CN115124041A - Method for purifying polycrystalline silicon waste by using solar cell waste glass - Google Patents
Method for purifying polycrystalline silicon waste by using solar cell waste glass Download PDFInfo
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- CN115124041A CN115124041A CN202210593958.0A CN202210593958A CN115124041A CN 115124041 A CN115124041 A CN 115124041A CN 202210593958 A CN202210593958 A CN 202210593958A CN 115124041 A CN115124041 A CN 115124041A
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- slag
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- 239000002699 waste material Substances 0.000 title claims abstract description 60
- 239000011521 glass Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 63
- 238000007670 refining Methods 0.000 claims abstract description 52
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910021419 crystalline silicon Inorganic materials 0.000 claims abstract description 21
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- 238000004321 preservation Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000006063 cullet Substances 0.000 claims abstract 2
- 230000008569 process Effects 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- 238000004064 recycling Methods 0.000 abstract description 5
- 210000004027 cell Anatomy 0.000 description 19
- 239000012535 impurity Substances 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 239000002210 silicon-based material Substances 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 210000003850 cellular structure Anatomy 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000002313 adhesive film Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000003181 co-melting Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229920006342 thermoplastic vulcanizate Polymers 0.000 description 1
Images
Classifications
-
- 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
- C01B33/02—Silicon
- C01B33/037—Purification
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/20—Waste processing or separation
Abstract
The invention belongs to the field of recycling of solar waste components, and particularly relates to a method for purifying polycrystalline silicon waste by using waste glass of a solar cell. The method comprises the following steps: (1) obtaining crystalline silicon waste for later use; (2) obtaining glass cullet; (3) mixing the glass broken slag and auxiliary materials uniformly to obtain refining slag; (4) putting the crystalline silicon waste and the refining slag into a crucible according to a certain mass ratio, wherein the mass ratio of the refining slag to the crystalline silicon waste is 1-10: 1; (5) putting the crucible containing the crystalline silicon waste and the refining slag into a high-temperature furnace, setting the working temperature of the high-temperature furnace at 1450-1700 ℃, preserving the heat for 0.5-5h, carrying out heat preservation refining for 1-5 times, and then separating the two phases of the silicon slag. The method can directly utilize the glass slag as the main component of the refining slag, is convenient to use and operate, greatly improves the removal rate of nonmetallic inclusions, and improves the quality of polycrystalline silicon, and the purity of silicon is 2N-6N, wherein the inclusions are lower than 1%.
Description
Technical Field
The invention belongs to the field of recycling of solar waste components, and particularly relates to a method for purifying polycrystalline silicon waste by using waste glass of a solar cell.
Background
In recent years, with the continuous development of new energy industries, the demand and the specific gravity of solar modules are increased, and a large amount of crystalline silicon waste materials and waste solar cell modules are generated.
The service life of the solar cell module is 20 years, but the actual service life is only about 10 years. With the gradual retirement of the earliest batch of solar cell modules, a recycling technology for solar cell modules is urgently developed. The crystalline silicon solar cell component mainly comprises the following components: the solar cell module comprises an aluminum frame, glass, an EVA (ethylene vinyl acetate) packaging adhesive film, a TPT (thermoplastic vulcanizate) back plate, a wire connector and a silicon-based solar cell. Wherein, aluminium frame and connector accessible mechanical automation's equipment is got rid of and is retrieved, and the technique is comparatively mature. The remaining materials are not effectively utilized, and particularly, the material of glass accounts for 70% of the scrapped solar cell module, and the direct discarding causes great resource waste. Therefore, it is necessary to dispose of these failed battery modules and recover and reuse the materials of the respective members.
In the manufacture of the solar cell industry, the main silicon waste materials include ingot casting waste materials and crystal silicon cutting waste materials generated in the crystal silicon slicing process. In the ingot casting process for preparing the solar grade polysilicon, the yield of the ingot casting is only 70%, and most factories directly discard the part of the side skin material due to the overhigh content of impurities at the top, the bottom and the periphery to finally become waste. During the production of the polycrystalline silicon slice by the multi-wire cutting method, at least more than 40% of silicon powder and silicon carbide abrasive are mixed to form cutting waste, and the cutting waste is basically in a stacking or low-value utilization state at present. The silicon scrap contains metal impurities such as Al and inclusions such as silicon carbide and silicon nitride. Therefore, the selection of an appropriate method for separating inclusions such as SiC is important for recovering and purifying the waste silicon material of the solar cell.
