CN105920986A - Process and device for treating tail gas and/or residual liquid in polycrystalline silicon production - Google Patents
Process and device for treating tail gas and/or residual liquid in polycrystalline silicon production Download PDFInfo
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- CN105920986A CN105920986A CN201610341094.8A CN201610341094A CN105920986A CN 105920986 A CN105920986 A CN 105920986A CN 201610341094 A CN201610341094 A CN 201610341094A CN 105920986 A CN105920986 A CN 105920986A
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- acid water
- tail gas
- water
- eluting column
- filtrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/40—Alkaline earth metal or magnesium compounds
- B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a process and device for treating tail gas and/or residual liquid in polycrystalline silicon production. According to the process, firstly, the tail gas and/or the residual liquid are fed into an elution column, weak-acid water with the mass concentration being 2-5% is used for carrying out spraying and washing at a countercurrent state, washed gas enters a liquid sealing tank to be purified through clean water, the finally released gas is discharged into air, and washed liquid serves as weak-acid water to carry out circular spraying; after the weak-acid water for circular spraying in the first step exceeds the limited concentration, part of waste acid water is drained, water is added to dilute the weak-acid water until the needed concentration is achieved, then, the weak-acid water continues to be used, lime emulsion is added into the exhausted waste acid water to neutralize the exhaust waste acid water, then, a pressure filter is used for carrying out filtering, part of filtrate is reused, and other filtrate and filter residues are discharged. The process and the device ensure that the treated tail gas reaches the standard and then is discharged; blockage of a spray head, a pipeline and equipment is avoided, and operation is safe and easy; part of the filtrate is reused, the chemical engineering waste acetylene sludge emulsion is recovered and used, the water consumption is reduced, and the treating cost for tail and/or residual liquid is saved.
Description
Technical field
The invention belongs to tail gas and residual liquid process field in production of polysilicon, be specifically related to tail gas and/or residual liquid in production of polysilicon
Process technique and device.
Background technology
At present in the vent gas treatment in production of polysilicon, in the Sealing Arrangement of water seal, using two-step purification to process, one-level is used
10% lime slurry circulated sprinkling under concurrent flow conditions, two grades purify with 10% lime slurry of circulation in liquid seal can, produce
Incoagulable gas emptying；When, after circulation fluid PH=6-9, being sent directly into pressure filter solid-liquid separation, arranging outside filtrate, waste residue is straight
Connect outward transport.It is in the Sealing Arrangement of the band stirring paddle of nitrogen envelope that residual liquid processes, and neutralizes with 10% lime slurry, then uses nitrogen
Being pressed in collecting tank by waste liquid, send into pressure filter solid-liquid separation, arrange outside filtrate, waste residue is directly transported outward.
During 10% lime slurry processes tail gas and residual liquid, due to the agglomeration problems of hydrolysate, it is easy to cause equipment,
Pipeline, the blocking of nozzle；After blocking, the effect of equipment drip washing is bad, and tail gas absorption is incomplete, and the tail gas of discharge is difficult to reach
Mark, and the workload of block clearing is big, load weight, material waste is serious.
Summary of the invention
It is an object of the invention to provide in a kind of production of polysilicon tail gas and/or residual liquor treating process and device；Can effectively process many
Tail gas and/or residual liquid in crystal silicon production, equipment is less scaling and blocks, and extends service life, and operates safe and simple.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: in production of polysilicon, tail gas and/or residual liquid process
Technique, it is characterised in that specifically include following steps:
1) tail gas and/or residual liquid are sent in eluting column, use mass concentration 2-5% weak acid water to carry out spray at reverse flow state clear
Washing, the gas after cleaning uses clear water to purify in entering liquid seal can, gas emptying the most out；Liquid after cleaning
As weak acid water circulated sprinkling；
2) step 1) in after the weak acid water of circulated sprinkling exceedes limiting concentration, be diluted with water to required after discharging part waste acid water
Concentration is continuing with, and it is 7-8 that the waste acid water of discharge add lime slurry to be neutralized to pH, then uses pressure filter to carry out
Filter, reuse portion filtrate, remaining filtrate and filtering residue carry out outer row.
Further, during described weak acid water cleaning showers, use hollow cone eddy current spraying nozzle spray weak acid water.Can change existing
Spiral nozzle easily block, blocking cleaning work amount is big and feature frequently.Hollow cone eddy current spraying nozzle is under the influence of centrifugal force
It is operated, its material spray angle, area coverage, uninterrupted, sets according to design parameter.During spray, material will not block
Shower nozzle, drip washing is effective, it is ensured that equipment and the tank connected exhausting pipeline of fluid-tight unobstructed.
