Preparation method of 3-(phenyl amino) propyl alkoxy silane, and recycling technology of by-product

A technology of propylalkoxysilane and chloropropylalkoxysilane, which is applied in the field of organic chemistry, can solve the problems of high production cost, no reuse of by-products, and the inability of ordinary silane coupling agents to meet the needs of special industries. To achieve the effect of reducing production costs and solving environmental problems

Active Publication Date: 2012-11-14
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a simple preparation method with low cost to solve the problem that the existing common silane coupling agent cannot meet the needs of special industries, and the by-products produced in the preparation of the

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 1000ml reaction vessel equipped with heating, stirring, and refluxing devices, add 465.5g of aniline liquid, and heat up to 130℃ at a stirring speed of 90rpm, and then add 198.7g of 3-chloropropyltrimethoxysilane Add dropwise to the container within 2 hours through a constant pressure dropping funnel. After the addition, continue to keep the temperature at 130℃ and react for 2 hours, then cool to room temperature and filter to filter out the by-product aniline hydrochloride produced by the reaction. . The filtrate was introduced into a distillation flask, and the filtrate was distilled at a pressure of -0.1Mpa and a temperature of 120°C to obtain 264.5 g of aniline; then the filtrate was continued to heat up and distilled again under the conditions of a pressure of -0.1Mpa and a temperature of 150°C to obtain 3 -229.1 grams of 3-(phenylamino)propyltrimethoxysilane in (phenylamino)propylalkoxysilane. The appearance of 3-(phenylamino)propyltrimethoxysilane is a color...

Embodiment 2

[0026] In a 1000ml reaction vessel equipped with heating, stirring, and refluxing devices, add 465.5g of aniline liquid, and heat up to 130℃ at a stirring speed of 90 rpm, and then 240.5g of 3-chloropropyltriethoxysilane Add dropwise to the container within 2 hours through a constant pressure dropping funnel. After the addition, continue to keep the temperature at 130℃ and react for 2 hours, then cool to room temperature and filter to filter out the by-product aniline hydrochloride produced by the reaction. . The filtrate was introduced into a distillation flask, and the filtrate was distilled at a pressure of -0.1Mpa and a temperature of 120°C to obtain 266.3 grams of aniline; then the filtrate was continued to heat up and distilled again at a pressure of -0.1Mpa and a temperature of 170°C to obtain 255.5 grams of 3-(phenylamino)propyltriethoxysilane product in 3-(phenylamino)propylalkoxysilane. The appearance of the 3-(phenylamino)propyltriethoxysilane product is a slightly ...

Embodiment 3

[0029] In a 1000ml reaction vessel equipped with heating, stirring and refluxing devices, add 465.5g of aniline liquid, heat up to 125℃ at a stirring speed of 90rpm, and then add 182.7g of 3-chloropropylmethyldimethoxy Silane was added dropwise to the container within 2 hours through the constant pressure dropping funnel. After the addition, the temperature was kept at 125°C and reacted for 2 hours, then cooled to room temperature and filtered to filter out the by-product aniline hydrochloric acid. salt. The filtrate was introduced into a distillation flask, and the filtrate was distilled at a pressure of -0.1Mpa and a temperature of 120°C to obtain 264.2 g of aniline; then the filtrate was continued to heat up and distilled again under the conditions of a pressure of -0.1Mpa and a temperature of 150°C to obtain 218.2 grams of 3-(phenylamino)propylmethyldimethoxysilane in 3-(phenylamino)propylalkoxysilane. The appearance of the 3-(phenylamino)propylmethyldimethoxysilane produc...

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Abstract

The invention relates to a preparation method of 3-(phenyl amino) propyl alkoxy silane, and recycling technology of a by-product, belonging to the technical field of organic chemistry. The preparation method comprises the steps of: using aniline and 3-chlorine propyl alkoxy silane for carrying out ammonolysis reaction to generate the solid of 3-(phenyl amino) propyl alkoxy silane and aniline hydrochloride; filtering the aniline hydrochloride; and distilling filtrate to obtain the 3-(phenyl amino) propyl alkoxy silane product, wherein the 3-(phenyl amino) propyl alkoxy silane product contains phenyl, amino, alkoxy or methyl, can provide and improve special functional properties for polyurethane material, adhesive, and reinforced phenolic composite material. The invention can be used for neutralizing treatment of the by-product aniline hydrochloride, so that the environmental pollution can be avoided, and the industrial wastewater directly enters a sewage treatment system; furthermore, aniline can be recovered and recycled, so that the production cost is reduced.

Description

Technical field [0001] The invention relates to a process for the preparation of 3-(phenylamino)propyl alkoxysilane and the recycling of by-products, belonging to the technical field of organic chemistry. Background technique [0002] Silane coupling agent is a chemical product with a wide range of industrial uses. It is used in coatings, rubber, textile, glass fiber, ceramics, electronics, medical materials, construction, etc., and is known as industrial monosodium glutamate. With the development of the chemical industry, ordinary silane coupling agents can no longer meet the needs of some special industries, such as polyurethane, epoxy, acrylic, phenolic and glass, metal, glass fiber, inorganic filler adhesion promoters; adhesives, sealing Glue, coating, glass fiber sizing agent and surface treatment agent, primer treatment agent and casting sand binder; improve the high temperature aging performance of glass fiber reinforced phenolic composites. At present, customers need to ...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07C211/46C07C209/86
Inventor 胡江华秦传俊刘宇阮少阳王灿汤艳甘俊陈圣云
Owner JINGZHOU JIANGHAN FINE CHEM
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