Supercharge Your Innovation With Domain-Expert AI Agents!

Method for preparing trichlorosilane by virtue of silicon tetrachloride liquid-phase cold hydrogenation in ionic liquid medium

A technology of silicon tetrachloride liquid and ionic liquid, which is applied in the direction of silicon halide compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., which can solve the problem of difficult batch storage and transportation, and difficult separation and recovery of catalysts , equipment is easy to block and wear, etc., to achieve the effect of reducing preparation cost, lowering temperature and pressure, and strong dissolving ability

Inactive Publication Date: 2015-05-06
HENAN UNIV OF SCI & TECH
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silicon tetrachloride is a liquid under normal pressure, with a low boiling point, easy to vaporize and deliquescent, highly corrosive and toxic, and difficult to store and transport in batches
Although several catalyst solutions suitable for cold hydrogenation have been proposed at home and abroad, mainly nickel-based catalysts, these catalysts themselves or the catalytic process still have high temperature pre-activation, high cost, low conversion rate, and easy blockage of equipment and wear, catalysts are difficult to separate and recycle, etc.

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Take 100g of silicon powder and 100g of catalyst respectively, put them into different corundum porcelain boats, and spread them evenly to 0.5mm. Pressurized hydrogen, activation pretreatment at constant temperature and pressure for 2 hours;

[0042] In a vacuum glove box, take 10g of silicon powder and 0.1g of catalyst and add it to a 500ml volume autoclave, then add 50g of 1-butyl-3-methylimidazole bis-trifluoromethanesulfonimide salt, after that, 184g Add silicon tetrachloride to the reaction kettle, after the reaction kettle is sealed, stir at a speed of 100rpm, the temperature rises to 70°C, and hydrogen gas with a pressure of 0.5MPa is introduced. During the reaction, the hydrogen pressure is kept constant, and the hydrogenation reaction starts and is timed. Regular sampling every 10 minutes for component analysis. The duration of the entire catalytic hydrogenation reaction is 2 hours; during the reaction process, the gas product obtained from the reaction is draw...

Embodiment 2

[0046] Take 100g of silicon powder and 100g of catalyst respectively, put them into different corundum porcelain boats, spread them evenly to 1mm, put the porcelain boats into the tube furnace, seal the furnace mouth end, raise the furnace temperature to 200°C, and introduce a pressure of 1.5MPa Hydrogen, activation pretreatment at constant temperature and pressure for 3h;

[0047] In a vacuum glove box, get 10g of silicon powder and 1g of catalyst and add it to a 500ml volume autoclave, then add 150g of 1-butyl-3-methylimidazolium dicyanamide salt, and then add 306g of silicon tetrachloride to the reaction Kettle, after the reaction kettle is sealed, stir at a speed of 300rpm, the temperature rises to 200°C, and hydrogen gas at a pressure of 2.5MPa is introduced. During the reaction, the hydrogen pressure is kept constant. Composition analysis was carried out, and the duration of the entire catalytic hydrogenation reaction was 3 hours; during the reaction process, the gaseous...

Embodiment 3

[0051] Take 100g of silicon powder and 100g of catalyst respectively, put them into different corundum porcelain boats, and spread them evenly to 0.7mm. Pressurized hydrogen, activation pretreatment at constant temperature and pressure for 2.5 hours;

[0052] In a vacuum glove box, take 10g of silicon powder and 0.5g of catalyst and add it to a 500ml volume autoclave, then add 100g of 1-butyl-3-methylimidazolium tetrafluoroborate, and then add 245g of silicon tetrachloride Add the reaction kettle, after the reaction kettle is sealed, stir at a speed of 200rpm, the temperature rises to 140°C, and hydrogen gas with a pressure of 1.5MPa is introduced. During the reaction, the hydrogen pressure is kept constant, and the hydrogenation reaction starts and is timed every 10 minutes. Sampling, component analysis of the sample by gas chromatographic analysis, the duration of the entire catalytic hydrogenation reaction is 2.5h; during the reaction process, the gas product obtained by th...

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

PropertyMeasurementUnit
specific surface areaaaaaaaaaaa
particle sizeaaaaaaaaaa
particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention provides a process method for preparing trichlorosilane by virtue of silicon tetrachloride liquid-phase cold hydrogenation in an ionic liquid medium based on the unique physicochemical properties of an ionic liquid such as non-volatility and strong dissolving capacity. The implementation result proves that the process method provided by the invention has excellent beneficial effects. Compared with the existing gas solid phase cold hydrogenation catalytic hydrogenation process, the method can be used for not only remarkably reducing the temperature and pressure of the catalytic hydrogenation reaction, but also improving the conversion rate of silicon tetrachloride and the selectivity of trichlorosilane. In the embodiment of the invention, the conversion rate of the obtained silicon tetrachloride is 20-40%, and the selectivity of trichlorosilane can reach 90-96%.

Description

technical field [0001] The invention relates to a process method for preparing trichlorosilane by liquid-phase cold hydrogenation of silicon tetrachloride based on an ionic liquid medium by means of catalytic reaction, and belongs to the technical field of chemical industry. Background technique [0002] At present, most of the production processes adopted by my country's polysilicon enterprises are the improved Siemens method, that is, mixed chlorosilanes (silicon tetrachloride, trichlorosilane, etc.) , to separate trichlorosilane, and then reduce trichlorosilane with high-purity hydrogen at high temperature, and the silicon vapor in the product is subjected to chemical vapor deposition to obtain high-purity polysilicon rods. A large number of by-products are produced during the reaction process of this process, that is, more than 10 tons of silicon tetrachloride and 1 to 5 tons of hydrogen chloride will be associated with every 1 ton of polysilicon produced. Silicon tetrac...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/107B01J23/89
Inventor 张军李晶晶杜西刚米刚宋帮才牛睿祺
Owner HENAN UNIV OF SCI & TECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com