Branched benzene siliconic oil

Abstract

This invention relates to a branch-type silicone oil with a structural formula which R1, R2 and R3 represent alkyl or aryl and methyl, ethyl and phenyl are considered in prior. R1, R2 and R3 can be the same or not. The polymerization degree n is an integral between 1 and 100. This invention also relates to the method to prepare the branch-type phenyl silicone oil. The branch-type phenyl silicone oil is smell-less and colorless transparent liquid, with the characteristics of low viscosity and high refractive index. It is compatible with kinds of cosmetic raw materials and contains no heavy metal.

Description

technical field

[0001] The invention relates to a silicone oil and a preparation method thereof, in particular to a branched-chain phenyl silicone oil and a preparation method thereof. Background technique

[0002] Phenyl silicone oil is one of the main varieties of silicone oil. Because of its good chemical stability, high and low temperature resistance, electrical insulation, radiation resistance and physiological inertness, it is widely used in daily chemicals, electronics, machinery etc.

[0003] The traditional phenyl silicone oil is a linear polydimethylsiloxane with some methyl groups replaced by phenyl groups. Its structure is as follows:

[0004]

[0005] Where R can be methyl or phenyl, and m, n, p may also be 0.

[0006] Their synthetic routes are divided into two types: hydrolytic polycondensation and ring-opening polymerization:

[0007] 1. Obtained by hydrolysis polycondensation reaction

[0008] Dimethyldichlorosilane, dimethyldialkoxysilane, phenylmeth...

Examples

Embodiment 1

[0060] Add 565g of deionized water into a 1L four-necked flask and stir, mix 131g of phenyltrichlorosilane and 174g of trimethylchlorosilane evenly, and uniformly drop them into the flask within 8 hours, and control the reaction temperature at 5°C; After the temperature is raised to 60°C, react for another 1 hour. After the reaction, let stand to separate the water; wash the oil phase repeatedly with alkali and water until neutral; then distill under reduced pressure at 1.3KPa and 100°C for 4 hours; , adding activated carbon, raising the temperature to 50°C, stirring for 0.5 hours, and then suction filtering to obtain 132 g of a colorless and odorless product with a viscosity of 28 mPa.s, a refractive index of 1.4669, and a specific gravity of 1.005.

Embodiment 2

[0062] Add 290g of deionized water and 52g of hydrochloric acid with a mass concentration of 36% into a 1L four-necked flask and stir, mix 162g of phenyltriethoxysilane and 350g of trimethylethoxysilane evenly, and drop them evenly within 1 hour into the flask, control the reaction temperature at 50°C; after the dropwise addition, raise the temperature to 80°C, and react for another 6 hours; after the reaction, let stand to separate the water; wash the oil phase repeatedly with alkali and water until it is neutral; Distill under reduced pressure at ℃ for 4 hours; after cooling down to room temperature, add activated carbon, raise the temperature to 80 ℃, stir for 2 hours, and then filter with suction to obtain 160 g of a colorless and odorless product with a viscosity of 15 mPa.s, a refractive index of 1.4552, and a specific gravity of 0.9726.

Embodiment 3

[0064]Add 222g of deionized water and 72g of hydrochloric acid with a mass concentration of 38% into a 1L four-necked flask and stir, mix 196g of phenyltriethoxysilane and 400g of hexamethyldisiloxane evenly, and drop them evenly within 2 hours Into the flask, control the reaction temperature at 60°C; after the dropwise addition, raise the temperature to 75°C, and then react for 3 hours. Distill under reduced pressure at ℃ for 2 hours; after cooling down to room temperature, add activated carbon, raise the temperature to 40 ℃, stir for 4 hours, and then filter with suction to obtain 210 g of a colorless and odorless product with a viscosity of 20 mPa.s, a refractive index of 1.4600, and a specific gravity of 0.9804.

technical field

[0001] The invention relates to a silicone oil and a preparation method thereof, in particular to a branched-chain phenyl silicone oil and a preparation method thereof. Background technique

[0002] Phenyl silicone oil is one of the main varieties of silicone oil. Because of its good chemical stability, high and low temperature resistance, electrical insulation, radiation resistance and physiological inertness, it is widely used in daily chemicals, electronics, machinery etc.

[0003] The traditional phenyl silicone oil is a linear polydimethylsiloxane with some methyl groups replaced by phenyl groups. Its structure is as follows:

[0004]

[0005] Where R can be methyl or phenyl, and m, n, p may also be 0.

[0006] Their synthetic routes are divided into two types: hydrolytic polycondensation and ring-opening polymerization:

[0007] 1. Obtained by hydrolysis polycondensation reaction

[0008] Dimethyldichlorosilane, dimethyldialkoxysilane, phenylmeth...

Examples

Embodiment 1

[0060] Add 565g of deionized water into a 1L four-necked flask and stir, mix 131g of phenyltrichlorosilane and 174g of trimethylchlorosilane evenly, and uniformly drop them into the flask within 8 hours, and control the reaction temperature at 5°C; After the temperature is raised to 60°C, react for another 1 hour. After the reaction, let stand to separate the water; wash the oil phase repeatedly with alkali and water until neutral; then distill under reduced pressure at 1.3KPa and 100°C for 4 hours; , adding activated carbon, raising the temperature to 50°C, stirring for 0.5 hours, and then suction filtering to obtain 132 g of a colorless and odorless product with a viscosity of 28 mPa.s, a refractive index of 1.4669, and a specific gravity of 1.005.

Embodiment 2

[0062] Add 290g of deionized water and 52g of hydrochloric acid with a mass concentration of 36% into a 1L four-necked flask and stir, mix 162g of phenyltriethoxysilane and 350g of trimethylethoxysilane evenly, and drop them evenly within 1 hour into the flask, control the reaction temperature at 50°C; after the dropwise addition, raise the temperature to 80°C, and react for another 6 hours; after the reaction, let stand to separate the water; wash the oil phase repeatedly with alkali and water until it is neutral; Distill under reduced pressure at ℃ for 4 hours; after cooling down to room temperature, add activated carbon, raise the temperature to 80 ℃, stir for 2 hours, and then filter with suction to obtain 160 g of a colorless and odorless product with a viscosity of 15 mPa.s, a refractive index of 1.4552, and a specific gravity of 0.9726.

Embodiment 3

[0064]Add 222g of deionized water and 72g of hydrochloric acid with a mass concentration of 38% into a 1L four-necked flask and stir, mix 196g of phenyltriethoxysilane and 400g of hexamethyldisiloxane evenly, and drop them evenly within 2 hours Into the flask, control the reaction temperature at 60°C; after the dropwise addition, raise the temperature to 75°C, and then react for 3 hours. Distill under reduced pressure at ℃ for 2 hours; after cooling down to room temperature, add activated carbon, raise the temperature to 40 ℃, stir for 4 hours, and then filter with suction to obtain 210 g of a colorless and odorless product with a viscosity of 20 mPa.s, a refractive index of 1.4600, and a specific gravity of 0.9804.

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