Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of vinyl-terminated methyl phenyl polysiloxane

A technology of terminal methyl phenyl and vinyl sealing, applied in the field of organosilicon synthesis, can solve problems such as unreasonable use of catalysts, and achieve the effects of easy recovery and reuse, good loading effect, and satisfying industrial production.

Active Publication Date: 2021-02-26
ZHEJIANG QUZHOU ZHENGBANG ORGANOSILICON CO LTD +1
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is in order to solve the unreasonable problem that the catalyzer that exists in the synthetic process of prior art is used unreasonably, adopts halloysite nanotube loading catalyst in reaction, avoids adopting H 2 SO 4 , HCl, tetramethylammonium hydroxide or tetramethylammonium hydroxide alkali gel as a catalyst, reduce the corrosion of equipment, reduce the discharge of three wastes, improve the yield of the reaction and the quality of the product, and provide a simple and reasonable process, the reaction yield Industrialized production method of vinyl-terminated methylphenyl polysiloxane with high efficiency, less waste, and low cost

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of vinyl-terminated methyl phenyl polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 500g of methylphenyldimethoxysilane and 400g of deionized water into the reactor, stir, add 2.5g of halloysite nanotube-supported catalyst, heat to 70°C, react for 2h, and collect the distillate with a condenser , after the reaction is over, adjust the system pressure to -0.096Mpa, remove water and low boilers by distillation under reduced pressure, and obtain a colorless and transparent hydroxyl-terminated methylphenyl siloxane oligomer intermediate, and then add 30g of tetramethyl phenylsiloxane Divinyl disiloxane, nitrogen protection, control the reaction temperature at 80°C, stir the reaction for 3h, after the reaction is completed, filter, recover the rockite nanotube-supported catalyst, adjust the pressure of the system to -0.096Mpa, at 180°C Under reduced pressure, the low boilers were removed by distillation under reduced pressure to obtain a colorless oily liquid vinyl-terminated methylphenylpolysiloxane. The yield is 83.6%, and the refractive index (20°C) ...

Embodiment 2

[0031] Add 500g of methylphenyldimethoxysilane and 500g of deionized water into the reactor, add 5g of halloysite nanotube-supported catalyst under stirring, heat to 80°C, react for 2h, and collect the distillate with a condenser , after the reaction is over, adjust the system pressure to -0.096Mpa, remove water and low boilers by distillation under reduced pressure, and obtain a colorless and transparent hydroxyl-terminated methylphenyl siloxane oligomer intermediate, and then add 25g tetramethyl phenylsiloxane Divinyl disiloxane, nitrogen protection, control the reaction temperature at 85°C, stir the reaction for 5h, after the reaction, filter, recover the rockite nanotube-supported catalyst, adjust the system pressure to -0.096Mpa, at 200°C Under reduced pressure, the low boilers were removed by distillation under reduced pressure to obtain a colorless oily liquid vinyl-terminated methylphenylpolysiloxane. The yield is 87.6%, and the refractive index (20°C) is 1.551.

[00...

Embodiment 3

[0037] Add 500g of methylphenyldimethoxysilane and 450g of deionized water into the reactor, add 4g of halloysite nanotube-supported catalyst under stirring, heat to 70-80°C, react for 2h, collect the distillate with a condenser After the reaction is finished, adjust the system pressure to -0.096Mpa, remove water and low boilers by distillation under reduced pressure, and obtain a colorless and transparent hydroxyl-terminated methylphenyl siloxane oligomer intermediate, and then add 40g Tetramethyldivinyldisiloxane, under the protection of nitrogen gas, under the condition of reaction temperature of 82 ℃, stirred and reacted for 4h, after the reaction was completed, filtered and recovered the catalyst supported by calcite nanotubes, adjusted the system pressure to -0.096Mpa, At 190°C, the low boilers were removed by distillation under reduced pressure to obtain a colorless oily liquid vinyl-terminated methylphenylpolysiloxane with a yield of 85.9% and a refractive index (20°C) ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
refractive indexaaaaaaaaaa
refractive indexaaaaaaaaaa
refractive indexaaaaaaaaaa
Login to View More

Abstract

The invention relates to a preparation method of vinyl-terminated methylphenyl polysiloxane, and the method comprises the following steps: adding 500 parts by mass of methylphenyl dimethoxysilane and400-500 parts by mass of deionized water into a reactor, adding 2.5-5 parts by mass of halloysite nanotube supported catalyst while stirring, heating to 70-80 DEG C, reacting for 2 hours, and collecting the distillate by using a condenser; after the reaction is finished, regulating the pressure of the system to -0.096 Mpa, carrying out reduced pressure distillation to remove water and low-boiling-point substances to obtain a colorless transparent hydroxyl-terminated methyl phenyl siloxane oligomer intermediate, adding 30-50 parts of tetramethyl divinyl disiloxane, introducing nitrogen for protection, carrying out stirring reaction for 3-5 hours under the condition that the reaction temperature is 80-85 DEG C, and after the reaction is finished, filtering and recovering the loess nanotube supported catalyst, adjusting the pressure of the system to -0.096 Mpa, and carrying out reduced pressure distillation at the temperature of 180-200 DEG C to remove low-boiling-point substances, so asto obtain colorless oily liquid vinyl-terminated methylphenyl polysiloxane. The method has the characteristics of simple and reasonable process, high reaction yield, less three wastes, low cost and easiness in industrial production.

Description

technical field [0001] The invention relates to the technical field of organosilicon synthesis, in particular to a preparation method of vinyl-terminated methylphenyl polysiloxane. Background technique [0002] Vinyl-terminated methylphenyl polysiloxane (Poly(phenylmenthylsiloxane), divinylterminated) is a vinyl-terminated linear methylphenyl silicone oil, mainly used for the preparation of addition-type liquid silicone rubber, high-power / high-refraction light-emitting diodes ( LED) packaging materials have good application prospects in ultra-low temperature sealing, damping and shock-absorbing materials and optoelectronic fields. [0003] Ganfangshu et al. (Organosilicon Materials, 2015, 29(2): 105-109) reported the preparation of vinyl-terminated compounds with different molar masses by hydrolysis-polycondensation method using methylphenyldimethoxysilane as raw material. Methylphenyl polysiloxane has low production cost, the refractive index of the product is above 1.51, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/08
CPCC08G77/20C08G77/08
Inventor 郑启波冯晓亮郑一凡李军勇池云丰
Owner ZHEJIANG QUZHOU ZHENGBANG ORGANOSILICON CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com