CN115124041B - Method for purifying polycrystalline silicon waste by utilizing waste glass of solar cell - Google Patents
Method for purifying polycrystalline silicon waste by utilizing waste glass of solar cell Download PDFInfo
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- CN115124041B CN115124041B CN202210593958.0A CN202210593958A CN115124041B CN 115124041 B CN115124041 B CN 115124041B CN 202210593958 A CN202210593958 A CN 202210593958A CN 115124041 B CN115124041 B CN 115124041B
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- slag
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- refining
- glass
- crystalline silicon
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- 239000002699 waste material Substances 0.000 title claims abstract description 57
- 239000011521 glass Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 14
- 239000002893 slag Substances 0.000 claims abstract description 61
- 238000007670 refining Methods 0.000 claims abstract description 47
- 229910021419 crystalline silicon Inorganic materials 0.000 claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 21
- 239000010703 silicon Substances 0.000 claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004321 preservation Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 12
- 229920005591 polysilicon Polymers 0.000 claims abstract description 8
- 239000006063 cullet Substances 0.000 claims abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 238000004064 recycling Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000926 separation method 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
- 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
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011084 recovery 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 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
- 239000002210 silicon-based material Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000003082 abrasive agent 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
- 238000007796 conventional method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005288 electromagnetic effect Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 239000012528 membrane 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
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000000746 purification Methods 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
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 utilizing 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) uniformly mixing the glass slag and auxiliary materials to obtain refined 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) Placing the crucible containing the crystalline silicon waste and the refining slag into a high-temperature furnace, setting the temperature to be 1450-1700 ℃ at Wen Lugong ℃, 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 glass slag as the main component of refining slag, is convenient to use and operate, greatly improves the removal rate of nonmetallic inclusion and improves the quality of polysilicon, and the silicon purity of the method is 2N-6N, wherein the inclusion is 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 utilizing waste glass of a solar cell.
Background
In recent years, with the continuous development of new energy industry, the demand and specific gravity of solar modules are increasing, and a large amount of crystalline silicon waste and waste solar 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 progressive retirement of the earliest batch of solar cell modules, development of recycling technologies for solar cell modules is urgent. The crystalline silicon solar cell module mainly comprises the following components: aluminum frame, glass, EVA encapsulation glued membrane, TPT backplate, connector, silicon-based solar cell piece. Wherein, aluminium frame and connector accessible mechanical automation's equipment get rid of and retrieve, and the technique is comparatively mature. The rest materials are not effectively utilized, particularly glass, accounting for 70% of the scrapped solar cell module, and the direct discarding can cause great resource waste. Therefore, it is necessary to dispose of these failed battery modules and recycle the materials of the respective components.
In the solar cell industry manufacturing, the main silicon scraps include ingot casting scraps and crystalline silicon cutting scraps generated in the process of slicing crystalline silicon. 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 offal material due to the excessive impurity content at the top, the bottom and the periphery, so that the offal is finally formed. In the process of producing polycrystalline silicon chips by a multi-wire cutting method, at least more than 40% of silicon powder and silicon carbide abrasive materials are mixed to form cutting waste materials, and the cutting waste materials are 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 a proper method for separating inclusions such as SiC is important for recycling 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 in photovoltaic modules. The technology for purifying the crystalline silicon waste is not mature, and the recovery treatment means for the waste glass is deficient, so the conventional method is directly abandoned, but the available materials in the waste glass are lost, so that the resource waste and the environmental burden are caused. On the other hand, aiming at hard inclusions such as silicon carbide, silicon nitride and the like in the polycrystalline silicon tailings, the emerging slag refining method achieves a certain effect, but the 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 recycling the silicon waste is one of the important research directions at present.
Disclosure of Invention
The invention provides a method for purifying polysilicon waste by utilizing waste glass of a solar cell, which uses the waste glass as refining slag, has simple operation and no pollutant in the process. The glass refining slag has low melting point and low viscosity, has good wettability with inclusions and strong affinity with impurities such as Al, and can effectively remove the inclusions and metal impurities in the crystalline silicon waste.
In order to achieve the above object, the technical scheme of the present invention is as follows:
a method for purifying polysilicon waste by using solar cell waste glass, the method comprising the steps of:
(1) Obtaining crystalline silicon waste for standby;
(2) Crushing and stripping the waste solar cell modules to obtain glass slag;
(3) Uniformly mixing the glass slag and auxiliary materials to obtain refined 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) Placing the crucible containing the crystalline silicon waste and the refining slag into a high-temperature furnace, setting the temperature to be 1450-1700 ℃ at Wen Lugong, preserving 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 above technical scheme, further, the diameter of the glass slag in the step (2) is 0.6-1mm.
In the above technical scheme, further, in the step (3), the glass content in the refining slag is 50-95%.
In the above technical solution, in step (3), the auxiliary material includes one or more of fluoride, chloride and oxide.
In the technical scheme, further, after each heat preservation refining is finished, the slag is poured off, and meanwhile, newly prepared refining slag is put in to continue the heat preservation refining.
In the technical scheme, further, the heat preservation refining process is performed under the air atmosphere.
