CN106583031A - Process for purifying ganister sand from silicon carbide reclamation sand - Google Patents

Process for purifying ganister sand from silicon carbide reclamation sand Download PDF

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Publication number
CN106583031A
CN106583031A CN201611107931.7A CN201611107931A CN106583031A CN 106583031 A CN106583031 A CN 106583031A CN 201611107931 A CN201611107931 A CN 201611107931A CN 106583031 A CN106583031 A CN 106583031A
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CN
China
Prior art keywords
silicon carbide
sand
carborundum
silica flour
silicon
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201611107931.7A
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Chinese (zh)
Inventor
高增禄
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XINZHENG BAODE HIGH-TECH Co Ltd
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XINZHENG BAODE HIGH-TECH Co Ltd
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Priority to CN201611107931.7A priority Critical patent/CN106583031A/en
Publication of CN106583031A publication Critical patent/CN106583031A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00General arrangement of separating plant, e.g. flow sheets
    • B03B9/06General arrangement of separating plant, e.g. flow sheets specially adapted for refuse
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B1/00Conditioning for facilitating separation by altering physical properties of the matter to be treated
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B5/00Washing granular, powdered or lumpy materials; Wet separating
    • B03B5/28Washing granular, powdered or lumpy materials; Wet separating by sink-float separation
    • B03B5/30Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions
    • B03B5/32Washing granular, powdered or lumpy materials; Wet separating by sink-float separation using heavy liquids or suspensions using centrifugal force
    • B03B5/34Applications of hydrocyclones
    • 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
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/52Mechanical processing of waste for the recovery of materials, e.g. crushing, shredding, separation or disassembly

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  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a process for purifying ganister sand from silicon carbide reclamation sand. The process includes the following steps that silicon carbide reclamation sand mortar is subjected to filter pressing, so that a silicon carbide filter cake is obtained; the silicon carbide filter cake and water are put into a ground pool at the weight ratio of 1:8, mixed and thoroughly stirred evenly; silicon carbide filter cake suspension liquid obtained after stirring is conveyed to a swirling tank through a pump to be swirled; obtained upper-layer ganister sand suspension liquid is subjected to filter pressing, and wet raw ganister sand is obtained; the wet raw ganister sand, industrial bromine and water are added into an agitator at the weight ratio of 4:1:5 and stand after being thoroughly stirred evenly; and high-purity ganister sand separated from the upper layer is subjected to filter pressing through a filter press and then collected. The process for purifying the ganister sand from the silicon carbide reclamation sand can improve the resource utilization rate, reduce environment pollution, turn waste into wealth and enable crystalline silicon and silicon carbide to be used reasonably, so that the long-term problem of waste pollution is solved.