Further, described hollow cone eddy current spraying nozzle is from top to bottom set to multistage in eluting column.General employing three grades is hollow
Cone eddy current spraying nozzle design, multilevel design, by increasing capacitance it is possible to increase the contact area of tail gas and/or residual liquid and weak acid water so that tail gas and/
Or the poisonous and harmful element in residual liquid can enter in weak acid water after as much as possible being cleaned by.
Further, described mass concentration 10% lime slurry uses industrial waste carbide slag to be prepared and forms.Due to industry
The carbide quantity of slag is big, and processing cost is high, is used in acid-base neutralization environment, just turns waste into wealth, reduce tail in the present invention
Gas and the processing cost of residual liquid.Industrial electro rock ballast is processed simultaneously；The carbide slag cream of outward transport is after over cleaning, first
Send in the dump skip of band agitating device and configure, after concentration meets requirement, sent into by loop network and use point to use.
Further, described step 2) in reuse portion filtrate be to be used for configuring lime slurry by filtrate.By reclaiming filtrate,
Minimizing water consumption, reduces processing cost.The mass concentration of configuration lime slurry is 10%.
The invention still further relates to tail gas and/or residual liquid processing apparatus in production of polysilicon, including eluting column and the fluid-tight that is attached thereto
Tower, eluting column is also associated with circulatory pool, and circulatory pool connects neutralization pond, and neutralization pond connects pressure filter；This device also includes stone
Ash breast make-up tank, lime cream make-up tank connects neutralization pond by pump and pipeline.
Further, this device also includes that accident pool, lime cream make-up tank are connected to accident pool by pump and pipeline.Accident pool
For emergency disposal, when emergency episode (as having a power failure suddenly) occurs, for the equipment of keeping the scene intact or avoid generating process, peace
Full accidents etc., can process on-the-spot tail gas incision equipped with the accident pool of lime slurry immediately.
Further, this device is additionally provided with tail gas buffer, and it is arranged on the front end of eluting column, described eluting column and fluid-tight
Tower everybody two set, can be used for processing tail gas and residual night respectively.
Further, the liquid outlet of described fluid-tight tower is connected to the spray inlet of eluting column；Water in liquid seal can drench
Washing in tower and recycle, the generation of minimizing waste liquid is with outer, and using water wisely.
Further, being additionally provided with Buffer Pool between described eluting column and circulatory pool, Buffer Pool is also associated with inlet channel.Drench
Wash and be all connected by overflow pipe between tower with Buffer Pool, Buffer Pool and circulatory pool, when the liquid in eluting column arrives certain
During storage capacity, overflow to Buffer Pool, subsequently into circulatory pool.Again pumped into by circulating pump in eluting column tail gas and/or residual
Liquid is carried out, when the weak acid temperature detected in Buffer Pool and content exceed technic index, if do not processed,
The effect that weak acid absorbs will decline, it should will discharge a part of liquid to neutralization pond, then addition service water in Buffer Pool
It is diluted and lowers the temperature.The lime slurry of liquid in neutralization pond addition simultaneously is stirred neutralizing, and is then pumped into pressure filter
In filter, carry out solid-liquid separation, filtrate portion reuse, the outer row of part, waste residue outward transport is buried.
Under involved technological principle, tail gas and/or residual liquid interact with aqueous solution, there is the exothermic reaction of hydrolyzing chlorosilane,
So that the reaction equation that tail gas is cleaned is as follows:
SiH2Cl2+3H2O=SiO2·H2O+2HCl+2H2↑
SiHCl3+3H2O=SiO2·H2O+3HCl+H2↑
SiCl4+3H2O=SiO2·H2O+4HCl
The hydrogen chloride gas that hydrolysis generates is only absorbed by the water, and generates weak hydrochloric acid solution, is neutralized by Calx by following reaction equation:
2HCl+Ca(OH)2=CaCl2+2H2O
The invention have the benefit that
Using weak acid water spray chlorosilane tail gas and/or residual liquid, with traditional with compared with lime cream spray, one effectively reduces
The consumption of lime cream, owing to lime cream easily precipitates, its effective ingredient does not has fully utilized during circulated sprinkling, thus
Causing consuming height, processing cost is the highest；And spray with weak acid water, add the sour water that clear water cements out, directly stir neutralization,
Avoid lime cream precipitation, reduce lime cream consumption, reduce processing cost；Two solve glass during lime cream spray
Temperature rise problem faster in glass steel equipment, particularly solve the winter inside and outside temperature difference of equipment big, and equipment expands with heat and contract with cold and causes
Material ageing problem, it is ensured that the service life of equipment；During three avoid lime cream spray, easy fouling in equipment,
Occluding device, pipeline, the problem of nozzle, reduce the workload of block clearing equipment, it is ensured that operation safe, simple.
