CN206985725U - Silicon tetrachloride devil liquor recovery processing unit - Google Patents
Silicon tetrachloride devil liquor recovery processing unit Download PDFInfo
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- CN206985725U CN206985725U CN201720886842.0U CN201720886842U CN206985725U CN 206985725 U CN206985725 U CN 206985725U CN 201720886842 U CN201720886842 U CN 201720886842U CN 206985725 U CN206985725 U CN 206985725U
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Abstract
The utility model provides a kind of silicon tetrachloride devil liquor recovery processing unit, wherein, after silicon tetrachloride waste liquid enters rectifying column, the reboiler is used to be evaporated it processing to form gas phase silicon tetrachloride and be exported from tower top, and the silicon tetrachloride waste liquid after handling is discharged from tower bottom of rectifying tower；It is output after liquid phase silicon tetrachloride to silicon tetrachloride return tank that first condenser, which is used for gas phase silicon tetrachloride condensation,；Partial Liquid Phase silicon tetrachloride in the silicon tetrachloride return tank is back to rectifying column tower top, and another part liquid phase silicon tetrachloride is produced to silicon tetrachloride recycling can；The residue hydrolyzer is used to the silicon tetrachloride waste liquid after the processing be hydrolyzed processing to form raffinate；The candle filter is used to carry out separation of solid and liquid processing to the raffinate and discharged respectively.It is silicon tetrachloride devil liquor recovery processing unit economy described in the utility model, environmental protection, easy to operate.
Description
Technical field
It the utility model is related to technical field of polysilicon production, and in particular to a kind of silicon tetrachloride devil liquor recovery processing dress
Put.
Background technology
At present, the international market price of polysilicon persistently drops, and each production of polysilicon manufacturer typically adopts to enhance the competitiveness
Taking reduces production cost and both approach of raising product quality.
With gradually reducing for production of polysilicon cost, using the Main By product four of improved Siemens production polysilicon
The problem of silicon chloride, its safety and environmental protection and recycling, causes everybody extensive concern.Wherein, silicon tetrachloride is high toxicity thing
Matter, easily deliquescence, react generation silicic acid and hydrogen chloride with water, if directly discharge can to human and environment generation high risks, it is necessary to
It is recycled.
Although each manufacturer has been able to be converted into silicon tetrachloride as by-product by cold hydrogenation process, or hot hydrogenation process
Production of polysilicon raw material trichlorosilane, but substantial amounts of silicon tetrachloride waste liquid is still inevitably produced in the conversion process, this
Have become the bottleneck for restricting polysilicon development.
Mainly there is the source of silicon tetrachloride waste liquid in polysilicon production process：The ring waste of chlorosilane synthesizing section, four
Silicon chloride rectifying dedirt raffinate and tail gas condensing recovered liquid.Silicon tetrachloride waste liquid composition mainly includes：Silicon tetrachloride, diatomic silicon
Chlorosilane and polyatom silicon chlorosilane, metallic chloride impurities, silica flour, polychlorostyrene silane and dust etc..
The difficult point and key of silicon tetrachloride liquid waste processing are that impurity is more, complicated components, and boiling point approaches between each component, are separated
Recovery difficult is big.In addition, the metal chloride in waste liquid easily deposits on condensing plant wall, equipment is caused to block.
Prior art predominantly stays in the hydrolysis stage of extensive style to the processing mode of silicon tetrachloride waste liquid or produced low
The white carbon of poor products matter, this is both the waste to raw material, and also human and environment will be damaged.
Therefore, the technology that a kind of device that can effectively recycle silicon tetrachloride waste liquid turns into urgently to be resolved hurrily at present is designed
Problem.
Utility model content
Technical problem to be solved in the utility model is to be directed to the drawbacks described above in the presence of prior art, there is provided a kind of
Economic, environmentally friendly, easy-operating silicon tetrachloride devil liquor recovery processing unit.
