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Method for preparing methyl acryloyl o-propyl dimethylchlorosilane

A technology of methacryloxypropyl dimethyl chlorosilane and dimethyl chlorosilane, which is applied in the field of preparation of methacryloxypropyl dimethyl chlorosilane, can solve the problem of temperature rise in the reaction system and many by-products , poor selectivity and other problems, to achieve the effect of mild conditions, high selectivity and easy recovery

Inactive Publication Date: 2011-05-04
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 easily lead to a rapid rise in the temperature of the reaction system, causing the raw material The side reaction of self-polymerization of allyl methacrylate and the self-polymerization of the target product, which leads to poor selectivity of the reaction and many by-products, has no value for popularization and application

Method used

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  • Method for preparing methyl acryloyl o-propyl dimethylchlorosilane
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Experimental program
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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...

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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

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 黄莹廖本仁蒋旭亮
Owner SHANGHAI CHEM REAGENT RES INST