Preparation process of trimethylethoxysilane

A technology for the preparation of trimethylethoxysilane and its preparation process, which is applied in the field of preparation of trimethylethoxysilane, and can solve the problems of increased by-products and waste residues, increased addition of neutralizing agents, and increased waste residues generated. , to achieve the effect of improved distillation yield, easy control and reduced investment

Inactive Publication Date: 2012-10-10
XINYAQIANG SILICON CHEM JIANGSU
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The biggest problem of the traditional preparation process is that there are side reactions in the reaction process, and water is produced after the side reactions occur, so that the raw materials (or products) are hydrolyzed to form linear organosiloxanes
At the same time, because there is a large amount of hydrogen chloride in the system, it is not easy to remove, and the occurrence of side reactions is promoted at a certain temperature, resulting in a vicious circle.
In addition, due to the large amount of hydrogen chloride contained in the system, the amount of neutralizing agent added increases, and the amount of waste residue generated also increases. As a result, the operation is difficult to control, the process flow is long, the product yield is greatly reduced, and by-products and waste residues increase.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation process of trimethylethoxysilane
  • Preparation process of trimethylethoxysilane
  • Preparation process of trimethylethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: As shown in the figure, the preparation process steps of trimethylethoxysilane are:

[0033] 1. Response: First, to 1m 3 Put 700kg of trimethylchlorosilane and 450kg of urea into the enamel stirred tank, mix and stir; then add 400kg of ethanol dropwise into the stirred tank, and the dropwise addition is completed within two hours. Or the method of jacket cold water cooling is controlled below 60 °C; the hydrogen chloride gas that has not reacted with urea is absorbed by water through the falling film absorber; after the reaction is completed, stop stirring, keep the layers for 20 minutes, release the acidic liquid at the bottom, and remove the crude product from the upper layer Import the neutralization kettle.

[0034] 2. Neutralization: Analyze the content of trimethylethoxysilane and hydrogen chloride before neutralization to determine the amount of neutralizing agent. The neutralizing agent is potassium alkoxide, sodium alkoxide or alkaline earth meta...

Embodiment 2

[0037] Embodiment two: as shown in the figure, the preparation process steps of trimethylethoxysilane are:

[0038] 1. Response: First, to 1m 3 Put 700kg of trimethylchlorosilane and 450kg of urea into the enamel stirred tank, mix and stir; then add 410kg of ethanol dropwise into the stirred tank, and the dropwise addition is completed within two hours. Below ℃, the temperature is controlled below 60℃ by means of dropping speed or cooling with jacketed cold water; the hydrogen chloride gas that has not reacted with urea is absorbed by water through the falling film absorber; after the reaction is over, stop stirring, keep the stratification for 60 minutes, and release the bottom Acidic liquid, the crude product of the upper layer is introduced into the neutralization tank.

[0039] 2. Neutralization: Analyze the content of trimethylethoxysilane and hydrogen chloride before neutralization to determine the amount of neutralizing agent. The neutralizing agent is potassium alkoxi...

Embodiment 3

[0042] Embodiment three: as shown in the figure, the preparation process steps of trimethylethoxysilane are:

[0043] 1. Response: First, to 1m 3 Put 700kg of trimethylchlorosilane and 450kg of urea into the enamel stirred tank, mix and stir; then add 430kg of ethanol dropwise into the stirred tank, and the dropwise addition is completed within two hours. Below ℃, the temperature is controlled below 60℃ by way of dropping speed or cooling with jacketed cold water; the hydrogen chloride gas that has not reacted with urea is absorbed by water through the falling film absorber; after the reaction is over, stop stirring, keep the stratification for 45 minutes, and release the bottom Acidic liquid, the crude product of the upper layer is introduced into the neutralization tank.

[0044] 2. Neutralization: analyze the content of trimethylethoxysilane and hydrogen chloride before neutralization to determine the amount of neutralizing agent. The neutralizing agent is potassium alkoxi...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a preparation process of trimethylethoxysilane, which comprises the following specific steps of: (1) reaction: firstly adding 14 parts of trimethylchlorosilane and 9 parts of urea in a stirring kettle, mixing and agitating; then dropwise adding 8-9 parts of ethanol into the stirring kettle, finishing adding within 2 hours, stop agitating after reaction, standing and layering for 20-60 minutes, discharging bottom acid liquid and introducing an upper coarse product into a neutralization kettle; (2) neutralization: terminating the neutralization reaction when a system is neutral or alkalescent; standing and settling after reaction, rectifying supernatant liquor, uniformly filtering a lower sediment after accumulation, rectifying generated liquid and recovering solid residues; (3) rectification: adding the supernatant liquor into a rectifying tower kettle to produce the trimethylethoxysilane. The preparation method has the beneficial effects that the reaction can be carried out at a normal temperature, so that the concentration of the hydrogen chloride in the system is reduced, and the generation of secondary reaction is avoided; and the rectification yield is greatly improved, and the production cost is reduced.

Description

technical field [0001] The invention relates to a preparation process of trimethylethoxysilane. Background technique [0002] The traditional preparation process of trimethylethoxysilane adopts the direct alcoholysis fatification method, that is, under the condition of heating and vaporization, ethanol directly reacts with trimethylchlorosilane (or adopts double-tower fatification, that is, adopts two-stage reaction, different lipidation temperature), after the product is condensed, add a neutralizing agent to remove the hydrogen chloride, and at the same time make the unreacted ones continue to react completely, filter to remove the slag, and the liquid is rectified to obtain the product. [0003] The biggest problem of the traditional preparation process is that there are side reactions in the reaction process, and water is generated after the side reactions occur, so that the raw materials (or products) are hydrolyzed to form linear organosiloxanes. Simultaneously, becau...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07F7/18
Inventor 初亚军
Owner XINYAQIANG SILICON CHEM JIANGSU
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap