A kind of preparation method of epoxy end-capped side chain vinyl methyl phenyl silicone oil
A technology of chain vinyl methyl phenyl silicon and terminal methyl phenyl siloxane, which is applied in the field of preparation of epoxy-terminated side chain vinyl methyl phenyl silicone oil, and can solve the problem that economic indicators are difficult to estimate and have no reports , high market prices and other issues, to achieve the effect of mass production process promotion, reduction of production, and less content
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0040] The preparation method of the present invention will be further described below in conjunction with the accompanying drawings.
[0041] A preparation method of epoxy-terminated side chain vinyl methyl phenyl silicone oil, comprising steps:
[0042] (1) Hydrolysis, that is, the use of hydrolysis to prepare hydroxyl-terminated methylphenylsiloxane oligomers, with methylphenyldimethoxysilane and diphenyldimethoxysilane containing at least methylphenyl Dimethoxysilane or a mixture of two monomers, at 50-90 ° C, with dilute acid or dilute alkali aqueous solution as a catalyst, the above-mentioned one monomer or a mixture of two monomers is hydrolyzed and removed. Low-boiling substances such as small molecule alcohols are washed, dried, and hot-filtered to obtain a colorless and transparent hydroxyl-terminated methylphenylsiloxane oligomer;
[0043] (2) Telomerization, the hydroxyl-terminated methylphenylsiloxane oligomer and methylvinylsiloxane ring body (D 4 Me,Vi ) and ...
Embodiment 1
[0046] Add 29.0g (0.1mol / L) hydrochloric acid to a 250ml three-necked flask, raise the temperature to 50°C, and add 82.0gMePhSi(OMe) dropwise 2 , the dropwise addition is completed within 0.5h, keep the reaction at 50°C for 1h, then raise the temperature to 70°C, keep it warm for 2h, then vacuum distill water and by-products, add 0.41g (0.1mol / L) hydrochloric acid, keep 70°C to continue hydrolysis After reacting for 2 hours, the by-products were distilled out again in vacuum, washed with hot water at 50°C for 3 times until neutral, and after liquid separation, the organic phase was washed with anhydrous CaCl 2 and anhydrous MgSO 4 Dry and filter with a membrane filtration device at 50°C. The pore size of the polytetrafluoroethylene microporous filter membrane is 1 μm to obtain 60.5g of hydroxyl-terminated methylphenylsiloxane oligomer. 1 Characterized by NMR, number average molecular weight: 800, viscosity 300mPa·s. 15.0g hydroxyl-terminated methyl phenyl silicone oil, 2.4g ...
Embodiment 2
[0048] Add 14.425g of deionized water and 0.202g of concentrated sulfuric acid to a 250ml three-necked flask, raise the temperature to 50°C, and add 36.4g of MePhSi(OMe) dropwise 2 , the dropwise addition is completed within 0.5h, keep the reaction at 50°C for 1h, then raise the temperature to 70°C, keep the temperature for 2h, then vacuum distill water and by-products, wash with hot water at 60°C for 3 times until neutral, after liquid separation, put Anhydrous Na for organic phase 2 SO 4 Dry and filter with a membrane filtration device at 60°C. The polyvinylidene fluoride microporous membrane has a pore size of 0.8 μm to obtain 25.5 g of a group-terminated methylphenylsiloxane oligomer. 1 Characterized by NMR, number average molecular weight: 1200, viscosity 600mPa·s. 22.9g hydroxyl-terminated methyl phenyl silicone oil, 2.3g epoxy-terminated agent, 1.5g D 4 Vi and 10mg Bu 4 Add 20% methanol solution of NOH into the three-necked flask, react at 95°C for 6h, after the re...
PUM
| Property | Measurement | Unit |
|---|---|---|
| viscosity | aaaaa | aaaaa |
| viscosity | aaaaa | aaaaa |
| porosity | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More