At present, no clear and effective recycling means exists for waste glass and crystalline silicon waste materials in photovoltaic modules. The industrial technology for purifying the crystalline silicon waste is not mature, and the recovery and treatment means of the waste glass is deficient, so that the conventional method is directly abandoned, but the loss of available materials is caused, so that the resource waste is caused, and the environmental burden is increased. On the other hand, aiming at hard inclusions such as silicon carbide, silicon nitride and the like in the polycrystalline silicon tailings, a certain effect is achieved by a novel slagging and refining method, but the used slag dosage is large, and the cost is increased for waste recovery. Therefore, the selection of a novel slag agent with low cost and high efficiency for silicon waste recovery is one of the currently important research directions.
Disclosure of Invention
The invention provides a method for purifying polycrystalline silicon waste by using solar cell waste glass, which uses the waste glass as refining slag, is simple to operate and does not generate pollutants in the process. The glass refining slag has low melting point and small viscosity, has good wettability with impurities and strong affinity with impurities such as Al, and can effectively remove the impurities and metal impurities in the crystalline silicon waste.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for purifying polycrystalline silicon waste by using waste glass of solar cells comprises the following steps:
(1) obtaining crystalline silicon waste for later use;
(2) crushing and stripping the waste solar cell module to obtain glass broken slag;
(3) uniformly mixing the glass slag and auxiliary materials to obtain refining slag;
(4) putting the waste crystalline silicon material and the refining slag into a crucible according to a certain mass ratio, wherein the mass ratio of the refining slag to the waste crystalline silicon material is 1-10: 1;
(5) and (3) placing the crucible containing the crystalline silicon waste and the refining slag into a high-temperature furnace, setting the working temperature of the high-temperature furnace at 1450-1700 ℃, preserving the heat for 0.5-5h, carrying out heat preservation refining for 1-5 times, and then separating the two phases of the silicon slag.
In the technical scheme, furthermore, the diameter of the glass slag in the step (2) is 0.6-1 mm.
In the technical scheme, furthermore, in the step (3), the glass accounts for 50-95% of the refining slag.
In the above technical solution, further, in the step (3), the auxiliary material includes one or more of fluoride, chloride and oxide.
In the technical scheme, furthermore, after heat preservation refining is finished each time, the slag is poured, and meanwhile, newly prepared refining slag is added to continue heat preservation refining.
In the technical scheme, the heat preservation refining process is further carried out in an air atmosphere.
The method comprises the steps of forming refining slag by waste glass and auxiliary materials in the solar cell module, co-melting the crystalline silicon waste and the refining slag under the action of high temperature, removing impurities and metal impurities in the crystalline silicon waste by using the refining slag by utilizing good wettability between the refining slag and the nonmetallic impurities and good affinity between oxygen, aluminum and other impurities in the refining slag, finally obtaining a high-purity crystalline silicon material by separating silicon from slag, and recycling the crystalline silicon waste and the waste glass of the solar cell module in one step. The method has the advantages of low cost, high removal efficiency of impurities and metal impurities, no pollution in the process, and capability of reproducing the separated refining slag agent as a raw material of glass, marble and the like, thereby increasing the technical economy.
The invention has the beneficial effects that:
the traditional slagging refining is mainly used for removing impurities such as Al, Mg, Ba, Ca, B, P and the like, the follow-up directional solidification method is still needed for removing nonmetallic inclusions, and the traditional slagging method needs to prepare a slag agent for slagging refining, so that the slag agent has high melting point, high viscosity and limited separation effect; the method can directly utilize the waste glass slag as the main component of the refining slag, is convenient to operate, greatly improves the removal rate of non-metallic inclusions, improves the quality of polycrystalline silicon, ensures that the purity of silicon purified by the method is 2N-6N, wherein the content of the inclusions is lower than 1%, and realizes the reutilization of solar cell component waste by selecting the slag agent, thereby greatly reducing the recovery cost.
The invention is a low-cost and environment-friendly production method, and belongs to an energy-saving and environment-friendly green manufacturing technology. The large-scale application and popularization of the technology can improve the market competitiveness of enterprises and protect the environment.
Drawings
FIG. 1 is a flow chart of the method for purifying polysilicon waste by using waste glass of solar cells according to the present invention.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
(1) Taking 6kg of silicon chips for later use;
(2) crushing and stripping a waste solar cell module to obtain 10kg of broken glass slag after treatment, and uniformly mixing the broken glass slag with 2kg of auxiliary materials consisting of 45% of calcium oxide, 45% of silicon dioxide and 10% of calcium fluoride in percentage by mass to obtain refining slag;
(3) putting the silicon chips and the refining slag into an alumina crucible;
(4) the crucible is placed in the central position of the induction furnace cavity, so that the crucible is uniformly heated, and the migration effect of non-metallic inclusions is improved by utilizing the electromagnetic action;
(5) setting working parameters of an induction furnace, wherein the working temperature is 1600 ℃, the heat preservation time is 2 hours, the heat preservation process is carried out in the air atmosphere, and the first heat preservation refining is carried out;
(6) after the heat preservation is finished, pouring the slag-silicon mixed melt in the crucible into a water-cooled copper crucible outside the furnace at high temperature, pouring out the slag melt, continuously adding new refining slag into the silicon melt for secondary heat preservation refining, and continuously operating at high temperature;
(7) after the secondary refining is finished, the slag melt is poured out at high temperature to realize silicon slag separation, the purified silicon is used as a raw material for subsequent process production, and the refining slag agent is used for industrial production of glass and the like.
