CN104841195A - Purification and recovery device for chlorosilane waste liquid and purification and recovery method for chlorosilane waste liquid - Google Patents

Purification and recovery device for chlorosilane waste liquid and purification and recovery method for chlorosilane waste liquid Download PDF

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Publication number
CN104841195A
CN104841195A CN201510296174.1A CN201510296174A CN104841195A CN 104841195 A CN104841195 A CN 104841195A CN 201510296174 A CN201510296174 A CN 201510296174A CN 104841195 A CN104841195 A CN 104841195A
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chlorosilane
waste liquid
filter
recovery device
purification
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CN201510296174.1A
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Chinese (zh)
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张升学
杨永亮
严大洲
万烨
曾晓国
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China ENFI Engineering Corp
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China ENFI Engineering Corp
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Priority to CN201510296174.1A priority Critical patent/CN104841195A/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals

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Abstract

The invention provides a purification and recovery device for chlorosilane waste liquid and a purification and recovery method for chlorosilane waste liquid. The purification and recovery device comprises a filtering unit and a purification tower, wherein the filtering unit comprises one or more filters arranged in parallel connection, a chlorosilane waste liquid inlet is formed in each filter, solid residue and filtrate are obtained after the chlorosilane waste liquid passes through each filter, a solid residue outlet is formed in the bottom of each filter, and a filtrate outlet is formed in the top of each filter; and an inlet of the purification tower is communicated with the filtrate outlet, chlorosilane liquid and purified residual liquid are obtained after the filtrate passes through the purification tower, a purified residual liquid outlet is formed in the bottom of the purification tower, a chlorosilane liquid outlet is formed in the top of the purification tower, and the purified residual liquid outlet is communicated with the chlorosilane waste liquid inlet. The whole system can be operated and run reliably, is high in chlorosilane recovery rate and high in purity, and has significant effects in aspects of energy conservation and consumption reduction, and environmental protection.

