CN113582185A - Method for preparing solar-grade silicon raw material by using silicon mud waste - Google Patents
Method for preparing solar-grade silicon raw material by using silicon mud waste Download PDFInfo
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- CN113582185A CN113582185A CN202110907864.1A CN202110907864A CN113582185A CN 113582185 A CN113582185 A CN 113582185A CN 202110907864 A CN202110907864 A CN 202110907864A CN 113582185 A CN113582185 A CN 113582185A
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/037—Purification
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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
- 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
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Abstract
The invention discloses a method for preparing a solar-grade silicon raw material by using silicon sludge waste, which comprises the following steps: mixing and stirring silicon mud waste of the monocrystalline silicon slices with water to obtain a suspension solution A; mixing the first gas with hydrogen peroxide to obtain a first gas-liquid mixture; introducing the first gas-liquid mixture into the suspension solution A, stirring, standing, and cleaning oil stains to obtain a suspension solution B; mixing the second gas with ammonia water to obtain a second gas-liquid mixture; introducing a second gas-liquid mixture into the suspension solution B, stirring, standing, and cleaning oil stains to obtain a suspension solution C; carrying out filter pressing on the suspension solution C, cleaning and drying to obtain silicon mud; die-casting and granulating the silicon mud to obtain silicon mud particles; putting the silicon mud particles into a vacuum directional solidification furnace for heating, melting and directional solidification to obtain a polycrystalline silicon ingot; and removing the top and the side skin of the polycrystalline silicon cast ingot, and then breaking the polycrystalline silicon cast ingot to obtain the solar-grade silicon raw material.
Description
Technical Field
The invention belongs to the technical field of silicon material purification, and particularly relates to a method for preparing a solar-grade silicon raw material by using silicon mud waste.
Background
Solar photovoltaic power generation is one of reliable renewable energy sources at present, and with gradual depletion of coal and petroleum energy sources, solar energy is rapidly developed in the field of new energy sources, and annual capacity is more than 50 ten thousand tons. In order to enable the power generation to be on line at a low price, the cost is reduced to the utmost extent in each production link of the whole solar energy manufacturing process. In recent two years, the conversion efficiency of more crystalline silicon of solar cells manufactured by using monocrystalline silicon as a base material is high, and polycrystalline silicon is replaced to become the mainstream of the market. During the process of processing the silicon single crystal rod into the battery piece, silicon mud with ultrafine particles is inevitably generated due to the cutting of the diamond wire. Under the catalysis of environmental protection pressure and economic power, the recycling of silicon sludge has become an important subject in the industry.
At present, the wire diameter of diamond wire has been reduced to around 50 μm, even so, 15 ten thousand tons of silicon sludge waste (after dehydration) are produced per year with a loss of 35%. The silicon mud of the solar monocrystalline silicon slice contains diamond particles, metal impurities and organic matter impurities for lubricating and cooling during cutting, however, the silicon purity of the silicon mud is the same as that of monocrystalline silicon, and how to convert the silicon mud into a solar-grade polycrystalline silicon raw material with low cost and high efficiency is a problem to be solved urgently by improving the value of the waste silicon mud in the photovoltaic industry.
Disclosure of Invention
In view of the above, an object of the embodiments of the present application is to provide a method for preparing a solar grade silicon raw material from silicon sludge waste, so as to improve the value of silicon sludge.
According to an embodiment of the application, a method for preparing solar-grade silicon raw material by using silicon sludge waste is provided, wherein the method comprises the following steps:
mixing and stirring silicon mud waste of the monocrystalline silicon slices with water to obtain a suspension solution A;
mixing a first gas with hydrogen peroxide to obtain a first gas-liquid mixture, wherein the first gas is N2HCL gas and HF gas are mixed;
introducing the first gas-liquid mixture into the suspension solution A, stirring, standing, and then cleaning oil stains on the surface of the salvaging solution to obtain a suspension solution B;
mixing a second gas with ammonia water to obtain a second gas-liquid mixture, wherein the second gas is composed of N2And Ar gas are mixed;
introducing the second gas-liquid mixture into the suspension solution B, stirring, standing, and then cleaning oil stains on the surface of the salvaging solution to obtain a suspension solution C;
carrying out filter pressing on the suspension solution C, cleaning and drying to obtain silicon mud;
die-casting and granulating the silicon mud to obtain silicon mud particles;
putting the silicon mud particles into a vacuum directional solidification furnace for heating, melting and directional solidification to obtain a polycrystalline silicon ingot;
and removing the top and the side skin of the polycrystalline silicon cast ingot, and then breaking the polycrystalline silicon cast ingot to obtain the solar-grade silicon raw material.
