CN104649483A - Treatment method of silicon-containing alkali wastewater in polycrystalline silicon production process - Google Patents
Treatment method of silicon-containing alkali wastewater in polycrystalline silicon production process Download PDFInfo
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- CN104649483A CN104649483A CN201510094331.0A CN201510094331A CN104649483A CN 104649483 A CN104649483 A CN 104649483A CN 201510094331 A CN201510094331 A CN 201510094331A CN 104649483 A CN104649483 A CN 104649483A
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- waste water
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Abstract
The invention discloses a treatment method of silicon-containing alkali wastewater in a polycrystalline silicon production process. The method comprises the following steps: S101, primary pressure filtration, namely carrying out primary pressure filtration on the silicon-containing alkali wastewater through a primary filter press, and separating solid from liquid in the silicon-containing alkali wastewater to obtain primary supernate; S102, neutralization reaction, namely carrying out neutralization reaction on residual NaOH and Na2SiO3 in the primary supernate with an acid liquid, and continuously stirring until the supernate is neutral to form a suspension liquid; S103, secondary pressure filtration, namely carrying out secondary pressure filtration on the suspension liquid in the step S102 through a second filter press, and realizing secondary solid-liquid separation to obtain secondary supernate; and S104, electrolytic reaction, namely conveying the secondary supernate obtained from the step S103 to an electrolytic tank to carry out electrolytic reaction. Comprehensive treatment of the silicon-containing alkali wastewater is realized by the processes of primary pressure filtration, acid neutralization, secondary pressure filtration and electrolysis; comprehensive recovery and application of resources are realized; and an accident of environmental pollution is prevented.
Description
Technical field
The present invention relates to the comprehensive processing technique relating to siliceous alkaline waste water, be specifically related to the treatment process of siliceous alkaline waste water in polysilicon production process.
Background technology
The waste gas main component produced in polysilicon production process is chlorosilane, hydrogenchloride, hydrogen and nitrogen, domestic conventional processing mode is: with alkali lye (NaOH) drip washing, chlorosilane in hydrolysis and in waste gas and hydrogen chloride gas, the silicon in waste gas and chlorine are finally dissolved or suspended in buck with the form of water glass, silicic acid and sodium-chlor.
When NaOH concentration drops to 4 ~ 5%, be dissolved in buck mesosilicic acid sodium and just can discharge, the jellied vitreum of shape; The silicic acid generated also can produce a large amount of white sediment in pond, and blocking spray pump, pipeline and nozzle, cause alkali lye elution circuit normally to carry out, the alkali lye drip washing that therefore must more renew.Changing the leacheate of discharging is strong basicity, and NaOH concentration is 4 ~ 5%, and is dissolved with a large amount of silicate, as direct discharge, can produce a large amount of white sediment, cause serious environmental pollution accident.
Summary of the invention
The technical problem to be solved in the present invention is to provide the treatment process of siliceous alkaline waste water in polysilicon production process, by process implementations such as one-level press filtration, acid neutralization, secondary press filtration, electrolysis to the comprehensive treating process of siliceous alkaline waste water, realize the comprehensive reutilization of resource, the accident that prevents the pollution of the environment occurs.
For achieving the above object, technical scheme of the present invention is as follows:
The treatment process of siliceous alkaline waste water in polysilicon production process, comprises the following steps:
S101, one-level press filtration: siliceous alkaline waste water is carried out a press filtration by one-level pressure filter, is separated by the solid-liquid in siliceous alkaline waste water, obtain one-level supernatant liquor;
S102, neutralization reaction: utilize residual NaOH and Na in acidic liquid neutralization reaction one-level supernatant liquor
2siO
3, and constantly stir until neutral, form suspension;
S103, secondary press filtration: the suspension in step S102 is carried out secondary press filtration by secondary pressure filter, realize solid-liquid secondary separation, obtains secondary supernatant;
S104, electrolytic reaction: the secondary supernatant obtained in step S103 is delivered to electrolytic tank electrolysis reaction.
In a preferred embodiment of the invention, the step of alkali lye drip washing chlorosilane waste gas was also set before step S101.
In a preferred embodiment of the invention, the acidic liquid of described step S102 adopts hydrochloric acid.
In a preferred embodiment of the invention, the Na dissolved in described hydrochloric acid and one-level supernatant liquor
2siO
3can react and generate white H
2siO
3precipitation, and at the effect low suspension stirred in a liquid, form suspension.
In a preferred embodiment of the invention, in described neutralization reaction, PH is adjusted to 6-9.
