CN114054030A - Preparation method of two-dimensional nickel-aluminum LDH composite material and application of two-dimensional nickel-aluminum LDH composite material in photocatalytic degradation of antibiotics - Google Patents
Preparation method of two-dimensional nickel-aluminum LDH composite material and application of two-dimensional nickel-aluminum LDH composite material in photocatalytic degradation of antibiotics Download PDFInfo
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- CN114054030A CN114054030A CN202111282492.4A CN202111282492A CN114054030A CN 114054030 A CN114054030 A CN 114054030A CN 202111282492 A CN202111282492 A CN 202111282492A CN 114054030 A CN114054030 A CN 114054030A
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- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003242 anti bacterial agent Substances 0.000 title claims abstract description 10
- 229940088710 antibiotic agent Drugs 0.000 title claims abstract description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 150000002815 nickel Chemical class 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 230000001699 photocatalysis Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 5
- YYCNOHYMCOXPPJ-UHFFFAOYSA-N alumane;nickel Chemical class [AlH3].[Ni] YYCNOHYMCOXPPJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 12
- 239000002028 Biomass Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 4
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000033444 hydroxylation Effects 0.000 claims description 3
- 238000005805 hydroxylation reaction Methods 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 2
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 2
- 244000105624 Arachis hypogaea Species 0.000 claims description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 2
- 235000018262 Arachis monticola Nutrition 0.000 claims description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- 235000021307 Triticum Nutrition 0.000 claims description 2
- 241000209140 Triticum Species 0.000 claims description 2
- 240000008042 Zea mays Species 0.000 claims description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 229940118662 aluminum carbonate Drugs 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 235000005822 corn Nutrition 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 238000005336 cracking Methods 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 159000000000 sodium salts Chemical class 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 238000005067 remediation Methods 0.000 description 2
- 229910000943 NiAl Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004941 influx Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
- B01J27/236—Hydroxy carbonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
- B01J27/25—Nitrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a preparation method of a two-dimensional nickel aluminum LDH composite material and application thereof in photocatalytic degradation of antibiotics, which mainly comprises the following steps: 1) obtaining biochar by a high-temperature cracking method; 2) mixing and stirring the biochar and the nickel/aluminum salt aqueous solution, and standing to obtain a reaction solution; 3) adding a sodium salt aqueous solution into the reaction solution to prepare a modified material by a coprecipitation method; 4) the biochar modified nickel-aluminum LDH material is obtained through the steps of washing, centrifuging, drying and the like, and the sheet structure of the two-dimensional layered hydroxide is maintained. The invention adopts a small amount of biochar to realize effective modification of the layered hydroxide, improves the specific surface area of the layered hydroxide, increases the surface active sites of the material, promotes the separation and charge transmission efficiency of photoproduction electron hole pairs on the surface of the material, has high efficiency of removing antibiotics under the illumination condition, and has potential application in the field of photocatalytic wastewater treatment.
Description
Technical Field
The invention relates to the technical field of layered metal hydroxide materials, in particular to a preparation method of a two-dimensional nickel aluminum LDH composite material and application of the two-dimensional nickel aluminum LDH composite material in photocatalytic degradation of antibiotics.
Background
In recent years, population growth, industrial expansion and demand for more food sources have led to the influx of various pollutants into water resources, and antibiotics are now considered as a large challenging class of pollutants that are widely used in agriculture to treat diseases and protect animal health, but such drugs can be discharged as parent compounds or metabolites out of the body and directly deposited into the environment, causing serious environmental pollution. Photocatalysis as an Advanced Oxidation Process (AOP) is a rapid, efficient method of degrading these non-biodegradable contaminants. The method has the advantages of no toxicity, easy operation, mild reaction conditions and the like, and only utilizes solar energy to decompose pollutants, thereby having low cost. Layered Double Hydroxides (LDHs) as a two-dimensional layered compound have the advantages of wide sources, stable chemical properties, low synthesis cost, no toxicity and the like, and are widely applied to the fields of adsorption, catalysts, pharmacology and the like, but single LDHs are difficult to further popularize in the practical application of the field of environmental remediation due to the defects of few surface functional groups, poor acid and alkali resistance, low reuse rate, easy aggregation and the like, so how to improve the adsorption performance of the LDHs is how to construct a functional layered metal hydroxide material by using the layered double hydroxides as a base material becomes one of the hotspots of the research of the field of recent environmental remediation.