Optionally, the first gas is composed of 50-90% by volume of N25 to 10 percent of HCL gas and 5 to 40 percent of HF gas.
Optionally, the first gas and hydrogen peroxide are mixed according to the volume fraction of 100 (5-10).
Optionally, the first gas-liquid mixture is introduced into the suspension solution a at a pressure of 0.1MPa to 0.5 MPa.
Optionally, the stirring time is 30min-2h, and the standing time is 1h-5 h.
Optionally, the second gas consists of 80-90% N by volume fraction2And 10% -20% of Ar gas.
Optionally, the second gas is mixed with ammonia water according to the volume fraction of 100 (3-10).
Optionally, the second gas-liquid mixture is introduced into the suspension solution B at a pressure of 0.1MPa to 0.5 MPa.
Optionally, the water content of the silicon mud obtained after drying is less than 3%.
Optionally, the silicon mud particles are 5mm-10 mm.
The technical scheme provided by the embodiment of the application can have the following beneficial effects:
according to the embodiment, the silicon mud is stirred and broken up to form the silicon mud solution A, hydrogen peroxide is blown into the silicon mud solution by taking mixed gas of HCL and HF as power in the first stage, and impurities such as oil stains and the like are removed to obtain the treated silicon mud solution B; in the second stage, ammonia water is blown into the treated silicon sludge solution B by taking mixed gas of N2 and Ar as power, and impurities such as oil stains and the like are removed to obtain a silicon sludge solution C; and carrying out filter pressing, drying and granulating on the silicon mud solution C to obtain silicon mud particles, and carrying out vacuum directional solidification treatment on the silicon mud particles to obtain the high-purity polycrystalline silicon raw material.
Stirring and scattering the silicon mud to uniformly distribute the silicon body and impurities in the silicon mud solution; in the first stage, hydrogen peroxide, HCL and HF are mixed and blown in to break most of oil stain molecular bonds in the silicon mud to form organic molecules with low molecular bonds, so that the silicon mud is easier to float upwards, and metal impurities in the silicon mud can be ionized; and in the second stage, ammonia water is further combined with oil stains to further remove impurities such as the oil stains. And in the process of carrying out filter pressing on the treated silicon mud solution, removing ionized metal impurities and the like in the silicon mud, and discharging the impurities and water together through the filter pressing process.
The operation is used for treating impurities in the silicon mud in a targeted manner, so that the impurities such as oil stains and the like are stripped from the silicon mud, and the reaction with a silicon body in the silicon mud in the high-temperature directional solidification process is avoided. Meanwhile, impurities in the silicon mud are removed, and the high-purity polycrystalline silicon ingot is obtained after high-temperature directional solidification and reaches the level of solar grade application.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
(1) gradually putting 650kg of silicon mud waste of the monocrystalline silicon slices into an acid-proof container filled with 1 ton of pure water, and continuously stirring the top of the container for 30min to obtain a suspension solution A;
(2) mixing a first gas and hydrogen peroxide according to a volume fraction of 100:5 to obtain a first gas-liquid mixture, wherein the volume of the gas isFraction of N90%2The hydrogen peroxide consists of 5% HCL gas in volume fraction and 5% HF gas in volume fraction, and the mass of the hydrogen peroxide is 400 g;
(3) blowing the gas-liquid mixture obtained in the step (2) from the bottom of the suspension solution A obtained in the step (1) at 0.2MPa until the hydrogen peroxide is completely blown, and meanwhile, continuously stirring for 0.5 h;
(4) standing the suspension solution obtained in the step (3) for 1h, and then fishing out surface oil stains and top suspended matters to obtain a suspension solution B;
(5) mixing the second gas with ammonia water according to the volume fraction of 100:3 to obtain a second gas-liquid mixture; the second gas volume fraction is 90% N2Ar with the volume fraction of 10 percent, wherein the mass of the ammonia water is 1 kg;
(6) blowing the second gas-liquid mixture obtained in the step (5) from the bottom of the suspension solution B obtained in the step (4) at 0.1MPa until the ammonia water is blown off, and meanwhile, continuously stirring for 2 hours;
(7) standing the suspension solution obtained in the step (6) for 2 hours, and then fishing out surface oil stains and top suspended matters to obtain a suspension solution C;
(8) carrying out primary filter pressing on the suspension solution C, adding 1 ton of water into the filter-pressed silicon mud, and stirring; secondary filter pressing is carried out after stirring, and 1 ton of water is added into the filter-pressed silicon mud for stirring; stirring, carrying out third-time filter pressing to obtain silicon mud with the water content of 45%, and drying by using a roller to obtain silicon mud with the water content of 3%;