Technical scheme is used by solving the utility model technical problem：
The utility model provides a kind of silicon tetrachloride devil liquor recovery processing unit, and it includes rectifying column, positioned at rectifying tower
The reboiler of kettle, the first condenser positioned at rectifying column tower top, silicon tetrachloride return tank, silicon tetrachloride recycling can, residue hydrolysis
Device and candle filter, after silicon tetrachloride waste liquid enters rectifying column, the reboiler is used to be evaporated it processing to be formed
Gas phase silicon tetrachloride is simultaneously exported from tower top, and the silicon tetrachloride waste liquid after handling is discharged from tower bottom of rectifying tower；First condensation
It is output after liquid phase silicon tetrachloride to silicon tetrachloride return tank that device, which is used for gas phase silicon tetrachloride condensation,；The silicon tetrachloride
Partial Liquid Phase silicon tetrachloride in return tank is back to rectifying column tower top, and another part liquid phase silicon tetrachloride is produced to silicon tetrachloride
Recycling can；The residue hydrolyzer is used to the silicon tetrachloride waste liquid after the processing be hydrolyzed processing to form raffinate；Institute
Candle filter is stated to be used to carry out separation of solid and liquid processing to the raffinate and discharge respectively.
Alternatively, silicon tetrachloride waste liquid enters wherein from the middle and lower part of rectifying column, and the reboiler is specifically used for entering
To form silicon tetrachloride vapor, the silicon tetrachloride of rising steams for part heating vaporization in the silicon tetrachloride waste liquid of tower bottom of rectifying tower
During vapour and the silicon tetrachloride waste liquid counter current contacting declined, the part silicon tetrachloride in waste liquid is transferred to silicon tetrachloride vapor
In, while the impurity in silicon tetrachloride vapor is transferred in waste liquid, so as to form pure gas phase silicon tetrachloride and from rectifying column
Tower top exports, after absorbing waste liquid that the impurity in silicon tetrachloride vapor and part silicon tetrachloride separate therefrom as handling
Silicon tetrachloride waste liquid is discharged from tower bottom of rectifying tower.
Alternatively, the reflux ratio of the rectifying column is 2~3.
Alternatively, it is provided with reflux pump on the silicon tetrachloride return tank to the pipeline of rectifying column tower top.
Alternatively, the solids that the candle filter is isolated directly discharges after centralized burning, and isolates
Liquid is emitted into waste water downstream treatment process after pH value is adjusted to neutrality.
Alternatively, it is provided with Pulp pump on the residue hydrolyzer to the pipeline of candle filter.
Alternatively, the pipeline of the residue hydrolyzer to candle filter is managed using CPVC.
Alternatively, in addition to activated carbon feeding device, it is connected with tower bottom of rectifying tower, for the inlet amount according to rectifying column
The activated carbon granule of predetermined amount, the tetrachloro after the processing of the activated carbon granule and tower bottom of rectifying tower are periodically added into tower
After silicon tetrachloride high polymer in SiClx waste liquid is adsorbed, discharged from tower reactor.
Alternatively, in addition to plate-type evaporator and the second condenser, the plate-type evaporator are used to arrange tower bottom of rectifying tower
Silicon tetrachloride waste liquid after the processing gone out carries out intermittent-heating evaporation, and the gas phase silicon tetrachloride obtained after evaporation is exported to the
Two condensers, and the residue obtained after evaporating is exported to residue hydrolyzer, and processing is hydrolyzed by residue hydrolyzer；Described second
Condenser is used to return the gas phase silicon tetrachloride condensation of plate-type evaporator output for output after liquid phase silicon tetrachloride to silicon tetrachloride
Closed cans.
Alternatively, second condenser is located at the top of plate-type evaporator.
Beneficial effect：
Silicon tetrachloride devil liquor recovery processing unit described in the utility model can efficiently separate the silicon tetrachloride in waste liquid,
Other materials in can also preferably disposing waste liquid, there is economic, environmental protection, and silicon tetrachloride rate of recovery height, quality are good in waste liquid
The advantages that.
Brief description of the drawings
Fig. 1 is the schematic diagram for the silicon tetrachloride devil liquor recovery processing unit that the utility model embodiment provides.
