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Fluorine-contained phenyl hydrogen-contained silicone oil cross-linking agent and preparing method thereof

A technology of phenyl hydrogen-containing silicone oil and cross-linking agent, which is applied in the field of fluorine-containing phenyl hydrogen-containing silicone oil cross-linking agent and its preparation, and can solve the problem that it is difficult to obtain completely transparent Products, phenylcyclosiloxane ring body stress, hydrogen-containing silicone oil cross-linking and other problems, to improve product quality and stability, high product yield, avoid residue effects

Inactive Publication Date: 2015-12-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process cannot use alkaline catalysts, which will easily lead to hydrogen loss and crosslinking of hydrogen-containing silicone oil, and because phenyl cyclosiloxane is solid, it is incompatible with fluorine-containing cyclosiloxane, methyl cyclosiloxane, and hydrogen-containing silicone oil. soluble, and the stress of the phenylcyclosiloxane ring is large, it is difficult to completely open the ring under acidic conditions, and it is difficult to obtain a completely transparent product even if the reaction time is prolonged

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Under the condition of stirring (stirring speed is 80 rpm), add 200g of methyl silicone oil (molecular weight 800) with a viscosity of 5mPa.s, 200g of octaphenylcyclotetrasiloxane and 100g of a viscosity of 5mPa. s methyl fluorosilicone oil (molecular weight 730), then add 0.25g potassium hydroxide, stir for 10min and mix well; heat up to 150°C, stir at constant temperature for 8h, stop heating, cool to room temperature, add 20g concentrated sulfuric acid (mass concentration is 98% ) and 500g of hydrogen-containing silicone oil (molecular weight: 4800) with a hydrogen content of 1.6%, equilibrated at room temperature for 4h, added 80g of sodium carbonate for neutralization for 1h, and vacuum filtered to obtain a colorless and transparent fluorine-containing phenyl hydrogen-containing silicone oil. Weighing 950g, the yield is 95%. The silicone oil has a refractive index of 1.4644 at 25° C., a viscosity of 35 mPa.s, and a hydrogen content of 0.79%.

Embodiment 2

[0031] Under stirring conditions (stirring speed is 100 rpm), add 200g of methyl silicone oil (molecular weight 1300) with a viscosity of 10mPa.s, 200g of octaphenylcyclotetrasiloxane and 100g of a viscosity of 50mPa. s methyl fluorosilicone oil (molecular weight 3500), then add 0.5g potassium hydroxide, stir for 10min to mix; heat up to 160°C, stir at constant temperature for 7h, stop heating, cool to room temperature, add 50g concentrated sulfuric acid (mass concentration is 98% ) and 500g of hydrogen-containing silicone oil (molecular weight: 5000) with a hydrogen content of 0.6%, equilibrated at room temperature for 5 hours, added 100g of sodium carbonate to neutralize for 2 hours, and vacuum filtered to obtain a colorless and transparent fluorine-containing phenyl hydrogen-containing silicone oil. Weighing 955g, the yield is 95.5%. The silicone oil has a refractive index of 1.4641 at 25° C., a viscosity of 55 mPa.s, and a hydrogen content of 0.28%.

Embodiment 3

[0033] Under the condition of stirring (stirring speed is 120 rpm), add 150g of methyl silicone oil (molecular weight 3800) with a viscosity of 50mPa.s, 250g of octaphenylcyclotetrasiloxane and 100g of a viscosity of 100mPa.s in a 2L three-necked flask. s of methyl fluorosilicone oil (molecular weight 5500), then add 0.25g of lithium hydroxide, stir for 8min to mix; heat up to 180°C, stir at constant temperature for 5h, stop heating, cool to room temperature, add 18g of concentrated sulfuric acid (mass concentration is 98% ) and 100g of hydrogen-containing silicone oil (molecular weight: 4800) with a hydrogen content of 1.6%, equilibrated reaction at room temperature for 6h, added 54g of sodium bicarbonate for neutralization for 1.5h, and vacuum filtration to obtain a colorless and transparent fluorine-containing phenyl hydrogen-containing silicone oil. Weighing 952g, the yield was 95.2%. The silicone oil has a refractive index of 1.4932 at 25° C., a viscosity of 176 mPa.s, an...

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Abstract

The invention belongs to the technical field of cross-linking agents and discloses a fluorine-contained phenyl hydrogen-contained silicone oil cross-linking agent and a preparing method thereof. According to the method, a base catalyst is added into low-viscosity methyl silicone oil, phenyl cyclosiloxane and fluorosilicone oil, the mixture is mixed uniformly, temperature is raised, the mixture is stirred at constant temperature and cooled, an acid catalyst and hydrogen-contained silicone oil are sequentially added into the mixture, a balanced reaction is carried out, and follow-up treatment is carried out after the reaction is finished, so that the colorless and transparent fluorine-contained phenyl hydrogen-contained silicone oil cross-linking agent is obtained. According to the preparing method, methyl cyclosiloxane and an end-capping agent do not needed to be added, the technology is simplified, and the product quality and stability are improved; the adopted raw materials do not contain chlorine or alkoxy, and therefore introduction of chloride ions and residues of alkoxy are avoided; as no solvent is adopted, harm to the human body and pollution to the environment are avoided; the yield of the prepared cross-linking agent is high.

Description

technical field [0001] The invention belongs to the technical field of crosslinking agents, and relates to a fluorine-containing phenyl hydrogen-containing silicone oil crosslinking agent, in particular to a fluorine-containing phenyl hydrogen-containing silicone oil crosslinking agent and a preparation method thereof. The fluorine-containing phenyl hydrogen-containing silicone oil crosslinking agent specifically refers to a hydrogen-containing silicone oil crosslinking agent containing fluorine groups and phenyl co-modified. Background technique [0002] Phenyl silicone rubber is one of the main varieties of silicone rubber. It has good high and low temperature resistance, radiation resistance, etc., and is widely used in electronics, machinery, aerospace and other fields. Low phenyl silicone rubber has remarkable low temperature resistance and is also elastic at -110°C; high phenyl silicone rubber can be used for a long time at 350°C; under γ-ray irradiation, phenyl silico...

Claims

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Application Information

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IPC IPC(8): C08G77/44
Inventor 涂伟萍朱淮军戴子林
Owner SOUTH CHINA UNIV OF TECH
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