CN101618874B - Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride - Google Patents
Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride Download PDFInfo
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- CN101618874B CN101618874B CN2009100657614A CN200910065761A CN101618874B CN 101618874 B CN101618874 B CN 101618874B CN 2009100657614 A CN2009100657614 A CN 2009100657614A CN 200910065761 A CN200910065761 A CN 200910065761A CN 101618874 B CN101618874 B CN 101618874B
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- silicon tetrachloride
- trichlorosilane
- hydrogenation reactor
- cold hydrogenation
- tubbiness
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Abstract
The invention relates to a method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride. The method comprises the following steps: mixing and vaporizing the silicon tetrachloride and hydrogen before entering a high-pressure state together with silicon powder and catalyst copper powder and entering a barrel-shaped cold hydrogenation reactor; continuously reacting in the barrel-shaped cold hydrogenation reactor under the conditions that temperature is 300-500 DEG C, pressure is 1.5-5.5 MPa, pH value is 5-7, and mixing gas velocity is 12 m/s to generate the trichlorosilane. The method can produce trichlorosilane directly for producing polysilicon at an electronic grade, improves the conversion efficiency (achieves 30-35 percent), circularly utilizes materials in the whole process, has no pollution, is beneficial to environmental protection, reduces enterprise cost and increases enterprise benefits.
Description
Technical field
The present invention relates to a kind of production method of trichlorosilane, especially producing trichlorosilane by coldly hydrogenating silicon tetrachloride.
Background technology
In the production process of polysilicon, can produce a large amount of silicon tetrachloride (SiCl
4), will produce the silicon tetrachloride (SiCl of 14-20kg as one kilogram of polysilicon of every production
4) and can't use.Silicon tetrachloride (SiCl
4) be by trichlorosilane (SiHCl
3) transform, if silicon tetrachloride (SiCl
4) carry out water treatment, these silicon tetrachlorides (SiCl
4) also to pay many expenses, it is the mass consumption raw material not only, again severe contamination surrounding enviroment; If allow silicon tetrachloride (SiCl
4) mixing hydrogen (H
2) be converted into polysilicon, then the mass consumption electric energy is not calculated at economic aspect.Therefore, solve this difficult problem, the current relatively way of reality is utilized silicon tetrachloride (SiCl exactly
4) production trichlorosilane (SiHCl
3).
At present, universal method in the world is hot hydrogenation, promptly adopt high temperature (nearly 1250 ℃) hydrogenation, but transformation efficiency is not high, and the cost height.The bell jar reflecting device is adopted in hot hydrogenation, and the gas that generates at this reactor reaction is trichlorosilane (SiHCl
3) and hydrogenchloride (HCl) gas, hydrogenchloride (HCl) can't discharge in removal process, need carry out neutralizing treatment.So present method adopts cold method for hydrogenation to transform silicon tetrachloride (SiCl
4).
Common cold hydrogenation is to adopt nickel powder to carry out catalyzed reaction as catalyzer, but this catalyst reaction rate is not high; In the domestic cold hydriding process,, cause unnecessary parking loss for it, cause loss of material again often because obstruction causes parking.
Summary of the invention
The present invention is problems such as existing producing trichlorosilane by using silicon tetrachloride ground method efficient is low, production cost height for solving, and have proposed producing trichlorosilane by coldly hydrogenating silicon tetrachloride.
In order to realize the object of the invention, the technical scheme of technical solution problem of the present invention need be implemented following steps:
1. vaporization: is 1～10: 1 mixing vaporization with hydrogen (H2) and silicon tetrachloride (SiCl4) with mol ratio;
2. feed: the mixed gas (H2, SiCl4) of silica flour (Si) material, catalyst copper powder, hydrogen and silicon tetrachloride is sent to high pressure conditions and enters into the cold hydrogenation reactor of tubbiness;
3. reaction: carry out successive reaction under the condition that in the cold hydrogenation reactor of tubbiness, be in temperature that 300 ℃ to 500 ℃, pressure are 1.5 to 5.5MPa, PH is 5 to 7, the mixed air rate of flow of fluid is 12m/s, generate trichlorosilane (SiHCl3);
4. dedusting: will follow silica flour (Si) that reactant gases comes out intussusception and utilizing again in dust removal installation, reactant gases is purified;
5. gas delivery purifying: will not have absorbed reactant gases to carry out subzero fractionation, compress gas behind the subzero fractionation with compressor then, enter into hydrogenchloride (HCl) knockout tower absorbing hydrogen chloride (HCl) gas, carry out adsorption cleaning at last hydrogen (H2);
6. rectifying: chlorosilane and the freezing chlorosilane that gets off after absorbing are carried out rectifying separation;
7. purify: silicon tetrachloride pure (SiCl4) is sent in the cold hydrogenation reactor of tubbiness after purifying, and trichlorosilane (SiHCl3) is purified obtains product.
The invention has the beneficial effects as follows: the trichlorosilane of producing with present method (SiHCl3) can reach the trichlorosilane (SiHCl3) that is directly used in the production electronic-grade polycrystalline silicon; improve transformation efficiency (reaching 30 ~ 35%); material recycle in the whole process; pollution-free; help environment protection, reduce enterprise cost, increase the performance of enterprises.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Following examples are used to illustrate the present invention, limit the scope of the invention but be not used in.
