CN113443621A - Method for recovering nano carbon material in magnesium-based composite material - Google Patents
Method for recovering nano carbon material in magnesium-based composite material Download PDFInfo
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- CN113443621A CN113443621A CN202110837598.XA CN202110837598A CN113443621A CN 113443621 A CN113443621 A CN 113443621A CN 202110837598 A CN202110837598 A CN 202110837598A CN 113443621 A CN113443621 A CN 113443621A
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- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 229910021392 nanocarbon Inorganic materials 0.000 title claims abstract description 46
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 43
- 239000011777 magnesium Substances 0.000 title claims abstract description 33
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 28
- 150000003839 salts Chemical class 0.000 claims abstract description 52
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 38
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 38
- 229910000861 Mg alloy Inorganic materials 0.000 claims abstract description 22
- 239000001103 potassium chloride Substances 0.000 claims abstract description 19
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 19
- 239000011780 sodium chloride Substances 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 11
- 230000008018 melting Effects 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 50
- 229910021389 graphene Inorganic materials 0.000 claims description 34
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 16
- 239000002041 carbon nanotube Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- 238000007711 solidification Methods 0.000 claims description 7
- 230000008023 solidification Effects 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 238000004064 recycling Methods 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000002787 reinforcement Effects 0.000 description 14
- 239000011159 matrix material Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 230000001737 promoting effect Effects 0.000 description 4
- 239000012266 salt solution Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000011156 metal matrix composite Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
- C01B32/196—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/17—Purification
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for recovering a nano carbon material in a magnesium-based composite material, relates to the field of nano material manufacturing, and aims to solve the problem of waste of a large amount of resources because a high-content nano carbon material in the magnesium-based composite material cannot be reused after the magnesium-based composite material loses efficacy. The method comprises the following steps: heating and melting the magnesium-based composite material containing the nano carbon material in a crucible; mixing and grinding sodium chloride and potassium chloride, then adding the mixture into the magnesium alloy melt, gradually stirring, and standing after the molten salt is completely melted. The crucible containing the metal melt and the molten salt was water cooled. And finally, soaking the cast ingot in the aqueous solution to completely dissolve the crystal salt on the surface of the cast ingot into the aqueous solution to obtain the suspension containing the nano carbon material. And washing the suspension for multiple times to recover the suspension. The invention is a simple and efficient nano carbon material recycling technology. Has great economic benefit for recycling the nano carbon material with high added value. The invention is applied to the field of material recovery.
Description
Technical Field
The invention relates to the field of nano material manufacturing, in particular to a method for recovering a nano carbon material in a magnesium-based composite material.
Background
In recent years, a metal matrix composite material formed by combining a metal and a reinforcement at an excellent interface by using a composite technology greatly improves various properties such as thermal expansion, strength, fracture toughness, impact toughness, abrasion resistance, electrical properties, magnetic properties, etc. of a single metal material, and thus is widely applied to products in industrial fields such as petroleum, chemical industry, ships, metallurgy, mines, machine manufacturing, electric power, water conservancy, etc. The mechanical properties of metal matrix composites are generally proportional to the amount of reinforcement present in the composite. Therefore, in order to obtain a more excellent composite effect, it is often necessary to add a large amount of reinforcement/functional body to the metal matrix. In particular, in recent years, a novel carbon material represented by graphene and carbon nanotubes is considered to be an ideal reinforcement for composite materials due to its unique physical and chemical properties. Currently, reinforcements represented by graphene and carbon nanotubes are introduced into the manufacturing process of metal matrix composites in a large amount. However, these reinforcements have a serious problem while achieving a good effect. The recycling of waste composite materials is difficult, if the waste composite materials cannot be well treated, the ecological environment can be seriously harmed, a large amount of resource waste can be caused, and the production cost of the novel nano carbon materials is very high due to the limitation of the preparation process. With the increasing application of magnesium-based composite materials prepared by using the novel carbon materials, the recycling problem of the nano carbon materials becomes very urgent. However, no effective method for solving the problem of difficult recovery of the nano-carbon material exists at present, and the technology for recycling the nano-carbon material in the magnesium-based composite material, which has low cost and high efficiency and is environmentally friendly, has great economic and social values.