In a preferred embodiment of the invention, described secondary supernatant main ingredient is NaCl solution, and its concentration is 160000-180000mg/l.
By technique scheme, the invention has the beneficial effects as follows:
The present invention has environmental protection and economical effects, can not only process siliceous alkaline waste water in polysilicon production process, make its qualified discharge, avoid the generation of pollution incident, and can also synthetical recovery NaOH, hydrogen and chlorine etc. as byproduct, reduce running cost, decrease the wasting of resources.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is process flow sheet of the present invention.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
With reference to Fig. 1, the treatment process of siliceous alkaline waste water in polysilicon production process, comprises the following steps:
S101, one-level press filtration: siliceous alkaline waste water is carried out a press filtration by one-level pressure filter, is separated by the solid-liquid in siliceous alkaline waste water, obtain one-level supernatant liquor;
S102, neutralization reaction: utilize residual NaOH and Na in acidic liquid neutralization reaction one-level supernatant liquor
2siO
3, and constantly stir until neutral, form suspension;
S103, secondary press filtration: the suspension in step S102 is carried out secondary press filtration by secondary pressure filter, realize solid-liquid secondary separation, obtains secondary supernatant;
S104, electrolytic reaction: the secondary supernatant obtained in step S103 is delivered to electrolytic tank electrolysis reaction.
Particularly, for the press filtration of step S010 one-level: when drip washing waste gas alkali lye (NaOH) density loss to 4 ~ 5% time, with pump, siliceous alkaline waste water is squeezed into one-level pressure filter, carries out a press filtration, realize solid-liquid separation.In a pressure-filtering process, not tolerant in siliceous alkaline waste water, tackled by pressure filter in solid form, its main component is silicon-dioxide and silicic acid; In siliceous alkaline waste water can be tolerant, then through one-level pressure filter in liquid form by Filter Press, form one-level supernatant liquor.
The chemical reaction occurred with alkali lye (NaOH) drip washing chlorosilane waste gas is as follows:
SiHCl
3+2H
2O→SiO
2+3HCl+H
21
SiH2Cl
2+2H
2O→SiO
2+2HCl+2H
22
SiCl
4+2H
2O→SiO
2+4HCl 3
HCl+NaOH→NaCl+H
2O 4
SiO
2+2NaOH→Na
2SiO
3+H
2O 5
2, for step S010 neutralization reaction and S103 bis-press filtrations.Acid adding secondary press filtration: the one-level supernatant liquor that one-level press filtration produces to reactor by pump delivery, under the stirring action of stirrer, is added hydrochloric acid, makes the remaining hydrogen sodium oxide in supernatant liquor and hydrochloric acid that uniform neutralization reaction occur in reactor.
In and stirring reaction process in, along with the reduction gradually of supernatant liquor basicity, the Na dissolved in supernatant liquor
2siO
3total overall reaction can generate white H
2siO
3precipitation, and at the effect low suspension stirred in a liquid.
When the PH of neutralization reaction is adjusted to 6 ~ 9, by the H of neutrality
2siO
3suspension carries out secondary press filtration by pump delivery to secondary pressure filter, realizes solid-liquid secondary separation.
In secondary pressure-filtering process, the white H that neutralization reaction generates
2siO
3precipitation, is tackled by pressure filter in solid form; And the solvable NaCl that neutralization reaction generates, then pass secondary pressure filter in liquid form by Filter Press, form the secondary supernatant containing NaCl.The chemical reaction that acid neutralization one-level supernatant liquor occurs is as follows:
NaOH+HCl→NaCl+H
2O 6
Na
2SiO
3+2HCl→2NaCl+H
2SiO
37
3, electrolytic recovery: the secondary supernatant that secondary press filtration produces is water white transparency, and PH is between 6 ~ 9, and main ingredient is NaCl solution, and its concentration is between 160000-180000mg/l.This water white transparency sodium chloride solution is delivered to electrolytic tank electrolysis, and anode generates chlorine, and negative electrode generates hydrogen, and sodium ion is combined with hydroxide radical and generates NaOH in the process.Secondary supernatant electrolytic reaction is as follows:
Negative electrode: 2H
++ 2e
-=H
2↑ 8
Anode: 2Cl
--2e
-=Cl
2↑ 9
Total reaction: NaCl+H
2o====2NaOH+H
2↑+Cl
2↑
The present invention is by processes such as one-level press filtration, acid neutralization, secondary press filtration, electrolysis, achieve the comprehensive treating process to alkaline waste water siliceous in polysilicon production process, the siliceous alkaline waste water that can not only produce in process polysilicon production process up to standard, avoid the generation of environmental pollution accident, can also synthetical recovery NaOH, hydrogen and chlorine etc. as byproduct, reduce running cost, decrease the wasting of resources, there is the double benefit of environmental protection and economic two aspects.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. the treatment process of siliceous alkaline waste water in polysilicon production process, is characterized in that, comprise the following steps:
S101, one-level press filtration: siliceous alkaline waste water is carried out a press filtration by one-level pressure filter, is separated by the solid-liquid in siliceous alkaline waste water, obtain one-level supernatant liquor;
S102, neutralization reaction: utilize residual NaOH and Na in acidic liquid neutralization reaction one-level supernatant liquor
2siO
3, and constantly stir until neutral, form suspension;
S103, secondary press filtration: the suspension in step S102 is carried out secondary press filtration by secondary pressure filter, realize solid-liquid secondary separation, obtains secondary supernatant;
S104, electrolytic reaction: the secondary supernatant obtained in step S103 is delivered to electrolytic tank electrolysis reaction.