Description

A kind of carborundum reclaims sand purification silica flour technique
Technical field
The present invention relates to the purification field of waste mortar, more particularly to a kind of carborundum recovery sand purification silica flour technique.
Background technology
In recent years, domestic and international photovoltaic direction research worker is devoted to solid phase particles (silicon in multi-thread saw cut waste mortar always And carborundum) Separation Research, to seek silicon and the carbon that a kind of practical and economic method is come in separating-purifying mortar SiClx.Yang Jianfeng et al. has applied for the special of entitled " a kind of method that silica flour and carborundum powder are reclaimed in waste mortar from cutting " Profit.Main contents include carrying out solid-liquid separation to saw blade cutting waste mortar, remove the suspending agent in waste mortar using organic solvent And binding agent, gained solid formation is carried out into air-flow purification by floatation then, the silica flour of certain purity is obtained, further to the silica flour Liquid floatation and gravity separation are carried out, and highly purified silica flour are obtained eventually through pickling.By the carborundum obtained by gravity separation Powder carries out magnetic separation with the mixed-powder of metal impurities, obtains pure carborundum powder.By the isolated silica flour of the method and Carborundum powder, finally reclaims the silica flour purity for obtaining more than 98%wt, and carborundum powder can be prepared into mortar and re-apply in silicon The cutting of piece or other purposes.But the reagents such as the bromoform in the method selected by liquid liquid flotation it is not only sufficiently expensive and It is toxic, furthermore the silicon bits granularity produced by during polysilicon scroll saw is more in micron to submicron order, from universal experience, Its liquid liquid purification by floatation is very difficult.
External T.Y Wang et al. are condensed using chemical treatment, high speed centrifugation, high temperature and directional solidification technique is to silicon chip Silicon bits in scroll saw mortar are reclaimed and are finally made silicon chip of solar cell.They remove what is remained in mortar using acetone PEG and other oiliness pollutant, dissolve metal impurities with nitric acid, obtain solid mixture using the method for centrifugation;To this Liquid of the density between Si and SiC is added in solid mixture, high speed centrifugation is carried out again, final SiC sinks to bottom substantially Portion, and top layer is then mainly Si.As the SiC microgranules of partial crushing in slurry are very thin, after causing centrifugation, top layer is still containing about 10% SiC.The so isolated product rich in Si powder is carried out into 1460 DEG C of high-temperature process under argon protection so that Si powder melts and assembles, and SiC powder remains solid and it is disconnected, the people such as Wang claims Si and SiC be kept completely separate, after cooling Only pure Si just need to can be isolated by washing;And most of other impurity can be deposited on Si frit tables in cooling procedure Face, can be removed with HF acid cleaning;The Si for obtaining material are oriented into solidification growth finally, be can be ultimately utilized in and made solar-electricity Pond piece.But this material and level of efficiency are overall or low, reason is that the content of the impurity such as phosphorus is higher.The process has carried out height Temperature is processed, and the impurity diffusion that can be made surface contaminant unavoidably and remain in carborundum is penetrated into inside originally high-purity silicon grain, and And SiC particulate is entrained into silicon melt or the probability that is bonded in its surface and can not be washed with water can be present unavoidably.Therefore, the method It is not a kind of preferable recovery technology.
Silicon chip is the main production material of photovoltaic art, and silicon chip cutting is then the key of crystal silicon solar cell sheet manufacture One of operation;The silicon material for having at least 40% during silicon wafer wire saw is cut enters cutting mortar in the form of sawdust, while In remaining cutting mortar, more than 90% silicon carbide abrasive is not fully utilized.Therefore, recycle solaode In piece saw blade cutting mortar, silicon is significant with carborundum;Hydrochloric acid system pickling of this project by crystal silicon cutting waste material Remove impurity, water base liquid phase deposition and double-deck organic reagent divided silicon and carborundum, crystalline silicon material and carborundum material to enrichment Material carries out the modes such as further Refining, obtains the crystal silicon cutting waste material with practicality and reclaims silicon and silicon carbide products;No But resource utilization can be improved, and environmental pollution can be reduced, be turned waste into wealth, crystalline silicon and carborundum is rationally utilized, be solved Certainly waste entrainment problem for a long time, benefits the nation and the people.
The content of the invention
