CN105152171A - Special system and method for continuously recovering chlorosilane containing slurry in polycrystalline silicon production process - Google Patents
Special system and method for continuously recovering chlorosilane containing slurry in polycrystalline silicon production process Download PDFInfo
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- CN105152171A CN105152171A CN201510483600.2A CN201510483600A CN105152171A CN 105152171 A CN105152171 A CN 105152171A CN 201510483600 A CN201510483600 A CN 201510483600A CN 105152171 A CN105152171 A CN 105152171A
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Abstract
The invention provides a special system and method for continuously recovering chlorosilane containing slurry in a polycrystalline silicon production process. The slurry is continuously conveyed to a dryer according to designed flow, steam is adopted for indirect heating, chlorosilane with a low boiling point is condensed and recovered, and the solid containing rate of a material discharged from the dryer is detected through material sampling at a discharge port of the dryer, so that the temperature of the dryer is adjusted and the slurry is treated into slag slurry with the solid containing rate of 80%; the slag slurry is discharged by a screw pump to a spray tower circulating tank for hydrolysis and neutralization reaction, hydrolyzed gas is subjected to high altitude discharge after being leached with a calcium hydroxide solution, and recovered chlorosilane which is qualified after detection is conveyed to a main technological unit for recycling. According to the special system and the method, continuous drying processing of the slurry is realized, the slurry processing capacity is greatly improved, the recovering rate of the slurry is high, the recovering quality of chlorosilane is good, recycling by the main technological unit is guaranteed, the dried slag slurry is slowly conveyed by the screw pump to a hydrolysis system for the hydrolysis and neutralization reaction, accordingly, hydrogen and heat produced through the hydrolysis reaction of one-time slag discharge of the dryer are avoided, and the system operates more safely and more stably.
Description
Technical field
The invention belongs to technical field of polysilicon production, be specifically related to chlorine-containing silane slurry in a kind of polysilicon production process and reclaim patent system and method continuously.
Background technology
In the cold hydrogenation process of production of polysilicon, the stripping tower of trichlorosilane synthesizing section can discharge a large amount of slurry, and slurry is primarily of impurity compositions such as trichlorosilane, silicon tetrachloride, dichlorosilane, silica flour, a small amount of metal chlorides; Slurry has severe corrosive, is volatile poisonous and harmful liquid, very large to environmental hazard.At present, polysilicon industry process slurry common method has two kinds: the first to be wet processing, slurry is delivered in drying plant in batches, heated up by dryer steam jacket indirect heating, reclaim most of chlorosilane, solid slag after oven dry is disposable enters hydrolysis system, neutralization reaction is carried out with basic solution, the uncontrollable rate of recovery of this method is within target zone, operation maneuvering ability is more weak, solid slag after oven dry is disposable enters hydrolysis system and alkali lye carries out neutralization reaction, react very violent, and produce a large amount of hydrogen and heat, there is potential safety hazard in system, this method belongs to intermittent operation, slurry processing efficiency is lower, second is dry process, is delivered in batches in drying plant by slurry, and heated up by dryer steam jacket indirect heating, reclaim whole chlorosilane, the solid slag after oven dry enters solid slag gathering barrel, transports landfill through cooling post-tensioning outside the venue to slag, still the uncontrollable rate of recovery is within target zone for this method, and operation maneuvering ability is strong, and the solid slag possibility attachment portion chlorosilane of discharge, cause environmental pollution, this method still belongs to intermittent operation, and slurry processing efficiency is lower.Above-mentioned two kinds of methods are intermittent operation, and processing efficiency is lower, cannot meet large-scale, successional explained hereafter demand, are therefore necessary to propose to improve.
Summary of the invention
The technical problem that the present invention solves: provide chlorine-containing silane slurry in a kind of polysilicon production process to reclaim patent system and method continuously, by the continuous indirect heating of steam, make the lower boiling chlorosilane entered continuously in dryer in slurry enter withdrawing can after evaporative condenser and be delivered to upstream recycling, solid slag continuous print after oven dry enters spiral pump, delivers into eluting column circulation groove to be hydrolyzed neutralization reaction by spiral pump.