Embodiment 1:
1. vaporization: is 1～10: 1 mixing vaporization with hydrogen (H2) and silicon tetrachloride (SiCl4) with mol ratio;
2. feed: the mixed gas (H2, SiCl4) of silica flour (Si) material, catalyst copper powder, hydrogen and silicon tetrachloride is sent to high pressure conditions and enters into the cold hydrogenation reactor of tubbiness;
3. reaction: carry out successive reaction under the condition that in the cold hydrogenation reactor of tubbiness, be in temperature that 300 ℃ to 500 ℃, pressure are 1.5 to 5.5MPa, PH is 5 to 7, the mixed air rate of flow of fluid is 12m/s, generate trichlorosilane (SiHCl3);
4. dedusting: will follow silica flour (Si) that reactant gases comes out intussusception and utilizing again in dust removal installation, reactant gases is purified;
5. gas delivery purifying: will not have absorbed reactant gases to carry out subzero fractionation, compress gas behind the subzero fractionation with compressor then, enter into hydrogenchloride (HCl) knockout tower absorbing hydrogen chloride (HCl) gas, carry out adsorption cleaning at last hydrogen (H2);
6. rectifying: chlorosilane and the freezing chlorosilane that gets off after absorbing are carried out rectifying separation;
7. purify: silicon tetrachloride pure (SiCl4) is sent in the cold hydrogenation reactor of tubbiness after purifying, and trichlorosilane (SiHCl3) is purified obtains product.
Embodiment 2:
The mixed gas inlet amount is 100～30000kg/h.
Embodiment 3:
Pure the purifying to of silicon tetrachloride enters into the cold hydrogenation reactor of tubbiness again more than 99.99%.
Embodiment 4:
Trichlorosilane is purified to boracic≤0.05ppb, phosphorus≤0.1ppb.
Claims (4)
1. the technology of producing trichlorosilane by coldly hydrogenating silicon tetrachloride, flow process is: vaporization, feed, reaction, dedusting, gas delivery purifying, rectifying, purification is characterized in that:
Vaporization: is 1～10: 1 mixing vaporization with hydrogen and silicon tetrachloride with mol ratio;
Feed: the mixed gas of silica flour material, catalyst copper powder, hydrogen and silicon tetrachloride is sent to high pressure conditions and enters into the cold hydrogenation reactor of tubbiness;
Reaction: carry out successive reaction under the condition that in the cold hydrogenation reactor of tubbiness, be in temperature that 300 ℃ to 500 ℃, pressure are 1.5 to 5.5MPa, pH is 5 to 7, the mixed gas flow velocity is 12m/s, generate trichlorosilane;
Dedusting: the silica flour that will follow reactant gases to come out absorbs in dust removal installation and utilizes, and reactant gases is purified;
Gas delivery purifying: will not have absorbed reactant gases to carry out subzero fractionation, and compress gas behind the subzero fractionation with compressor then, and enter into hydrogenchloride knockout tower absorbing hydrogen chloride gas, and carry out adsorption cleaning at last to hydrogen;
Rectifying: chlorosilane and the freezing chlorosilane that gets off after absorbing are carried out rectifying separation;
Purify: be sent to after the pure purification of silicon tetrachloride in the cold hydrogenation reactor of tubbiness, trichlorosilane is purified obtains product.
2. the technology of producing trichlorosilane by coldly hydrogenating silicon tetrachloride according to claim 1, it is characterized in that: described mixed gas inlet amount is 100～30000kg/h.
3. the technology of producing trichlorosilane by coldly hydrogenating silicon tetrachloride according to claim 1, it is characterized in that: described silicon tetrachloride purifies to and enters into the cold hydrogenation reactor of tubbiness more than 99.99% again.
4. the technology of producing trichlorosilane by coldly hydrogenating silicon tetrachloride according to claim 1, it is characterized in that: described trichlorosilane purifies to boracic≤0.05ppb, phosphorus≤0.1ppb.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100657614A CN101618874B (en) | 2009-08-13 | 2009-08-13 | Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100657614A CN101618874B (en) | 2009-08-13 | 2009-08-13 | Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101618874A CN101618874A (en) | 2010-01-06 |
| CN101618874B true CN101618874B (en) | 2011-04-27 |
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| CN2009100657614A Expired - Fee Related CN101618874B (en) | 2009-08-13 | 2009-08-13 | Method for producing trichlorosilane by coldly hydrogenating silicon tetrachloride |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941702B (en) * | 2010-09-08 | 2012-09-05 | 洛阳晶辉新能源科技有限公司 | Method for producing trichlorosilane by converting silicon tetrachloride |
| CN102815707B (en) * | 2012-08-10 | 2014-09-10 | 中国恩菲工程技术有限公司 | Method for preparing trichlorosilane through silicon tetrachloride cold hydrogenation |
| CN102815711B (en) * | 2012-08-10 | 2014-03-26 | 中国恩菲工程技术有限公司 | Cold hydrogenation system for preparing trichlorosilane from silicon tetrachloride |
| CN102786055A (en) * | 2012-09-03 | 2012-11-21 | 内蒙古盾安光伏科技有限公司 | Method and device for heat utilization in polycrystalline silicon production process |
| CN102974569B (en) * | 2012-11-14 | 2015-06-03 | 内蒙古盾安光伏科技有限公司 | Online cleaning method of cold hydrogenation electric heater and online cleaning device of the cold hydrogenation electric heater |
| CN103449447B (en) * | 2013-08-23 | 2016-06-29 | 中国恩菲工程技术有限公司 | Prepare the equipment of trichlorosilane |
| CN103449448B (en) * | 2013-08-23 | 2016-07-06 | 中国恩菲工程技术有限公司 | Equipment for purification trichlorosilane |
| CN110980740A (en) * | 2019-11-01 | 2020-04-10 | 新疆东方希望新能源有限公司 | Trichlorosilane production process and production system |
| CN112374502B (en) * | 2020-11-16 | 2023-02-21 | 天津大学 | Polycrystalline silicon cold hydrogenation method adopting gas-solid parallel flow downer reactor |
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2009
- 2009-08-13 CN CN2009100657614A patent/CN101618874B/en not_active Expired - Fee Related
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