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Method for preparing naphthyl alkoxy silane monomers

A technology of naphthylalkoxysilane and alkoxysilane, which is applied in the field of preparation of naphthylalkoxysilane monomers, can solve the problems of a large number of high-cost solvents and environmental pollution, and achieve the reduction of solvent consumption and evaporation cost , Conducive to the effect of cleaner production

Active Publication Date: 2016-12-07
JIUJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inventors found that the synthesis methods used in patents WO2013 / 005858 and CN104788488A need to use a large amount of high-cost solvents and reactants such as magnesium, which may cause potential environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Synthesis and Purification of Naphthyltrimethoxysilane

[0022] 1) Synthesis of naphthyltrimethoxysilane: add 8.2g (0.36mol) sodium flakes, 100ml tetramethoxy Heat the silane to 70°C; keep the temperature at 70°C, add 25ml of 1-bromonaphthalene to the constant pressure dropping funnel, and slowly drop it into the four-neck bottle, control the dropping speed, after dropping, raise the temperature to 80°C for 2 hours ; Cool down to 50°C. 8.3ml of tetrachlorosilane was added dropwise, stirred and refluxed, and the reaction temperature was controlled not to exceed 80°C. The reddish-brown crude product was filtered by suction. The reddish-brown crude product was distilled to remove the remaining tetramethoxysilane under normal pressure, then distilled under reduced pressure, and the fraction at 130-135°C was collected at 5 mmHg to obtain 25 g of the crude product of naphthyltrimethoxysilane.

[0023] 2) Purification of naphthyltrimethoxysilane: Add 20 g of the crude produ...

Embodiment 2

[0025] Synthesis and Purification of Naphthylmethyldimethoxysilane

[0026] 1) Synthesis of naphthylmethyldimethoxysilane: Add 8.2g of sodium flakes and 100ml of methyltrimethoxysilane to a four-neck flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel and a spherical condenser And heat to 75°C; keep the temperature at 75°C, add 25ml of 1-bromonaphthalene into the constant pressure dropping funnel, and slowly drop it into the four-necked bottle, control the dropping speed, after the drop, raise the temperature to 80°C for 1 hour ; Cool down to 50°C. 8.3ml of tetrachlorosilane was added dropwise, stirred and refluxed, and the reaction temperature was controlled not to exceed 80°C. The reddish-brown crude product was filtered by suction. Then filter the mixed solution obtained after the reaction, and distill the resulting solution under normal pressure to remove the remaining methyltrimethoxysilane, distill under reduced pressure, collec...

Embodiment 3

[0029] Synthesis and Purification of Naphthyltriethoxysilane

[0030] 1) Synthesis of naphthyltriethoxysilane: Add 8.2g of sodium flakes and 100ml of tetraethoxysilane to a 1L four-neck flask equipped with a mechanical stirrer, a thermometer, a constant pressure dropping funnel and a spherical condenser and heat to 70°C; keep the temperature at 70°C, add 25ml of 1-bromonaphthalene into the constant pressure dropping funnel, and slowly drop it into the four-neck bottle, control the dropping speed, after the drop, raise the temperature to 70°C for 2 hours; 8.3ml of tetrachlorosilane was added dropwise, stirred and refluxed, and the reaction temperature was controlled not to exceed 80°C. Then filter the mixed liquid obtained after the reaction, and distill the resulting liquid under normal pressure to remove the remaining tetraethoxysilane, distill under reduced pressure, collect 150-135 ° C fractions at 5 mmHg to obtain naphthyl triethoxysilane The crude product is 30g.

[0031]...

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PUM

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Abstract

The invention relates to a method for preparing naphthyl alkoxy silane monomers. The method comprises the following step: mixing alkoxy silane, sodium and 1-naphthalene halide to be reacted to obtain naphthyl alkoxy silane in an organic solvent, wherein the alkoxy silane is selected any one of tetramethoxysilane, methyltrimethoxysilane, tetraethoxysilane and methyl triethoxysilane. The method is easy to operate.

Description

technical field [0001] The invention relates to a preparation method of a naphthylalkoxysilane monomer, and specifically belongs to the technical field of organosilicon materials. Background technique [0002] Semiconductor lighting based on light-emitting diodes (LEDs) has the characteristics of high light efficiency and long life, and has become the fourth generation of lighting sources. The aging resistance of packaging materials has a very important impact on the light efficiency and service life of LED lighting devices. In the past few decades, epoxy resin has been widely used as an LED packaging material due to its good mechanical properties, high transparency, and low cost. However, with the continuous improvement of people's requirements for LED power and brightness, traditional epoxy resin packaging materials can no longer meet the requirements of power LEDs in terms of aging resistance. For example, epoxy resin is prone to yellowing and light transmittance decr...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1876
Inventor 彭游尹健美其他发明人请求不公开姓名
Owner JIUJIANG UNIVERSITY
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