A kind of siloxane copolymer containing ethylphenyl siloxane chain unit and preparation method thereof

Abstract

The invention relates to the field of organic polymer chemistry, and specifically relates to a siloxane copolymer containing ethyl phenyl silica chain links and a preparation method thereof. The preparation method comprises the following steps: taking ethyl phenyl dialkoxysilane and dimethyl dialkoxysilane as the raw materials, carrying out hydrolysis condensation reactions in the presence of an anionic type or cationic type hydrolysis catalyst to generate oligomer composed of ethyl phenyl silica chain links and dimethyl silica chain links, then mixing the obtained oligomer with end-capping reagents with different structural types, carrying out reactions in the presence of an anionic type or cationic type polymerization catalyst, and subjecting the reaction products to neutralization / catalyst decomposition and reduced pressured distillation to remove low-boiling-point substances so as to obtain poly(dimethyl-ethylphenyl)siloxane copolymer with ends capped by different functional groups. The species of the monomer used in the provided method are few, the polymerization reaction conditions are mild, the reaction process control is simple, the copolymer structure is uniform, and the performance of the copolymer is excellent, and the provided method is suitable for massive industrial production.

Description

technical field

[0001] The invention relates to the field of organic polymer chemistry, in particular to a siloxane copolymer containing ethylphenylsiloxane chain segments and a preparation method thereof. Background technique

[0002] Silicone polymers with Si-O-Si as the main chain structure combine the comprehensive properties of inorganic materials and organic materials, and have basic properties such as low surface tension, small viscosity-temperature coefficient, high compressibility and high gas permeability, and are resistant High and low temperature, electrical insulation, oxidation resistance stability, weather resistance, flame retardant, hydrophobic, corrosion resistance, non-toxic and tasteless and physiological inertness and other excellent characteristics, therefore, it is widely used in aerospace, electrical and electronic, construction, transportation, Chemical, textile, food, light industry and medical industries.

[0003] From the perspective of molecular...

Examples

Embodiment 1

[0063] Add 8.02g (0.0357mol) ethylphenyldiethoxysilane, 500.5g (3.3754mol) dimethyldiethoxysilane, 130g (7.2222mol) deionized water and 5g (0.2088mol) lithium hydroxide In a 1000mL four-necked round-bottomed flask equipped with a thermometer, constant pressure dropping funnel, mechanical stirring and distillation device, slowly raise the temperature until the material in the flask boils and refluxes, adjust the reflux ratio of the distillation device, and partially receive the overhead fraction, while opening the constant pressure drop The feed valve of the liquid funnel was used to slowly add deionized water dropwise to maintain the liquid level of the material in the round bottom flask basically unchanged. As the hydrolysis process proceeds, the temperature is gradually raised to keep the material in the round bottom flask always in a reflux state. The refractive index (nD 25 ), when the instantaneous refractive index of the sample (n D 25 ) close to 1.3325 (1.3325-1.3330...

Embodiment 2

[0066] 25g (0.1114mol) ethylphenyldiethoxysilane, 17.5g (0.1180mol) dimethyldiethoxysilane, 82.5g (4.5833mol) deionized water and 1.1g (0.0459mol) lithium hydroxide Add it into a 250mL four-neck round bottom flask equipped with a thermometer, constant pressure dropping funnel, mechanical stirring and distillation device, slowly raise the temperature until the material in the flask boils and reflux, adjust the reflux ratio of the distillation device, partially receive the overhead fraction, and open the constant pressure at the same time The feeding valve of the dropping funnel is used to slowly add deionized water dropwise to maintain the liquid level of the material in the round bottom flask basically unchanged. As the hydrolysis process proceeds, the temperature is gradually raised to keep the material in the round bottom flask always in a reflux state. The refractive index (n D 25 ), when the instantaneous refractive index of the sample (n D 25 ) close to 1.3325 (1.3325...