Disclosure of Invention
The invention aims to provide a method for solving the problem of waste of a large amount of resources due to the fact that high-content nano carbon materials in a magnesium-based composite material cannot be reused after the magnesium-based composite material loses efficacy. Thereby providing a method for recycling the high-content nano carbon material in the magnesium-based composite material with simple process, low cost and feasibility.
The invention relates to a method for recovering a nano carbon material in a magnesium-based composite material, which comprises the following steps:
firstly, placing the magnesium-based composite material containing the nano carbon material in a crucible, and heating and melting at the temperature of 650-;
mixing and grinding sodium chloride and potassium chloride, drying, adding the mixed metal salt into the magnesium alloy melt under the condition of mechanical stirring, stopping stirring after the mixed salt is completely melted, and standing;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano carbon material and the mixed salt of sodium chloride and potassium chloride to obtain an ingot;
soaking the cast ingot in the aqueous solution for 0.5-48h to obtain a suspension containing the nano-carbon material, and filtering the suspension to obtain the nano-carbon material;
and fifthly, washing the nano carbon material in distilled water, filtering, repeating the washing and filtering steps for 3-5 times, and drying to obtain the clean nano carbon material.
Further, the heating melting temperature in the first step is 750 ℃.
Further, the mass ratio of the sodium chloride to the potassium chloride in the second step is 1: 1-3.
Further, the mass ratio of the sodium chloride to the potassium chloride in the second step is 1: 2.
Further, in the second step, after mixing sodium chloride and potassium chloride according to a ratio of 1:2, adding magnesium chloride accounting for 10% of the total mass of the two mixed salts for grinding.
And further, adding mixed salt of sodium chloride and potassium chloride into the magnesium alloy melt in the second step, stirring for 10-20 min, and standing for 5-15 min after the mixed salt is completely melted.
Further, the drying temperature in the second step is 250 ℃.
Further, in the fourth step, the ingot is soaked in the aqueous solution for 3-10 h.
Further, in the fourth step, the ingot is soaked in the aqueous solution for 3-5 h.
Further, the magnesium-based composite nano-carbon material is a graphene and carbon nano tube hybrid reinforced magnesium-based composite or a graphene reinforced copper-based composite.
The invention has the following beneficial effects:
the invention provides a new idea for recycling the nano-carbon material with high added value, and directly realizes large-batch green extraction and utilization of the nano-carbon material in the magnesium melt by utilizing the difference of wettability of the mixed molten salt and the magnesium melt with the nano-carbon material. At present, no mature recovery technology for the nanocarbon material in the metal matrix exists, and generally, in the known technology in the field, in order to obtain the nanocarbon material powder in the metal matrix, an acid solution extraction process is generally needed, which is not only high in cost, but also causes damage and destruction of the carbon material in the soaking process of the acid solution, and besides, the process also causes a serious pollution problem to the environment. The invention utilizes the adsorption effect of the reinforcement on the mixed molten salt, realizes the extraction of the reinforcement in one step, does not weaken the quality of the reinforcement in the recovery process, has very low cost, has lower requirements of related processes on experimental conditions, and is very suitable for being popularized to industrial production. In addition to this. The whole preparation process does not need strong acid and strong alkali solution which are extremely harmful to the environment, and the requirements of environment-friendly and green chemistry are met.
Drawings
FIG. 1 is a schematic view of the recycling of a nanocarbon material; wherein (a) a heating and melting operation of the composite material; (b) adding mixed salt for mixing sodium chloride and potassium chloride into the magnesium alloy melt; (c) mechanical stirring operation of the composite melt; (d) standing and extracting the composite melt;
FIG. 2 is a macroscopic optical topography of the metal salt of example 1 before and after addition to the composite melt to recover graphene; wherein (a) before addition and (b) after addition;
FIG. 3 is a graph of the morphology of the graphene extracted in different states of example 2; wherein (a) an aqueous solution of graphene; (b) drying the graphene powder;
fig. 4 is a graph of the morphology of the graphene recovered from the composite material of example 2.
Detailed Description
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.
To make the objects, aspects and advantages of the embodiments of the present invention more apparent, the following detailed description clearly illustrates the spirit of the disclosure, and any person skilled in the art, after understanding the embodiments of the disclosure, may make changes and modifications to the technology taught by the disclosure without departing from the spirit and scope of the disclosure.