In figure：1- rectifying columns；2- reboilers；The condensers of 3- first；4- silicon tetrachloride recycling cans；5- activated carbons add
Expect device；6- plate-type evaporators；The condensers of 7- second；8- silicon tetrachloride recycling cans；9- residue hydrolyzers；10- candle formulas
Filter；11- reflux pumps；12- Pulp pumps.
Embodiment
To make those skilled in the art more fully understand the technical solution of the utility model, with reference to the accompanying drawings and examples
The utility model is described in further detail.
The utility model embodiment provides a kind of economic, environmental protection, the silicon tetrachloride devil liquor recovery processing unit of easy-operation type.
Wherein, silicon tetrachloride waste liquid include silicon tetrachloride, diatomic silicon chlorosilane and polyatom silicon chlorosilane, metallic chloride impurities,
Silica flour, polychlorostyrene silane and dust etc..
As shown in figure 1, the recycling and processing device includes rectifying column 1, the reboiler 2 positioned at tower bottom of rectifying tower, positioned at essence
Evaporate the first condenser 3, silicon tetrachloride return tank 4, silicon tetrachloride recycling can 8, residue hydrolyzer 9 and the candle filter of column overhead
10.After silicon tetrachloride waste liquid enters rectifying column 1, the reboiler 2 is used to be evaporated it processing to form not dust-laden, purity
Higher gas phase silicon tetrachloride is simultaneously exported from tower top, and the silicon tetrachloride waste liquid after handling is discharged from tower bottom of rectifying tower；Described
It is output after liquid phase silicon tetrachloride to silicon tetrachloride return tank 4 that one condenser 3, which is used for gas phase silicon tetrachloride condensation,；It is described
Partial Liquid Phase silicon tetrachloride in silicon tetrachloride return tank 4 is back to rectifying column tower top, the extraction of another part liquid phase silicon tetrachloride
To silicon tetrachloride recycling can 8 with recycling；The residue hydrolyzer 9 is used to lead to the silicon tetrachloride waste liquid after the processing
Cross aqua calcis and processing is hydrolyzed to form raffinate；The candle filter 10 is used to carry out solid-liquid point to the raffinate
Discharge from processing and respectively.
Specifically, silicon tetrachloride waste liquid enters wherein from the middle and lower part of rectifying column 1, i.e., is fed from rectifying column middle and lower part, essence
Tower atmospheric operation is evaporated, operating temperature is 60~70 DEG C, and the reboiler 2 is specifically used for that the silicon tetrachloride of tower bottom of rectifying tower will be entered
Part heating in waste liquid is vaporized to form silicon tetrachloride vapor (wherein containing gas phase silicon tetrachloride and some gaseous impurities),
During the silicon tetrachloride vapor of rising and the silicon tetrachloride waste liquid counter current contacting declined, the part silicon tetrachloride in waste liquid turns
Move on in silicon tetrachloride vapor, while the impurity in silicon tetrachloride vapor is transferred in waste liquid, so as to form pure gas phase four
Silicon chloride simultaneously exports from rectifying column tower top, absorbs the impurity in silicon tetrachloride vapor and part silicon tetrachloride separates therefrom
Waste liquid is discharged as the silicon tetrachloride waste liquid (alternatively referred to as kettle raffinate, it is solidliquid mixture) after processing from tower bottom of rectifying tower；
And the liquid phase silicon tetrachloride also silicon tetrachloride vapor counter current contacting with rising to flow back, to supplement liquid phase.
In the present embodiment, the general principle of rectifying is by liquid mixture (i.e. silicon tetrachloride waste liquid) partial gasification, is utilized
The wherein different characteristic of each component volatility, realize the purpose of component separation.The process of rectifying is：What tower bottom of rectifying tower evaporated
Gas phase (i.e. silicon tetrachloride vapor) carries out adverse current with lower descending liquid (including silicon tetrachloride waste liquid and liquid phase silicon tetrachloride of backflow) and connect
To touch, in two-phase contact process, volatile (low boiling) component in lower descending liquid constantly shifts into gas phase, and in gas phase
Hardly possible volatilization (higher boiling) component is constantly shifted in downward descending liquid, therefore gas phase is closer to tower top, its volatile components (i.e. tetrachloro
SiClx) concentration is higher, and lower descending liquid is then more enriched with closer to tower reactor, its difficult volatile component, so as to reach the purpose of component separation.
