CN105858602A - Polycrystalline silicon cutting waste material treatment method - Google Patents
Polycrystalline silicon cutting waste material treatment method Download PDFInfo
- Publication number
- CN105858602A CN105858602A CN201610219288.0A CN201610219288A CN105858602A CN 105858602 A CN105858602 A CN 105858602A CN 201610219288 A CN201610219288 A CN 201610219288A CN 105858602 A CN105858602 A CN 105858602A
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- CN
- China
- Prior art keywords
- polycrystalline silicon
- waste material
- leaching
- cutting waste
- sodium silicate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a polycrystalline silicon cutting waste material treatment method, and relates to comprehensive utilization of resources. According to the method, a polycrystalline silicon cutting waste material is taken as a main raw material, is leached with an alkali solution, and is filtered so as to obtain a mixture of hydrogen, a sodium silicate solution, silicon carbide and iron directly. Specifically, the method comprises the following steps: within a temperature range of 20-95 DEG C, leaching the cutting waste material with a 5-15% sodium hydroxide (or potassium hydroxide) solution, after the leaching is completed, filtering, and separating the filtrate from the leached waste material, wherein Si in the waste material can react with the NaOH solution in the alkali leaching process to generate sodium silicate and hydrogen; the filtrate can be used for preparing sodium silicate or taken as a raw material for preparing white carbon black; the waste material obtained after alkali leaching comprises main components of Fe and SiC, and pure silicon carbide can be prepared after acid leaching separation of iron. The invention provides a technique for resource utilization of polycrystalline silicon cutting waste materials with low cost, valuable elements in the polycrystalline silicon cutting waste materials can be recycled to the maximum extent, and waste can be turned into wealth.
Description
Technical field
The invention belongs to solid waste resource recovery and utilize field, a kind of method being specifically related to recycling polycrystalline silicon cut waste.
Background technology
Solar energy industry and the high speed development of semiconductor industry, crystalline silicon is as important photoelectric material, semi-conducting material, the demand of crystalline silicon is got more and more by the whole world, these industries need be cut to satisfactory silicon chip, but in cutting process, the crystalline silicon of about about 50% loses with the form of silica flour becomes slug, these waste slurry bulk depositions, easily cause certain safety and environmental problem, soil, air and water resource are polluted.
Polycrystalline silicon wastes be mainly composed of silicon, carborundum and ferriferous oxide.Owing to the physicochemical property of silicon and carborundum is close, and the particle diameter of waste material is very thin, and the difficulty of high separation silicon and carborundum is higher.At present with polycrystalline silicon cut waste as raw material, the method that silicon therein and carborundum are carried out separating-purifying, including froth flotation method, centrifugal separation, heavy-fluid isolation technics, high temperature filtration method and fractionation etc., but these method high costs, complex process, and some method is still in conceptual phase, it separates and purification process still needs further to be improved.
Hydrogen is a kind of important industrial gasses, but at present due to the restriction of preparation method, such as electrolysis water, cracking natural gas, cracking ammonia etc. so that its price is higher.Carborundum, as a kind of conventional high-temperature refractory, has the performances such as good heat endurance, wearability and creep resistance, is widely used in the fields such as metallurgy, chemical industry, biology.The purposes of waterglass the most widely, almost throughout each department of national economy.Such as chemical system is used to manufacture the various silicates products such as silica gel, white carbon, zeolite molecular sieve, metasilicate pentahydrate sodium, Ludox, layer silicon and instant powdery sodium silicate, sodium potassium silicate, is the base stock of silicon compound.
Summary of the invention
The present invention provides the processing method of a kind of polycrystalline silicon cut waste, with polycrystalline silicon cut waste as raw material, leached by alkali and obtain sodium silicate solution leachate, can directly prepare hydrogen and waterglass, can also react to prepare white carbon with acid, the waste material after alkali leaches can get pure carborundum through acidleach, is possible not only to the pollution problem reducing waste material for environment, and can fully recycle resource, low cost prepares the higher hydrogen of industrial value, waterglass and carborundum.
The present invention is achieved by the following technical solutions:
With polycrystalline silicon cut waste as primary raw material, it is carried out aqueous slkali leaching and filtration, the mixture of hydrogen, sodium silicate solution, carborundum and iron can be directly obtained.
Polycrystalline silicon cut waste processing method comprises the concrete steps that:
(1) configure certain density aqueous slkali, and make solution temperature stable at 20-95 DEG C；
(2) under conditions of stirring, polycrystalline silicon cut waste is added in aqueous slkali；
(3) to during produce hydrogen be collected, reaction terminate after, reactant is carried out filter separate, obtain sodium silicate solution leachate；
(4) waste material being filtrated to get in step (3) carries out acidleach, obtains pure carborundum.Described aqueous slkali includes NaOH, potassium hydroxide or both mixed solutions, and its concentration is 5-15%.