Disclosure of Invention
The invention aims to solve the problems that: the preparation method of the two-dimensional nickel-aluminum LDH composite material and the application of the two-dimensional nickel-aluminum LDH composite material in photocatalytic degradation of antibiotics are provided, the problems of small specific surface area, poor adsorption performance and the like of the existing layered hydroxide can be effectively solved, and the two-dimensional nickel-aluminum LDH composite material is applied to catalytic degradation of antibiotics, so that the problem of environmental pollution is effectively solved.
The technical scheme provided by the invention for solving the problems is as follows: a method for the preparation of a two-dimensional nickel aluminium LDH composite material, said method comprising the steps of,
step S1, preparation of charcoal powder: crushing, grinding and sieving biomass raw materials to obtain biomass powder, then carrying out oxygen-limited pyrolysis on the biomass powder at 400-900 ℃ to obtain a biochar precursor, adding 0.5-1.5 mol/L acid solution into the biochar precursor, carrying out hydroxylation treatment for 12-20 h, and finally washing, centrifuging and drying to obtain biochar powder;
step S2, preparation of the nickel-aluminum LDH composite material: firstly, mixing and dissolving a certain amount of nickel salt and aluminum salt and the biochar in the step S1 in deionized water, dropwise adding a mixed aqueous solution of sodium hydroxide and sodium carbonate into the mixed solution at a certain speed under the stirring condition, stirring for 1-3 h at 40-50 ℃, then continuously stirring for 10-14 h at 50-70 ℃, and finally washing, centrifuging and drying to obtain the nickel-aluminum LDH/biochar composite material.
Preferably, the biomass raw material is selected from one or more of corn, wheat, bamboo, rice hull, wood and peanut shell.
Preferably, the acid is selected from one or more of sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid.
Preferably, the nickel salt is selected from one or more of nickel nitrate, nickel chloride, nickel sulfate and nickel carbonate.
Preferably, the aluminum salt is selected from one or more of aluminum nitrate, aluminum chloride, aluminum sulfate and aluminum carbonate.
Preferably, the mass ratio of the biochar to the nickel salt is (0.1-1): 100.
Preferably, the biochar modified nickel aluminum LDH material retains the original two-dimensional sheet structure.
The invention also discloses application of the two-dimensional nickel-aluminum LDH composite material prepared by any one of the methods in photocatalytic degradation of antibiotics, and the two-dimensional nickel-aluminum LDH composite material is applied to the field of photocatalytic treatment of wastewater.
Compared with the prior art, the invention has the advantages that:
(1) compared with the nickel-aluminum layered hydroxide, the nickel-aluminum LDH modified by a proper amount of biochar keeps the original two-dimensional layered sheet structure.
(2) Compared with the nickel-aluminum layered hydroxide, the nickel-aluminum LDH modified by a proper amount of charcoal has a larger specific surface area, and the adsorption performance is effectively improved.
(3) The existence of the biochar promotes the photoproduction electron hole separation and the charge transmission efficiency, thereby promoting the photocatalytic activity of the nickel-aluminum LDH.
(4) The preparation method has simple and convenient process, and the prepared photocatalyst has good photocatalytic performance, less impurities and complete reaction.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a TEM image of a sample obtained in example 2;
FIG. 2 is a graph showing the adsorption rate of samples obtained in example 1, example 2 and example 3 as a function of time, wherein the adsorption rate of example 2 after reaction for 1.5h in the dark is 1.7 times that of pure nickel aluminum layered hydroxide;
FIG. 3 is a graph showing the change of the intensity of photocurrent with time under the condition of alternating light and no light of the samples obtained in example 1, example 2 and example 3;
fig. 4 is a graph showing the photocatalytic degradation efficiency of the samples obtained in example 1, example 2, and example 3 as a function of time, and the degradation rate of the antibiotic after the example 2 is catalytically reacted for 1.5h under the illumination condition is 94.4%.