The technical solution used in the present invention: in polysilicon production process, chlorine-containing silane slurry reclaims dedicated system continuously, there is sizing agent-agitating tank, described slurry agitation tank top is provided with recirculated water cooling condenser I, sizing agent-agitating tank exit end is communicated with dryer inlet end, an exit end of described dryer is communicated with the inlet end of spiral pump, the exit end of described spiral pump is communicated with spray column circulation groove inlet end, an exit end of described spray column circulation groove is communicated with spray column, and another exit end of spray column circulation groove is communicated with waste water downstream unit inlet end; Another exit end of described dryer is communicated with recirculated water cooling condenser II inlet end being arranged on chlorosilane withdrawing can top, and described chlorosilane withdrawing can top is also provided with ethylene glycol interchanger.
The continuous recovery method of chlorine-containing silane slurry in a kind of polysilicon production process is also provided, slurry according to design discharge continus convergence to dryer, utilize 3bar steam indirect heating, lower boiling chlorosilane condensate is reclaimed, the solid content that material discharged by dryer is detected by the sampling of dryer discharge gate material, thus regulate dryer temperature slurry process to be reached the slag slurry of solid content 80%, use spiral pump to drain into spray column circulation groove in slag slurry to be again hydrolyzed neutralization reaction, water decomposition gas is high altitude discharge after aqua calcis drip washing, be delivered to main technique unit after the chlorosilane detection of reclaiming is qualified to recycle.
Specifically comprise following step:
1) first chlorine-containing silane slurry enters sizing agent-agitating tank storage, and the chlorosilane gas produced in storage process enters sizing agent-agitating tank again by recirculated water cooling condenser I condensation of slurry agitation tank top;
2) slurry in sizing agent-agitating tank relies on deadweight to enter dryer continuously according to design discharge, described dryer uses 3bar steam indirect heating slurry, described slurry fully stirs in dryer inside, the chlorosilane gas evaporated cools and returns the main technique workshop section of polysilicon after the assay was approved and recycles, and is controlled the temperature of dryer by dryer discharge gate sampling test slurry solid content simultaneously;
3) the described dryer slag slurry of discharging slowly is pushed by spiral pump and to be hydrolyzed reaction in spray column circulation groove, the waste gas that hydrolysis reaction produces uses qualified discharge after lime milk solution drip washing through spray column, and the waste water that hydrolysis produces is delivered to waste water downstream unit and processed.
Above-mentioned steps 2) in, the lower boiling chlorosilane gas that described slurry evaporates after dryer inside is fully stirred enters recirculated water cooling condenser II through vent line and carries out just cold, deep cooling is carried out again through ethylene glycol interchanger, the gas be not condensed enters waste gas header through chlorosilane withdrawing can vent line and continues process, the chlorosilane liquid produced that condensation is got off is back to chlorosilane withdrawing can and stores, and returns the main technique workshop section of polysilicon and recycle after the chlorosilane liquid produced in chlorosilane withdrawing can is qualified after testing.
Above-mentioned steps 2) in, detect by the sampling of dryer discharge gate slurry the solid content that material discharged by dryer, thus slurry is treated to the slag slurry that solid content reaches 80% by adjustment dryer temperature.
Above-mentioned steps 3) in, waste gas qualified discharge after the lime milk solution drip washing that spray column working concentration is 10% that hydrolysis reaction produces.
The present invention compared with prior art realizes the continuous drying process of slurry, it is good that the processing power of slurry promotes greatly, the rate of recovery is high, chlorosilane reclaims quality, ensure that main technique unit is recycled, slag slurry after oven dry is slowly delivered to hydrolysis system by spiral pump and is hydrolyzed neutralization reaction, avoid the disposable deslagging hydrolysis reaction of dryer to produce hydrogen and heat, system cloud gray model is safety and stability more.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Embodiment
Below in conjunction with accompanying drawing 1, a kind of embodiment of the present invention is described.