According to the invention, the waste glass and auxiliary materials in the solar cell module form refining slag, the crystalline silicon waste material and the refining slag are subjected to eutectic melting under the action of high temperature, the good wettability between the refining slag and nonmetallic inclusion and the good affinity between oxygen and aluminum and other impurities in the refining slag are utilized, the impurities and metal impurities in the crystalline silicon waste material are removed by utilizing the refining slag, and finally, the high-purity crystalline silicon material is obtained through slag-silicon separation, so that the recycling of the crystalline silicon waste material and the waste glass of the solar cell module can be realized in one step. The method has low cost, high efficiency of removing impurities and metal impurities, no pollution in the process, and the separated refining slag can be used as raw materials for reproducing glass, marble and the like, thereby increasing the economical efficiency of the technology.
The beneficial effects of the invention are as follows:
the traditional slag-making refining is mainly used for removing Al, mg, ba, ca, B, P and other impurities, the non-metallic inclusions still need to be removed by a directional solidification means in the follow-up process, and the traditional slag-making means needs to prepare slag agents for slag-making refining, and the slag agents have high melting point, high viscosity and limited separation effect; the method can directly utilize the waste glass slag as the main component of refining slag, is convenient to operate, greatly improves the removal rate of nonmetallic inclusion, improves the quality of polysilicon, and has the purity of 2N-6N after purification, wherein the purity of the inclusion is lower than 1 percent, and secondly, the slag agent is selected to realize the reutilization of solar cell module waste, thereby greatly reducing the recovery cost.
The invention relates to a low-cost and environment-friendly production method, which belongs to an energy-saving and environment-friendly 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 of the present invention for purifying polysilicon waste using solar cell waste glass.
Detailed Description
The following examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
(1) Taking 6kg of silicon scraps for standby;
(2) Crushing and stripping the waste solar cell module, treating to obtain 10kg of glass slag, and uniformly mixing with 2kg of auxiliary materials consisting of 45% of calcium oxide, 45% of silicon dioxide and 10% of calcium fluoride by mass to obtain refined slag;
(3) Placing the silicon scraps and refining slag into an alumina crucible;
(4) The crucible is placed in the central position of the furnace chamber of the induction furnace, so that the crucible is uniformly heated, and meanwhile, the migration effect of nonmetallic inclusion is improved by utilizing the electromagnetic effect;
(5) Setting working parameters of an induction furnace, wherein the working temperature is 1600 ℃, the heat preservation time is 2 hours, and the heat preservation process is carried out in air atmosphere to carry out primary heat preservation refining;
(6) Pouring the slag-silicon mixed melt in the crucible into the water-cooled copper crucible outside the furnace at high temperature after heat preservation is finished, 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 second refining is finished, pouring out slag melt at high temperature to realize silicon slag separation, and taking the purified silicon as a raw material for subsequent process production, wherein 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 scraps for standby;
(2) Crushing and stripping the waste solar cell module, treating to obtain 10kg of glass slag, and uniformly mixing with 2kg of auxiliary materials consisting of 45% of calcium oxide, 45% of silicon dioxide and 10% of calcium fluoride by mass to obtain refined slag;
(3) Placing the silicon scraps and refining slag into an alumina crucible;
(4) Placing the crucible in the center of a furnace chamber of a muffle furnace 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, and the heat preservation process is carried out in air atmosphere to carry out primary heat preservation refining;
(6) Pouring the slag-silicon mixed melt in the crucible into the water-cooled copper crucible outside the furnace at high temperature after heat preservation is finished, 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 second refining is finished, pouring out slag melt at high temperature to realize silicon slag separation, and taking the purified silicon as a raw material for subsequent process production, wherein the refining slag agent is used for industrial production of glass and the like.
The above examples are only preferred embodiments of the present invention and are not limiting of the implementation. The protection scope of the present invention shall be subject to the scope defined by the claims. Other variations or modifications may be made in the various forms based on the above description. Obvious variations or modifications of the embodiments are within the scope of the invention.
Claims (5)
1. A method for purifying polysilicon waste by using solar cell waste glass, which is characterized by comprising the following steps:
(1) Obtaining crystalline silicon waste for standby;
(2) Crushing and stripping the waste solar cell modules to obtain glass slag;
(3) Uniformly mixing the glass slag and auxiliary materials to obtain refined 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) Placing the crucible containing the crystalline silicon waste and the refining slag into a high-temperature furnace, setting the temperature to be 1450-1700 ℃ at Wen Lugong ℃, preserving heat for 0.5-5h, carrying out heat preservation refining for 1-5 times, and then separating two phases of the silicon slag;
in the step (3), the auxiliary materials are calcium oxide, silicon dioxide and calcium fluoride.
2. The method of claim 1, wherein the diameter of the glass cullet in step (2) is 0.6-1mm.
3. The method of claim 1, wherein in step (3), the glass content of the refining slag is 50-95%.
4. The method of claim 1, wherein after each heat preservation refining is completed, the slag is poured off, and simultaneously newly prepared refining slag is put in, and heat preservation refining is continued.
5. The method of claim 1, wherein the insulated refining process is performed under an air atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
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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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| CN115124041A CN115124041A (en) | 2022-09-30 |
| CN115124041B true CN115124041B (en) | 2023-11-17 |
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|---|---|---|---|---|
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| 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 |
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2022
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