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Fluoroalkyl alkoxy silane and preparation method thereof

A technology of fluoroalkylalkoxysilane and hydroalkoxysilane, which is applied in the field of organosilicon chemical synthesis, can solve the problems of three wastes, complicated processes, poor product color and luster, etc., and achieves good product quality, low corrosion, Stable effect

Inactive Publication Date: 2015-05-20
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In addition, WO2008017553 and WO2005058919 propose a method for preparing perfluorooctyltrimethoxysilane by reacting perfluorohexyl iodide and vinyltrimethoxysilane. In this method, the yield can reach more than 90%, and the process is relatively complicated, and The color of its products is poor, and there are more three wastes

Method used

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  • Fluoroalkyl alkoxy silane and preparation method thereof
  • Fluoroalkyl alkoxy silane and preparation method thereof
  • Fluoroalkyl alkoxy silane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 0.2g of isopropanol solution of 0.5% Pt-C complex with Pt content and 5g of trimethoxysilane into a 500ml three-necked flask with a stirring and reflux tube, heat at 80°C, and add 73g of trimethoxysilane (0.6mol) dropwise and 223g of 1H, 1H, 2H-perfluoro-1-decene (0.5mol), keep warm for 4 hours after completion, and distill to collect fractions above 100°C to obtain 256g of perfluorodecyltrimethoxysilane, based on 1H, 1H, 2H-perfluoro-1-decene The calculated yield of fluoro-1-decene is 91%.

[0030] The position and assignment of the characteristic absorption peaks in the GC-MS spectrum of perfluorodecyltrimethoxysilane (m / z): 517 (0.25, M-51), 369 (0.55, CF3CF2CF2CF2CF2CF2CF2), 141 (M1, 4625), 121 (100, Si (OCH 3 ) 3 ), 91 (35.45, Si (OCH 3 ) 2 ), 59 (5.85, SiOCH3). 1H NMR spectrum see attached figure figure 1 .

Embodiment 2

[0032] According to the method of Example 1, add 0.2 g of Pt Pt-C complex isopropanol solution, 5 g of triethoxysilane, stir, heat to 100 ° C, drop 82 g of triethoxysilane (0.5 mol) from the dropping funnel and 173g 1H, 1H, 2H-perfluoro-1-octene (0.5mol), stirring for 2 hours after the dropwise addition, cooling and atmospheric pressure distillation to remove low-boiling impurities, and then vacuum distillation to collect fractions above 80°C to obtain perfluorooctane Base triethoxysilane 227g, calculated yield 85% based on trimethoxysilane.

Embodiment 3

[0034] Add the isopropanol solution of 0.4g Pt-C complex 5g methyldimethoxysilane according to the method of Example 1, stir, heat to 60 ℃, from the dropping funnel 53g methyldimethoxysilane (0.5 mol) and 223g of 1H, 1H, 2H-perfluoro-1-decene (0.5mol), after the completion of the heat preservation for 2h, distilled to collect fractions above 100°C to obtain 230g of perfluorodecylmethyldimethoxysilane, based on 1H, The calculated yield of 1H,2H-perfluoro-1-decene is 83.3%.

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Abstract

The invention provides fluoroalkyl alkoxy silane and a preparation method thereof. The fluoroalkyl alkoxy silane has a structural formula (I) as shown in the specification, wherein substituents are defined in the specification. The fluoroalkyl alkoxy silane prepared by the invention has the advantages of good quality, strong stability, high yield of the preparation method, safety and environmental protection.

Description

technical field [0001] The invention belongs to the field of organosilicon chemical synthesis, and relates to a method for preparing fluoroalkylalkoxysilane by hydrosilylation. Background technique [0002] Fluoroalkylsilane can chemically bond with hydroxyl, carboxyl and oxygen-containing groups in many inorganic and organic substrates, forming a self-assembled monomolecular fluorosilicon film layer on the surface of inorganic substances. The treated substrate has extremely low surface energy and poor wettability, and has excellent hydrophobic, oil-repellent and antifouling properties, and is favored by coatings, construction, medicine and other fields. [0003] The method of preparing alkylsilane by hydrosilylation has been documented for a long time and has become an important method for preparing silane. In the early stage, it was mainly aimed at the addition between hydrochlorosilane and unsaturated carbon-carbon bond, and then carried out alcoholysis reaction to produ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 冯锦财陈清蒋云菊鲍樟水
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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