Description

The purification recovery device of chlorosilane waste liquid and the method for purifying and recovering of chlorosilane waste liquid
Technical field
The present invention relates to Recovery Purifying technical field, in particular to a kind of purification recovery device of chlorosilane waste liquid and the method for purifying and recovering of chlorosilane waste liquid.
Background technology
In production polysilicon process, a large amount of accessory substances (being generally silicon tetrachloride) can be produced.At present, the production of polysilicon enterprise of more than 90% all adopts silicon tetrachloride cold hydrogenation technology to process accessory substance, is translated into the raw material trichlorosilane producing polysilicon.Silicon tetrachloride cold hydrogenation technology is by metallurgical grade silica flour, hydrogen, silicon tetrachloride under certain temperature, pressure condition, and under catalyst action, reaction generates trichlorosilane.But, containing metal impurities in metallurgical grade silica flour, in hydrogenation of silicon tetrachloride process, easily introduce trickle silica flour and metal impurities.Slightly heat up in a steamer in process at quench tower or eluting column and follow-up chlorosilane, for preventing occluding device and removing metal impurities, these fine silicon powder and metal impurities will be discharged by the bottom of tower with silicon tetrachloride liquid, and this part solidliquid mixture of discharge is raffinate.If this partially liq directly carries out outer row process, the loss of silicon tetrachloride raw material can be caused on the one hand, the more important thing is that silicon tetrachloride belongs to noxious material, after contacting with air or water, form acid mist, cause environmental pollution.
At present, the approach reclaiming chlorosilane raffinate is many, and major part all adopts raffinate evaporation, namely by additional heat, is evaporated by chlorosilane, thus realizes solid-liquor separation by condensation chlorosilane steam from raffinate.But adopt evaporation process raffinate energy consumption higher, steam consumption is larger, and the method needs to improve caloic exchange efficiency by mechanical agitation, and the sealing of device is poor, easily reveals, and causes device damage and environmental pollution.In addition, the chlorosilane steam of evaporation easily brings the powder of trace and metal impurities into follow-up system, causes separation not thorough.
Summary of the invention
Main purpose of the present invention there are provided a kind of purification recovery device of chlorosilane waste liquid and the method for purifying and recovering of chlorosilane waste liquid, to solve the problem that in prior art, the rate of recovery of chlorosilane is lower.
To achieve these goals, according to an aspect of the present invention, provide a kind of purification recovery device of chlorosilane waste liquid, this purification recovery device comprises: filter element, comprise one or more filter be arranged in parallel, each filter is provided with chlorosilane waste liquid entrance, and chlorosilane waste liquid is by obtaining solid slag and filtered fluid after each filter, and the bottom of filter is provided with solid slag outlet, the top of filter is provided with filtrate outlet; Purifying column, the entrance of purifying column is connected with filtrate outlet, filtered fluid is by obtaining chlorosilane liquid produced and residual solution after purifying after purifying column, residual solution outlet after the bottom of purifying column is provided with and purifies, the top of purifying column is provided with chlorosilane liquid produced outlet, and after purifying, residual solution outlet is connected with chlorosilane waste liquid entrance.
Further, each filter comprises filter housings and is arranged at the filter core unit in filter housings, the floral disc that filter core unit comprises multiple filter core and is arranged between adjacent filter core and between outermost filter core and filter housings.
Further, filter core is selected from cloth bag, metal filtering core or ceramic element.
Further, each filter comprises the blowback entrance be arranged at above filter core, and chlorosilane waste liquid entrance is arranged at the below of filter core, and purification recovery device also comprises blowback bottle and is arranged at the blowback pipeline between blowback bottle and blowback entrance.
Further, inert gas or chlorosilane is filled in blowback bottle.
Further, between filtrate outlet and the entrance of purifying column, be provided with filtered fluid pipeline, after purifying, between residual solution outlet and chlorosilane waste liquid entrance, be provided with residual solution pipeline after purifying.
Further, purifying column is sieve-plate tower.
Further, purification recovery device also comprises chlorosilane waste tank and the waste liquid delivery pump of the upstream being arranged at filter element.
Further, chlorosilane waste liquid comprises dust, metallic compound and chlorosilane, and the key component of solid slag is dust, and the key component of filtered fluid is chlorosilane, and after purifying, residual solution comprises dust and metallic compound.
According to a further aspect in the invention, provide a kind of method for purifying and recovering of chlorosilane waste liquid, this method for purifying and recovering comprises the following steps: by chlorosilane waste liquid by obtaining solid slag and filtered fluid after each filter of purification recovery device provided by the invention; By filtered fluid by obtaining chlorosilane liquid produced after the purifying column of purification recovery device and residual solution after purifying, and residual solution after purification is passed in each filter.
Apply technical scheme of the present invention, by adopting filter, pretreatment is carried out to chlorosilane waste liquid, the thing major part that admittedly contains in chlorosilane waste liquid is deviate to obtain filtered fluid, the dust of the metallic compound do not filtered out in filtrate and trace is removed by recycling purifying column, obtains pure chlorosilane liquid produced.Whole system operation, reliable, the chlorosilane rate of recovery is high, and purity is high, and has significant effect in energy-saving and cost-reducing, environmental protection.
Accompanying drawing explanation
The Figure of description forming a application's part is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows the cross-sectional view according to purification recovery device of the present invention; And
Fig. 2 shows the filter profile structural representation in purification recovery device of the present invention.
Detailed description of the invention
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.Below with reference to the accompanying drawings and describe the application in detail in conjunction with the embodiments.