The present invention is applicable to polycrystalline silicon producing device, is effectively increased the cycle of operation of equipment, solves equipment, pipeline, spray
Mouth holds susceptible to plugging problem.Relative to 10% current lime slurry spray process, all of equipment each 1 with 1 standby totally 2,
Number of devices is few, and cost is low, and safely, simply, drip washing is effective, without block clearing in the cycle of operation of half a year in operation；Disappear
Consumption cost, maintenance cost are the most both economical rationally.
Accompanying drawing explanation
Fig. 1 is assembly of the invention structural representation.
Fig. 2 is the process chart of the present invention.
Detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment and attached Fig. 1 and 2, but the scope of protection of present invention not office
It is limited to the scope of embodiment statement.
Tail gas and/or residual liquor treating process in production of polysilicon, specifically include following steps:
1) tail gas and/or residual liquid are sent in eluting column, use mass concentration 2-5% weak acid water to carry out spray at reverse flow state clear
Washing, the gas after cleaning uses clear water to purify in entering liquid seal can, gas emptying the most out；Liquid after cleaning
As weak acid water circulated sprinkling；
2) step 1) in after the weak acid water of circulated sprinkling exceedes limiting concentration, be diluted with water to required after discharging part waste acid water
Concentration is continuing with, and the waste acid water of discharge adds lime slurry and is neutralized, and then uses pressure filter to filter, reuse portion
Dividing filtrate, remaining filtrate and filtering residue carry out outer row.
During described weak acid water cleaning showers, use hollow cone eddy current spraying nozzle spray weak acid water.
Described hollow cone eddy current spraying nozzle is from top to bottom set to multistage in eluting column.
Described lime slurry uses industrial waste carbide slag to be prepared and forms.
Described step 2) in reuse portion filtrate be that filtrate is used for configuration quality concentration 10% lime slurry.
Concrete technological process explanation:
1, prepared by carbide slag emulsion: the carbide slag cream of outward transport, after over cleaning, is sent in the dump skip of band agitating device and carried out
Configuration, after concentration meets technological requirement, is sent into by loop network and uses point to use.
2, vent gas treatment: tail gas enters after tail gas buffer, sends in eluting column, weak acid water under reverse flow state with three grades
Hollow cone eddy current spraying nozzle cleans, and removes in tail gas after poisonous and harmful element, and tail gas enters back into liquid seal can by double purification, tail gas
Thoroughly cleaned up, last incoagulable gas emptying.
3, residual liquid processes: residual liquid is sent in eluting column, and weak acid water cleans with three grades of hollow cone eddy current spraying nozzles under reverse flow state,
After removing its poisonous and harmful element, tail gas enters back into liquid seal can and is thoroughly cleaned up by double purification, tail gas, last not
Solidifying property gas emptying.
4, waste collection and process: in lessivation, chlorosilane tail gas and residual liquid hydrolysate, the weak acid water band circulated
Entering Buffer Pool, enter circulatory pool by overflow and be circulated spray again, in pond being detected, weak acid temperature and density once exceed
Technic index, the effect that weak acid absorbs will decline, and just add plant water cooling, dilution weak acid concentration in pond.Meanwhile, put
The spent acid swapped out enters neutralization pond by overflow, after being neutralized on the spot by carbide slag emulsion in the neutralization pond of band agitating device,
Sending into pressure filter with centrifugal pump and carry out solid-liquid separation, filtrate portion reuse, the outer row of part, waste residue outward transport is buried.
5, emergency disposal: when emergency episode (as having a power failure suddenly) occurs, for the equipment of keeping the scene intact or avoid generating process,
Security incidents etc., can process on-the-spot tail gas incision equipped with the accident pool of lime slurry immediately.
Tail gas and/or residual liquid processing apparatus in production of polysilicon, including eluting column 1 and the fluid-tight tower 2 that is attached thereto, eluting column
1 is also associated with circulatory pool 3, and circulatory pool 3 connects neutralization pond 4, and neutralization pond connects pressure filter 5；This device also includes Calx
Breast make-up tank 6, lime cream make-up tank 6 connects neutralization pond 4 by pump and pipeline.
