CN204824191U - Dedicated system is retrieved in succession to chloride silane thick liquids in polycrystalline silicon production process - Google Patents
Dedicated system is retrieved in succession to chloride silane thick liquids in polycrystalline silicon production process Download PDFInfo
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- CN204824191U CN204824191U CN201520601149.5U CN201520601149U CN204824191U CN 204824191 U CN204824191 U CN 204824191U CN 201520601149 U CN201520601149 U CN 201520601149U CN 204824191 U CN204824191 U CN 204824191U
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Abstract
The utility model provides a dedicated system is retrieved in succession to chloride silane thick liquids in polycrystalline silicon production process, thick liquids agitator tank top is equipped with water cooling circulation and congeals ware I, thick liquids agitator tank exit end and drying -machine entry end intercommunication, the exit end of drying -machine and the entry end intercommunication of screw pump, the exit end and the spray column circulating slot entry end intercommunication of screw pump, exit end and spray column intercommunication, another exit end and the low reaches waste water unit entry end intercommunication of spray column circulating slot of spray column circulating slot, the water cooling circulation that tank deck portion was retrieved at the chlorosilane to another exit end and the setting of drying -machine congeals II entry ends of ware intercommunication, and the chlorosilane is retrieved tank deck portion and still is equipped with the ethylene glycol heat exchanger. The utility model discloses can realize the continuous drying process of thick liquids, ensure main technique unit recycle, the sediment thick liquid after the stoving is avoided the drying -machine once only to arrange sediment hydrolysis reaction and is produced hydrogen and heat through the slow transport of screw pump to the hydrolyze neutralization reaction of system that hydrolysises, and the system moves safety and stability more.
Description
Technical field
The utility model belongs to technical field of polysilicon production, is specifically related to chlorine-containing silane slurry in a kind of polysilicon production process and reclaims patent system 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.
Utility model content
The technical problem that the utility model solves: provide chlorine-containing silane slurry in a kind of polysilicon production process to reclaim dedicated system 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 adopted in the utility model: 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 utility model 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 the utility model structural representation.
Embodiment
Below in conjunction with accompanying drawing 1, a kind of embodiment of the present utility model 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 utility model 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 utility model, 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 utility model, is not used for limiting the utility model practical range, therefore all equivalence changes done with content described in the utility model claim, all should be included within the utility model right.
Claims (1)
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).
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| CN201520601149.5U CN204824191U (en) | 2015-08-10 | 2015-08-10 | Dedicated system is retrieved in succession to chloride silane thick liquids in polycrystalline silicon production process |
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| CN201520601149.5U CN204824191U (en) | 2015-08-10 | 2015-08-10 | Dedicated system is retrieved in succession to chloride silane thick liquids in polycrystalline silicon production process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043406A (en) * | 2022-06-24 | 2022-09-13 | 新疆协鑫新能源材料科技有限公司 | Treatment device and method for polycrystalline silicon waste |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115043406A (en) * | 2022-06-24 | 2022-09-13 | 新疆协鑫新能源材料科技有限公司 | Treatment device and method for polycrystalline silicon waste |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP02 | Change in the address of a patent holder |
Address after: 712038 Xianyang city of Shaanxi province Zhengyang town Weicheng District East Road Embankment Patentee after: Shaanxi Tianhong Silicon Material Co., Ltd. Address before: High road high tech Zone of Xi'an City, Shaanxi province 710006 Xianyang City No. 51 Gaoxin building 6 floor Patentee before: Shaanxi Tianhong Silicon Material Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151202 Termination date: 20190810 |
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| CF01 | Termination of patent right due to non-payment of annual fee |