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High viscosity phenyl methyl silicone oil and preparing method thereof

A technology of phenylmethyl silicone oil and high viscosity, which is applied in the field of phenylmethyl silicone oil and its preparation, can solve the problem that high-viscosity phenylmethyl silicone oil is not suitable for use, and cannot prepare high-viscosity phenylmethyl silicone oil, viscosity Problems such as poor control technology are achieved to achieve low cost, high phenyl content, and improved transparency

Inactive Publication Date: 2018-03-06
SHANGHAI RESIN FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The silicone oil prepared by the above method is mainly used as a crosslinking agent for LED encapsulation liquid, and the cost is relatively high, so it is not suitable for the use of the above-mentioned high-viscosity phenylmethyl silicone oil
In addition, most of the products currently on the market are made of a mixture of phenylmethyl silicone oils with different viscosities, and the actual application effect is not good.
The viscosity control technology in the preparation of this type of product is not good, and most of the end-capping agents are added in the early stage of the reaction, so that high-viscosity phenylmethyl silicone oil cannot be prepared.

Method used

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  • High viscosity phenyl methyl silicone oil and preparing method thereof
  • High viscosity phenyl methyl silicone oil and preparing method thereof
  • High viscosity phenyl methyl silicone oil and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] formula:

[0038]

[0039] Add dimethyldiphenyl mixed cyclosiloxane and octamethylcyclotetrasiloxane into the reactor, mix and dehydrate for 1 hour at 40°C and -0.09MPa.

[0040] After the dehydration is completed, the temperature of the reaction system is raised to 90°C, tetramethylammonium hydroxide silicon alkoxide is added, and the reaction is carried out at -0.09MPa. When the viscosity of the system increases rapidly, add 5 parts of hexamethyldisiloxane, and continue to react for 2 hours under normal pressure and 90°C. After the reaction, the temperature of the reaction system was raised to 150° C. to decompose (inactivate) tetramethylammonium hydroxide silicon alkoxide for 30 minutes. Then the temperature of the reaction system was raised to 180°C, and the pressure was reduced to -0.09MPa to remove small molecular compounds for 30 minutes to obtain high-viscosity phenylmethyl silicone oil. After measurement, the product has a refractive index of 1.4959, a vis...

Embodiment 2

[0043] formula:

[0044]

[0045] 100 parts of dimethyldiphenyl mixed cyclosiloxane was added to the reactor, and dehydration was carried out at 30°C and -0.09MPa for 2 hours.

[0046] After the dehydration is complete, the temperature of the reaction system is raised to 80°C, 1 part of tetramethylammonium hydroxide silicon alkoxide is added, and the reaction is carried out at -0.09MPa. When the viscosity of the system increases rapidly, add 10 parts of hexamethyldisiloxane, and continue to react for 3 hours at normal pressure and 80°C. After the reaction, the temperature of the reaction system was raised to 150° C. to decompose (deactivate) tetramethylammonium hydroxide silicon alkoxide for 35 minutes. Then the temperature of the reaction system was raised to 175°C, and the pressure was reduced to -0.09MPa to remove small molecular compounds for 35 minutes to obtain high-viscosity phenylmethyl silicone oil. After measurement, the refractive index is 1.4984 and the viscos...

Embodiment 3

[0048] formula:

[0049]

[0050] Add 100 parts of dimethyldiphenyl mixed cyclosiloxane and 20 parts of octamethylcyclotetrasiloxane into the reactor, mix and dehydrate for 1.5 hours at 35°C and -0.09MPa.

[0051] After dehydration is complete, the temperature of the reaction system is raised to 85°C, 1.2 parts of tetramethylammonium hydroxide silicon alkoxide is added, and the reaction is carried out at -0.09MPa. When the viscosity of the system increases rapidly, add 5 parts of hexamethyldisiloxane, and continue to react at normal pressure and 85°C for 2 hours. After the reaction, the temperature of the reaction system was raised to 150° C. to decompose (deactivate) tetramethylammonium hydroxide silicon alkoxide for 40 minutes. Then the temperature of the reaction system was raised to 170°C, and the small molecule compounds were removed for 40 minutes under the condition of reducing the pressure to -0.09MPa to obtain high-viscosity phenylmethyl silicone oil. After measu...

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Abstract

The invention discloses high viscosity phenyl methyl silicone oil and a preparing method thereof. The high viscosity phenyl methyl silicone oil is prepared from, by weight, 70-100 parts of dimethyl diphenyl mixed cyclosiloxane, 0-20 parts of octamethyl cyclotetrasiloxane, 0.7-1.2 parts of tetramethyl ammonium hydroxide silanol salt and 1-10 parts of hexamethyldisiloxane. The preparing method is simple in raw material, low in cost, simple in technology and mild in reaction condition. The phenyl content is high, and the prepared phenyl methyl silicone oil is high in refractive index; the conducted polymerization mode is cyclosiloxane ring opening polymerization, the polymerization yield is high, the molecular weight distribution is small, and the homogeneity and the viscosity are high. The synthesized silicone oil is high in refractive index (1.49-1.51) and high in viscosity (the rotary viscosity reaches 100 mPa.s or above), and the visible light transmittance reaches 80% or above.

Description

technical field [0001] The invention relates to a phenylmethyl silicone oil and a preparation method thereof. Background technique [0002] Phenyl methyl silicone oil is a product in which some methyl groups in methyl silicone oil are replaced by phenyl groups. It has the advantages of high temperature resistance, radiation resistance, lubricity, and high refractive index. The rotational viscosity of high-viscosity phenylmethyl silicone oil can reach more than 1000mPa s. Due to its high viscosity, this type of silicone oil is used in nuclear power plant special radiation protection, high heat carrier, and structural sealing under continuous high temperature. After use, the sealing structure is not easy to fall off, and The radioactive substances in it are not easy to leak, and it has the function that low-viscosity phenylmethyl silicone oil cannot replace. It is currently a high-end application product of phenylmethyl silicone oil. This type of silicone oil is a promising p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/08C08G77/04
CPCC08G77/04C08G77/06C08G77/08
Inventor 何辛周亦文姚慧敏高晟弢王立伟吴蓁
Owner SHANGHAI RESIN FACTORY
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