2. the treatment process of siliceous alkaline waste water in polysilicon production process according to claim 1, is characterized in that, also arrange the step of alkali lye drip washing chlorosilane waste gas before step S101.
3. in the polysilicon production process according to right 1, the treatment process of siliceous alkaline waste water, is characterized in that, the described acidic liquid employing hydrochloric acid requiring step S102.
4. the treatment process of siliceous alkaline waste water in polysilicon production process according to claim 3, is characterized in that, the Na dissolved in described hydrochloric acid and one-level supernatant liquor
2siO
3can react and generate white H
2siO
3precipitation, and at the effect low suspension stirred in a liquid, form suspension.
5. the treatment process of siliceous alkaline waste water in polysilicon production process according to claim 1, is characterized in that, in described neutralization reaction, PH is adjusted to 6-9.
6. the treatment process of siliceous alkaline waste water in polysilicon production process according to claim 1, it is characterized in that, described secondary supernatant main ingredient is NaCl solution, and its concentration is 160000-180000mg/l.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668862A (en) * | 2016-04-15 | 2016-06-15 | 林淑录 | Method for recycling sodium hydroxide containing waste water in silicon wafer production process |
| CN105731487A (en) * | 2016-03-07 | 2016-07-06 | 四川理工学院 | Method for resource utilization of exhaust gas alkaline-washing waste residues generated in polysilicon production |
| CN110615517A (en) * | 2019-09-07 | 2019-12-27 | 山东九思新材料科技有限责任公司 | Alkaline silicon washing alkaline sewage treatment device and use method thereof |
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| US20070256972A1 (en) * | 2003-06-19 | 2007-11-08 | Kansai Paint Co., Ltd. | Process for Purification Treatment of Wastewater Containing Organic Substance |
| CN203899432U (en) * | 2013-09-16 | 2014-10-29 | 陕西天宏硅材料有限责任公司 | Waste gas leaching wastewater treatment device for polycrystalline silicon production |
| CN104230049A (en) * | 2014-09-01 | 2014-12-24 | 上海希瑞歌恩环境技术有限公司 | Wastewater treatment method in photovoltaic industry |
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2015
- 2015-03-03 CN CN201510094331.0A patent/CN104649483A/en active Pending
Patent Citations (3)
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| US20070256972A1 (en) * | 2003-06-19 | 2007-11-08 | Kansai Paint Co., Ltd. | Process for Purification Treatment of Wastewater Containing Organic Substance |
| CN203899432U (en) * | 2013-09-16 | 2014-10-29 | 陕西天宏硅材料有限责任公司 | Waste gas leaching wastewater treatment device for polycrystalline silicon production |
| CN104230049A (en) * | 2014-09-01 | 2014-12-24 | 上海希瑞歌恩环境技术有限公司 | Wastewater treatment method in photovoltaic industry |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731487A (en) * | 2016-03-07 | 2016-07-06 | 四川理工学院 | Method for resource utilization of exhaust gas alkaline-washing waste residues generated in polysilicon production |
| CN105731487B (en) * | 2016-03-07 | 2018-02-09 | 四川理工学院 | A kind of method utilized to waste gas in production of polycrystalline silicon alkali cleaning waste residue resource |
| CN105668862A (en) * | 2016-04-15 | 2016-06-15 | 林淑录 | Method for recycling sodium hydroxide containing waste water in silicon wafer production process |
| CN110615517A (en) * | 2019-09-07 | 2019-12-27 | 山东九思新材料科技有限责任公司 | Alkaline silicon washing alkaline sewage treatment device and use method thereof |
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Application publication date: 20150527 |
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