It should be noted that used term is only to describe detailed description of the invention here, and be not intended to the illustrative embodiments of restricted root according to the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative is also intended to comprise plural form, in addition, it is to be further understood that, " comprise " when using term in this manual and/or " comprising " time, it indicates existing characteristics, step, operation, device, assembly and/or their combination.
For convenience of description, here can usage space relative terms, as " ... on ", " in ... top ", " at ... upper surface ", " above " etc., be used for the spatial relation described as a device shown in the figure or feature and other devices or feature.Should be understood that, space relative terms is intended to comprise the different azimuth in use or operation except the described in the drawings orientation of device.Such as, " in other devices or structure below " or " under other devices or structure " will be positioned as after if the device in accompanying drawing is squeezed, being then described as the device of " above other devices or structure " or " on other devices or structure ".Thus, exemplary term " in ... top " can comprise " in ... top " and " in ... below " two kinds of orientation.This device also can other different modes location (90-degree rotation or be in other orientation), and relatively describe space used here and make respective explanations.
From background technology, in prior art, the rate of recovery of chlorosilane is lower.The present inventor provides a kind of purification recovery device of chlorosilane waste liquid.As depicted in figs. 1 and 2, this purification recovery device comprises: filter element, comprise one or more filter 2 be arranged in parallel, each filter 2 is provided with chlorosilane waste liquid entrance 3, chlorosilane waste liquid is by obtaining solid slag and filtered fluid after each filter 2, and the bottom of filter 2 is provided with solid slag outlet 5, the top of filter 2 is provided with filtrate outlet 12; Purifying column 7, the entrance of purifying column 7 is connected with filtrate outlet 12, filtered fluid is by obtaining chlorosilane liquid produced and residual solution after purifying after purifying column 7, residual solution outlet after the bottom of purifying column 7 is provided with and purifies, the top of purifying column 7 is provided with chlorosilane liquid produced outlet 8, and after purifying, residual solution outlet is connected with chlorosilane waste liquid entrance 3.
The present invention carries out pretreatment by adopting filter 2 pairs of chlorosilane waste liquids, the thing major part that admittedly contains in chlorosilane waste liquid is deviate to obtain filtered fluid, the dust of the metallic compound do not filtered out in filtrate and trace is removed by recycling purifying column 7, obtains pure chlorosilane liquid produced.Whole system operation, reliable, the chlorosilane rate of recovery is high, and purity is high, and has significant effect in energy-saving and cost-reducing, environmental protection.
More specifically, the present invention is based in chlorosilane waste liquid containing dust, metallic compound and chlorosilane, the filter 2 utilizing filtering accuracy higher, by being admittedly separated containing thing in raffinate, containing a small amount of metallic compound in the liquid that filter 2 is separated, this part liquid enters purifying column 7, utilize the boiling point difference of metallic compound and chlorosilane, purify through tower, tower top obtains pure chlorosilane, the enrichment of tower reactor metallic compound is discharged with chlorosilane liquid produced, enters raffinate filter 2 carry out filtered and recycled again through pump.
Illustrative embodiments according to purification recovery device provided by the invention will be described in more detail below.But these illustrative embodiments can be implemented by multiple different form, and should not be interpreted as being only limited to embodiment set forth herein.Should be understood that, provide these embodiments be in order to make the application open thorough and complete, and the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
In above-mentioned purification recovery device, the filter core unit that each filter 2 comprises filter housings 9 and is arranged in filter housings 9, the floral disc 15 that filter core unit comprises multiple filter core 11 and is arranged between adjacent filter core 11 and between outermost filter core 11 and filter housings 9.Preferably, filter core 11 is selected from cloth bag, metal filtering core or ceramic element.
In a preferred embodiment, each filter 2 comprises the blowback entrance 10 be arranged at above filter core 11, chlorosilane waste liquid entrance 3 is arranged at the below of filter core 11, and purification recovery device also comprises blowback bottle and is arranged at the blowback pipeline 1 between blowback bottle and blowback entrance 10.Preferably, inert gas or chlorosilane is filled in blowback bottle.
Particularly, between the entrance of filtrate outlet 12 and purifying column 7, be provided with filtered fluid pipeline 6, after purifying, between residual solution outlet and chlorosilane waste liquid entrance 3, be provided with residual solution pipeline 4 after purifying.Purifying column 7 can be sieve-plate tower etc.Purification recovery device also comprises chlorosilane waste tank and the waste liquid delivery pump of the upstream being arranged at filter element.Chlorosilane waste liquid comprises dust, metallic compound and chlorosilane, and the key component of solid slag is dust, and the key component of filtered fluid is chlorosilane, and after purifying, residual solution comprises dust and metallic compound.
According to a further aspect in the invention, provide a kind of method for purifying and recovering of chlorosilane waste liquid, this method for purifying and recovering comprises the following steps: by chlorosilane waste liquid by obtaining solid slag and filtered fluid after each filter 2 of purification recovery device provided by the invention; By filtered fluid by obtaining chlorosilane liquid produced after the purifying column 7 of purification recovery device and residual solution after purifying, and residual solution after purification is passed in each filter 2.
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
(1) filter: be delivered to filter 2 containing the chlorosilane waste liquid admittedly containing thing through chlorosilane waste liquid entrance 3, in filter 2, adopt cloth bag or metal filtering core or ceramic element, filtered by chlorosilane waste liquid, after chlorosilane liquid produced is separated, (i.e. filtered fluid) enters in purifying column 7 through filtered fluid pipeline 6; Admittedly be retained down by cloth bag containing thing and fall into filter lower space, from solid slag outlet 5 discharge.Raffinate filter the using and the reserved, an operation, another carries out slagging-off cleaning filter core, to realize system continuity; Filter 2 is provided with blowback pipeline 1, adopts the chlorosilane liquid produced of inert gas (as nitrogen) or cleaning to carry out blowback or backwash, prevents the blocked up pressure reduction that causes of filter cake excessive, realizes continuously large flux and runs.