The exemplary embodiments of the present invention and the description thereof are provided to explain the present invention and not to limit the present invention.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
The method for recovering the nano-carbon material in the magnesium-based composite material is carried out according to the following steps:
firstly, heating and melting a failed graphene reinforced magnesium-based composite material member in a crucible at 700 ℃;
mixing and grinding two metal salts of sodium chloride and potassium chloride according to a ratio of 1:1, heating and drying at 250 ℃, then sequentially adding the metal salts into the magnesium alloy melt and gradually stirring for 10min, standing for 5min after the mixed salts are completely melted, and promoting the graphene reinforcement to spontaneously move from the magnesium alloy matrix to the mixed molten salt;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano carbon material and the mixed salt;
soaking the cast ingot in the aqueous solution for 3-5 hours to completely dissolve the crystal salt on the surface of the cast ingot into the aqueous solution to obtain a suspension containing graphene, and filtering the salt solution to obtain graphene slurry;
fifthly, washing the graphene slurry with distilled water, filtering, and repeating for 3-5 times to obtain clean graphene.
A schematic diagram of a process for recovering graphene by adding mixed metal molten salt to a composite material melt in the embodiment is shown in fig. 1, and specifically includes (a) heating and melting a composite material; (b) adding a mixed salt of mixed sodium chloride and potassium chloride to the magnesium alloy melt; (c) mechanically stirring the composite melt; (d) and (5) standing and extracting the composite melt.
The macro-optical morphology of the selected mixed metal salt before and after the mixed metal salt is added to the composite material melt to recover graphene is shown in fig. 2, and it can be obtained from fig. 2(a) that the mixed molten salt is entirely represented as a clean and dispersed white crystal particle. After the mixed molten salt is added into the composite melt to extract graphene, the mixed salt is turned into black block-shaped characteristics as shown in fig. 2 (a). The molten salt is melted on the surface of the magnesium alloy after the mixed molten salt is added into the magnesium-based composite material matrix, and gradually diffuses from the composite material melt into the mixed molten salt along with the graphene so as to be converted into black characteristics.
Example 2
The method for recovering the nano-carbon material in the magnesium-based composite material is carried out according to the following steps:
firstly, heating and melting a failed graphene reinforced magnesium-based composite material member in a crucible at 700 ℃;
secondly, mixing two metal salts of sodium chloride and potassium chloride according to the ratio of 2: 5, mixing and grinding in proportion, heating and drying at 250 ℃, then sequentially adding the mixture into the magnesium alloy melt and gradually stirring for 10min, standing for 8min after the mixed salt is completely melted, and promoting the reinforcement to move from the magnesium alloy matrix to the mixed molten salt;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano carbon material and the mixed salt;
soaking the cast ingot in the aqueous solution for 10 hours to completely dissolve the crystal salt on the surface of the cast ingot into the aqueous solution to obtain a suspension containing graphene, and filtering the salt solution to obtain graphene slurry;
fifthly, washing the graphene slurry with distilled water, filtering, and repeating for 3-5 times to obtain clean graphene.
The morphology of the black bulk mixed molten salt dissolved in an aqueous solution obtained in this example is shown in fig. 3(a), which illustrates that the bulk containing graphene is soluble in water after solidification, which is the basis for further obtaining the nanocarbon material powder. The morphology of the dried powder is shown in fig. 3 (b). The feasibility of recycling the nano-carbon material by using the mixed salt is fully proved.
A scanning electron micrograph of the dried black powder obtained in this example is shown in fig. 4, which shows a typical morphology of graphene. The extracted black reinforcement powder is further proved to be graphene in the composite material, and the feasibility of the recovery process is fully proved.
