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Preparation method of methacryloyloxypropyltriacetoxysilane

A technology of methacryloxypropyltriacetoxysilane and methacryloxypropyltrimethoxysilane, which is applied in the field of preparation of methacryloxypropyltriacetoxysilane and can solve industrial problems Difficult production, long synthetic process route, easy cross-linking and polymerization, etc., to achieve the effects of easy storage and transportation, reduced reaction time, and high yield

Pending Publication Date: 2022-04-12
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Usually, there are two synthetic methods of methacryloyloxypropyltriacetoxysilane, one is the addition-acylation method, that is, allyl methacrylate and trichlorosilane are first obtained by hydrosilylation Methacryloyloxypropyl trichlorosilane is synthesized by acylation reaction with glacial acetic acid or acetic anhydride. It is easy to cross-link and solidify, so industrial production is difficult; another synthesis method is the acylation-condensation method, that is, chloropropyl trichlorosilane is acylated with glacial acetic acid or acetic anhydride to obtain chloropropyl triacetoxysilane , and then prepared by condensation reaction with sodium methacrylate, this method also has the problems of long process route and prone to cross-linking polymerization

Method used

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  • Preparation method of methacryloyloxypropyltriacetoxysilane
  • Preparation method of methacryloyloxypropyltriacetoxysilane

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Embodiment 1

[0050] A method for preparing methacryloxypropyltriacetoxysilane provided in the embodiment of the present invention comprises:

[0051] Step S1, add 200 g (0.80 mol) of methacryloxypropyltrimethoxysilane, 2,6-di 0.25 g of tert-butyl-p-cresol, 0.30 g of ytterbium trifluoromethanesulfonate, and 250 g (2.45 mol) of acetic anhydride were weighed and added to the dropping funnel to wait for dropwise addition. Turn on the stirring and oil bath heating device, and when the temperature of the system rises to 80°C, turn on the vacuum pump, and start to add acetic anhydride slowly and uniformly under the negative pressure condition of vacuum degree -0.02MPa, and the dropping time is controlled at 2h; , heat up to 100°C, continue to age for 2 hours, and at the same time, distill all the by-product methyl acetate to collect;

[0052] Step S2, after the aging is completed, distill out the residual acetic anhydride in the system at a temperature of 75°C and a pressure of -0.098MPa;

[00...

Embodiment 2

[0056] A method for preparing methacryloxypropyltriacetoxysilane provided in the embodiment of the present invention comprises:

[0057] Step S1. Add 400 g (1.61 mol) of methacryloxypropyl trimethoxysilane, 2,6-di-tert-tert 0.50 g of butyl-p-cresol, 0.46 g of ytterbium trifluoromethanesulfonate, and 510 g (5.00 mol) of acetic anhydride were weighed and added to the dropping funnel to wait for dropwise addition. Turn on the stirring and oil bath heating device, and when the temperature of the system rises to 85°C, turn on the vacuum pump, and start to add acetic anhydride slowly and uniformly under the negative pressure condition of vacuum degree -0.03MPa, and the dropping time is controlled at 2.5h; the dropping is completed Afterwards, raise the temperature to 105°C, continue to age for 2.5 hours, and at the same time distill all the by-product methyl acetate to collect;

[0058] Step S2, after the aging is completed, distill out the residual acetic anhydride in the system a...

Embodiment 3

[0062] A method for preparing methacryloxypropyltriacetoxysilane provided in the embodiment of the present invention comprises:

[0063] Step S1. Add 400 g (1.61 mol) of methacryloxypropyltrimethoxysilane, 2-tert-butyl p- 0.50 g of hydroquinone, 0.50 g of lanthanum trifluoromethanesulfonate, weighed 510 g (5.00 mol) of acetic anhydride, added them to the dropping funnel and waited for dropwise addition. Turn on the stirring and oil bath heating device, and when the temperature of the system rises to 75°C, turn on the vacuum pump, and start to add acetic anhydride slowly and uniformly under the negative pressure condition of vacuum degree -0.04MPa, and the dropping time is controlled at 2.5h; the dropping is completed After that, raise the temperature to 95°C, continue to age for 2.5 hours, and at the same time, distill all the by-product methyl acetate to collect;

[0064] Step S2, after the aging is completed, distill out the residual acetic anhydride in the system at a temp...

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Abstract

The invention provides a preparation method of methacryloyloxypropyltriacetoxysilane, which comprises the following steps: uniformly mixing methacryloyloxypropyltrimethoxysilane, a polymerization inhibitor and a catalyst, adding acetic anhydride, and carrying out acyloxy exchange reaction under the conditions of stirring, heating and micro-negative pressure to obtain a reaction product; carrying out reduced pressure distillation on the reaction product to remove and recover residual acetic anhydride so as to obtain a crude product; and adding activated carbon into the crude product to adsorb the residual catalyst, and then filtering to obtain the methacryloyloxypropyltriacetoxysilane. According to the method, acetic anhydride reacts with methacryloyloxypropyltrimethoxysilane, acetoxyl is used for replacing methoxyl, the substituted methoxyl reacts with acetic anhydride to generate methyl acetate, the methyl acetate continuously overflows through micro-negative pressure under the low-temperature condition, the reaction continuously moves rightwards, the reaction speed is increased, the reaction time is shortened, and the yield of methyl acetate is increased. The thermosensitive polymerization is completely avoided; and the product has the advantages of high yield, high content, safety and environmental protection.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, and more specifically, to a preparation method of methacryloyloxypropyltriacetoxysilane. Background technique [0002] UV curing adhesive has the advantages of fast curing, less energy consumption, and no solvent pollution. It is a new type of energy-saving and environmentally friendly adhesive. The curing principle is that the photoinitiator forms excited state molecules under ultraviolet light irradiation, decomposes into free radicals, and makes unsaturated organic compounds undergo chemical reactions such as polymerization, grafting, and crosslinking to achieve the purpose of curing. UV curing adhesives are mainly composed of photoinitiators, reactive diluents, prepolymers and adhesion promoters, among which acrylate compounds containing conjugated double bonds are an important part of UV curing adhesives. Methacryloyloxypropyltriacetoxysilane has the ability to cross-link with UV res...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07C67/11C07C69/14
CPCY02P20/584
Inventor 文少卿胡江华甘俊甘书官陈圣云
Owner JINGZHOU JIANGHAN FINE CHEM