Method for preparing methyl acryloyl o-propyl dimethylchlorosilane

A technology for methacryloyloxypropyl dimethyl chlorosilane and dimethyl chlorosilane is applied in the field of preparing methacryloyloxypropyl dimethyl chlorosilane, and can solve the problem of the temperature rise of the reaction system and the large amount of by-products. , poor selectivity and other problems, to achieve the effect of mild conditions, easy recovery and high selectivity

Inactive Publication Date: 2008-04-09
SHANGHAI CHEM REAGENT RES INST
View PDF1 Cites 12 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The study found that the method reported in this patent still has shortcomings, such as the preparation of the catalyst is cumbersome, it is difficult to recycle and reuse, and the cost is high, especially when the hydrosilylation of olefins is catalyzed, there will be a strong instantaneous heat release, which will easil

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
  • Method for preparing methyl acryloyl o-propyl dimethylchlorosilane
  • Method for preparing methyl acryloyl o-propyl dimethylchlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) SiO 2 The preparation of supported type chloroplatinic acid catalyst: in the reaction vessel with stirring, add 1g hexahydrate chloroplatinic acid respectively, 120ml isopropanol aqueous solution (isopropanol and deionized water are prepared in a volume ratio of 1:5), 75.25g dried SiO 2 Stir well at room temperature, and after standing for 24 hours, evaporate the contained water at 130 ° C to obtain 73.5 g of SiO containing 1% chloroplatinic acid (mass ratio). 2 Supported chloroplatinic acid catalyst.

[0019] (2) Add 12.6g (0.10mol) allyl methacrylate, 0.1g (0.0009mol) hydroquinone and 0.17g SiO to the reactor equipped with reflux condenser, stirrer and thermometer respectively 2 Supported chloroplatinic acid catalyst, introduce nitrogen gas at the same time, under nitrogen atmosphere, heat to 50~53 ℃, slowly add dropwise the mixed solution of 44g allyl methacrylate and dimethyl chlorosilane (allyl methacrylate / Preparation of dimethylchlorosilane mixed solution...

Embodiment 2

[0021] (1) SiO 2 The preparation of the supported chloroplatinic acid catalyst is the same as in Example 1.

[0022] (2) Add 37.8g (0.30mol) allyl methacrylate, 0.1g (0.0009mol) hydroquinone, 0.17g SiO to the reactor equipped with reflux condenser, stirrer and thermometer respectively 2 Supported chloroplatinic acid catalyst, introduce nitrogen at the same time, under nitrogen atmosphere, heat to 50~55 ℃, slowly add dropwise the mixed solution of 44g allyl methacrylate and dimethyl chlorosilane (allyl methacrylate / Preparation of dimethylchlorosilane mixed solution: 25.2g (0.2mol) allyl methacrylate and 18.8g (0.2mol) dimethylchlorosilane are mixed at room temperature in a molar ratio of 1:1 and stirred evenly), Control and maintain the reaction temperature at 60-70°C. Continue to drop 28.4g (0.3mol) dimethyl chlorosilane to react for 2 hours, distill the obtained reaction solution under reduced pressure, collect 116~120°C / 10mm Hg fraction, and obtain 94.8g methacryloxypropy...

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

No PUM Login to view more

Abstract

The invention discloses a preparation method of dimethoxymethylsilyl propyl methacrylate. The method takes the allyl methacrylate as the raw materials, the hydroquinone is taken as the polymerization inhibitor, the reaction is carried out with the dimethylchlorosilane with the presence of the catalyst, and the target product can be obtained by vacuum distillation. The purity of the product can achieve more than 98.5 percent (GC) and the yield is 85 to 90 percent. Compared with the prior art, the invention overcomes the shortcomings of cumbersome preparation of the catalysts, poor selectivity of the reaction and more by-products in the prior art; furthermore, the reaction process of the invention has mild conditions and no reaction solvent, the invention adopts the SiO2 load-type chloroplatinic acid as the catalyst, the selectivity of the catalyst is high, the catalyst is easy to reclaim, so the invention is in line with the requirements of green chemistry and is applicable to the industrialization scale production.

Description

technical field [0001] The invention relates to the field of organic chemical industry, in particular to a method for preparing methacryloyloxypropyl dimethylchlorosilane. Background technique [0002] Methacryloxypropyl dimethyl chlorosilane is a widely used silane coupling agent, especially as a surface treatment for glass fiber, improving the bonding performance of glass fiber and resin, and improving the mechanical properties of composite materials , the effect of enhancing the strength, electrical and waterproof properties of composite materials is very significant. Its structural formula is as follows: [0003] [0004] In the prior art, the preparation method disclosed in European Patent EP 0775708 uses allyl methacrylate as a raw material, n-hexane as a solvent, phenothiazine as a polymerization inhibitor, platinum / 1,3-divinyltetramethyldimethacrylate The complex compound of siloxane is used as a catalyst, reacts with dimethyl chlorosilane, and undergoes vacuum ...

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
IPC IPC(8): C07F7/12
Inventor 黄莹廖本仁蒋旭亮
Owner SHANGHAI CHEM REAGENT RES INST
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap