CN202208647U - Chlorosilane recovery system - Google Patents
Chlorosilane recovery system Download PDFInfo
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- CN202208647U CN202208647U CN201120298860XU CN201120298860U CN202208647U CN 202208647 U CN202208647 U CN 202208647U CN 201120298860X U CN201120298860X U CN 201120298860XU CN 201120298860 U CN201120298860 U CN 201120298860U CN 202208647 U CN202208647 U CN 202208647U
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- chlorosilane
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Abstract
The utility model discloses a chlorosilane recovery system capable of recovering chlorosilane with lower impurity content, which includes a first liquid storage container used for collecting waste chlorosilane, an evaporator used for converting the collected chlorosilane liquid into chlorosilane gas, a reactor used for removing impurities from the chlorosilane gas through moisture reaction, a second liquid storage container used for collecting reaction product, and a separator capable of performing gas-solid separation of the gas in the reaction product, which are connected sequentially. The chlorosilane recovery system can remove the chlorosilane impurities contaminated during the production process and with higher impurity content, so as to meet the requirement on the impurity content of the chlorosilane raw material in the Siemens method production polysilicon technology.
Description
Technical field
The application relates to the chlorosilane recovery system in the production of improvement Siemens process polycrystalline silicon.
Background technology
Can produce a large amount of discarded chlorosilanes in the improvement Siemens process polycrystalline silicon production process.Contain a large amount of available trichlorosilanes, part silicon tetrachloride and dichloro-dihydro silicon in these discarded chlorosilanes.A polysilicon factory that produces 3000 tons per year can produce the discarded chlorosilane of thousands of tons of, and the relatively poor factory of some process operation levels even can produce the discarded chlorosilanes of tens thousand of tons.Therefore, reclaiming and utilize this part discarded chlorosilane is an important research project.
The utility model content
The application aims to provide a kind of recyclable recovery system that obtains the lower chlorosilane of foreign matter content.
For this reason, this chlorosilane recovery system comprises and being linked in sequence:
A, be used to collect first liquid storage container of discarded chlorosilane;
B, be used for the chlorosilane liquid of collecting is changed into the vaporizer of chlorosilane gas;
C, be used for chlorosilane gas is carried out the reactor drum of moisture impurity removal reaction;
D, be used for collecting reaction product second liquid storage container;
E, be used for the gas of reaction product is carried out gas-solid isolating separator.
In technique scheme, the chlorosilane liquid in first liquid storage container can be transported in the vaporizer through pumping mode, for this reason, also should on the pipeline that connects first liquid storage container and vaporizer, pump be set.
Certainly, the chlorosilane liquid in first liquid storage container also can be transported to vaporizer through other modes, and the below that is reduced to first liquid storage container such as pneumatic conveying mode or with the mounting height of vaporizer is so that chlorosilane liquid nature inflow evaporator.
In addition, vaporizer can adopt multiple type of heating to make chlorosilane vaporizing liquid wherein become chlorosilane gas.Such as gas heating, heat-conducting oil heating, nichrome wire heating in addition, inductance heating, Infrared Heating etc.Perhaps, also can adopt vaporizer is pumped into negative pressure, make chlorosilane liquid direct boiling wherein become chlorosilane gas.
When the moisture impurity removal reaction, said moisture is the mixed gas of a kind of and water vapor in hydrogen, carbonic acid gas, nitrogen, the rare gas element, and its humidity is 8%～90%RH.
For the gas in the reaction product being carried out gas-solid separation through separator; Can adopt filtering elements such as cloth bag, ceramic porous material, also can directly in separator, establish the chlorosilane spray equipment and remove the micro-solid impurity in the chlorosilane liquid with washing through clean chlorosilane.Certainly, also can be with the chlorosilane spray as carrying out filtering assist measure through filtering element.
Owing to have the higher noncondensable gas of portion temperature in first liquid storage container, therefore can on the top vent of first liquid storage container, connect water cooler, thereby make noncondensable gas after the water cooler cooling, carry out harmless treatment.
In addition, be provided with the chlorosilane spray equipment in the reactor drum.
For fear of impurity caking blocking pipe, on first liquid storage container whipping appts is installed.Based on same reason, whipping appts is installed also on the vaporizer.
Further, second liquid storage container adopts bubbler.
The application's beneficial effect is:
1, can chlorosilane Impurity removal contaminated in the production process and that foreign matter content is high be reached the improvement Siemens Method and produce chlorosilane raw material impurity content requirement in the polysilicon process;
2, fully reclaim the improvement Siemens Method and produce element silicon, protium and chlorine element in the polysilicon process, reduced production material consumption and energy consumption, have remarkable economic efficiency;
3, reduce the quantity that the improvement Siemens Method is produced harmless treatment chlorosilane in the polysilicon process, reduced the required alkali lye of neutralization, practiced thrift resource; Reduce slag and effluent quantity, alleviated environmental stress, had the remarkable environmental safety benefit.
Description of drawings
Fig. 1 is the structural representation of the application's chlorosilane retrieving arrangement.
Be labeled as among the figure: whipping appts 1, first liquid storage container 2, pump 3, whipping appts 4, vaporizer 5, reactor drum 6, separator 7, second liquid storage container 8, water cooler 9.
Embodiment
Below in conjunction with accompanying drawing and embodiment the structure and the method for use of this chlorosilane recovery system are described further.
As shown in Figure 1, the step that adopts the chlorosilane recovery system to reclaim trichlorosilane is:
1) collects discarded chlorosilane (the discarded chlorosilane of the discarded chlorosilane that the discarded chlorosilane that rectification working process produces, maintenance produce, the chlorosilane phlegma in the waste gas, synthesis procedure silicon tetrachloride washings or the like) pneumatic conveying mode and be transported to first liquid storage container 2.For fear of impurity caking blocking pipe, container for storing liquid is equipped with whipping appts 1.First liquid storage container, 2 tops are equipped with water cooler 9, and noncondensable gas carries out harmless treatment after cooling.In order to guarantee to discard the normal conveying of chlorosilane and avoid the air anti-channeling to go into storage tank and blast, first liquid storage container, 2 pressure-controlling are at 50-150kpa.Waste liquid foreign matter content in first liquid storage container 2: boron content is less than 750ppb, and phosphorus content is less than 550ppb.
2) the discarded chlorosilane (employing pumping mode) in first liquid storage container 2 is transported in the vaporizer 5.There is whipping appts 4 vaporizer 5 inside, avoid solid impurity caking blocking pipe to conduct heat with influence.
3) vaporizer heating.Adopt steam heating, heating makes chlorosilane vapourizing production chlorosilane steam in the vaporizer, and temperature is controlled at 110 ℃, and pressure-controlling is at 300kPa; Debris in the vaporizer is a mud or Powdered, mainly is impurity such as silica flour, metal chloride, and processing is hydrolyzed.The purpose of heating is to make that chlorosilane vapourizing is a chlorosilane steam in the vaporizer, and waste residue enters hydrolyzing process and carries out harmless treatment.
4) chlorosilane steam (the flow 200NM after the vaporization
3/ h, foreign matter content: boron is less than 700ppb, and phosphorus is less than 500ppb) and moisture (temperature: 32 ℃, humidity: 15%RH, flow: 25NM
3/ h) feed in the reactor drum 6 reaction and spray silicon tetrachloride (flow: 1M respectively
3/ h, temperature: 25 ℃).
5) gas recovery.The gas that has high boiling material gets into separator 7; In separator 7 by after silicon tetrachloride (temperature: the 25 ℃) washing; Foreign matter content in the purified gas is: boron content is less than 400ppb; The phosphorus saltiness is less than 300ppb, and phlegma boron, phosphorus content that purified gas entering condensate recovery system obtains behind deep cooling (temperature :-50 ℃) are low, can be used for improveing Siemens Method and produce in the polysilicon process.The effusive impure silicon tetrachloride washings of separator is collected in second liquid storage container 8 (bubbler), sends into rectifying tower and separates purification, the silicon tetrachloride after cat head obtains purifying.Tower bottoms obtains containing impurity liquid such as silica dust particle and metal chloride, continue to reclaim chlorosilane wherein through such scheme again, and remaining solid impurity discharges after with the alkali lye harmless treatment through the hydrolysis treatment system.
As shown in Figure 1, the step that adopts the chlorosilane recovery system to reclaim trichlorosilane is:
1) collects discarded chlorosilane (the discarded chlorosilane of the discarded chlorosilane that the discarded chlorosilane that rectification working process produces, maintenance produce, the chlorosilane phlegma in the waste gas, synthesis procedure silicon tetrachloride washings or the like) pump delivery mode and be transported to first liquid storage container 2.For fear of impurity caking blocking pipe, first liquid storage container 2 is equipped with whipping appts 1.First liquid storage container, 2 tops are equipped with water cooler 9, and noncondensable gas carries out harmless treatment after cooling.In order to guarantee to discard the normal conveying of chlorosilane and avoid the air anti-channeling to go into storage tank and blast, first liquid storage container, 2 pressure-controlling are at 400-550kpa.Waste liquid foreign matter content in first liquid storage container 2: boron content is less than 750ppb, and phosphorus content is less than 550ppb.
2) the discarded chlorosilane (employing pneumatic conveying mode) in first liquid storage container 2 is transported in the vaporizer 5.There is whipping appts 4 vaporizer 5 inside, avoid solid impurity caking blocking pipe to conduct heat with influence.
3) vaporizer heating.Vaporizer is used the heating medium heat-conducting oil heating, makes chlorosilane vapourizing production chlorosilane steam in the vaporizer, and temperature is controlled at 140 ℃, pressure 400KPa.Debris in the vaporizer is a mud or Powdered, mainly is impurity such as silica flour, metal chloride, and processing is hydrolyzed.The purpose of heating is to make that chlorosilane vapourizing is a chlorosilane steam in the vaporizer, and waste residue enters hydrolyzing process and carries out harmless treatment.
4) chlorosilane steam (the flow 230NM after the vaporization
3/ h, foreign matter content: boron is less than 700ppb, and phosphorus is less than 500ppb) and moisture (temperature: 32 ℃, humidity: 15%RH, flow: 25NM
3/ h) feed in the reactor drum 6 reaction and spray silicon tetrachloride (flow: 1.2M respectively
3/ h, temperature: 25 ℃).
5) gas recovery.The gas that has high boiling material gets into separator 7; In separator 7 by after silicon tetrachloride (temperature: the 25 ℃) washing; Foreign matter content in the purified gas is: boron is less than 450ppb; Phosphorus is less than 310ppb, and phlegma boron, phosphorus content that purified gas entering condensate recovery system obtains behind deep cooling (temperature :-50 ℃) are low, can be used for improveing Siemens Method and produce in the polysilicon process.The effusive impure silicon tetrachloride washings of separator is collected in second liquid storage container 8 (bubbler), sends into rectifying tower and separates purification, the silicon tetrachloride after cat head obtains purifying.Tower bottoms obtains containing impurity liquid such as silica dust particle and metal chloride, continue to reclaim chlorosilane wherein through such scheme again, and remaining solid impurity discharges after with the alkali lye harmless treatment through the hydrolysis treatment system.
Embodiment 3
As shown in Figure 1, the step that adopts the chlorosilane recovery system to reclaim trichlorosilane is:
1) collects discarded chlorosilane (the discarded chlorosilane of the discarded chlorosilane that the discarded chlorosilane that rectification working process produces, maintenance produce, the chlorosilane phlegma in the waste gas, synthesis procedure silicon tetrachloride washings or the like) pneumatic conveying mode and be transported to first liquid storage container 2.For fear of impurity caking blocking pipe, first liquid storage container 2 is equipped with whipping appts 1.Tank top is equipped with water cooler, and noncondensable gas carries out harmless treatment after cooling.In order to guarantee to discard the normal conveying of chlorosilane and avoid the air anti-channeling to go into storage tank and blast, first liquid storage container, 2 pressure-controlling are at 50-150kpa.Waste liquid foreign matter content in first liquid storage container 2: boron benefit 750ppb, phosphorus is less than 550ppb.
2) the discarded chlorosilane (employing pumping mode) in first liquid storage container 2 is transported in the vaporizer 4.There is whipping appts 4 vaporizer 4 inside, avoid solid impurity caking blocking pipe to conduct heat with influence.
3) vaporizer 4 heating: vaporizer 4 usefulness heating mediums (adopting the nichrome wire heating) heating makes vaporizer 4 interior chlorosilane vapourizings produce chlorosilane steam, and temperature is controlled at 110 ℃, and pressure-controlling is at 300kpa; Debris in the vaporizer 4 is a mud or Powdered, mainly is impurity such as silica flour, metal chloride, and processing is hydrolyzed.The purpose of heating is to make that chlorosilane vapourizing is a chlorosilane steam in the vaporizer, and waste residue enters hydrolyzing process and carries out harmless treatment.
4) chlorosilane steam (the flow 100NM after the vaporization
3/ h, foreign matter content: boron content is less than 700ppb, and phosphorus is less than 500ppb) and moisture (temperature: 32 ℃, humidity: 15%RH, flow: 25NM
3/ h) feed in the reactor drum 6 reaction and spray silicon tetrachloride (flow: 0.5M respectively
3/ h, temperature: 25 ℃).
5) gas recovery.The gas that has high boiling material gets into separator 7; In separator 7 by after silicon tetrachloride (temperature: the 25 ℃) washing; Foreign matter content in the purified gas is: boron content is less than 380ppb; Phosphorus content is less than 200ppb, and phlegma boron, phosphorus content that purified gas entering condensate recovery system obtains behind deep cooling (temperature :-50 ℃) are low, can be used for improveing Siemens Method and produce in the polysilicon process.The effusive impure silicon tetrachloride washings of separator is collected in second liquid storage container 8 (bubbler), sends into rectifying tower and separates purification, the silicon tetrachloride after cat head obtains purifying.Tower bottoms obtains containing impurity liquid such as silica dust particle and metal chloride, continue to reclaim chlorosilane wherein through such scheme again, and remaining solid impurity discharges after with the alkali lye harmless treatment through the hydrolysis treatment system.
Claims (8)
1. chlorosilane recovery system is characterized in that it comprises to be linked in sequence:
A, be used to collect first liquid storage container (2) of discarded chlorosilane;
B, be used for the chlorosilane liquid of collecting is changed into the vaporizer (5) of chlorosilane gas;
C, be used for chlorosilane gas is carried out the reactor drum (6) of moisture impurity removal reaction;
D, be used for collecting reaction product second liquid storage container (8);
E, be used for the gas of reaction product is carried out gas-solid isolating separator (7).
2. recovery system as claimed in claim 1 is characterized in that: the pipeline that connects first liquid storage container (2) and vaporizer (5) is provided with pump (3).
3. recovery system as claimed in claim 1 is characterized in that: be connected with water cooler (9) on the top vent of first liquid storage container (2).
4. recovery system as claimed in claim 1 is characterized in that: reactor drum is provided with the chlorosilane spray equipment in (6).
5. recovery system as claimed in claim 1 is characterized in that: separator is provided with the chlorosilane spray equipment in (7).
6. recovery system as claimed in claim 1 is characterized in that: whipping appts (1) is installed on first liquid storage container (2).
7. recovery system as claimed in claim 1 is characterized in that: whipping appts (4) is installed on the vaporizer (5).
8. recovery system as claimed in claim 1 is characterized in that: second liquid storage container (8) adopts bubbler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120298860XU CN202208647U (en) | 2011-08-17 | 2011-08-17 | Chlorosilane recovery system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120298860XU CN202208647U (en) | 2011-08-17 | 2011-08-17 | Chlorosilane recovery system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202208647U true CN202208647U (en) | 2012-05-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201120298860XU Expired - Fee Related CN202208647U (en) | 2011-08-17 | 2011-08-17 | Chlorosilane recovery system |
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| CN (1) | CN202208647U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927469A (en) * | 2017-04-12 | 2017-07-07 | 中国恩菲工程技术有限公司 | The recovery system of chlorosilane waste liquid |
-
2011
- 2011-08-17 CN CN201120298860XU patent/CN202208647U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106927469A (en) * | 2017-04-12 | 2017-07-07 | 中国恩菲工程技术有限公司 | The recovery system of chlorosilane waste liquid |
| CN106927469B (en) * | 2017-04-12 | 2023-12-15 | 中国恩菲工程技术有限公司 | Recovery system of chlorosilane waste liquid |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120502 Termination date: 20160817 |
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| CF01 | Termination of patent right due to non-payment of annual fee |