In polysilicon production process, chlorine-containing silane slurry reclaims dedicated system continuously, there is sizing agent-agitating tank 1, described sizing agent-agitating tank 1 top is provided with recirculated water cooling condenser I 2, sizing agent-agitating tank 1 exit end is communicated with dryer 3 inlet end, an exit end of described dryer 3 is communicated with the inlet end of spiral pump 4, the exit end of described spiral pump 4 is communicated with spray column circulation groove 8 inlet end, an exit end of described spray column circulation groove 8 is communicated with spray column 9, and another exit end of spray column circulation groove 8 is communicated with waste water downstream unit 10 inlet end; Another exit end of described dryer 3 is communicated with recirculated water cooling condenser II 5 inlet end being arranged on chlorosilane withdrawing can 6 top, and described chlorosilane withdrawing can 6 top is also provided with ethylene glycol interchanger 7.
Utilize the continuous recovery method of chlorine-containing silane slurry in special recovery system recoveries polysilicon production process, slurry according to design discharge continus convergence to dryer 3, utilize 3bar steam indirect heating, lower boiling chlorosilane condensate is reclaimed, the solid content that material discharged by dryer 3 is detected by the sampling of dryer 3 discharge gate material, thus regulate dryer temperature slurry process to be reached the slag slurry of solid content 80%, use spiral pump to drain into spray column circulation groove in slag slurry to be again hydrolyzed neutralization reaction, water decomposition gas is high altitude discharge after aqua calcis drip washing, be delivered to main technique unit after the chlorosilane detection of reclaiming is qualified to recycle.
Concrete steps are as follows:
1) first chlorine-containing silane slurry enters sizing agent-agitating tank 1 and stores, and the chlorosilane gas produced in storage process enters sizing agent-agitating tank 1 again by recirculated water cooling condenser I 2 condensation at sizing agent-agitating tank 1 top;
2) slurry in sizing agent-agitating tank in 1 relies on deadweight to enter dryer 3 continuously according to design discharge, described dryer 3 uses 3bar steam indirect heating slurry, described slurry fully stirs in dryer 3 inside, the chlorosilane gas evaporated cools and returns the main technique workshop section of polysilicon after the assay was approved and recycles, specifically, the lower boiling chlorosilane gas that described slurry evaporates after dryer inside is fully stirred enters recirculated water cooling condenser II 5 through vent line and carries out just cold, deep cooling is carried out again through ethylene glycol interchanger 7, the gas be not condensed enters waste gas header through chlorosilane withdrawing can 6 vent line and continues process, the chlorosilane liquid produced that condensation is got off is back to chlorosilane withdrawing can 6 and stores, return the main technique workshop section of polysilicon after chlorosilane liquid produced in chlorosilane withdrawing can 6 is qualified after testing to recycle, detect by the sampling of dryer 3 discharge gate slurry the solid content that material discharged by dryer, thus slurry is treated to the slag slurry that solid content reaches 80% by adjustment dryer temperature simultaneously,
3) the described dryer slag slurry of discharging slowly is pushed by spiral pump 4 and to be hydrolyzed reaction in spray column circulation groove 8, waste gas qualified discharge after the lime milk solution drip washing that spray column 9 working concentration is 10% that hydrolysis reaction produces, the waste water that hydrolysis produces is delivered to waste water downstream unit 10 and is processed.
By facts have proved, adopt the present invention can reach more than 70% to the rate of recovery of chlorosilane in trichlorosilane synthesis procedure discharge chlorine-containing silane slurry, the reuse that the quality reclaiming chlorosilane after testing can reach upstream process requires (silicon tetrachloride molar fraction reaches more than 90%, and boron, phosphorus and metals content impurity are ppbw level).The present invention, by the indirect heating of steam, achieves the solid-liquid separation of slurry, has recycled useful chlorosilane, has added the effective rate of utilization of resource, achieves the continuous process of slurry simultaneously, greatly improves the processing power of slurry.By the conveying of spiral pump, the slag slurry after drying is delivered to hydrolysis neutralized system slowly, avoids slag slurry disposable with basic solution generation intense reaction, produce a large amount of hydrogen and heat, avoid potential safety hazard, reach safety and economic double benefit.
