CN1045077C - Tail gas recovery method and device in production of silicon carbide fibre - Google Patents
Tail gas recovery method and device in production of silicon carbide fibre Download PDFInfo
- Publication number
- CN1045077C CN1045077C CN95115643A CN95115643A CN1045077C CN 1045077 C CN1045077 C CN 1045077C CN 95115643 A CN95115643 A CN 95115643A CN 95115643 A CN95115643 A CN 95115643A CN 1045077 C CN1045077 C CN 1045077C
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- CN
- China
- Prior art keywords
- tail gas
- absorption tower
- silicon carbide
- condensed
- high boiling
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- Treating Waste Gases (AREA)
- Inorganic Fibers (AREA)
Abstract
The present invention provides a tail gas recovery method and a device in the production of silicon carbide fiber. Through a condensing device with the temperature of-40 to-80 DEG C, tail gas is condensed to separate CH3SiCl3, CH3 SiHCl2 and substances with high boiling points; then substances which can not be condensed, such as HCl, H2, etc., are conveyed to an absorption tower with 10% of alkaline liquor; after the HCl and the H2 are removed, the tail gas is conveyed to a purifier for purification and is condensed to separate silicane; through precise distillation, substances with high boiling points are removed and the tail gas is reused. The recovered CH3SiCl3 and CH3SiHCl2 take 95% of the total amount of the tail gas, and the utilization rate is 65%. After the tail gas recovery of the present invention, environment detection can achieve national standards.
Description
The invention belongs to the tail gas recycle in the Chemical Manufacture, particularly chemical Vapor deposition process is produced the method for recovering tail gas and the device of silicon carbide fiber.
Adopting chemical Vapor deposition process to produce silicon carbide fiber is that the tungsten filament matrix is passed through reactor continuously, feeds proper C H in reactor
3SiCl
3, CH
3SiHCl
2With the mixed gas of hydrogen, silane generates SiC in tungsten filament surface pyrolysis under 1100-1300 ℃ temperature.In the production process of silicon carbide fiber, the requirement of unstripped gas is less than 10% of input, and most of unstripped gas is then along with the waste gas that reaction is produced is discharged from the reaction tubes exhaust port.The tail gas of discharging mainly contains 95% silane, the product that in addition also has hydrogen, hydrogenchloride and synthesize or decompose in reaction.These tail gas, also can be detrimental to health except the significant wastage that causes raw material as not reclaimed and utilizing, and etching apparatus causes severe contamination to environment.Up to the present, yet there are no the relevant report that this part tail gas is recycled.
The object of the present invention is to provide the recovery method and the device of tail gas in a kind of silicon carbide fiber production, this method can make the tail gas recycle rate reach more than 95%, and utilization ratio reaches 65% again, and the discharging environment reaches GB.
The recovery method that silicon carbide fiber of the present invention is produced tail gas comprises the steps:
(1). with the condensing works condensation of tail gas by-40～-80 ℃, separation of C H
3SiCl
3, CH
3SiHCl
2And high boiling substance;
(2). the HCl that can not be condensed, H
2Enter the absorption tower that contains 10% alkali lye Deng material, remove HCl;
(3) .H
2Send into purification utensil;
(4). the silane that condensation separation goes out re-uses after high boiling substance is removed in the process precise distillation.
The device for recovering tail gas that designs according to aforesaid method, comprise a condensate trap, the bottom of condensate trap connects a collection container, collection container is connected with rectifying tower, the upper end of condensate trap links to each other with the absorption tower, the hydrogen that the absorption tower upper air vent gives off enters hydrogen gas cleaner, and the hydrogen after the purification still can use, and alkali lye recycles by being pumped into the absorption tower.
Tail gas recycle employing condensation separation of the present invention and rectifying, caustic washing method make the unstripped gas of the overwhelming majority obtain reclaiming.CH by the present invention's recovery
3SiCl
3And CH
3SiHCl
2Account for 95% of tail gas total amount, utilization ratio is 65% again.All can utilize through the hydrogen after purifying.Be up to state standards through the environment measuring after the tail gas recycle.Device for recovering tail gas of the present invention control simple in structure, easy is used this device to reclaim tail gas and has been improved economic benefit, has prolonged service life of equipment, has reduced environmental pollution.
Describe method of the present invention and device in detail below in conjunction with accompanying drawing.
Accompanying drawing is depicted as the silicon carbide fiber device for recovering tail gas synoptic diagram that proposes according to the present invention.