(2) purify: from the dust containing trace in the chlorosilane liquid produced (i.e. filter liquide) of raffinate filter and a small amount of metallic compound, enter after purifying column 7 through filtrate conduit 6, utilize the boiling point difference admittedly containing thing and chlorosilane, realize being separated.After pure chlorosilane liquid produced is separated from chlorosilane liquid produced outlet 8 out, the raffinate of tower reactor enrichment higher boiling metallic compound and dust delivers to raffinate filter chlorosilane waste liquid entrance 3 through filtrate conduit 4, to realize circulation and stress, improves the rate of recovery of chlorosilane.Raffinate purifying column adopts common sieve-plate tower.
As can be seen from the above embodiments, the above-mentioned example of the present invention achieves following technique effect: carry out pretreatment by adopting filter to chlorosilane waste liquid, the thing major part that admittedly contains in chlorosilane waste liquid is deviate to obtain filtered fluid, the dust of the metallic compound do not filtered out in filtrate and trace is removed by recycling purifying column, obtains pure chlorosilane liquid produced.Whole system operation, reliable, the chlorosilane rate of recovery is high, and purity is high, and has significant effect in energy-saving and cost-reducing, environmental protection.
These are only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. a purification recovery device for chlorosilane waste liquid, is characterized in that, described purification recovery device comprises:
Filter element, comprise one or more filter (2) be arranged in parallel, each described filter (2) is provided with chlorosilane waste liquid entrance (3), described chlorosilane waste liquid obtains solid slag and filtered fluid by after each described filter (2), and the bottom of described filter (2) is provided with solid slag outlet (5), the top of described filter (2) is provided with filtrate outlet (12);
Purifying column (7), the entrance of described purifying column (7) is connected with described filtrate outlet (12), described filtered fluid is by obtaining chlorosilane liquid produced and residual solution after purifying after described purifying column (7), residual solution outlet after the bottom of described purifying column (7) is provided with and purifies, the top of described purifying column (7) is provided with chlorosilane liquid produced outlet (8), and after described purification, residual solution outlet is connected with described chlorosilane waste liquid entrance (3).
2. purification recovery device according to claim 1, it is characterized in that, the filter core unit that each described filter (2) comprises filter housings (9) and is arranged in described filter housings (9), described filter core unit comprises multiple filter core (11) and is arranged at the floral disc (15) between adjacent described filter core (11) and between outermost described filter core (11) and described filter housings (9).
3. purification recovery device according to claim 2, is characterized in that, described filter core (11) is selected from cloth bag, metal filtering core or ceramic element.
4. purification recovery device according to claim 2, it is characterized in that, each described filter (2) comprises the blowback entrance (10) being arranged at described filter core (11) top, described chlorosilane waste liquid entrance (3) is arranged at the below of described filter core (11), and described purification recovery device also comprises blowback bottle and is arranged at the blowback pipeline (1) between described blowback bottle and described blowback entrance (10).
5. purification recovery device according to claim 4, is characterized in that, fills inert gas or chlorosilane in described blowback bottle.
6. purification recovery device according to claim 1, it is characterized in that, be provided with filtered fluid pipeline (6) between the entrance of described filtrate outlet (12) and described purifying column (7), after described purification, between residual solution outlet and described chlorosilane waste liquid entrance (3), be provided with residual solution pipeline (4) after purifying.
7. purification recovery device according to claim 1, is characterized in that, described purifying column (7) is sieve-plate tower.
8. purification recovery device according to claim 1, is characterized in that, described purification recovery device also comprises chlorosilane waste tank and the waste liquid delivery pump of the upstream being arranged at described filter element.
9. purification recovery device according to any one of claim 1 to 8, it is characterized in that, described chlorosilane waste liquid comprises dust, metallic compound and chlorosilane, the key component of described solid slag is described dust, the key component of described filtered fluid is described chlorosilane, and after described purification, residual solution comprises described dust and described metallic compound.
10. a method for purifying and recovering for chlorosilane waste liquid, is characterized in that, described method for purifying and recovering comprises the following steps:
By chlorosilane waste liquid by obtaining solid slag and filtered fluid after each described filter (2) of the purification recovery device according to any one of claim 1 to 9;
By described filtered fluid by obtaining chlorosilane liquid produced after the purifying column (7) of described purification recovery device and residual solution after purifying, and residual solution after described purification is passed in each described filter (2).
CN201510296174.1A 2015-06-02 2015-06-02 Purification and recovery device for chlorosilane waste liquid and purification and recovery method for chlorosilane waste liquid Pending CN104841195A (en)

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Cited By (6)

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CN107758673A (en) * 2017-11-03 2018-03-06 洛阳中硅高科技有限公司 Chlorosilane Recovery Purifying device and method
CN110589838A (en) * 2019-10-22 2019-12-20 中国恩菲工程技术有限公司 Method for treating chlorosilane residual liquid
CN110624268A (en) * 2019-09-16 2019-12-31 广州汇富研究院有限公司 Chlorosilane purifying device and purifying method thereof
CN111072031A (en) * 2019-12-10 2020-04-28 新疆东方希望新能源有限公司 Chlorosilane silicon powder filtering system and filtering method thereof
CN111228932A (en) * 2020-01-19 2020-06-05 四川永祥多晶硅有限公司 Silica flour filtration system
CN115970489A (en) * 2022-12-18 2023-04-18 石河子大学 Process for separating silicon powder by ceramic microfiltration membrane

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CN111228932A (en) * 2020-01-19 2020-06-05 四川永祥多晶硅有限公司 Silica flour filtration system
CN115970489A (en) * 2022-12-18 2023-04-18 石河子大学 Process for separating silicon powder by ceramic microfiltration membrane

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Application publication date: 20150819