(9) die-casting and granulating the silicon mud with the water content of less than 3% obtained in the step (8) to obtain silicon mud particles with the granularity of 5 mm;
(10) putting the silicon sludge particles into a vacuum directional solidification furnace for heating, melting and directional solidification to obtain square cast ingots with the size of 960mm x 340 mm;
(11) removing 70mm from the top of the ingot obtained in the step (10) by using a wire saw, removing 20mm from the bottom of each side skin to obtain polycrystalline silicon raw materials with the thickness of 920mm 270mm, and detecting the materials, wherein the boron content is 0.12ppm, the total impurity content is less than 1ppm, and the requirements of the raw materials of CZ Faraday monocrystals can be met;
example 2:
(1) gradually putting 700kg of silicon mud waste of monocrystalline silicon slices into an acid-proof container filled with 1.2 tons of pure water, and continuously stirring the top for 40min to obtain a suspension solution A;
(2) mixing the first gas with hydrogen peroxide according to the volume fraction of 100:5 to obtain a first gas-liquid mixture; the first gas volume fraction is 50% N2The hydrogen peroxide consists of 10% by volume of HCL gas and 40% by volume of HF gas, and the mass of the hydrogen peroxide is 500 g;
(3) blowing the first gas-liquid mixture obtained in the step (2) from the bottom of the suspension solution A obtained in the step (1) at 0.4MPa until the hydrogen peroxide is blown off, and meanwhile, continuously stirring for 2 hours;
(4) standing the suspension solution obtained in the step (3) for 5 hours, and then fishing out surface oil stains and top suspended matters to obtain a suspension solution B;
(5) mixing the second gas with ammonia water according to the volume fraction of 100:3 to obtain a second gas-liquid mixture; the second gas volume fraction is 80% N2Ar with the volume fraction of 20 percent, wherein the mass of the ammonia water is 1.5 kg;
(6) blowing the second gas-liquid mixture obtained in the step (5) from the bottom of the suspension solution B obtained in the step (4) at 0.4MPa until the ammonia water is completely blown, and meanwhile, continuously stirring for 3 hours;
(7) standing the suspension solution obtained in the step (6) for 5 hours, and then fishing out surface oil stains and top suspended matters to obtain a suspension solution C;
(8) carrying out primary filter pressing on the suspension solution C, adding 1.2 tons of water into the filter-pressed silicon sludge, and stirring; secondary filter pressing is carried out after stirring, and 1.2 tons of water are added into the filter-pressed silicon mud for stirring; stirring and carrying out third-time filter pressing to obtain silicon mud with the water content of 45%; drying in a roller to obtain silicon mud with the water content of 3 percent;
(9) die-casting and granulating the silicon mud with the water content of less than 3% obtained in the step (8) to obtain silicon mud particles with the granularity of 10 mm;
(10) placing the silicon mud particles into a vacuum directional solidification furnace for heating, melting and directional solidification to obtain square cast ingots with the size of 960mm x 360 mm;
removing 60mm from the top of the ingot obtained in the step (10) by using a wire saw, removing 20mm from the bottom of each side skin to obtain polycrystalline silicon raw materials with the thickness of 920mm 300mm, and detecting the materials, wherein the boron content is 0.15ppm, the total impurity content is less than 1ppm, and the requirements of the raw materials of CZ Faraday monocrystals can be met;
example 3:
(1) gradually putting 680kg of silicon mud waste of monocrystalline silicon slices into an acid-proof container filled with 1.1 ton of pure water, and continuously stirring the top of the container for 35min to obtain a suspension solution A;
(2) mixing the first gas with hydrogen peroxide according to the volume fraction of 100:5 to obtain a first gas-liquid mixture; the first gas has a volume fraction of 80% N210% of HCL gas and 10% of HF gas, wherein the mass of the hydrogen peroxide is 600 g;
(3) blowing the gas-liquid mixture obtained in the step (2) from the bottom of the suspension solution A obtained in the step (1) at 0.5MPa until the hydrogen peroxide is completely blown, and meanwhile, continuously stirring for 3 hours;
(4) standing the suspension solution obtained in the step (3) for 4 hours, and then fishing out surface oil stains and top suspended matters to obtain a suspension solution B;
(5) mixing the second gas with ammonia water according to the volume fraction of 100:3 to obtain a second gas-liquid mixture; the second gas volume fraction is 85% N2The volume fraction of Ar is 15 percent, and the mass of the ammonia water is 1.2 kg;
