CN108963270A - A kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material - Google Patents
A kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material Download PDFInfo
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- CN108963270A CN108963270A CN201810763676.4A CN201810763676A CN108963270A CN 108963270 A CN108963270 A CN 108963270A CN 201810763676 A CN201810763676 A CN 201810763676A CN 108963270 A CN108963270 A CN 108963270A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8647—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites
- H01M4/8652—Inert electrodes with catalytic activity, e.g. for fuel cells consisting of more than one material, e.g. consisting of composites as mixture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/02—Details
- H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
- H01M8/0204—Non-porous and characterised by the material
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- H01M8/0226—Composites in the form of mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/18—Regenerative fuel cells, e.g. redox flow batteries or secondary fuel cells
- H01M8/184—Regeneration by electrochemical means
- H01M8/188—Regeneration by electrochemical means by recharging of redox couples containing fluids; Redox flow type batteries
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention provides a kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material, follows the steps below: the preparation of nitrogen-doped graphene；Nitrogen-doped graphene secondary oxidation；The preparation of nitrogen-doped graphene/di-iron trioxide combination electrode material.A kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method of the invention, with high-specific surface area and good three-dimensional structure channel, place can be provided for the storage and transport of electrolyte, it is integrated with active material that electrode realizes collector, the comprehensive performance of electrode material is provided, it can be looked forward to and had broad application prospects in the new energy field of batteries such as flow battery.
Description
Technical field
The present invention relates to novel energy resource material technology fields, and in particular to a kind of nitrogen-doped graphene/di-iron trioxide is compound
The preparation method of electrode material.
Background technique
Liquid flow energy storage battery technology is as solution renewable energy system randomness and intermittent unstable state feature
Effective ways, power industry, electric car power supply, emergency power system, in terms of have a wide range of applications before
Scape.As one of electrode of liquid flow cell critical component, electrode is only used as the place of electrochemical reaction, is not involved in electrochemical reaction,
It is required that it is with excellent electro-chemical activity, electric conductivity, reproducibility, stability and mechanical strength.
Two iron of titanium dioxide becomes one kind by wide due to low cost, non-toxic, high chemical stability and high theoretical capacity
The electrode material of general concern.Graphene resistivity is extremely low, and the speed of electron transfer is exceedingly fast, and has unusual electrical property.Stone
For black two iron combination electrode of alkene/titanium oxide while keeping two kinds of component advantages, di-iron trioxide nano particle is distributed in stone
Between black alkene lamella, it can effectively inhibit the lamella of graphene to stack and reunite, improve pore structure, increasing specific surface area.Simultaneously
The three-dimensional conductive network that two iron composite material of graphene/titanium oxide constructs can effectively overcome di-iron trioxide low electric conductivity etc.
Disadvantage, porous structure also are used as the buffer-stored pond of ion, are conducive to ion transmission, can have and alleviate di-iron trioxide nanometer
Grain volume expansion during charge discharge, improves flow battery comprehensive performance.
Nitrogen-doped graphene/di-iron trioxide combination electrode has the characteristic of superelevation specific capacity at higher current densities.Together
When nitrogen atom doping in graphene-structured, electrode-electric solution liquid wetting situation can be optimized, make electrode material have good length
Phase operation stability.Nitrogen-doped graphene/di-iron trioxide meets electrode activity and is obviously improved.
Current most composite material is all the nano particle shape by the way that dissimilar materials is deposited or be anchored on graphene
At powder body material, thus cause graphene directly by it is irreversible reunion and accumulation, cause the specific surface area of composite material
It is remarkably decreased, limits graphene composite material in the application in certain fields, the present invention is capable of providing a kind of inexpensive, simple process
The effective solution to this problem of nitrogen.
Summary of the invention
The purpose of the present invention is to provide a kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation sides
Method has high-specific surface area and good three-dimensional structure channel, can provide place for the storage and transport of electrolyte, electrode is real
Show that collector is integrated with active material, has provided the comprehensive performance of electrode material, it can be looked forward in flow battery etc.
New energy field of batteries has broad application prospects.