In addition, the pure gas phase silicon tetrachloride exported by rectifying column tower top enters the first condenser, condensed liquid phase silicon tetrachloride
A part be back to as phegma through tower top in rectifying column, remaining part then as distillate take out, be stored in tetrachloro
In SiClx recycling can；And entering the waste liquid of tower bottom of rectifying tower, a part therein is sent into reboiler, and heating evaporation returns into gas phase
In tower, another part is discharged as kettle raffinate.
In distillation operation, the ratio that phegma flow L and top gaseous phase flow D in tower are returned through rectifying column tower top is
Reflux ratio R, i.e. R=L/D.
Why rectifying column can realize that component separation is due to gas in tower (D) liquid (L) two-phase after the contact of each layer column plate, more
Number light component rises after turning into gas phase, and most heavy constituents turn into liquid, so as the number of plates raises, its light component after being condensed
Content is higher, and heavy constituent is fewer, so as to reach separating effect.But if liquid phase is insufficient, it is possible to be not enough to condense
Uprising gas, the separating effect before weakening, tower top is caused to distillate heavy constituent too many, it is unqualified, and overhead reflux is exactly to be
Rectifying column provides enough liquid phases, and it is qualified that appropriate backflow ensures that tower top distillates.It can be seen that the size of reflux ratio, to distillation process
Separating effect and economy have important influence, therefore, in distillation design, reflux ratio is a ginseng that need to conscientiously select
Number.In the present embodiment, more preferably, the reflux ratio R of rectifying column is 2~3.
In addition, in order to preferably adjust reflux ratio, set on the pipeline of the silicon tetrachloride return tank 4 to the tower top of rectifying column 1
It is equipped with reflux pump 11.
Understood through described above, backflow had both included the liquid-phase reflux of tower top, gas phase caused by also being vaporized including tower reactor part
Backflow.Backflow is to form vapour, liquid two-phase contact mass transfer to enable the necessary condition that distillation process is carried out continuously.If tower top does not have liquid
Mutually flow back, or tower reactor does not have opposing steam flow caused by reboiler, then and the gas-liquid mass transfer on column plate has just lacked interaction
One side, also just lose the centrifugation of column plate.Therefore, the step by step tray of phegma declines and the rising of the step by step tray of steam is to realize rectifying
Necessary condition.
In the present embodiment, the solids that the candle filter 10 is isolated can be handled as industrial refuse, example
Such as directly discharged after centralized burning, and the liquid isolated is emitted into waste water downstream processing after pH value is adjusted to neutrality
Process.Pulp pump 12 is provided with the residue hydrolyzer 9 to the pipeline of candle filter 10, residue hydrolyzer 9 is exported
Raffinate be pumped into candle filter 10.The pipeline of the residue hydrolyzer 9 to candle filter 10 uses CPVC (chlorinated polyvinyl chloride second
Olefine resin) manage, the CPVC is made by polyvinyl chloride (PVC) resin is chlorination modified.
As shown in figure 1, the recycling and processing device also includes activated carbon feeding device 5, it is connected with tower bottom of rectifying tower, uses
The activated carbon of predetermined amount is periodically added into tower in the inlet amount (i.e. the inlet of silicon tetrachloride waste liquid) according to rectifying column 1
, the silicon tetrachloride high polymer in the silicon tetrachloride waste liquid after the processing of the activated carbon granule and tower bottom of rectifying tower is carried out
After absorption, discharged from tower reactor.
