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Vinyl silicone oil and synthetic method thereof

A technology of vinyl silicone oil and synthesis method, applied in the field of silicone oil and its synthesis, can solve the problems of high cost, low product yield and the like, and achieve the effects of low cost, high product yield and high reactivity

Active Publication Date: 2013-10-02
JIANGSU TIANCHEN NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, synthetic vinyl silicone oil is generally made of methyl cyclosiloxane and methyl vinyl cyclosiloxane as raw materials, and vinyl siloxane is used as an end-capping agent. into, the product yield is low, and the cost is high

Method used

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  • Vinyl silicone oil and synthetic method thereof
  • Vinyl silicone oil and synthetic method thereof
  • Vinyl silicone oil and synthetic method thereof

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preparation example Construction

[0026] The synthetic method of above-mentioned vinyl silicone oil comprises the following steps:

[0027] a, the synthesis of basic catalyst

[0028] Mix octamethylcyclotetrasiloxane and alkali metal hydroxide in a mass ratio of 1-10:1, polymerize at 40-80°C for 2-8 hours, then raise the temperature to 150-180°C, in N 2 Remove oligomers under protection for 3-6 hours to obtain the basic catalyst, preferably polymerize at 50-70°C for 3-4 hours, then raise the temperature to 150-170°C, remove low polymer for 3-5 hours, wherein the alkali metal hydroxide may be potassium hydroxide or sodium hydroxide. The degree of polymerization of the basic catalyst is 10-70.

[0029] b. Synthesis of vinyl silicone oil

[0030] Step 1. In parts by weight, 100 parts of methylcyclosiloxane and 10-40 parts of tetramethyltetravinylcyclotetrasiloxane are used as reaction monomers, and 1-20 parts of vinyl end-capping agent are added, 0.1 - 1 part of basic catalyst, polymerized at 90-150°C for 2-6...

Embodiment 1

[0034] (1) Synthesis of basic catalyst

[0035] Put 100g of octamethylcyclotetrasiloxane and 25g of potassium hydroxide in a three-necked flask, polymerize at 40°C for 3 hours, then raise the temperature to 150°C, under N 2 The oligomer was removed under protection for 4 hours to obtain the basic catalyst.

[0036] (2) Synthesis of vinyl silicone oil

[0037] Step 1. Take 100g octamethylcyclotetrasiloxane and 15g tetramethyltetravinylcyclotetrasiloxane as reaction monomers, and add 4g dimethylvinylethoxysilane, 0.5g of the base synthesized above catalyst, polymerized at 100°C for 3 hours;

[0038] Step 2. After the polymerization reaction is completed, cool to room temperature, add 10wt% dilute hydrochloric acid to neutralize, adjust pH = 7, wash with water three times, and after separation, remove the low boilers from the obtained polymerization solution at 160°C for 4 hours. Vinyl silicone oil can be obtained.

[0039] The vinyl silicone oil synthesized in this example h...

Embodiment 2

[0041] (1) Synthesis of basic catalyst

[0042] Put 100g of octamethylcyclotetrasiloxane and 40g of potassium hydroxide in a three-necked flask, polymerize at 60°C for 3 hours, then raise the temperature to 170°C, 2 The oligomer was removed under protection for 4 hours to obtain the alkali gel catalyst.

[0043] (2) Synthesis of vinyl silicone oil

[0044] Step 1. Take 50g of octamethylcyclotetrasiloxane, 50g of dodecamethylcyclohexasiloxane and 30g of tetramethyltetravinylcyclotetrasiloxane as reaction monomers, and add 7g of dimethylvinyl Ethoxysilane, 1g of the basic catalyst synthesized above, polymerized at 100°C for 3 hours;

[0045] Step 2. After the polymerization reaction is completed, cool to room temperature, add 10wt% dilute hydrochloric acid to neutralize, adjust pH = 7, wash with water three times, and after separation, remove the low boilers from the obtained polymerization solution at 160°C for 4 hours. Vinyl silicone oil can be obtained.

[0046] The vinyl...

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Abstract

The invention discloses vinyl silicone oil and a synthetic method thereof. The vinyl silicone oil comprises the following ingredients in parts by weight: 100 parts of dimethylcydosiloxane, 10-40 parts of tetravinyl tetramethylcyelo tetrasiloxane, 1-20 parts of vinyl end-capping agent, and 0.1-1 part of basic catalyst, wherein the basic catalyst is a basic rubber catalyst which is formed by ring opening polymerization of octamethylcyclotetrasiloxane under the catalysis of basic hydroxide. The synthetic method of the vinyl silicone oil comprises the steps of taking dimethylcydosiloxane and tetravinyl tetramethylcyelo tetrasiloxane as reactive monomers, performing polymerization reaction in the presence of the vinyl end-capping agent and the basic catalyst, after the polymerization reaction, cooling, performing diluted acid neutralization, washing, separating, rectifying polymerization liquid, removing low-boiling-point substances, and obtaining the vinyl silicone oil. The method is simple in technology process, low in cost and high in product yield, the viscosity of the vinyl silicone oil is easy to control, and the vinyl silicone oil is high in reactive activity and good in storage stability, and can be widely applied to synthesis and modifying of new materials such as silicon rubber, polyurethane and polyacrylate.

Description

technical field [0001] The invention relates to a silicone oil and a synthesis method thereof, in particular to a vinyl silicone oil and a synthesis method thereof. Background technique [0002] Silicone oil usually refers to linear polysiloxane that remains liquid at room temperature. It is a type of silicone product with many varieties and a wide range of applications. The organic groups of the most commonly used silicone oil are all methyl groups, called methyl silicone oil. Vinyl silicone oil is the product of part of the methyl groups in methyl silicone oil being replaced by vinyl groups. It has excellent high and low temperature resistance, lubricity, radiation resistance and compatibility, and is a product with broad development prospects. Vinyl silicone oil is mainly used as an additive for addition-type silicone rubber to enhance the strength and hardness of silicone rubber; and can be used to make liquid silicone rubber; react with polyurethane, acrylic and other ...

Claims

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Application Information

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IPC IPC(8): C08G77/20
Inventor 王超陆磊王芳
Owner JIANGSU TIANCHEN NEW MATERIALS
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