In order to achieve the above objectives, the technical solution adopted by the present invention:
A kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method of the invention, according to the following steps into
Row:
(1) preparation of nitrogen-doped graphene: graphene oxide is made by Humers, by the graphite powder and 10-16 of 20-30 parts of weight
The sodium nitrate mixing drying 8-12h of part weight, is transferred in three-necked flask, and be added 10-17 parts thereto under condition of ice bath
The concentrated sulfuric acid of weight is slowly uniformly added into the potassium permanganate of 10-17 parts of weight, ice bath device is removed, by mixed solution in 60-80
Incubation water heating 6-9h at DEG C is slowly added to the ice water of 100-120 parts of weight again, after transfer the solution into after the completion of exothermic heat of reaction
In beaker, the hydrogen peroxide of 20-30 parts of weight is added dropwise into solution while stirring, removes extra potassium permanganate, solution has reflected
It is in glassy yellow after complete, filters bright yellow solution with sand core funnel, and with salt acid elution five times, then is molten with deionized water dilution washing
Remaining chloride ion in liquid；After eliminating extra metal ion and chloride ion, graphene filter cake is dispersed in deionized water
It is dispersed with stirring 30min, then filtering and washing；By the graphene dispersion of 20-35 parts of weight in the concentrated ammonia liquor of 100-150 parts of weight
20-40min is stirred, then ultrasound 20-60min, finely dispersed solution is transferred in polytetrafluoroethyl-ne acid water heating kettle, 180 DEG C
High temperature hydro-thermal, which reflects after 12-18h, hydro-thermal reaction stop, being cooled to room temperature solution；
(2) nitrogen-doped graphene secondary oxidation: by the preparatory ultrasonic disperse 30- in the reaction vessel of dispersion liquid obtained by step (1)
60min, it is then cooling under the conditions of -15--5 DEG C, the concentrated sulfuric acid of 5-8 part weight, the concentrated nitric acid and lane nitre of 1-5 part weight is added
Sour mixed solution, standing make its reaction sufficiently, and solution is then transferred to water-bath water-bath, and bath temperature is 25-50 DEG C；It is added
The hydrogen peroxide of 10-20 parts of weight, stirring, standing keep its reaction abundant；
(3) nitrogen-doped graphene/di-iron trioxide combination electrode material preparation: by the soluble ferrite of 1-3 parts of weight,
The graphene oxide dispersion of 400-600 parts of weight ratios is added in dispersion liquid, heats handle magnetic agitation；Transfer the solution into poly- four
In vinyl fluoride reaction kettle, it is cooled to room temperature after 120-140 DEG C of sealed thermal insulating 3-6h, obtains nitrogen-doped graphene/tri- oxidations two
Molten iron gel；By hydrogel liquid nitrogen pre-freeze 4-7min, it is then transferred to freeze drier, dry 48h, obtains nitrogen at -80 DEG C
Doped graphene/di-iron trioxide combination electrode material.
Further, a kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method, the step (3)
The soluble ferrite is one of ferrous sulfate, ferrous oxalate, frerrous chloride, ferrous nitrate.
Further, a kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method, the step
Suddenly the concentration of graphene oxide dispersion is 1-8mg/ml in (3).
The invention has the following advantages: a kind of nitrogen-doped graphene of the invention/di-iron trioxide combination electrode material
The preparation method of material has high-specific surface area and good three-dimensional structure channel, can provide for the storage of electrolyte with transport
Place, electrode realize that collector is integrated with active material, provide the comprehensive performance of electrode material, can look forward to its
The new energy field of batteries such as flow battery has broad application prospects.
Specific embodiment
Embodiment 1
Kind nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method, follows the steps below:
(1) preparation of nitrogen-doped graphene: graphene oxide is made by Humers, by the graphite powder and 10 parts of weight of 20 parts of weight
Sodium nitrate mixing drying 8h, be transferred in three-necked flask, and the concentrated sulfuric acid of 10 parts of weight is added thereto under condition of ice bath,
Slowly be uniformly added into the potassium permanganate of 10 parts of weight, remove ice bath device, by mixed solution at 60 DEG C incubation water heating 6h, again
It is slowly added to the ice water of 100 parts of weight, after be transferred the solution into beaker after the completion of exothermic heat of reaction, is dripped while stirring into solution
The hydrogen peroxide for adding 20 parts of weight removes extra potassium permanganate, is in glassy yellow after solution reflection completely, is filtered with sand core funnel bright
Yellow solution, and remaining chloride ion in washing solution is diluted with salt acid elution five times, then with deionized water；It is extra when eliminating
After metal ion and chloride ion, graphene filter cake, which is dispersed in deionized water, is dispersed with stirring 30min, then filtering and washing；It will
The graphene dispersion of 20 parts of weight stirs 20min in the concentrated ammonia liquor of 100 parts of weight, then ultrasound 20min, will be finely dispersed
Solution is transferred in polytetrafluoroethyl-ne acid water heating kettle, and 180 DEG C of high temperature hydro-thermals, which reflect after 12h, hydro-thermal reaction stop, being cooled to solution
Room temperature；
(2) nitrogen-doped graphene secondary oxidation: by the preparatory ultrasonic disperse 30min in the reaction vessel of dispersion liquid obtained by step (1),
Then cooling under the conditions of -15 DEG C, the concentrated sulfuric acid of 5 parts of weight, the concentrated nitric acid of 1 part of weight is added and does nitric acid mixed solution, it is quiet
Setting makes its reaction sufficiently, and solution is then transferred to water-bath water-bath, and bath temperature is 25 DEG C；The dioxygen of 10 parts of weight is added
Water, stirring, standing keep its reaction abundant；
(3) nitrogen-doped graphene/di-iron trioxide combination electrode material preparation: by the ferrous sulfate of 1 part of weight, 400 parts of weights
The graphene oxide dispersion for measuring ratio is added in dispersion liquid, heats handle magnetic agitation；Transfer the solution into polytetrafluoroethyl-ne alkene reaction
In kettle, it is cooled to room temperature after 120-140 DEG C of sealed thermal insulating 3-6h, obtains nitrogen-doped graphene/di-iron trioxide hydrogel；It will
Hydrogel liquid nitrogen pre-freeze 4-7min, is then transferred to freeze drier, the dry 48h at -80 DEG C, obtain nitrogen-doped graphene/
Di-iron trioxide combination electrode material；The concentration of graphene oxide dispersion is 1-8mg/ml.