The tail gas that CVD SiC fiber-reactive device is discharged is sent into condensing temperature and is-70 ℃ condensate trap 5, CH
3SiC
3And CH
3SiHCl
2Condensation here also is collected in the container 6, at this moment 95% CH in the tail gas
3SiCl
3And CH
3SiHCl
2Recovery is condensed.Condensed silane is sent into retort 1 again through rectifying tower 3 rectifying, and smart distilled silane enters stationary tank 2 through condenser 4 condensations, removes high boiling material, and available silane reaches 65%.The gaseous matter that is not condensed is sent into absorption tower 7, injects the HCl gas that 10% sodium hydroxide solution absorbs gas in the tower, and alkali lye recycles by lye pump 9 and lye vat 8, is in operation regularly to detect naoh concentration in the solution.Fail absorbed hydrogen and send into and still can use after hydrogen gas cleaner 10 is removed the impurity of moisture content and other.Surrounding environment detects the requirement that can be up to state standards.
Each unit equipment in apparatus of the present invention all can be selected for use from known technology.
Claims (2)
1. the recovery method of a silicon carbide fiber production tail gas is characterized in that comprising the steps:
(1). with the condensing works condensation of tail gas by-40～-80 ℃, separation of C H
3SiCl
3, CH
3SiHCl
2And high boiling substance;
(2). the HCl that can not be condensed, H
2Enter the absorption tower that contains 10% alkali lye Deng material, remove HCl;
(3) .H
2Send into purification utensil;
(4). the silane that condensation separation goes out, after removing high boiling substance, the process precise distillation reuses.
2. device for recovering tail gas that designs according to the described method of claim 1, it is characterized in that comprising a condensate trap (5), the bottom of condensate trap connects a collection container (6), collection container is connected with rectifying tower (3), the upper end of condensate trap links to each other with absorption tower (7), the hydrogen that the absorption tower upper air vent gives off enters hydrogen gas cleaner (10), and alkali lye is sent into the absorption tower by pump (9) and recycled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95115643A CN1045077C (en) | 1995-09-29 | 1995-09-29 | Tail gas recovery method and device in production of silicon carbide fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95115643A CN1045077C (en) | 1995-09-29 | 1995-09-29 | Tail gas recovery method and device in production of silicon carbide fibre |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1146503A CN1146503A (en) | 1997-04-02 |
| CN1045077C true CN1045077C (en) | 1999-09-15 |
Family
ID=5080589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95115643A Expired - Fee Related CN1045077C (en) | 1995-09-29 | 1995-09-29 | Tail gas recovery method and device in production of silicon carbide fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1045077C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1073458C (en) * | 1998-11-24 | 2001-10-24 | 西北工业大学 | CVI/CVD technological tail gas treating process and equipment |
| CN101377376B (en) * | 2007-08-29 | 2012-06-06 | 中国恩菲工程技术有限公司 | Method for recovering tail gas generated by polycrystalline silicon production |
| EP2484631B1 (en) * | 2009-09-30 | 2015-03-11 | Tokuyama Corporation | Method for reusing hydrogen |
| CN109939532B (en) * | 2019-04-17 | 2021-07-27 | 复旦大学 | Papermaking waste gas purification recovery plant |
| CN110860199A (en) * | 2019-12-19 | 2020-03-06 | 大连福佳·大化石油化工有限公司 | Reforming catalyst reduction tail gas purification and recovery system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU891126A1 (en) * | 1977-02-14 | 1981-12-23 | Государственный ордена Октябрьской Революции научно-исследовательский и проектный институт редкометаллической промышленности | Method of cleaning hydrogen from hydrogen chloride and silicium chloride |
| JPS58167418A (en) * | 1982-03-25 | 1983-10-03 | ゴスダルストウエンヌイ・ナウチノ−イスレドワ−チエルスキ−・イ・プロエクトヌイ・インスチツ−ト・レドコメタリチエスコイ・プロムイシユレンノスチ゛ギレドメト゛ | Regeneration of chlorosilane and hydrogen for semiconductor polycrystal silicon manufacturing process |
-
1995
- 1995-09-29 CN CN95115643A patent/CN1045077C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU891126A1 (en) * | 1977-02-14 | 1981-12-23 | Государственный ордена Октябрьской Революции научно-исследовательский и проектный институт редкометаллической промышленности | Method of cleaning hydrogen from hydrogen chloride and silicium chloride |
| JPS58167418A (en) * | 1982-03-25 | 1983-10-03 | ゴスダルストウエンヌイ・ナウチノ−イスレドワ−チエルスキ−・イ・プロエクトヌイ・インスチツ−ト・レドコメタリチエスコイ・プロムイシユレンノスチ゛ギレドメト゛ | Regeneration of chlorosilane and hydrogen for semiconductor polycrystal silicon manufacturing process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1146503A (en) | 1997-04-02 |
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