In addition, the recycling and processing device also includes the condenser 7 of plate-type evaporator 6 and second.The plate-type evaporator 6
It is connected by incomplete tube line with tower bottom of rectifying tower, its slag-drip opening is connected by pipeline with residue hydrolyzer 9, for rectifying tower
Silicon tetrachloride waste liquid after the processing of kettle discharge carries out intermittent-heating evaporation, the gas phase silicon tetrachloride output obtained after evaporation
To the second condenser 7, and the residue obtained after evaporating can be pushed into residue hydrolyzer 9 by the material-pulling device in it, by residue water
Processing is hydrolyzed in solution device 9, wherein, the silicon tetrachloride waste liquid after the processing of tower bottom of rectifying tower discharge may be set to periodically arrange
Enter plate-type evaporator 6.It is liquid phase four that second condenser 7, which is used for the gas phase silicon tetrachloride condensation that plate-type evaporator 6 exports,
Exported after silicon chloride to silicon tetrachloride recycling can 8.More preferably, second condenser 7 is located at the top of plate-type evaporator 6.
In the present embodiment, the liquid phase silicon tetrachloride in silicon tetrachloride recycling can 8 can both use as the raw material of rectifying column,
It can also be used as the raw material of chlorosilane derivative.
In summary, silicon tetrachloride devil liquor recovery processing unit described in the utility model is a kind of economic and environment-friendly type, capital
Less input, can in Recovery Purifying silicon tetrachloride waste liquid most of silicon tetrachloride processing unit, its innovation is：Utilize
The strong adsorptivity of activated carbon, after carrying out impurity absorption to the silicon tetrachloride waste liquid after the processing of tower bottom of rectifying tower, then carry out
Quantitative deslagging operation, it is solid to avoid tower bottoms coking, knot, solves that tower bottoms concentration is dilute the problem such as to be difficult to handle；Use activity
Charcoal adsorbs to the metal chloride in waste liquid, maximizes the volatilization for reducing volatile metal chloride to silicon tetrachloride production
The influence of product purity；Silicon tetrachloride waste liquid (alternatively referred to as inspissation residue liquid) after processing is after plate-type evaporator evaporates, condensed
The recyclable chlorosilane derivative chlorosilane product for obtaining high added value, the residue obtained after evaporation is by weak base or the water of water
After solution processing, can directly filtering emission or centralized burning, environment will not be polluted.
It is understood that embodiment of above is merely to illustrate that principle of the present utility model and used exemplary
Embodiment, but the utility model is not limited thereto.For those skilled in the art, this is not being departed from
In the case of the spirit and essence of utility model, various changes and modifications can be made therein, and these variations and modifications are also considered as this reality
With new protection domain.
Claims (10)
- A kind of 1. silicon tetrachloride devil liquor recovery processing unit, it is characterised in that boiling again including rectifying column, positioned at tower bottom of rectifying tower Device, the first condenser positioned at rectifying column tower top, silicon tetrachloride return tank, silicon tetrachloride recycling can, residue hydrolyzer and candle formula Filter, after silicon tetrachloride waste liquid enters rectifying column, the reboiler is used to be evaporated it processing to form gas phase tetrachloro SiClx is simultaneously exported from tower top, and the silicon tetrachloride waste liquid after handling is discharged from tower bottom of rectifying tower；First condenser is used for will The gas phase silicon tetrachloride condensation is output after liquid phase silicon tetrachloride to silicon tetrachloride return tank；In the silicon tetrachloride return tank Partial Liquid Phase silicon tetrachloride be back to rectifying column tower top, another part liquid phase silicon tetrachloride is produced to silicon tetrachloride recycling can； The residue hydrolyzer is used to the silicon tetrachloride waste liquid after the processing be hydrolyzed processing to form raffinate；The candle formula mistake Filter is used to carry out separation of solid and liquid processing to the raffinate and discharged respectively.
- 2. recycling and processing device according to claim 1, it is characterised in that silicon tetrachloride waste liquid is from the middle and lower part of rectifying column Into wherein, the reboiler be specifically used for entering part heating vaporization in the silicon tetrachloride waste liquid of tower bottom of rectifying tower with During forming silicon tetrachloride vapor, the silicon tetrachloride vapor of rising and the silicon tetrachloride waste liquid counter current contacting declined, waste liquid In part silicon tetrachloride be transferred in silicon tetrachloride vapor, while the impurity in silicon tetrachloride vapor is transferred in waste liquid, from And form pure gas phase silicon tetrachloride and exported from rectifying column tower top, absorb the impurity in silicon tetrachloride vapor and part four The waste liquid that silicon chloride separates therefrom is discharged as the silicon tetrachloride waste liquid after processing from tower bottom of rectifying tower.