The Advantageous Effects of the present invention:
The present invention directly utilizes polycrystalline silicon cut waste, it is not necessary to the pretreatment of waste material and pyroreaction.Sodium hydroxide solution is directly used to carry out alkali leaching at a lower temperature so that silica and silicon in waste material generate sodium metasilicate with NaOH, can be used for preparing the raw material of waterglass and white carbon, and silicon can be used for preparing hydrogen with the reaction of NaOH simultaneously.Unreacted carborundum can carry out separating-purifying by acidleach except iron.The invention provides the technology of a kind of low cost recycling polycrystalline silicon cut waste, can farthest reclaim the valuable element in polycrystalline silicon cut waste, it is achieved turn waste into wealth.
Accompanying drawing explanation
Fig. 1 is waste material XRD diffraction image after embodiment 1 filters.
Fig. 2 is waste material XRD diffraction image after embodiment 2 filters.
Fig. 3 is waste material XRD diffraction image after embodiment 3 filters.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is explained in further detail.Should be appreciated that specific embodiment described herein is used only for explaining the present invention, be not intended to limit the present invention.
On the contrary, the present invention contains any replacement made in the spirit and scope of the present invention, amendment, equivalent method and scheme being defined by the claims.Further, in order to make the public that the present invention to be had a better understanding, in below the details of the present invention being described, detailed describe some specific detail sections.The description not having these detail sections for a person skilled in the art can also understand the present invention completely.
Embodiment 1
Take 7.9g solid sodium hydroxide deionized water and be configured to the sodium hydroxide solution that mass fraction is 5%, and be heated to 75 DEG C with water-bath.Under conditions of stirring, take 4g silicon cutting waste material and add in sodium hydroxide solution, to during the hydrogen that produces be collected, after reaction 10min, obtain sodium silicate solution leachate, take out reactant and carry out suction filtration.Remaining solid waste material after suction filtration is dried, and carries out XRD analysis.Result is as it is shown in figure 1, be mainly SiC according to remaining material after leaching knowable to Fig. 1, and the iron in waste material cannot show due to the lowest diffraction maximum in XRD of content.
Embodiment 2
Take 7.9g solid sodium hydroxide deionized water and be configured to the potassium hydroxide solution that mass fraction is 5%, and be heated to 95 DEG C with water-bath.Under conditions of stirring, take 4g silicon cutting waste material and add in sodium hydroxide solution, to during the hydrogen that produces be collected, after reaction 20min, obtain sodium silicate solution leachate, take out reactant and carry out suction filtration.Remaining solid waste material after suction filtration is dried, and carries out XRD analysis.Result is as in figure 2 it is shown, be mainly SiC according to remaining material after leaching knowable to Fig. 2.
Embodiment 3
Take 7.9g solid sodium hydroxide deionized water and be configured to the sodium hydroxide solution that mass fraction is 15%, and be heated to 65 DEG C with water-bath.Under conditions of stirring, take 4g silicon cutting waste material and add in sodium hydroxide solution, to during the hydrogen that produces be collected, after reaction 10min, obtain sodium silicate solution leachate, take out reactant and carry out suction filtration.Remaining solid waste material after suction filtration is dried, and carries out XRD analysis.Result is as it is shown on figure 3, be mainly SiC according to remaining material after leaching knowable to Fig. 3.
Embodiment 4
Take 7.9g solid sodium hydroxide deionized water and be configured to the sodium hydroxide solution that mass fraction is 5%, and be heated to 25 DEG C with water-bath.Under conditions of stirring, take 4g silicon cutting waste material and add in sodium hydroxide solution, to during the hydrogen that produces be collected, after reaction 10min, obtain sodium silicate solution leachate, take out reactant and carry out suction filtration.Remaining solid waste material after suction filtration is dried.
Claims (3)
1. a polycrystalline silicon cut waste processing method, it is characterised in that with polycrystalline silicon cut waste as primary raw material, carries out aqueous slkali leaching and filtration to it, directly obtains the mixture of hydrogen, sodium silicate solution, carborundum and iron.
2. polycrystalline silicon cut waste processing method as claimed in claim 1, it is characterised in that comprise the concrete steps that:
1) configure certain density aqueous slkali, and make solution temperature stable at 20-95 DEG C；
2)) under conditions of stirring, polycrystalline silicon cut waste is added in aqueous slkali；
3) to during produce hydrogen be collected, reaction terminate after, reactant is carried out filter separate, obtain sodium silicate solution leachate；
4) waste material being filtrated to get in step 3) is carried out acidleach, obtain pure carborundum.
