CN201543362U - Treatment device for treating hydrogen in polysilicon tail gas through temperature and pressure variation method - Google Patents
Treatment device for treating hydrogen in polysilicon tail gas through temperature and pressure variation method Download PDFInfo
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- CN201543362U CN201543362U CN2009202560290U CN200920256029U CN201543362U CN 201543362 U CN201543362 U CN 201543362U CN 2009202560290 U CN2009202560290 U CN 2009202560290U CN 200920256029 U CN200920256029 U CN 200920256029U CN 201543362 U CN201543362 U CN 201543362U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The utility model relates to a treatment device for treating hydrogen in polysilicon tail gas through a temperature and pressure variation method. The purity of hydrogen recovered by the treatment device from tail gas is above 99.9999 percent. The treatment device comprises at least three adsorption towers which are connected in parallel. Active carbon is arranged in each adsorption tower. A heating/cooling device and a pressurizing/depressurizing device are arranged on the adsorption tower. The treatment device additionally comprises a hydrogen cleaning device. The hydrogen cleaning device is communicated with the adsorption towers and valves are arranged on passages. The utility model has the advantages that: 1. the purity of the recovered hydrogen is high and can reach 99.9999 percent, the recovered hydrogen can be directly returned back to the polysilicon reaction furnace and high-purity polysilicon can be produced; 2. the entire process is simple, the operation is easy and the process continuity can be kept; 3. the recovered hydrogen is used for regenerating adsorbent, the excessive hydrogen can be used by other devices and the energy is saved; and 4. the adsorbent is regenerated and the environmental pollution is reduced.
Description
Technical field
The utility model relates to the purifying process of hydrogen in a kind of improved tail gas, and the hydrogen purity of recovery is more than 99.9999%.
Technical background
Utilize the trichlorosilane cracking process to produce polysilicon, will produce a large amount of chlorosilane, hydrogen and a spot of hydrogen chloride.The tail gas of CVD at first sprays the condensation chlorosilane at low temperatures with silicon tetrachloride, again through the pressurization deep cooling, use the chlorosilane absorbing hydrogen chloride, recover hydrogen, after the silicon tetrachloride that is absorbed with hydrogen chloride parses hydrogen chloride, return absorption system and recycle, the hydrogen chloride that parses returns the production of polysilicon system.Still the silane, hydrogen chloride and other metal impurities that contain trace in the recover hydrogen.Purified by activated carbon adsorber, the hydrogen after the purification directly turns back to the CVD reacting furnace.Will the production high-purity polycrystalline, the hydrogen of recycling use has been proposed higher requirement.
In the polysilicon, metal ion contents such as boron, phosphorus higher greatly reduces silicon as semi-conductive performance.Well-known active carbon is widely used as adsorbent and adsorbs impurity.So we utilize the hydrogen of novel charcoal tower process and Preparation of Activated Carbon 99.9999% purity.
The utility model content
The utility model is at above-mentioned defective, and purpose is to provide a kind of alternating temperature transformation method that can improve hydrogen recovery purity to handle the treating apparatus of hydrogen in the polysilicon tail gas.
The technical solution of the utility model is: the utility model comprises at least three adsorption towers that are formed in parallel, be provided with active carbon in each adsorption tower, adsorption tower is provided with and heats/heat sink, pressurization/dropping equipment, described treating apparatus also is provided with a hydrogen clearing apparatus, and this hydrogen clearing apparatus and each adsorption tower are communicated with and are provided with valve on its passage.
The top and the bottom of active carbon are provided with silk screen in described each adsorption tower.
The utility model relates to one-level absorption and make high-purity hydrogen.Comprise the adsorption process of the lower hydrogen of purity in tower, the hydrogen that utilize to reclaim is to the regenerative process of tower with to the tower of the finishing regeneration set-up procedure of boosting.Detect through ICP-MS, active carbon not only has suction-operated to silane and hydrogen chloride, simultaneously metal ions such as boron, phosphorus is also had suction-operated.Whole technology is made up of three charcoal towers, a tower absorption, and a tower ramp regeneration, a tower cooling is prepared, and three towers recycle.Whole technology is simple, easy operating, and efficient is higher.Gas is through tower body absorption, and the hydrogen purity of coming out at last is more than 99.9999%.
Operation principle of the present utility model is as follows:
Absorption phase, in just entering preceding 10 minutes of adsorption process, the utility model has two towers all at adsorbed state, after the hydrogen adsorption terminal valve of two towers is all opened, previous tower at adsorbed state can enter into regeneration step, and a back tower that enters adsorbed state will carry out the absorption of 530min; Pressure during absorption is the pressure of system, and usually at 0.6～1.5Mpa, pressure is high more, and impurity-eliminating effect is good more; In-55 ℃～30 ℃ scopes, temperature is low more usually for the temperature of absorption, and impurity-eliminating effect is good more.In the throughput of design, can guarantee product quality, can keep the continuity of technology again.
In the regeneration stage, what the utility model adopted is the heating of step-down limit, limit, and pressure will be lower than 0.17Mpa, and pressure is low more, the easy more desorption of impurity, and what the utility model designed is slow step-down, prevents that excessive pressure drop from impacting the technology in downstream; Temperature will be heated to more than 170 ℃ at least, and temperature is low more, the easy more desorption of impurity, and what the utility model designed is wing formula heating tube, so it is better to add thermal effect.Carry out hydrogen purge then, also will continue heating simultaneously,, can cool off active carbon, be not easy to the desorption of impurity because the hydrogen temperature that reclaims is lower.The flow of hydrogen purge gas is greater than 300cm
3/ h.After purge time satisfied, the temperature of active carbon must be more than 170 ℃.
Loitering phase, what the utility model adopted is the cooling pressurization.Before tower entered absorption, the tower body temperature must be lower than 30 ℃, helped next step impurity absorption like this.Pressure must be more than or equal to system pressure, otherwise causes the instability of system easily, causes damage.
The utility model has the advantages that:
1, the hydrogen purity of Hui Shouing is higher, can reach 99.9999%, can directly turn back in the reactor for polycrystalline silicon, produces high-purity polycrystalline.
2, whole technology is simple, and easy operating can keep the continuity of technology.
3, utilize the hydrogen that reclaims to make adsorbent reactivation, unnecessary hydrogen can use for other device, saves the energy.
4, adsorbent is regenerated, reduced environmental pollution.
Content of the present utility model makes further instructions in conjunction with following example.
Description of drawings
Fig. 1 is a structural representation of the present utility model
1 is that tower A, 2 is that tower B, 3 is that tower C, 4 is that active carbon, 5 is that hydrogen terminal valve, 6 is that deep fat terminal valve, 7 is that blow down valve, 8 is the cold oil terminal valve among the figure.
The specific embodiment
Below in conjunction with Fig. 1 and with three adsorption towers the utility model is described in detail, is beneficial to correct understanding of the present utility model;
In the first step, move 10 minutes, tower A/B is in absorption phase, and tower C is in loitering phase.At this moment the hydrogen terminal valve of tower A/B is all opened, and this is in order to keep the continuity of technology.The cold oil outlet valve of tower A is being opened, and is that conduction oil is met heat can expansion because of tower A meeting heat release in adsorption process.The deep fat terminal valve of tower B is being opened, and prepares to enter heated condition.Tower C prepares to enter the pressurization cooling, and blow down valve is that opening to open with terminal valve cold oil.
In second step, move 320 minutes, tower A is in absorption phase.Valve does not change; Tower B is in step-down/heating period, and hydrogen purge valve is opened, and require the pressure of system must be lower than 0.17Mpa when the time satisfies, and temperature is more than 170 ℃; Tower C is in cooling/pressure period, and valve does not change.
In the 3rd step, move 10 minutes, tower A is in absorption phase, and valve does not change; Tower B is in step-down/heating period, and valve does not change; Tower C is in cooling stage, and at this moment the sweep gas intake valve is closed, and the hydrogen outlet valve is opened because when cooling pressure can descend, so carry out ftercompction from system, when tower C entered absorption, the pressure of system was more stable, the operation of whole technology will be stablized.
In the 4th step, move 200 minutes, tower A is in absorption phase, and valve does not change; Tower B is in purge stages, and the sweep gas intake valve is opened; Tower C is in cooling stage, and valve does not change.
In the 5th step, move 10 minutes, tower A/C is in absorption phase, and tower B is in loitering phase.At this moment the hydrogen terminal valve of tower A/C is all opened, and this is in order to keep the continuity of technology.The deep fat terminal valve of tower A is being opened, and prepares to enter heated condition.Tower B prepares to enter the pressurization cooling, and blow down valve is that opening to open with terminal valve cold oil.The cold oil outlet valve of tower C is being opened, and is that conduction oil is met heat can expansion because of tower C meeting heat release in adsorption process.
In the 6th step, move 320 minutes, tower A is in step-down/heating period, and the hydrogen purge air outlet valve is opened, and require the pressure of system must be lower than 0.17Mpa when the time satisfies, and temperature is more than 170 ℃.Tower B is in cooling/pressure period, and valve does not change.Tower A is in absorption phase.Valve does not change.
In the 7th step, move 10 minutes, tower A is in step-down/heating period, and valve does not change; Tower B is in cooling stage, and at this moment the sweep gas intake valve is closed, and the hydrogen outlet valve is opened because when cooling pressure can descend, so carry out ftercompction from system, when tower B entered absorption, the pressure of system was more stable, the operation of whole technology will be stablized; Tower C is in absorption phase, and valve does not change.
In the 8th step, move 200 minutes, tower A is in purge stages, and the sweep gas intake valve is opened; Tower B is in cooling stage, and valve does not change; Tower C is in absorption phase, and valve does not change.
In the 9th step, move 10 minutes, tower A is in loitering phase, and tower B/C is in absorption phase.At this moment the hydrogen terminal valve of tower B/C is all opened, and this is in order to keep the continuity of technology.Tower A prepares to enter the pressurization cooling, and blow down valve is that opening to open with terminal valve cold oil.The cold oil outlet valve of tower B is being opened, and is that conduction oil is met heat can expansion because of tower B meeting heat release in adsorption process.The deep fat terminal valve of tower C is being opened, and prepares to enter heated condition.
In the tenth step, move 320 minutes, tower A is in cooling/pressure period, and valve does not change.Tower B is in absorption phase.Valve does not change.Tower C is in step-down/heating period, and the hydrogen purge air outlet valve is opened, and require the pressure of system must be lower than 0.17Mpa when the time satisfies, and temperature is more than 170 ℃.
In the 11 step, move 10 minutes, tower A is in cooling stage, and at this moment the sweep gas intake valve is closed, the hydrogen outlet valve is opened because when cooling pressure can descend, so carry out ftercompction from system, when tower A entered absorption, the pressure of system was more stable, and the operation of whole technology will be stablized; Tower B is in absorption phase, and valve does not change; Tower C is in step-down/heating period, and valve does not change.
In the 12 step, move 200 minutes, tower A is in cooling stage, and valve does not change; Tower B is in absorption phase, and valve does not change; Tower C is in purge stages, and the sweep gas intake valve is opened.
So far, three towers have all been realized the circulation by adsorption process, regenerative process, set-up procedure.Guaranteed the continuity of whole explained hereafter.
Active carbon of the present utility model is a cocoanut active charcoal, and particle diameter is at 4～80 orders.
Claims (2)
1. an alternating temperature transformation method is handled the treating apparatus of hydrogen in the polysilicon tail gas, it is characterized in that, comprise at least three adsorption towers that are formed in parallel, be provided with active carbon in each adsorption tower, adsorption tower is provided with and heats/heat sink, pressurization/dropping equipment, described treating apparatus also is provided with a hydrogen clearing apparatus, and this hydrogen clearing apparatus and each adsorption tower are communicated with and are provided with valve on its passage.
2. a kind of alternating temperature transformation method according to claim 1 is handled the treating apparatus of hydrogen in the polysilicon tail gas, it is characterized in that, the top and the bottom of active carbon are provided with silk screen in each adsorption tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202560290U CN201543362U (en) | 2009-12-01 | 2009-12-01 | Treatment device for treating hydrogen in polysilicon tail gas through temperature and pressure variation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009202560290U CN201543362U (en) | 2009-12-01 | 2009-12-01 | Treatment device for treating hydrogen in polysilicon tail gas through temperature and pressure variation method |
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| CN201543362U true CN201543362U (en) | 2010-08-11 |
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| CN2009202560290U Expired - Fee Related CN201543362U (en) | 2009-12-01 | 2009-12-01 | Treatment device for treating hydrogen in polysilicon tail gas through temperature and pressure variation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102284225A (en) * | 2011-06-15 | 2011-12-21 | 四川瑞能硅材料有限公司 | Method for analyzing adsorbing column of polycrystalline silicon tail gas dry method separation system |
| CN104436992A (en) * | 2014-10-15 | 2015-03-25 | 北京氢璞创能科技有限公司 | Pressure swing adsorption gas purifier component with front gas component separator |
| CN105935537A (en) * | 2016-04-19 | 2016-09-14 | 杨皓 | Process for purifying chlorosilane and hydrogen chloride with hydrogen mixed gas |
| CN114146532A (en) * | 2021-12-17 | 2022-03-08 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
| CN114146532B (en) * | 2021-12-17 | 2024-04-26 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
-
2009
- 2009-12-01 CN CN2009202560290U patent/CN201543362U/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102284225A (en) * | 2011-06-15 | 2011-12-21 | 四川瑞能硅材料有限公司 | Method for analyzing adsorbing column of polycrystalline silicon tail gas dry method separation system |
| CN102284225B (en) * | 2011-06-15 | 2014-07-16 | 四川瑞能硅材料有限公司 | Method for analyzing adsorbing column of polycrystalline silicon tail gas dry method separation system |
| CN104436992A (en) * | 2014-10-15 | 2015-03-25 | 北京氢璞创能科技有限公司 | Pressure swing adsorption gas purifier component with front gas component separator |
| CN105935537A (en) * | 2016-04-19 | 2016-09-14 | 杨皓 | Process for purifying chlorosilane and hydrogen chloride with hydrogen mixed gas |
| CN105935537B (en) * | 2016-04-19 | 2018-10-02 | 杨皓 | A kind of technique of hydrogen mixed gas purified chlorosilane and hydrogen chloride |
| CN114146532A (en) * | 2021-12-17 | 2022-03-08 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
| CN114146532B (en) * | 2021-12-17 | 2024-04-26 | 新疆大全新能源股份有限公司 | Operation process of active carbon adsorption tower in polycrystalline silicon tail gas recovery process |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100811 Termination date: 20121201 |