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Method for preparing 3-(methacryloxy)propyltrimethoxysilane

A technology of propyltrimethoxysilane and methacryloxy, which is applied in the field of preparation of 3-propyltrimethoxysilane, can solve the problem of high performance of polymerization inhibitors and poor polymerization inhibition effect of polymerization inhibitors. Ideal, it is difficult to achieve the effect of polymerization inhibition, etc., to achieve the effect of reducing cost and production risk, easy to remove color, exothermic temperature and easy to control

Active Publication Date: 2008-02-13
湖北武大有机硅新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since this reaction itself is an exothermic reaction, it has high requirements on the polymerization inhibition performance of the polymerization inhibitor, and the polymerization inhibition effect of the polymerization inhibitor is not ideal, and the reaction is easy to gel
Some of the above documents use one of the above inhibitors or simply share several inhibitors together, and some use inhibitors with very complex structures, and the dosage is relatively large, and it is difficult to achieve ideal Polymerization effect, especially in the distillation process, it is easy to stick, which increases the production risk and increases the cost

Method used

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  • Method for preparing 3-(methacryloxy)propyltrimethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Preparation of catalyst: Using chloroplatinic acid, isopropanol, and compound A as raw materials, add compound A after dissolving chloroplatinic acid in isopropanol, and then heat to 65-85° C. for 1-3 hours to obtain liquid catalyst. The mass ratio of chloroplatinic acid, isopropanol and compound A is: 1:70~75:20~25.

[0018] The compound A is tetramethyldivinyldisiloxane or 1,3,5,7-tetramethyltetravinylcyclotetrasiloxane or 1,4-cyclooctadiene or 1,5-cyclo One of octadiene or acetylacetone or 2,5-dimethyl-2,4-hexadiene.

Embodiment 2

[0019] Embodiment 2: target product is synthesized

[0020] The reaction formula is as follows:

[0021]

[0022] In the reactor, add 85 grams to 330 kilograms of trimethoxysilane, and then add 0.0005 to 0.001 times the amount of catalyst (prepared in the embodiment), 0.0005 to 0.001 times the amount of polymerization inhibitor phenothiazine and 0.0005 to 0.001 times the amount of polymerization inhibitor ZJ-701, the temperature is raised to 70 to 85 ° C, and the methacrylic acid alkene mixed with 0.0005 to 0.001 times the amount of polymerization inhibitor N, N'-diphenyl-p-phenylenediamine is added dropwise. Propyl ester is added dropwise within 10 minutes to 3 hours. After the dropwise addition, keep warm at 85-95° C. for 2-3 hours. The product content in the reactant is 85-88% according to sampling analysis.

[0023] Add 0.0005-0.001 times the amount of polymerization inhibitor ZJ-701 and 0.001-0.002 times the amount of polymerization inhibitor ZJ-101 to the above react...

Embodiment 3

[0024] Embodiment 3: the preparation of novel catalyst: with 0.1g chloroplatinic acid (H 6 PtCl 6 ·6H 2 O) Add 7.5ml of isopropanol, after the chloroplatinic acid is completely dissolved, add 2.5ml of tetramethyldivinyldisiloxane or acetylacetone, and then heat to 65-85°C for 1 hour to prepare a liquid catalyst (number 1).

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Abstract

The invention discloses a preparation method of the 3-(methacryloyl oxygen) propyl tri-methoxy silane. The steps are: first the platinum chloride acid, isopropanol and the compound A are used as the raw materials; the platinum chloride acid is added into the isopropyl alcohol; after the dissolution, the compound A is added and then to be heated; secondly, the polymerization-preventing reagent phenothiazine and ZJ-701 are added into the tri-methoxy silane to dissolve the raw material X; thirdly, the polymerization-preventing reagent N, N'-drophenyl-p-phenylenediamine are added in the methacrylate allylic ester to dissolve the raw material Y; fourthly, the polymerization-preventing reagent ZJ-701 and ZJ-101 are added in the reaction materials after the reaction between the raw materials and the catalysts to dissolve to get the 3-(methacryloyl oxygen) propyl tri-methoxy silane. The invention is of the simple preparation, the high efficiency, the little consumption, the strong selectivity, and the high collection rate of the products; the polymerization-preventing effects of the polymerization-preventing technology are good; the polymerization-preventing reagents are not easy to be gelated; the consumption is little; the polymerization-preventing reagents are easily separated from the products; the products are easy to be decolorized, good in quality, and have no harm to the catalyst.

Description

technical field [0001] The invention relates to a preparation method of 3-(methacryloxy)propyltrimethoxysilane. Including the preparation of new catalysts and the application of compound inhibition technology. The catalyst and polymerization inhibition technology are suitable for a series of hydrosilylation reactions using hydrogen-containing siloxane and allyl methacrylate or unsaturated esters with similar structures as raw materials. Background technique [0002] 3-(Methacryloyloxy)propyltrimethoxysilane is a widely used organosilane coupling agent. It is mainly used as a tackifier for resins and polymeric materials; synthetic methacryloyloxyhydrocarbyl silicone oil; room temperature curing acrylic coatings and crosslinking agents for polyolefin methods; copolymerized with methyl methacrylate to make contact lenses; also used as Improve the hydrophobicity of insulating oil and fiber optic coatings and improve the mechanical properties of polyester concrete. [0003] Ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 廖俊董鹏杨金玉陈圣云何运凡刘巧云程鹏飞高胜波梁晶丁强张先亮张治民
Owner 湖北武大有机硅新材料股份有限公司
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