(6) blowing the second gas-liquid mixture obtained in the step (5) from the bottom of the suspension solution B obtained in the step (4) at 0.5MPa until the ammonia water is blown off, and meanwhile, continuously stirring for 2.5 h;
(7) standing the suspension solution obtained in the step (6) for 3 hours, and then fishing out surface oil stains and top suspended matters to obtain a suspension solution C;
(8) carrying out primary filter pressing on the suspension solution C, adding 1.1 ton of water into the filter-pressed silicon sludge, and stirring; secondary filter pressing is carried out after stirring, and 1.1 ton of water is added into the filter-pressed silicon mud for stirring; stirring and carrying out third-time filter pressing to obtain silicon mud with the water content of 45%; drying in a roller to obtain silicon mud with the water content of 3 percent;
(9) die-casting and granulating the silicon mud with the water content of less than 3% obtained in the step (8) to obtain silicon mud particles with the granularity of 8 mm;
(10) putting the silicon sludge particles into a vacuum directional solidification furnace for heating, melting and directional solidification to obtain square cast ingots with the size of 960mm x 340 mm;
removing 65mm from the top of the ingot obtained in the step (10) by using a wire saw, removing 20mm from the bottom of each side skin to obtain polycrystalline silicon raw materials with the thickness of 920mm 375mm, and detecting the materials, wherein the boron content is 0.13ppm, the total impurity content is less than 1ppm, and the requirements of the raw materials of CZ Faraday monocrystals can be met;
the method can remove organic and most metal impurities in the silicon mud at low temperature, maintains the body characteristics of silicon in the silicon mud, further creates conditions for the next step of vacuum directional solidification, becomes a method for stably and reliably recovering the silicon mud with low cost and high yield, and has higher technical advantages and economic value.
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.
Claims (10)
1. A method of producing solar grade silicon feedstock from silicon sludge waste, wherein the method comprises:
mixing and stirring silicon mud waste of the monocrystalline silicon slices with water to obtain a suspension solution A;
mixing a first gas with hydrogen peroxide to obtain a first gas-liquid mixture, wherein the first gas is N2HCL gas and HF gas are mixed;
introducing the first gas-liquid mixture into the suspension solution A, stirring, standing, and then cleaning oil stains on the surface of the salvaging solution to obtain a suspension solution B;
mixing a second gas with ammonia water to obtain a second gas-liquid mixture, wherein the second gas is composed of N2And Ar gas are mixed;
introducing the second gas-liquid mixture into the suspension solution B, stirring, standing, and then cleaning oil stains on the surface of the salvaging solution to obtain a suspension solution C;
carrying out filter pressing on the suspension solution C, cleaning and drying to obtain silicon mud;
die-casting and granulating the silicon mud to obtain silicon mud particles;
putting the silicon mud particles into a vacuum directional solidification furnace for heating, melting and directional solidification to obtain a polycrystalline silicon ingot;
and removing the top and the side skin of the polycrystalline silicon cast ingot, and then breaking the polycrystalline silicon cast ingot to obtain the solar-grade silicon raw material.
2. The method of claim 1, wherein the first gas consists of 50-90% N by volume fraction25 to 10 percent of HCL gas and 5 to 40 percent of HF gas.
3. The method of claim 1, wherein the first gas is mixed with hydrogen peroxide according to a volume fraction of 100 (5-10).
4. The method of claim 1, wherein the first gas-liquid mixture is introduced into the suspension solution A at a pressure of 0.1MPa to 0.5 MPa.
5. The method of claim 1, wherein the stirring time is 0.5h-2h and the standing time is 1h-5 h.
6. The method of claim 1, wherein the second gas consists of 80% to 90% N by volume fraction2And 10% -20% of Ar gas.
7. The method of claim 1, wherein the second gas is mixed with ammonia water in a volume fraction of 100 (3-10).
8. The method of claim 1, wherein the second gas-liquid mixture is introduced into the suspension solution B at a pressure of 0.1MPa to 0.5 MPa.
9. The method of claim 1, wherein the moisture content of the silicon sludge obtained after drying is less than 3%.
10. The method of claim 1, wherein the silicon sludge particles are 5mm to 10 mm.
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Effective date of registration: 20230801 Address after: Room 401D-22, Building 4, Core City Science Park, No. 588, Yuelu West Avenue, High tech Development Zone, Changsha City, Hunan Province, 410205 Patentee after: Hunan Lixin silicon material technology Co.,Ltd. Address before: 410205 room 401d-23, building 4, Xincheng Science Park, No. 588, Yuelu West Avenue, high tech Development Zone, Changsha, Hunan Patentee before: Changsha Xinli silicon material technology Co.,Ltd. |