3. polycrystalline silicon cut waste processing method as claimed in claim 1, it is characterised in that described aqueous slkali includes NaOH, potassium hydroxide or both mixed solutions, and its concentration is 5-15%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610219288.0A CN105858602A (en) | 2016-04-08 | 2016-04-08 | Polycrystalline silicon cutting waste material treatment method |
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| CN201610219288.0A CN105858602A (en) | 2016-04-08 | 2016-04-08 | Polycrystalline silicon cutting waste material treatment method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106916978A (en) * | 2017-01-25 | 2017-07-04 | 东北大学 | A kind of method for preparing silicon-containing alloy with the diamond wire cutting waste material slurry of crystalline silicon |
| CN107098783A (en) * | 2017-05-27 | 2017-08-29 | 镇江环太硅科技有限公司 | The technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting |
| CN107324337A (en) * | 2017-07-05 | 2017-11-07 | 镇江环太硅科技有限公司 | A kind of method that solar energy crystalline silicon cuts waste slurry recycling |
| CN107365156A (en) * | 2017-07-19 | 2017-11-21 | 北京科技大学 | A kind of method that silicon nitride is prepared using diamond wire saw polycrystalline silicon wastes |
| TWI618673B (en) * | 2016-09-20 | 2018-03-21 | 國立清華大學 | Method for generating hydrogen by chemical method and system thereof |
| CN109650331A (en) * | 2019-02-15 | 2019-04-19 | 嘉兴尚能光伏材料科技有限公司 | Hydrogen production process and hydrogen generating system based on silicon powder and silicon material |
| CN110342529A (en) * | 2019-08-12 | 2019-10-18 | 东北大学 | A method of white carbon black is prepared with crystalline silicon diamond wire cutting waste material |
| CN110734072A (en) * | 2018-07-19 | 2020-01-31 | 新特能源股份有限公司 | Method and device for recycling solid slag waste in polycrystalline silicon production |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
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| CN101691216A (en) * | 2009-10-05 | 2010-04-07 | 山东科技大学 | Method for recycling silicon carbide and co-producing white carbon black from waste mortar for wire cutting |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
| EP2474390A1 (en) * | 2011-01-06 | 2012-07-11 | Tzer-Huang Guo | Method and Apparatus for Recycling and Treating Waste Liquid that has been used in Cutting Mono Silicon |
| CN102976323A (en) * | 2012-11-16 | 2013-03-20 | 晶科能源有限公司 | Recovery technology of waste mortar used for solar silicon wafer cutting |
| CN103435050A (en) * | 2013-09-18 | 2013-12-11 | 天津大学 | Method for preparing white carbon black from monocrystalline silicon environment-friendly waste mortar |
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2016
- 2016-04-08 CN CN201610219288.0A patent/CN105858602A/en active Pending
Patent Citations (5)
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| CN101691216A (en) * | 2009-10-05 | 2010-04-07 | 山东科技大学 | Method for recycling silicon carbide and co-producing white carbon black from waste mortar for wire cutting |
| CN101804983A (en) * | 2010-04-23 | 2010-08-18 | 连云港佳宇电子材料科技有限公司 | Recovery, purification and classification method of high-purity silicon carbide micro-powder |
| EP2474390A1 (en) * | 2011-01-06 | 2012-07-11 | Tzer-Huang Guo | Method and Apparatus for Recycling and Treating Waste Liquid that has been used in Cutting Mono Silicon |
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| CN103435050A (en) * | 2013-09-18 | 2013-12-11 | 天津大学 | Method for preparing white carbon black from monocrystalline silicon environment-friendly waste mortar |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI618673B (en) * | 2016-09-20 | 2018-03-21 | 國立清華大學 | Method for generating hydrogen by chemical method and system thereof |
| CN106916978A (en) * | 2017-01-25 | 2017-07-04 | 东北大学 | A kind of method for preparing silicon-containing alloy with the diamond wire cutting waste material slurry of crystalline silicon |
| CN107098783A (en) * | 2017-05-27 | 2017-08-29 | 镇江环太硅科技有限公司 | The technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting |
| CN107324337A (en) * | 2017-07-05 | 2017-11-07 | 镇江环太硅科技有限公司 | A kind of method that solar energy crystalline silicon cuts waste slurry recycling |
| CN107324337B (en) * | 2017-07-05 | 2020-02-07 | 镇江环太硅科技有限公司 | Method for recycling waste solar crystalline silicon cutting slurry |
| CN107365156A (en) * | 2017-07-19 | 2017-11-21 | 北京科技大学 | A kind of method that silicon nitride is prepared using diamond wire saw polycrystalline silicon wastes |
| CN110734072A (en) * | 2018-07-19 | 2020-01-31 | 新特能源股份有限公司 | Method and device for recycling solid slag waste in polycrystalline silicon production |
| CN109650331A (en) * | 2019-02-15 | 2019-04-19 | 嘉兴尚能光伏材料科技有限公司 | Hydrogen production process and hydrogen generating system based on silicon powder and silicon material |
| CN110342529A (en) * | 2019-08-12 | 2019-10-18 | 东北大学 | A method of white carbon black is prepared with crystalline silicon diamond wire cutting waste material |
| CN114524408A (en) * | 2022-02-14 | 2022-05-24 | 浙江大学 | Environment-friendly comprehensive recycling method of organic silicon pulp residues |
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Application publication date: 20160817 |
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