Embodiment 2
A kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method of the invention, according to the following steps into
Row:
(1) preparation of nitrogen-doped graphene: graphene oxide is made by Humers, by the graphite powder and 16 parts of weight of 30 parts of weight
Sodium nitrate mixing dry 12h, be transferred in three-necked flask, and the concentrated sulfuric acid of 17 parts of weight is added thereto under condition of ice bath,
Slowly be uniformly added into the potassium permanganate of 17 parts of weight, remove ice bath device, by mixed solution at 80 DEG C incubation water heating 9h, again
It is slowly added to the ice water of 120 parts of weight, after be transferred the solution into beaker after the completion of exothermic heat of reaction, is dripped while stirring into solution
The hydrogen peroxide for adding 30 parts of weight removes extra potassium permanganate, is in glassy yellow after solution reflection completely, is filtered with sand core funnel bright
Yellow solution, and remaining chloride ion in washing solution is diluted with salt acid elution five times, then with deionized water；It is extra when eliminating
After metal ion and chloride ion, graphene filter cake, which is dispersed in deionized water, is dispersed with stirring 30min, then filtering and washing；It will
The graphene dispersion of 35 parts of weight stirs 40min in the concentrated ammonia liquor of 150 parts of weight, then ultrasound 60min, will be finely dispersed
Solution is transferred in polytetrafluoroethyl-ne acid water heating kettle, and 180 DEG C of high temperature hydro-thermals, which reflect after 18h, hydro-thermal reaction stop, being cooled to solution
Room temperature；
(2) nitrogen-doped graphene secondary oxidation: by the preparatory ultrasonic disperse 60min in the reaction vessel of dispersion liquid obtained by step (1),
Then cooling under the conditions of -5 DEG C, the concentrated sulfuric acid of 8 parts of weight, the concentrated nitric acid of 5 parts of weight is added and does nitric acid mixed solution, stands
Make its reaction sufficiently, solution is then transferred to water-bath water-bath, bath temperature is 50 DEG C；The hydrogen peroxide of 20 parts of weight is added,
Stirring, standing keep its reaction abundant；
(3) nitrogen-doped graphene/di-iron trioxide combination electrode material preparation: by the ferrous oxalate of 3 parts of weight, 600 parts of weights
The graphene oxide dispersion for measuring ratio is added in dispersion liquid, heats handle magnetic agitation；Transfer the solution into polytetrafluoroethyl-ne alkene reaction
In kettle, it is cooled to room temperature after 140 DEG C of sealed thermal insulating 6h, obtains nitrogen-doped graphene/di-iron trioxide hydrogel；By hydrogel
Liquid nitrogen pre-freeze 4-7min, is then transferred to freeze drier, and the dry 48h at -80 DEG C obtains nitrogen-doped graphene/tri- oxidations
Two iron combination electrode materials；The concentration of graphene oxide dispersion is 1-8mg/ml.