Detailed Description
The embodiments of the present invention will be described in detail with reference to the accompanying drawings and examples, so that how to implement the technical means for solving the technical problems and achieving the technical effects of the present invention can be fully understood and implemented.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the embodiments of the invention. As used in the description of embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Example 1:
preparing charcoal powder: crushing, grinding and sieving a biomass raw material to obtain biomass powder, then carrying out oxygen-limited pyrolysis on the biomass powder at 800 ℃ to obtain a biochar precursor, adding 1mol/L acid solution into the biochar precursor, carrying out hydroxylation treatment on the biochar precursor for 16h, and finally carrying out washing, centrifuging, drying and other steps to obtain the biochar powder.
Example 2:
4.653g Ni (NO)3·6H2O、3.001g Al(NO)3·9H2O and 0.005g of biochar is mixed and dissolved in 80mL of deionized water, and 2.40g of NaOH and 1.696g of Na are dropwise added into the mixed solution at a certain speed under the condition of stirring2CO3Stirring the aqueous solution at 45 ℃ for 2 hours, then continuously stirring the aqueous solution at 60 ℃ for 12 hours, and finally washing, centrifuging, drying and the like to obtain the nickel-aluminum LDH/biochar composite material.
Example 3:
the difference from the embodiment 2 is that: pure nickel aluminum LDH samples (NiAl-LDH) were prepared without adding biochar to the mixed solution.
Table 1: data on specific surface area of samples obtained in examples 1, 2 and 3
| Sample (I) | Specific surface area (m)2/g) |
| NiAl-LDH | 0.43 |
| NiAl/BC-0.5 | 87.28 |
| BC | 38.35 |
The foregoing is merely illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary. All changes which come within the scope of the invention as defined by the independent claims are intended to be embraced therein.
Claims (8)
1. A preparation method of a two-dimensional nickel aluminum LDH composite material is characterized by comprising the following steps: the method comprises the following steps of,
step S1, preparation of charcoal powder: crushing, grinding and sieving biomass raw materials to obtain biomass powder, then carrying out oxygen-limited pyrolysis on the biomass powder at 400-900 ℃ to obtain a biochar precursor, adding 0.5-1.5 mol/L acid solution into the biochar precursor, carrying out hydroxylation treatment for 12-20 h, and finally washing, centrifuging and drying to obtain biochar powder;
step S2, preparation of the nickel-aluminum LDH composite material: firstly, mixing and dissolving a certain amount of nickel salt and aluminum salt and the biochar in the step S1 in deionized water, dropwise adding a mixed aqueous solution of sodium hydroxide and sodium carbonate into the mixed solution at a certain speed under the stirring condition, stirring for 1-3 h at 40-50 ℃, then continuously stirring for 10-14 h at 50-70 ℃, and finally washing, centrifuging and drying to obtain the nickel-aluminum LDH/biochar composite material.
2. The method for preparing a two-dimensional nickel aluminum LDH composite material of claim 1, wherein: the biomass raw material is selected from one or more of corn, wheat, bamboo, rice hull, wood and peanut shell.
3. The method for preparing a two-dimensional nickel aluminum LDH composite material of claim 1, wherein: the acid is selected from one or more of sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid.
4. The method for preparing a two-dimensional nickel aluminum LDH composite material of claim 1, wherein: the nickel salt is selected from one or more of nickel nitrate, nickel chloride, nickel sulfate and nickel carbonate.
5. The method for preparing a two-dimensional nickel aluminum LDH composite material of claim 1, wherein: the aluminum salt is selected from one or more of aluminum nitrate, aluminum chloride, aluminum sulfate and aluminum carbonate.
6. The method for preparing a two-dimensional nickel aluminum LDH composite material of claim 1, wherein: the mass ratio of the biochar to the nickel salt is (0.1-1): 100.
7. The method for preparing a two-dimensional nickel aluminum LDH composite material of claim 1, wherein: the biochar modified nickel-aluminum LDH material keeps the original two-dimensional sheet structure.
8. The application of the two-dimensional nickel aluminum LDH composite material prepared by the method in any one of claims 1 to 7 in photocatalytic degradation of antibiotics is applied to the field of photocatalytic treatment of wastewater.
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| CN114733542A (en) * | 2022-04-26 | 2022-07-12 | 国家石油天然气管网集团有限公司 | Biochar composite catalyst and preparation method and application thereof |
Citations (10)
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