This device also includes that accident pool 7, lime cream make-up tank 6 are connected to accident pool by pump and pipeline.
This device is additionally provided with tail gas buffer 8, uses Q235 material, and it is arranged on the front end of eluting column, described eluting column
1 and liquid seal can 2 be respectively two sets.Eluting column, liquid seal can are FRP glass steel material, circulatory pool, neutralization pond, accident pool etc.
For mixed reinforced concrete structure.
The liquid outlet of described fluid-tight tower 2 is connected to the spray inlet of eluting column 1.
Being additionally provided with Buffer Pool 9 between described eluting column 1 and circulatory pool 3, Buffer Pool 9 is also associated with inlet channel.
Chamber-type press filter and centrifugal filter pressing pump is may select during filter pressing.
Claims (10)
1. tail gas and/or residual liquor treating process in production of polysilicon, it is characterised in that specifically include following steps:
1) sending in eluting column by tail gas and/or residual liquid, use mass concentration 2-5% weak acid water to carry out cleaning showers at reverse flow state, the gas after cleaning uses clear water to purify in entering liquid seal can, gas emptying the most out；Liquid after cleaning is as weak acid water circulated sprinkling；
2) after in step 1), the weak acid water of circulated sprinkling exceedes limiting concentration, it is diluted with water to desired concn after discharging part waste acid water be continuing with, discharge waste acid water add lime slurry be neutralized to pH be 7-8, then pressure filter is used to filter, reuse portion filtrate, remaining filtrate and filtering residue carry out outer row.
Technique the most according to claim 1, it is characterised in that: during described weak acid water cleaning showers, use hollow cone eddy current spraying nozzle spray weak acid water.
Technique the most according to claim 2, it is characterised in that: described hollow cone eddy current spraying nozzle is from top to bottom set to multistage in eluting column.
Technique the most according to claim 1, it is characterised in that: described mass concentration 10% lime slurry uses industrial waste carbide slag to be prepared and forms.
Technique the most according to claim 1, it is characterised in that: described step 2) in reuse portion filtrate be to be used for configuring lime slurry by filtrate.
6. tail gas and/or residual liquid processing apparatus in production of polysilicon, it is characterized in that: include eluting column (1) and the fluid-tight tower (2) being attached thereto, eluting column (1) is also associated with circulatory pool (3), and circulatory pool (3) connects neutralization pond (4), and neutralization pond connects pressure filter (5)；This device also includes lime cream make-up tank (6), and lime cream make-up tank (6) connects neutralization pond (4) by pump and pipeline.
Device the most according to claim 6, it is characterised in that: this device also includes that accident pool (7), lime cream make-up tank (6) are connected to accident pool by pump and pipeline.
Device the most according to claim 6, it is characterised in that: this device is additionally provided with tail gas buffer (8), its be arranged on the front end of eluting column, described eluting column (1) and fluid-tight tower (2) everybody two set.
Device the most according to claim 6, it is characterised in that: the liquid outlet of described fluid-tight tower (2) is connected to the spray inlet of eluting column (1).
Device the most according to claim 6, it is characterised in that: being additionally provided with Buffer Pool (9) between described eluting column (1) and circulatory pool (3), Buffer Pool (9) is also associated with inlet channel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610341094.8A CN105920986A (en) | 2016-05-20 | 2016-05-20 | Process and device for treating tail gas and/or residual liquid in polycrystalline silicon production |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610341094.8A CN105920986A (en) | 2016-05-20 | 2016-05-20 | Process and device for treating tail gas and/or residual liquid in polycrystalline silicon production |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108926960A (en) * | 2018-08-31 | 2018-12-04 | 四川永祥新能源有限公司 | A kind of processing method of cold hydrogenated tail gas |
| CN108947030A (en) * | 2018-09-27 | 2018-12-07 | 中石化南京工程有限公司 | A kind of polysilicon exhaust gas washing liquid processing device and method |
| CN114410704A (en) * | 2022-02-15 | 2022-04-29 | 上海云洛生物技术有限公司 | Method for biologically synthesizing vitronectin |
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|---|---|---|---|---|
| CN108926960A (en) * | 2018-08-31 | 2018-12-04 | 四川永祥新能源有限公司 | A kind of processing method of cold hydrogenated tail gas |
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| CN114410704A (en) * | 2022-02-15 | 2022-04-29 | 上海云洛生物技术有限公司 | Method for biologically synthesizing vitronectin |
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