Embodiment 3
A kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material, follows the steps below:
(1) preparation of nitrogen-doped graphene: graphene oxide is made by Humers, by the graphite powder and 13 parts of weight of 24 parts of weight
Sodium nitrate mixing drying 9h, be transferred in three-necked flask, and the concentrated sulfuric acid of 12 parts of weight is added thereto under condition of ice bath,
Slowly be uniformly added into the potassium permanganate of 12 parts of weight, remove ice bath device, by mixed solution at 65 DEG C incubation water heating 7h, again
It is slowly added to the ice water of 1100 parts of weight, after transfer the solution into beaker after the completion of exothermic heat of reaction, while stirring into solution
The hydrogen peroxide of 25 parts of weight is added dropwise, removes extra potassium permanganate, is in glassy yellow after solution reflection completely, is filtered with sand core funnel
Bright yellow solution, and remaining chloride ion in washing solution is diluted with salt acid elution five times, then with deionized water；It is extra when eliminating
Metal ion and chloride ion after, graphene filter cake, which is dispersed in deionized water, is dispersed with stirring 30min, then filtering and washing；
The graphene dispersion of 25 parts of weight is stirred into 25min in the concentrated ammonia liquor of 120 parts of weight, then ultrasound 30min, will be uniformly dispersed
Solution be transferred in polytetrafluoroethyl-ne acid water heating kettle, 180 DEG C of high temperature hydro-thermals reflect after 14h, hydro-thermal reaction stop that solution is cooling
To room temperature；
(2) nitrogen-doped graphene secondary oxidation: by the preparatory ultrasonic disperse 38min in the reaction vessel of dispersion liquid obtained by step (1),
Then cooling under the conditions of -10 DEG C, the concentrated sulfuric acid of 6 parts of weight, the concentrated nitric acid of 3 parts of weight is added and does nitric acid mixed solution, it is quiet
Setting makes its reaction sufficiently, and solution is then transferred to water-bath water-bath, and bath temperature is 30 DEG C；The dioxygen of 14 parts of weight is added
Water, stirring, standing keep its reaction abundant；
(3) nitrogen-doped graphene/di-iron trioxide combination electrode material preparation: by the frerrous chloride of 2 parts of weight, 450 parts of weights
The graphene oxide dispersion for measuring ratio is added in dispersion liquid, heats handle magnetic agitation；Transfer the solution into polytetrafluoroethyl-ne alkene reaction
In kettle, it is cooled to room temperature after 130 DEG C of sealed thermal insulating 4h, obtains nitrogen-doped graphene/di-iron trioxide hydrogel；By hydrogel
Liquid nitrogen pre-freeze 5min, is then transferred to freeze drier, and the dry 48h at -80 DEG C obtains nitrogen-doped graphene/tri- oxidations two
Iron combination electrode material, the concentration of graphene oxide dispersion are 1-8mg/ml.
Embodiment 4
A kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material, follows the steps below:
(1) preparation of nitrogen-doped graphene: graphene oxide is made by Humers, by the graphite powder and 14 parts of weight of 28 parts of weight
Sodium nitrate mixing drying 10h, be transferred in three-necked flask, and the dense sulphur of 15 parts of weight is added thereto under condition of ice bath
Acid is slowly uniformly added into the potassium permanganate of 15 parts of weight, removes ice bath device, by mixed solution at 75 DEG C incubation water heating 8h,
It is slowly added to the ice water of 116 parts of weight again, after transfer the solution into beaker after the completion of exothermic heat of reaction, while stirring to solution
The middle hydrogen peroxide that 27 parts of weight is added dropwise removes extra potassium permanganate, is in glassy yellow after solution reflection completely, is taken out with sand core funnel
Bright yellow solution is filtered, and with salt acid elution five times, then dilutes remaining chloride ion in washing solution with deionized water；It is more when eliminating
After remaining metal ion and chloride ion, graphene filter cake, which is dispersed in deionized water, is dispersed with stirring 30min, then filters and washes
It washs；The graphene dispersion of 32 parts of weight is stirred into 35min in the concentrated ammonia liquor of 145 parts of weight, then ultrasound 55min, will disperse
Uniform solution is transferred in polytetrafluoroethyl-ne acid water heating kettle, and 180 DEG C of high temperature hydro-thermals reflect 16h, by solution after hydro-thermal reaction stopping
It is cooled to room temperature；
(2) nitrogen-doped graphene secondary oxidation: by the preparatory ultrasonic disperse 55min in the reaction vessel of dispersion liquid obtained by step (1),
Then cooling under the conditions of -1 DEG C, the concentrated sulfuric acid of 7 parts of weight, the concentrated nitric acid of 4 parts of weight is added and does nitric acid mixed solution, stands
Make its reaction sufficiently, solution is then transferred to water-bath water-bath, bath temperature is 44 DEG C；The hydrogen peroxide of 18 parts of weight is added,
Stirring, standing keep its reaction abundant；
(3) nitrogen-doped graphene/di-iron trioxide combination electrode material preparation: by the ferrous nitrate of 2 parts of weight, 550 parts of weights
The graphene oxide dispersion for measuring ratio is added in dispersion liquid, heats handle magnetic agitation；Transfer the solution into polytetrafluoroethyl-ne alkene reaction
In kettle, it is cooled to room temperature after 135 DEG C of sealed thermal insulating 5h, obtains nitrogen-doped graphene/di-iron trioxide hydrogel；By hydrogel
Liquid nitrogen pre-freeze 6min, is then transferred to freeze drier, and the dry 48h at -80 DEG C obtains nitrogen-doped graphene/tri- oxidations two
Iron combination electrode material, the concentration of graphene oxide dispersion are 1-8mg/ml.