Embodiment 3

[0069] 10.8g (0.055mol) ethylphenyldimethoxysilane, 17.5g (0.1180mol) dimethyldiethoxysilane, 31.5g (1.75mol) deionized water and 0.05g (0.0009mol) hydroxide Potassium was added to a 250mL four-necked round-bottomed flask equipped with a thermometer, a constant pressure dropping funnel, mechanical stirring and a distillation device, and the temperature was slowly raised until the material in the flask boiled and refluxed, and the reflux ratio of the distillation device was adjusted to partially receive the overhead fraction. Press the feeding valve of the dropping funnel, and slowly add deionized water dropwise to keep the liquid level of the material in the round bottom flask basically unchanged. As the hydrolysis process proceeds, the temperature is gradually raised to keep the material in the round bottom flask always in a reflux state. The refractive index (n D 25 ), when the instantaneous refractive index of the sample (n D 25 ) close to 1.3325 (1.3325-1.3330), stop t...

technical field

[0001] The invention relates to the field of organic polymer chemistry, in particular to a siloxane copolymer containing ethylphenylsiloxane chain segments and a preparation method thereof. Background technique

[0002] Silicone polymers with Si-O-Si as the main chain structure combine the comprehensive properties of inorganic materials and organic materials, and have basic properties such as low surface tension, small viscosity-temperature coefficient, high compressibility and high gas permeability, and are resistant High and low temperature, electrical insulation, oxidation resistance stability, weather resistance, flame retardant, hydrophobic, corrosion resistance, non-toxic and tasteless and physiological inertness and other excellent characteristics, therefore, it is widely used in aerospace, electrical and electronic, construction, transportation, Chemical, textile, food, light industry and medical industries.

[0003] From the perspective of molecular...

Examples

Embodiment 1

[0063] Add 8.02g (0.0357mol) ethylphenyldiethoxysilane, 500.5g (3.3754mol) dimethyldiethoxysilane, 130g (7.2222mol) deionized water and 5g (0.2088mol) lithium hydroxide In a 1000mL four-necked round-bottomed flask equipped with a thermometer, constant pressure dropping funnel, mechanical stirring and distillation device, slowly raise the temperature until the material in the flask boils and refluxes, adjust the reflux ratio of the distillation device, and partially receive the overhead fraction, while opening the constant pressure drop The feed valve of the liquid funnel was used to slowly add deionized water dropwise to maintain the liquid level of the material in the round bottom flask basically unchanged. As the hydrolysis process proceeds, the temperature is gradually raised to keep the material in the round bottom flask always in a reflux state. The refractive index (nD 25 ), when the instantaneous refractive index of the sample (n D 25 ) close to 1.3325 (1.3325-1.3330...

Embodiment 2

[0066] 25g (0.1114mol) ethylphenyldiethoxysilane, 17.5g (0.1180mol) dimethyldiethoxysilane, 82.5g (4.5833mol) deionized water and 1.1g (0.0459mol) lithium hydroxide Add it into a 250mL four-neck round bottom flask equipped with a thermometer, constant pressure dropping funnel, mechanical stirring and distillation device, slowly raise the temperature until the material in the flask boils and reflux, adjust the reflux ratio of the distillation device, partially receive the overhead fraction, and open the constant pressure at the same time The feeding valve of the dropping funnel is used to slowly add deionized water dropwise to maintain the liquid level of the material in the round bottom flask basically unchanged. As the hydrolysis process proceeds, the temperature is gradually raised to keep the material in the round bottom flask always in a reflux state. The refractive index (n D 25 ), when the instantaneous refractive index of the sample (n D 25 ) close to 1.3325 (1.3325...

Embodiment 3

[0069] 10.8g (0.055mol) ethylphenyldimethoxysilane, 17.5g (0.1180mol) dimethyldiethoxysilane, 31.5g (1.75mol) deionized water and 0.05g (0.0009mol) hydroxide Potassium was added to a 250mL four-necked round-bottomed flask equipped with a thermometer, a constant pressure dropping funnel, mechanical stirring and a distillation device, and the temperature was slowly raised until the material in the flask boiled and refluxed, and the reflux ratio of the distillation device was adjusted to partially receive the overhead fraction. Press the feeding valve of the dropping funnel, and slowly add deionized water dropwise to keep the liquid level of the material in the round bottom flask basically unchanged. As the hydrolysis process proceeds, the temperature is gradually raised to keep the material in the round bottom flask always in a reflux state. The refractive index (n D 25 ), when the instantaneous refractive index of the sample (n D 25 ) close to 1.3325 (1.3325-1.3330), stop t...

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