Embodiment of the present invention technical problem to be solved is, there is provided one kind can improve resource utilization, and can Environmental pollution is reduced, is turned waste into wealth, crystalline silicon and carborundum is rationally utilized, solve the problems, such as the carbonization of waste entrainment for a long time Silicon reclaims sand purification silica flour technique.
To solve above-mentioned technical problem, the invention provides a kind of carborundum reclaims sand purification silica flour technique, the technique Comprise the steps:
(1)Silicon carbide filter cake is obtained after carborundum is reclaimed sand mortar filter pressing;
(2)By Silicon carbide filter cake and water by weight 1:8 ratio is thrown in into Di Chili and is mixed, and stirs;
(3)By step(2)The silicon carbide filter cake suspension obtained after stirring is entered by being pumped into eddy flow tank
Row eddy flow;
(4)By step(3)The upper strata silica flour suspension of acquisition obtains wet thick silica flour Jing after filter pressing;
(5)By step(4)The wet thick silica flour for obtaining and industrial bromine and water by weight 4:1:5 ratio adds stirred tank, fills Divide;
(6)By step(5)Collect after the high-purity silica flour pressure filter filter pressing that upper strata isolates.
Preferably, the step(2)Be sufficiently stirred for the time for 30 minutes.
Preferably, the step(5)Be sufficiently stirred for the time for 30 minutes, stand 1 hour.
Preferably, lower floor's silicon carbide suspension that the step (3) obtains obtains wet thick carborundum Jing after centrifugation.
Preferably, it is the recovered liquid after cutting monocrystal silicon, polysilicon that the carborundum reclaims sand mortar.
Preferably, the step(3)The eddy flow time be 1 hour.
Implement the embodiment of the present invention, have the advantages that:
The present invention can realize recycling to the silicon in solar energy crystal silicon cutting waste material and carborundum, reclaim work by the purification Skill, realizes reaching more than 90% to the response rate of carborundum in crystal silicon cutting waste material, and the response rate of silicon reaches more than 80%, recovery The purity of silica flour and carborundum powder can reach more than 93%, and especially silica flour can be made again through the purification of follow-up bromine water processed To produce the raw material of solar level crystal silicon, for the cost of electricity-generating and solar energy that further reduce crystal silicon solar batteries The extensive application of volt technology has highly important meaning.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment to the present invention It is described in further detail.
A kind of carborundum of the embodiment of the present invention reclaims sand purification silica flour technique, comprises the steps:
(1)Recovered liquid after cutting monocrystal silicon, polysilicon is processed into into Silicon carbide filter cake;
(2)By Silicon carbide filter cake and water by weight 1:8 ratio is thrown in and is mixed enter in holding vessel, is sufficiently stirred for 30 points Can not there is dead angle or interruption in clock, whipping process, at the uniform velocity stirring forms silicon carbide filter cake suspension;
(3)By step(2)The silicon carbide filter cake suspension obtained after stirring is entered by being pumped into eddy flow tank
Row eddy flow, eddy flow time are 1 hour, and different using carborundum, silica flour proportion, silica flour is separated with carborundum, carborundum Suspension is descending, and silica flour suspension is up, and in keeping eddy flow tank, pressure is 0.18-0.2MPa;Up silica flour suspension passes through Overflow head piece is entered in surge tank, carries out lower road filter pressing operation;
(4)By step(3)Silica flour suspension obtains wet thick silica flour after carrying out filter press filter pressing;
(5)By step(4)The wet thick silica flour for obtaining and industrial bromine and water by weight 4:1:5 ratio adds stirred tank, fills Divide stirring 30 minutes, stand 1 hour afterwards, using double layer separation technology, bromine water upper strata is the high-purity silica flour for isolating, under Layer is silicon carbide micro-powder, then all collecting after the high-purity silica flour pressure filter filter pressing for isolating.
In the same manner, step(3)In descending silicon carbide suspension obtain wet after underflow head piece is input into and is centrifuged in centrifuge Thick carborundum.
The present invention can realize recycling to the silicon in solar energy crystal silicon cutting waste material and carborundum, be reclaimed by the purification Technique, realizes reaching the response rate of carborundum in crystal silicon cutting waste material more than 90%, and the response rate of silicon reaches more than 80%, reclaims Silica flour and the purity of carborundum powder can reach more than 93%, especially silica flour can be again through the purification of follow-up bromine water processed As the raw material of production solar level crystal silicon, for the cost of electricity-generating and solar energy that further reduce crystal silicon solar batteries The extensive application of photovoltaic technology has highly important meaning.
Above disclosed is only a kind of preferred embodiment of the invention, and the power of the present invention can not be limited certainly with this Sharp scope, therefore the equivalent variations made according to the claims in the present invention, still belong to the scope covered by the present invention.