Above-described embodiment, just preferred embodiment of the present invention, is not used for limiting the scope of the present invention, therefore all equivalence changes done with content described in the claims in the present invention, all should be included within the claims in the present invention scope.
Claims (6)
1. in polysilicon production process, chlorine-containing silane slurry reclaims dedicated system continuously, there is sizing agent-agitating tank (1), it is characterized in that: described sizing agent-agitating tank (1) top is provided with recirculated water cooling condenser I (2), sizing agent-agitating tank (1) exit end is communicated with dryer (3) inlet end, an exit end of described dryer (3) is communicated with the inlet end of spiral pump (4), the exit end of described spiral pump (4) is communicated with spray column circulation groove (8) inlet end, an exit end of described spray column circulation groove (8) is communicated with spray column (9), another exit end of spray column circulation groove (8) is communicated with waste water downstream unit (10) inlet end, another exit end of described dryer (3) is communicated with recirculated water cooling condenser II (5) inlet end being arranged on chlorosilane withdrawing can (6) top, and described chlorosilane withdrawing can (6) top is also provided with ethylene glycol interchanger (7).
2. reclaim with chlorine-containing silane slurry in polysilicon production process according to claim 1 the method that dedicated system reclaims chlorosilane continuously, it is characterized in that slurry according to design discharge continus convergence to dryer (3), utilize 3bar steam indirect heating, lower boiling chlorosilane condensate is reclaimed, the solid content that material discharged by dryer (3) is detected by the sampling of dryer (3) discharge gate slurry, thus regulate dryer (3) temperature slurry process to be reached the slag slurry of solid content 80%, use spiral pump (4) to drain into spray column circulation groove (8) in slag slurry to be again hydrolyzed neutralization reaction, water decomposition gas is high altitude discharge after aqua calcis drip washing, be delivered to main technique unit after the chlorosilane detection of reclaiming is qualified to recycle.
3. the continuous recovery method of chlorine-containing silane slurry in polysilicon production process according to claim 1, is characterized in that comprising following step:
1) first chlorine-containing silane slurry enters sizing agent-agitating tank (1) storage, and the chlorosilane gas produced in storage process enters sizing agent-agitating tank (1) again by recirculated water cooling condenser I (2) condensation at sizing agent-agitating tank (1) top;
2) slurry in sizing agent-agitating tank in (1) relies on deadweight to enter dryer (3) continuously according to design discharge, described dryer (3) uses 3bar steam indirect heating slurry, described slurry fully stirs in dryer (3) inside, the chlorosilane gas evaporated cools and returns the main technique workshop section of polysilicon after the assay was approved and recycles, and is controlled the temperature of dryer by dryer (3) discharge gate sampling test slurry solid content simultaneously;
3) the described dryer slag slurry of discharging slowly is pushed by spiral pump (4) and to be hydrolyzed reaction in spray column circulation groove (8), the waste gas that hydrolysis reaction produces uses qualified discharge after lime milk solution drip washing through spray column (9), and the waste water that hydrolysis produces is delivered to waste water downstream unit (10) and processed.
4. the continuous recovery method of chlorine-containing silane slurry in polysilicon production process according to claim 1, it is characterized in that: above-mentioned steps 2) in, the lower boiling chlorosilane gas that described slurry evaporates after dryer inside is fully stirred enters recirculated water cooling condenser II (5) through vent line and carries out just cold, deep cooling is carried out again through ethylene glycol interchanger (7), the gas be not condensed enters waste gas header through chlorosilane withdrawing can (6) vent line and continues process, the chlorosilane liquid produced that condensation is got off is back to chlorosilane withdrawing can (6) and stores, return the main technique workshop section of polysilicon after chlorosilane liquid produced in chlorosilane withdrawing can (6) is qualified after testing to recycle.