- 3. recycling and processing device according to claim 1, it is characterised in that the reflux ratio of the rectifying column is 2~3.
- 4. recycling and processing device according to claim 1, it is characterised in that the silicon tetrachloride return tank to rectifying tower Reflux pump is provided with the pipeline on top.
- 5. recycling and processing device according to claim 1, it is characterised in that the solids that the candle filter is isolated Directly discharged after centralized burning, and the liquid isolated is emitted into waste water downstream processing work after pH value is adjusted to neutrality Sequence.
- 6. recycling and processing device according to claim 1, it is characterised in that the residue hydrolyzer to candle filter Pulp pump is provided with pipeline.
- 7. recycling and processing device according to claim 1, it is characterised in that the residue hydrolyzer to candle filter Pipeline is managed using CPVC.
- 8. according to the recycling and processing device any one of claim 1-7, it is characterised in that also feed and fill including activated carbon To put, it is connected with tower bottom of rectifying tower, for the activated carbon granule of predetermined amount periodically to be added into tower according to the inlet amount of rectifying column, The silicon tetrachloride high polymer in silicon tetrachloride waste liquid after the processing of the activated carbon granule and tower bottom of rectifying tower is inhaled It is attached, discharged from tower reactor.
- 9. according to the recycling and processing device any one of claim 1-7, it is characterised in that also including plate-type evaporator and Second condenser, the silicon tetrachloride waste liquid that the plate-type evaporator is used for after the processing to tower bottom of rectifying tower discharge enter in the ranks Have a rest heating evaporation, the gas phase silicon tetrachloride obtained after evaporation is exported to the second condenser, and the residue obtained after evaporating export to Residue hydrolyzer, processing is hydrolyzed by residue hydrolyzer；Second condenser is used for the gas phase for exporting plate-type evaporator Silicon tetrachloride condensation is output after liquid phase silicon tetrachloride to silicon tetrachloride recycling can.
- 10. recycling and processing device according to claim 9, it is characterised in that second condenser is located at plate evaporation The top of device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720886842.0U CN206985725U (en) | 2017-07-20 | 2017-07-20 | Silicon tetrachloride devil liquor recovery processing unit |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720886842.0U CN206985725U (en) | 2017-07-20 | 2017-07-20 | Silicon tetrachloride devil liquor recovery processing unit |
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| CN206985725U true CN206985725U (en) | 2018-02-09 |
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| CN201720886842.0U Active CN206985725U (en) | 2017-07-20 | 2017-07-20 | Silicon tetrachloride devil liquor recovery processing unit |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573172A (en) * | 2022-02-18 | 2022-06-03 | 福建钰融科技有限公司 | Waste liquid regeneration system |
| CN115321486A (en) * | 2022-07-23 | 2022-11-11 | 四川红华实业有限公司 | Electronic grade chlorine trifluoride purification method |
-
2017
- 2017-07-20 CN CN201720886842.0U patent/CN206985725U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573172A (en) * | 2022-02-18 | 2022-06-03 | 福建钰融科技有限公司 | Waste liquid regeneration system |
| CN115321486A (en) * | 2022-07-23 | 2022-11-11 | 四川红华实业有限公司 | Electronic grade chlorine trifluoride purification method |
| CN115321486B (en) * | 2022-07-23 | 2023-11-17 | 四川红华实业有限公司 | Method for purifying electronic grade chlorine trifluoride |
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| TR01 | Transfer of patent right |
Effective date of registration: 20200423 Address after: 831500 Urumqi City, Xinjiang Uygur Autonomous Region, China Patentee after: Xinjiang new special new material testing center Co., Ltd. Address before: 830011, the Xinjiang Uygur Autonomous Region Urumqi national hi tech Industrial Development Zone (new urban area) Ganquan Fort High-tech Industrial Park Patentee before: XINTE ENERGY Co.,Ltd. |
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| TR01 | Transfer of patent right |