Claims (3)
1. a kind of nitrogen-doped graphene/di-iron trioxide combination electrode material preparation method, which is characterized in that according to following step
It is rapid to carry out:
(1) preparation of nitrogen-doped graphene: graphene oxide is made by Humers, by the graphite powder and 10-16 of 20-30 parts of weight
The sodium nitrate mixing drying 8-12h of part weight, is transferred in three-necked flask, and be added 10-17 parts thereto under condition of ice bath
The concentrated sulfuric acid of weight is slowly uniformly added into the potassium permanganate of 10-17 parts of weight, ice bath device is removed, by mixed solution in 60-80
Incubation water heating 6-9h at DEG C is slowly added to the ice water of 100-120 parts of weight again, after transfer the solution into after the completion of exothermic heat of reaction
In beaker, the hydrogen peroxide of 20-30 parts of weight is added dropwise into solution while stirring, removes extra potassium permanganate, solution has reflected
It is in glassy yellow after complete, filters bright yellow solution with sand core funnel, and with salt acid elution five times, then is molten with deionized water dilution washing
Remaining chloride ion in liquid；After eliminating extra metal ion and chloride ion, graphene filter cake is dispersed in deionized water
It is dispersed with stirring 30min, then filtering and washing；By the graphene dispersion of 20-35 parts of weight in the concentrated ammonia liquor of 100-150 parts of weight
20-40min is stirred, then ultrasound 20-60min, finely dispersed solution is transferred in polytetrafluoroethyl-ne acid water heating kettle, 180 DEG C
High temperature hydro-thermal, which reflects after 12-18h, hydro-thermal reaction stop, being cooled to room temperature solution；
(2) nitrogen-doped graphene secondary oxidation: by the preparatory ultrasonic disperse 30- in the reaction vessel of dispersion liquid obtained by step (1)
60min, it is then cooling under the conditions of -15--5 DEG C, the concentrated sulfuric acid of 5-8 part weight, the concentrated nitric acid and lane nitre of 1-5 part weight is added
Sour mixed solution, standing make its reaction sufficiently, and solution is then transferred to water-bath water-bath, and bath temperature is 25-50 DEG C；It is added
The hydrogen peroxide of 10-20 parts of weight, stirring, standing keep its reaction abundant；
(3) nitrogen-doped graphene/di-iron trioxide combination electrode material preparation: by the soluble ferrite of 1-3 parts of weight,
The graphene oxide dispersion of 400-600 parts of weight ratios is added in dispersion liquid, heats handle magnetic agitation；Transfer the solution into poly- four
In vinyl fluoride reaction kettle, it is cooled to room temperature after 120-140 DEG C of sealed thermal insulating 3-6h, obtains nitrogen-doped graphene/tri- oxidations two
Molten iron gel；By hydrogel liquid nitrogen pre-freeze 4-7min, it is then transferred to freeze drier, dry 48h, obtains nitrogen at -80 DEG C
Doped graphene/di-iron trioxide combination electrode material.
2. a kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material according to claim 1,
It is characterized in that, the step (3) soluble ferrite is ferrous sulfate, in ferrous oxalate, frerrous chloride, ferrous nitrate
It is a kind of.
3. a kind of preparation method of nitrogen-doped graphene/di-iron trioxide combination electrode material according to claim 1,
It is characterized in that, the concentration of graphene oxide dispersion is 1-8mg/ml in the step (3).
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| CN113155931A (en) * | 2021-04-09 | 2021-07-23 | 国家烟草质量监督检验中心 | Method for detecting chloride ions in tobacco and tobacco planting soil |
| CN117482905A (en) * | 2023-12-30 | 2024-02-02 | 江西国中业伟环保科技有限公司 | Composite material for recycling rare earth in industrial and mining wastewater and preparation method thereof |
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