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Preparation method of phenyl silicone oil

A technology of phenyl silicone oil and diphenyl cyclosiloxane, which is applied in the field of phenyl silicone oil preparation, can solve the problem of difficult preparation of high-quality phenyl silicone oil containing diphenyl chain members, large difference in reactivity, and phenyl silicone oil Problems such as limited application, to achieve the effect of good transparency, easy access, and low polymerization temperature

Active Publication Date: 2014-04-09
SHANDONG DONGYUE ORGANIC SILICON MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The copolymerization of diphenylsiloxane ring body and dimethylcyclosiloxane needs to be polymerized at a higher temperature. Due to the steric hindrance effect of diphenylcyclosiloxane, the reactivity of the two is quite different, so it is difficult to Make the phenyl group evenly distributed among the molecules, and it is easy to leave a certain amount of diphenylcyclosiloxane without ring opening, and it is easy to precipitate white crystals to make the silicone oil opaque (Organosilicon Materials, 2012, 26(2): 117-121), Due to the high reaction temperature, yellowing of silicone oil is also prone to occur in the presence of catalysts
However, because the above-mentioned methods all use polydiphenyl-dimethyl polysiloxane with a low degree of polymerization terminated by hydroxyl groups, the silicone oil will often contain a certain amount of hydroxyl groups, and the viscosity range will also be limited to a certain extent.
[0006] At present, the existing phenyl silicone oil preparation process is difficult to prepare high-quality phenyl silicone oil containing diphenyl chain members. Due to the limitation of the quality of diphenyl silicone oil, phenyl silicone oil containing diphenyl chain members is used in many high-end fields. application limited

Method used

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  • Preparation method of phenyl silicone oil

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Experimental program
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Effect test

Embodiment 1

[0053] To prepare vinyl-terminated, phenyl silicone oil with a phenyl content of 35mol% and a degree of polymerization of 150, the steps are as follows:

[0054] (1) Take 96g of DMC and 139g of octaphenylcyclotetrasiloxane in a 500mL four-neck flask, add 2.3g of potassium hydroxide, mix well, and polymerize at 180°C for 6 hours to obtain a copolymer;

[0055] (2) In a closed reaction system isolated from air, the temperature of the copolymer is raised to 340°C for a cracking reaction, and the product is distilled during the cracking reaction to obtain diphenyl-dimethylcyclosiloxane;

[0056] (3) NMR 1 According to H-NMR analysis, the molar ratio of diphenylsiloxane chains to dimethylsiloxane chains is 1:1.85, and its phenyl content is 35mol%;

[0057] (4) Take 200g of diphenyl-dimethylcyclosiloxane, add 2.1g of divinyltetramethyldisiloxane, tetramethylammonium hydroxide silicon alkoxide (converted to tetramethylammonium hydroxide) 0.01g, stirring polymerization at 90°C for 4...

Embodiment 2

[0061] To prepare vinyl-terminated, phenyl silicone oil with a phenyl content of 30mol%, a degree of polymerization of 150, and side vinyl groups, the steps are as follows:

[0062] (1) Take 100g of D4 and 145g of octaphenylcyclotetrasiloxane in a 500mL four-necked flask, add 2.4g of potassium hydroxide, mix well, and polymerize at 180°C for 6 hours to obtain a copolymer;

[0063] (2) In a closed reaction system isolated from air, the temperature of the copolymer is raised to 320°C for a cracking reaction, and the product is distilled during the cracking reaction to obtain diphenyl-dimethylcyclosiloxane;

[0064] (3) NMR 1 According to H-NMR analysis, the molar ratio of diphenylsiloxane and dimethylsiloxane chains is 1:1.93, and its phenyl content is 34mol%;

[0065] (4) Take 200g of diphenyl-dimethylcyclosiloxane, add 8.8g of D4 to adjust the phenyl content, introduce 8.6g of tetramethyltetravinylcyclotetrasiloxane into side vinyl groups, add 2.4g of divinyl tetrasiloxane M...

Embodiment 3

[0069] To prepare hydrogen-terminated, phenyl silicone oil with a phenyl content of 38mol% and a degree of polymerization of 20, the steps are as follows:

[0070] (1) Take 100g of D5 and 150g of octaphenylcyclotetrasiloxane in a 500mL four-necked flask, add 2.4g of potassium hydroxide, mix well, and polymerize at 180°C for 4 hours to obtain a copolymer;

[0071] (2) In a closed reaction system isolated from air, the temperature of the copolymer is raised to 320°C for a cracking reaction, and the product is distilled during the cracking reaction to obtain diphenyl-dimethylcyclosiloxane;

[0072] (3) NMR 1 According to H-NMR analysis, the molar ratio of diphenylsiloxane and dimethylsiloxane chains is 1:1.83, and its phenyl content is 36mol%;

[0073] (4) Take 200g of diphenyl-dimethylcyclosiloxane, add 124.8g of methylphenylcyclosiloxane mixture to adjust the phenyl content, add 17.6g of tetramethyldisiloxane and 3g of 98wt% concentrated Sulfuric acid, stirring polymerization...

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Abstract

The invention relates to a preparation method of phenyl silicone oil. The method includes: mixing diphenyl cyclosiloxane with dimethyl cyclosiloxane according to certain proportion, adding an alkali catalyst to undergo copolymerization under certain temperature, then raising the temperature to 250-350DEG C, conducting cracking to obtain diphenyl-dimethyl cyclosiloxane, determining the proportions of a dimethyl chain link and a diphenyl chain link therein, mixing the diphenyl-dimethyl cyclosiloxane, an end-capping reagent, a catalyst or other cyclosiloxane and a promoter uniformly in proportion, carrying out polymerization under certain temperature, then deactivating the catalyst, conducting post-treatment, and removing low molecules, thus obtaining the target product phenyl silicone oil. The method provided by the invention can be used for preparing a variety of phenyl silicone oil, the obtained phenyl silicone oil has high quality and excellent transparency, and can be applied to optical packaging materials, personal care, lubricating oil and other fields.

Description

technical field [0001] The invention belongs to the field of polyorganosiloxane preparation and relates to a preparation method of phenyl silicone oil. Background technique [0002] Phenyl silicone oil is a linear polysiloxane in which part of the methyl group is substituted by phenyl in methyl silicone oil. Compared with methyl silicone oil, it has more excellent properties such as high and low temperature resistance, lubricity and radiation resistance. Development prospects, can be used in personal care products, defense industry, life sciences, aerospace and other fields. In recent years, as the demand for phenyl silicone oil has increased year by year, the research and development of its new varieties and new processes has become a hot spot. [0003] Phenyl silicone oil is divided into polymethylphenyl-dimethylsiloxane copolymers containing methylphenylsiloxane chains and polymethylphenyl-dimethylsiloxane copolymers containing diphenylsiloxane chains according to the di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/04C08G77/20C08G77/12
Inventor 高俊杰刘海龙付佃亮张停
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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