Preparation method, purification method and stabilization method in composition for acryloxy alkyl alkoxy silane, and application of the same
A technology of acryloyloxyalkylalkoxysilane and acryloyloxypropyl, used in the preparation of acryloyloxyalkylalkoxysilane, its purification, stabilization in compositions and its application fields , can solve the problem of unstable storage and so on
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 11
[0133] 86 g (1 mol) of methacrylic acid were neutralized with 280 g of a 25% potassium methacrylate solution in methanol under stirring. Then add 0.6 g of N, N'-diphenyl-p-phenylenediamine, 2.8 g (0.009 mol) of 1-(2'-ethyl-hexyl)-4-dimethyl Amino-pyridinium chloride and 198.5 g (1 mol) of 3-chloropropyltrimethoxysilane and the methanol was distilled off. The reaction mixture was kept at 125°C for 1.5 hours and after cooling the KCl formed was filtered. KCl was washed with methanol. Methanol was distilled off from the combined filtrates and the residue was distilled under reduced pressure.
[0134] 230 g of 3-methacryloxypropyltrimethoxysilane with a boiling point of 82° C. (0.4 mbar) were obtained, corresponding to a yield of 92.7%, based on the methacrylic acid used. The purity is 98.5%. Only traces of 4-dimethylaminopyridine and 0.01% of 2-ethylhexyl methacrylate could be detected in gas chromatography.
Embodiment 12
[0136] Make 110.2g (1mol) of potassium acrylate and 198.5g (1mol) of 3-chloropropyltrimethoxysilane, 2.8g (0.01mol) of 1-neopentyl-4-(4'-methyl-piper Pyridyl)-pyridinium chloride Mix with 0.3 g of N,N'-diphenyl-p-phenylenediamine and heat to 128°C with stirring. After 2 hours it was cooled and the KCl formed as a by-product was filtered. KCl was washed with 50 g methanol. Methanol was distilled off from the combined filtrates and the residue was distilled off under reduced pressure, whereby 108.5 g of 3-acryloyloxypropyltrimethoxysilane with a boiling point of 80° C. (0.5 mbar) were obtained. The yield was 92.7% based on the potassium acrylate used. The purity is 98.8%. Only traces of neopentyl acrylate and 4-(4'-methyl-piperidinyl)-pyridine could be detected in gas chromatography.
Embodiment 13
[0138] Make 54g (0.5mol) of sodium methacrylate and 99.3g (0.5mol) of 3-chloropropyltrimethoxysilane, 1.6g (0.006mol) of 1-(2'-ethylhexyl)-4- Dimethylamino-pyridinium chloride Mix with 0.4 g of N,N'-diphenyl-p-phenylenediamine and heat to 120°C for 1.5 hours with stirring. Sodium chloride formed as a by-product was filtered off and washed with 80 g of methanol. Methanol was distilled off from the combined filtrates and the residue was distilled off under reduced pressure, whereby 112 g of 3-methacryloxypropyltrimethoxysilane with a boiling point of 82° C. (0.4 mbar) were obtained. The yield was 90.3% based on the sodium methacrylate used. The purity is 98.5%. Only traces of 2-ethylhexyl acrylate and 4-dimethylaminopyridine could be detected in gas chromatography.
PUM
| Property | Measurement | Unit |
|---|---|---|
| Boiling point | aaaaa | aaaaa |
| Melting point | aaaaa | aaaaa |
| Melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More