned cyclosiloxane is tetramethyltetrahydrocyclotetrasiloxane, and its usage amount is 4.16 g (0.0173 mol). In phenylalkoxysilane and cyclosiloxane, the ratio of the total moles of phenyl groups to the total moles of Si—H groups is about 1.44:1.

[0056] Above-mentioned organic solvent ...

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Abstract

The invention discloses a preparation method for phenyl hydrogen-containing silicone oil, which comprises the steps as follows: firstly, phenyl alkoxyl silane and cyclosiloxane are used as basic reaction monomers; moreover, organic solvent, water and blocking agent are added to implement hydrolysis condensation reaction under the effect of acidic catalyst; secondarily, after the hydrolysis condensation reaction is completed, the reaction liquid obtained is washed to neutral and then low-boiling substances in the reaction liquid are removed, thus obtaining the phenyl hydrogen-containing silicone oil. The preparation method for phenyl hydrogen-containing silicone oil has the advantages of easily obtained material, simple operation, easy control, no pollution, gentle condition and convenientindustrialization. The number-average molar mass of the phenyl hydrogen-containing silicone oil prepared is between 0.5*103 and 5.0*103, the refractive index is adjustable between 1.41 and 1.60 and the hydrogen content is adjustable between 0.2 and 1.2wt percent. The phenyl hydrogen-containing silicone oil has excellent performances of high refractive index, high light transmittance, radiation resistance, high and low temperature resistance, weather resistance, etc. The phenyl hydrogen-containing silicone oil is suitable to be used as cosmetic additives, lubricant additives, cross-linking agent of electronic pouring sealant and cross-linking agent used for seal rings.

Description

technical field [0001] The invention relates to a method for preparing hydrogen-containing silicone oil, in particular to a method for preparing phenyl hydrogen-containing silicone oil. Background technique [0002] Phenyl silicone oil is one of the main varieties of silicone oil. It has excellent electrical insulation properties, excellent anti-ozone, corona resistance, hydrophobic and moisture-proof properties, and good chemical stability. Due to the introduction of phenyl groups into the molecular chain of phenyl silicone oil, it has better high temperature resistance, radiation resistance, lubricity and compatibility. In addition, phenyl silicone oil shows certain absorption to ultraviolet light, and the working temperature is -50℃~250℃. Therefore, phenyl silicone oil is widely used in daily chemical products, electronics, machinery and other fields. [0003] Among phenyl silicone oils, phenyl hydrogen-containing silicone oil is a linear polysiloxane in which some meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/12C08G77/32C08G77/06A61K8/891C10M155/02C09J11/08C09K3/10
Inventor 周振基周博轩
Owner NICHE TECH KAISER SHANTOU
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