5. the continuous recovery method of chlorine-containing silane slurry in polysilicon production process according to claim 1, it is characterized in that: above-mentioned steps 2) in, detect by the sampling of dryer (3) discharge gate slurry the solid content that material discharged by dryer, thus slurry is treated to the slag slurry that solid content reaches 80% by adjustment dryer temperature.
6. the continuous recovery method of chlorine-containing silane slurry in polysilicon production process according to claim 1, it is characterized in that: above-mentioned steps 3) in, waste gas qualified discharge after the lime milk solution drip washing that spray column (9) working concentration is 10% that hydrolysis reaction produces.
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| CN201510483600.2A CN105152171A (en) | 2015-08-10 | 2015-08-10 | Special system and method for continuously recovering chlorosilane containing slurry in polycrystalline silicon production process |
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| CN201510483600.2A CN105152171A (en) | 2015-08-10 | 2015-08-10 | Special system and method for continuously recovering chlorosilane containing slurry in polycrystalline silicon production process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106621757A (en) * | 2017-02-21 | 2017-05-10 | 德山化工（浙江）有限公司 | Recovery treatment device and treatment method of chlorosilane analysis waste gases |
| CN113967360A (en) * | 2021-10-22 | 2022-01-25 | 南通友拓新能源科技有限公司 | Slurry recovery system and method in electronic-grade polycrystalline silicon production |
| CN115820386A (en) * | 2022-11-23 | 2023-03-21 | 东莞市巴能检测技术有限公司 | Compound preprocessing device of large-scale marsh gas engineering raw materials |
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| CN103420381A (en) * | 2012-05-15 | 2013-12-04 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling disposal of silicon tetrachloride slag slurry produced in polycrystalline silicon production and device thereof |
| CN204058313U (en) * | 2014-06-24 | 2014-12-31 | 吴娟 | A kind of apparatus system recycling chlorosilane slag slurry raffinate |
| CN104692391A (en) * | 2015-03-03 | 2015-06-10 | 陕西天宏硅材料有限责任公司 | Dry-process recycling method for chloro-silicane-containing slurry in polycrystalline silicon production process |
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2015
- 2015-08-10 CN CN201510483600.2A patent/CN105152171A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103420381A (en) * | 2012-05-15 | 2013-12-04 | 天华化工机械及自动化研究设计院有限公司 | Method for recycling disposal of silicon tetrachloride slag slurry produced in polycrystalline silicon production and device thereof |
| CN204058313U (en) * | 2014-06-24 | 2014-12-31 | 吴娟 | A kind of apparatus system recycling chlorosilane slag slurry raffinate |
| CN104692391A (en) * | 2015-03-03 | 2015-06-10 | 陕西天宏硅材料有限责任公司 | Dry-process recycling method for chloro-silicane-containing slurry in polycrystalline silicon production process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106621757A (en) * | 2017-02-21 | 2017-05-10 | 德山化工（浙江）有限公司 | Recovery treatment device and treatment method of chlorosilane analysis waste gases |
| CN113967360A (en) * | 2021-10-22 | 2022-01-25 | 南通友拓新能源科技有限公司 | Slurry recovery system and method in electronic-grade polycrystalline silicon production |
| CN115820386A (en) * | 2022-11-23 | 2023-03-21 | 东莞市巴能检测技术有限公司 | Compound preprocessing device of large-scale marsh gas engineering raw materials |
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Address after: 712038 Xianyang city of Shaanxi province Zhengyang town Weicheng District East Road Embankment Applicant after: Shaanxi Tianhong Silicon Material Co., Ltd. Address before: 710006 Shaanxi city of Xi'an province high tech Zone High Road No. 51 building 6 floor Applicant before: Shaanxi Tianhong Silicon Material Co., Ltd. |
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Application publication date: 20151216 |