Example 3
The method for recovering the nano-carbon material in the magnesium-based composite material is carried out according to the following steps:
firstly, heating and melting a failed carbon nano tube reinforced magnesium-based composite material member in a crucible at 700 ℃;
secondly, mixing two metal salts of sodium chloride and potassium chloride according to the weight ratio of 1:1 proportion, mixing and grinding, heating and drying at 250 ℃, then sequentially adding the mixture into a magnesium alloy melt and gradually stirring for 10min, standing for 15min after the mixed salt is completely melted, and promoting the reinforcement to move from the magnesium alloy matrix to the mixed molten salt;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the carbon nano tube and the mixed salt;
soaking the cast ingot in the aqueous solution for 10 hours to completely dissolve the crystal salt on the surface of the cast ingot into the aqueous solution to obtain a suspension containing the carbon nano tubes, and filtering the salt solution to obtain the carbon nano tubes;
fifthly, washing the carbon nano tube by using distilled water, filtering and repeating for 3-5 times to obtain the clean carbon nano tube.
Example 4
The method for recovering the nano-carbon material in the magnesium-based composite material is carried out according to the following steps:
firstly, heating and melting a failed magnesium-based composite material member containing carbon nanotubes and graphene in a crucible at 700 ℃;
secondly, mixing two metal salts of sodium chloride and potassium chloride according to the weight ratio of 1:1 proportion, mixing and grinding, heating and drying at 250 ℃, then sequentially adding the mixture into a magnesium alloy melt and stirring for 10min, standing for 15min after the mixed salt is completely melted, and promoting the reinforcement to move from the magnesium alloy matrix to the mixed molten salt;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the carbon nano tube, the graphene and the mixed salt;
soaking the cast ingot in the aqueous solution for 10 hours to completely dissolve the crystal salt on the surface of the cast ingot into the aqueous solution to obtain a turbid liquid containing the carbon nano tubes, and filtering the salt solution to obtain a mixture of the carbon nano tubes and the graphene;
and fifthly, washing the mixture of the carbon nano tube and the graphene by using distilled water, filtering, and repeating for 3-5 times to obtain clean mixed powder of the graphene and the carbon nano tube.
Claims (10)
1. A method for recovering a nano carbon material in a magnesium-based composite material is characterized by comprising the following steps:
firstly, placing the magnesium-based composite material containing the nano carbon material in a crucible, and heating and melting at the temperature of 650-;
mixing and grinding sodium chloride and potassium chloride, drying, adding the mixed metal salt into the magnesium alloy melt under the condition of mechanical stirring, stopping stirring after the mixed salt is completely melted, and standing;
thirdly, performing water condensation solidification on the crucible containing the magnesium alloy, the nano carbon material and the mixed salt of sodium chloride and potassium chloride to obtain an ingot;
soaking the cast ingot in the aqueous solution for 0.5-48h to obtain a suspension containing the nano-carbon material, and filtering the suspension to obtain the nano-carbon material;
and fifthly, washing the nano carbon material in distilled water, filtering, repeating the washing and filtering steps for 3-5 times, and drying to obtain the clean nano carbon material.
2. The method as claimed in claim 1, wherein the heating and melting temperature in the first step is 750 ℃.
3. The method for recovering the nanocarbon material from the magnesium-based composite material as claimed in claim 1, wherein the mass ratio of sodium chloride to potassium chloride in the second step is 1: 1-3.
4. The method as claimed in claim 3, wherein the mass ratio of sodium chloride to potassium chloride in the second step is 1: 2.
5. The method as claimed in claim 1, wherein in the second step, the sodium chloride and the potassium chloride are mixed at a ratio of 1:2, and then the magnesium chloride is added in an amount of 10% by mass of the total amount of the two mixed salts to grind the mixture.
6. The method for recovering the nanocarbon material from the magnesium-based composite material as claimed in claim 1, wherein in the second step, the mixed salt of sodium chloride and potassium chloride is added to the magnesium alloy melt and stirred for 10-20 min, and the mixture is left to stand for 5-15 min after the mixed salt is completely melted.
7. The method as claimed in claim 1, wherein the drying temperature in step two is 250 ℃.
8. The method of claim 1, wherein the ingot is immersed in the aqueous solution for 3 to 10 hours.
9. The method of claim 1, wherein the ingot is immersed in the aqueous solution for 3 to 5 hours.
10. The method as claimed in claim 1, wherein the Mg-based composite material is a Mg-based composite material reinforced by graphene and carbon nanotubes or a Cu-based composite material reinforced by graphene.
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CN114522965A (en) * | 2022-03-12 | 2022-05-24 | 湖北智烨新能科技有限公司 | Green and environment-friendly recycling method for new energy material |
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