Method for preparing tetramethyl orthosilicate in direct method

A tetramethoxysilane, direct method technology, applied in the direction of silicon organic compounds, etc., can solve the problems of atmospheric environmental pollution, complex rectification and purification, complicated operation, etc., and achieves the effect of large contact surface, favorable reaction and low price.

Inactive Publication Date: 2017-09-29
JIANGSU UNIV
View PDF3 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional method of preparing tetramethoxysilane, due to the direct liquid phase reaction of silicon tetrachloride and methanol, produces hydrogen chloride gas, which causes great pollution to the atmospheric environment an

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
  • Method for preparing tetramethyl orthosilicate in direct method
  • Method for preparing tetramethyl orthosilicate in direct method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 40g of silicon powder and 3.2g of Cu on an electronic balance 2 O, mix, stir evenly, pour into pulverizer and pulverize, pulverize time 1min. Take 30mL of pulverized silicon powder and cuprous oxide and pour it into a fixed bed reactor, combine the fixed bed reactor, and place it in a circulating tube furnace. Nitrogen was introduced into the fixed bed reactor with a nitrogen flow rate of 15mL / min. The temperature program was started, with an initial temperature of 15°C and a final temperature of 240°C. The heating time was 1h, and the temperature was maintained at 240°C for 4h. Then, switch to methanol, methanol flow rate 0.1mL / min, first react for 0.5h, then start timing, react at 220°C for 1h, take samples with a centrifuge tube, and perform detection on a gas chromatograph. Calculate the conversion of methanol and the selectivity of tetramethoxysilane. Experimental results such as figure 1 .

Embodiment 2

[0033] Weigh 40g of silicon powder and 3.2g of Cu on an electronic balance 2 O, mix, stir evenly, pour into pulverizer and pulverize, pulverize time 1min. Take 30mL of pulverized silicon powder and cuprous oxide and pour it into a fixed bed reactor, combine the fixed bed reactor, and place it in a circulating tube furnace. Nitrogen was introduced into the fixed bed reactor with a nitrogen flow rate of 15mL / min. The temperature program was started, with an initial temperature of 15°C and a final temperature of 240°C. The heating time was 1h, and the temperature was maintained at 240°C for 4h. Then, switch to methanol, methanol flow rate 0.1mL / min, react for 0.5h first, then start timing, react at 240°C for 1h each, take samples with a centrifuge tube, and perform detection on a gas chromatograph. Calculate the conversion of methanol and the selectivity of tetramethoxysilane. Experimental results such as figure 1 .

Embodiment 3

[0035] Weigh 40g of silicon powder and 3.2g of Cu on an electronic balance 2 O, mix, stir evenly, pour into pulverizer and pulverize, pulverize time 1min. Take 30mL of pulverized silicon powder and cuprous oxide and pour it into a fixed bed reactor, combine the fixed bed reactor, and place it in a circulating tube furnace. Nitrogen was introduced into the fixed bed reactor with a nitrogen flow rate of 15mL / min. The temperature program was started, with an initial temperature of 15°C and a final temperature of 240°C. The heating time was 1h, and the temperature was maintained at 240°C for 4h. Then, switch to methanol, methanol flow rate 0.1mL / min, first react for 0.5h, then start timing, react at 260°C for 1h each, take samples with a centrifuge tube, and perform detection on a gas chromatograph. Calculate the conversion of methanol and the selectivity of tetramethoxysilane. Experimental results such as figure 1 .

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 provides a method for preparing tetramethyl orthosilicate in a direct method. The method comprises the following steps: (1) measuring silicon powder and catalyst, mixing and uniformly stirring, and then crushing in a crushing machine; (2) pouring the crushed silicon and catalyst mixture into a fixed-bed reactor, assembling an apparatus, and placing the reactor apparatus into a tubular heating furnace; (3) introducing nitrogen into the fixed-bed reactor, heating the tubular furnace by virtue of a program, heating to 240 DEG C, and processing for 2h at 240 DEG C; and (4) lowering the temperature in the fixed-bed reactor to 220 DEG C, beginning the introduction of methanol, performing the reaction timing in 0.5h, performing the reaction, wherein a reaction product is the tetramethyl orthosilicate. The raw materials adopted in the method are silicon powder and methanol and are synthesized to form the tetramethyl orthosilicate in one step. Compared with the traditional method, the method is more environment-friendly and green. No harmful gas hydrogen chloride is produced in the product.

Description

technical field [0001] The invention relates to the fields of organic chemistry and catalytic chemistry, in particular to a method for preparing tetramethoxysilane by a direct method. Background technique [0002] Tetramethoxysilane is tetramethoxysilane, which can be used as an insulating material in the fields of organic silicon synthesis, heat-resistant paint manufacturing, adhesives, electronics industry, etc. It is also an important raw material for optical glass treatment agents and coagulants. Therefore, its synthesis has always been concerned by the chemical industry. [0003] The traditional synthesis method is to react silicon tetrachloride and methanol directly in liquid phase, and control the reaction speed by controlling the ratio of silicon tetrachloride and methanol. The produced tetramethoxysilane needs to be further purified by distillation to achieve More than 99% purity. This traditional synthesis method of tetramethoxysilane is divided into two operatio...

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): C07F7/04
CPCC07F7/04
Inventor 张明明王爱丽殷恒波
Owner JIANGSU UNIV
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