Claims (6)

1. a kind of carborundum reclaims sand purification silica flour technique, it is characterised in that:The technique comprises the steps:
(1)Silicon carbide filter cake is obtained after carborundum is reclaimed sand mortar filter pressing;
(2)By Silicon carbide filter cake and water by weight 1:8 ratio is thrown in into Di Chili and is mixed, and stirs;
(3)By step(2)The silicon carbide filter cake suspension obtained after stirring carries out eddy flow by being pumped into eddy flow tank;
(4)By step(3)The upper strata silica flour suspension of acquisition obtains wet thick silica flour Jing after filter pressing;
(5)By step(4)The wet thick silica flour for obtaining and industrial bromine and water by weight 4:1:5 ratio adds stirred tank, fills Divide;
(6)By step(5)Collect after the high-purity silica flour pressure filter filter pressing that upper strata isolates.
2. carborundum as claimed in claim 1 reclaims sand purification silica flour technique, it is characterised in that:The step(2)It is abundant Mixing time is 30 minutes.
3. carborundum as claimed in claim 1 reclaims sand purification silica flour technique, it is characterised in that:The step(5)It is abundant Mixing time is 30 minutes, stands 1 hour.
4. carborundum as claimed in claim 1 reclaims sand purification silica flour technique, it is characterised in that:What the step (3) obtained Lower floor's silicon carbide suspension obtains wet thick carborundum Jing after centrifugation.
5. carborundum as claimed in claim 1 reclaims sand purification silica flour technique, it is characterised in that:The carborundum reclaims sand sand Slurry is the recovered liquid after cutting monocrystal silicon, polysilicon.
6. carborundum as claimed in claim 1 reclaims sand purification silica flour technique, it is characterised in that:The step(3)Eddy flow Time is 1 hour.
CN201611107931.7A 2016-12-06 2016-12-06 Process for purifying ganister sand from silicon carbide reclamation sand Pending CN106583031A (en)

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CN201611107931.7A CN106583031A (en) 2016-12-06 2016-12-06 Process for purifying ganister sand from silicon carbide reclamation sand

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108046269A (en) * 2018-01-16 2018-05-18 常州大学 A kind of technique of the useless powder separation and recovery of solar silicon wafers cutting
CN108285147A (en) * 2018-03-23 2018-07-17 河南易成新能源股份有限公司 The method that high-purity silicon powder is extracted from crystalline silicon mortar cutting waste material
CN109160759A (en) * 2018-10-12 2019-01-08 中水电第十工程局(郑州)有限公司 A kind of preparation method of silicon powder suspension

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101792142A (en) * 2009-12-31 2010-08-04 唐康宁 Method for recovering polysilicon ingots, carborundum powder and polyethylene glycol from cutting waste mortar
CN102530948A (en) * 2012-01-04 2012-07-04 浙江大学 Method for recycling silicon from filings obtained through silicon wafer cutting
CN102642837A (en) * 2012-04-27 2012-08-22 河南新大新材料股份有限公司 Method for recycling polysilicon from silicon wafer waste slurry cut by diamond wire saw
KR20130033290A (en) * 2011-09-26 2013-04-03 시나노 덴기 세이렌 가부시끼가이샤 Method for recovering a solid particle
CN104229801A (en) * 2013-06-17 2014-12-24 储晞 Method and device for recycling silicon cutting waste mortar

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101792142A (en) * 2009-12-31 2010-08-04 唐康宁 Method for recovering polysilicon ingots, carborundum powder and polyethylene glycol from cutting waste mortar
KR20130033290A (en) * 2011-09-26 2013-04-03 시나노 덴기 세이렌 가부시끼가이샤 Method for recovering a solid particle
CN102530948A (en) * 2012-01-04 2012-07-04 浙江大学 Method for recycling silicon from filings obtained through silicon wafer cutting
CN102642837A (en) * 2012-04-27 2012-08-22 河南新大新材料股份有限公司 Method for recycling polysilicon from silicon wafer waste slurry cut by diamond wire saw
CN104229801A (en) * 2013-06-17 2014-12-24 储晞 Method and device for recycling silicon cutting waste mortar

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108046269A (en) * 2018-01-16 2018-05-18 常州大学 A kind of technique of the useless powder separation and recovery of solar silicon wafers cutting
CN108285147A (en) * 2018-03-23 2018-07-17 河南易成新能源股份有限公司 The method that high-purity silicon powder is extracted from crystalline silicon mortar cutting waste material
CN109160759A (en) * 2018-10-12 2019-01-08 中水电第十工程局(郑州)有限公司 A kind of preparation method of silicon powder suspension
CN109160759B (en) * 2018-10-12 2021-04-20 中水电第十一工程局(郑州)有限公司 Preparation method of silicon powder suspension

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