The purity of the polysilicon purified by the method of example 1 reaches 99.99%.
Example 2
(1) Taking 6kg of silicon chips for later use;
(2) crushing and stripping the waste solar cell module to obtain 10kg of glass broken slag after treatment, and uniformly mixing the glass broken slag with 2kg of auxiliary materials consisting of 45 mass percent of calcium oxide, 45 mass percent of silicon dioxide and 10 mass percent of calcium fluoride to obtain refining slag;
(3) putting the silicon chips and the refining slag into an alumina crucible;
(4) placing the crucible into the central position of a muffle furnace chamber to ensure that the crucible is heated uniformly;
(5) setting working parameters of a muffle furnace, wherein the working temperature is 1600 ℃, the heat preservation time is 2 hours, the heat preservation process is carried out in an air atmosphere, and the first heat preservation refining is carried out;
(6) after the heat preservation is finished, pouring the slag-silicon mixed melt in the crucible into a water-cooled copper crucible outside the furnace at high temperature, pouring out the slag melt, continuously adding new refining slag into the silicon melt for secondary refining, and continuously operating at high temperature;
(7) after the secondary refining is finished, the slag melt is poured out at high temperature to realize silicon slag separation, the purified silicon is used as a raw material for subsequent process production, and the refining slag agent is used for industrial production of glass and the like.
The above examples are merely preferred embodiments of the present invention, and are not intended to limit the embodiments. The protection scope of the present invention shall be subject to the scope defined by the claims. Other variations and modifications may be made on the basis of the above description. Obvious variations or modifications derived therefrom are within the scope of the invention.
Claims (6)
1. A method for purifying polycrystalline silicon waste by using waste glass of solar cells is characterized by comprising the following steps:
(1) obtaining crystalline silicon waste for later use;
(2) crushing and stripping the waste solar cell module to obtain glass broken slag;
(3) uniformly mixing the glass slag and auxiliary materials to obtain refining slag;
(4) putting the crystalline silicon waste and the refining slag into a crucible according to a certain mass ratio, wherein the mass ratio of the refining slag to the crystalline silicon waste is 1-10: 1;
(5) and (3) placing the crucible containing the crystalline silicon waste and the refining slag into a high-temperature furnace, setting the working temperature of the high-temperature furnace at 1450-1700 ℃, preserving the heat for 0.5-5h, carrying out heat preservation refining for 1-5 times, and then separating the two phases of the silicon slag.
2. The method according to claim 1, wherein the diameter of the glass cullet in step (2) is 0.6-1 mm.
3. The method according to claim 1, wherein in the step (3), the glass content in the refining slag is 50-95%.
4. The method according to claim 1, wherein in the step (3), the auxiliary materials comprise one or more of fluoride, chloride and oxide.
5. The method according to claim 1, wherein after each heat-insulating refining, the slag is poured off and the newly prepared refining slag is added to continue the heat-insulating refining.
6. The method of claim 1, wherein the soaking refining process is performed under an air atmosphere.
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| CN202210593958.0A CN115124041B (en) | 2022-05-27 | 2022-05-27 | Method for purifying polycrystalline silicon waste by utilizing waste glass of solar cell |
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| CN202210593958.0A CN115124041B (en) | 2022-05-27 | 2022-05-27 | Method for purifying polycrystalline silicon waste by utilizing waste glass of solar cell |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8301207D0 (en) * | 1982-01-18 | 1983-02-16 | Sueddeutsche Kalkstickstoff | Process for purifying silicon |
| US4388286A (en) * | 1982-01-27 | 1983-06-14 | Atlantic Richfield Company | Silicon purification |
| JP2007191323A (en) * | 2006-01-17 | 2007-08-02 | Nippon Steel Materials Co Ltd | Method for refining silicon with slag and apparatus for producing high purity silicon |
| JP2008266075A (en) * | 2007-04-20 | 2008-11-06 | Shin Etsu Chem Co Ltd | Method for purifying silicon |
| CN102219221A (en) * | 2011-06-08 | 2011-10-19 | 大连理工大学 | Method for purifying polycrystalline silicon by directional solidification and slag refining |
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-
2022
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