CN114768756A - Thickness-controllable alumina/carbon nanosheet and application thereof in heavy metal adsorption - Google Patents
Thickness-controllable alumina/carbon nanosheet and application thereof in heavy metal adsorption Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000002135 nanosheet Substances 0.000 title claims abstract description 26
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 16
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 22
- 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 abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 11
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 9
- 239000005011 phenolic resin Substances 0.000 claims description 9
- 229920001568 phenolic resin Polymers 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 229960000502 poloxamer Drugs 0.000 claims description 4
- 229920001983 poloxamer Polymers 0.000 claims description 4
- VWWHFOBVDHPEKJ-UHFFFAOYSA-N aluminum ethanol trinitrate Chemical compound C(C)O.[N+](=O)([O-])[O-].[Al+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] VWWHFOBVDHPEKJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002064 nanoplatelet Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 241000446313 Lamella Species 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract description 2
- 238000005530 etching Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 48
- 239000011651 chromium Substances 0.000 description 29
- 239000000203 mixture Substances 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 238000002835 absorbance Methods 0.000 description 8
- 229910052593 corundum Inorganic materials 0.000 description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 description 8
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical group C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910001430 chromium ion Inorganic materials 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 206010028400 Mutagenic effect Diseases 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 231100000405 induce cancer Toxicity 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 231100000243 mutagenic effect Toxicity 0.000 description 1
- 230000003505 mutagenic effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 231100000378 teratogenic Toxicity 0.000 description 1
- 230000003390 teratogenic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000002912 waste gas Substances 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of nano materials, and particularly relates to an alumina/carbon nano sheet with controllable thickness and application thereof in heavy metal adsorption. The method utilizes the etching effect of ammonia water on aluminum oxide, takes aluminum nitrate as a copper source and acetylacetone as a complex, and obtains Al with a sheet structure after in-situ synthesis at room temperature and high-temperature heat treatment2O3The thickness of the lamella of the/C compound can be adjusted within the range of 5-50 nm by controlling the adding amount of the aluminum source and the compound, and the material is simple in preparation method and suitable for industrial application. The material is used for Cr (VI) adsorption, the removal rate of Cr (VI) can reach 100 percent in 3 hours at room temperature, and excellent adsorption is shownAnd (4) adhesion performance.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to an alumina/carbon nano sheet with controllable thickness and application thereof in heavy metal adsorption.
Background
Heavy metal contamination refers to environmental contamination caused by heavy metals or compounds thereof. Mainly caused by human factors such as mining, waste gas discharge, sewage irrigation, use of products with heavy metals exceeding standards and the like. The heavy metal content in the environment increases due to human activities, which exceeds the normal range, directly harms human health, and causes deterioration of environmental quality.
With the continuous development of the industry in China, the problem of heavy metal pollution needs to be solved urgently. A large amount of industrial wastewater containing chromium ions is discharged into the environment without being treated, resulting in increasing chromium pollution. Scientific research shows that Cr (VI) has strong toxicity and mobility, and in the pH range of normal human bodies, Cr (VI) easily penetrates through cell membranes to enter cells and reacts with intracellular substances to be reduced into Cr (III). The intermediate products generated in the process can react with DNA to cause the unwinding or the breaking of the DNA, thereby causing great harm to human bodies. In addition, cr (vi) can induce cancer, has potential teratogenic and mutagenic effects, and is one of three carcinogenic metal substances recognized internationally. Therefore, how to remove Cr (VI) in the environment by a simple and convenient method is significant.
Disclosure of Invention
The invention aims to provide an alumina/carbon nanosheet with controllable lamellar thickness for Cr (VI) adsorption, aluminum nitrate is used as a copper source, acetylacetone is used as a complex for in-situ synthesis at room temperature by utilizing the etching effect of ammonia water on alumina, and Al with a lamellar structure is obtained after high-temperature heat treatment2O3the/C composite can adjust the lamella thickness of the composite within the range of 5-50 nm by controlling the adding amount of the aluminum source and the complex, and the material has simple preparation method and is suitable for industrial application. The material is used for Cr (VI) adsorption, the removal rate of Cr (VI) can reach 100 percent at room temperature within 3 hours, and the material shows excellent adsorption performance.
The technical scheme of the invention is as follows:
the application of the thickness-controllable alumina/carbon nanosheet in heavy metal adsorption is disclosed, and the preparation method of the thickness-controllable alumina/carbon nanosheet comprises the following steps:
(1) adding poloxamer F127 ethanol solution into the phenolic resin ethanol solution, and uniformly stirring; slowly dripping an aluminum nitrate ethanol solution; then adding acetylacetone solution and stirring;
(2) after the reaction is finished, adding ammonia water to adjust the pH value, and continuously stirring;
(3) filtering and washing to neutrality; nitrogen atmosphere 500-800 after dryingoC, heat treatment;
the phenolic resin, poloxamer F127 and aluminum nitrate are added in a mass ratio of: 10-30: 0.5-2: 0.2-2; the molar ratio of the addition amount of the acetylacetone to the aluminum nitrate is 1-10: 1.
Preferably, the thickness of the alumina/carbon nano-sheet ranges from 5 nm to 50 nm.
Further, the adsorbent is used for adsorbing heavy metal Cr (VI).
The invention has the advantages of
A series of alumina carbon materials with different loading amounts are synthesized by a certain chemical method by utilizing the advantages of rich hydroxyl on the surface of the alumina, large specific surface area, high thermal stability, high specific surface area of the activated carbon material, good thermal stability and chemical stability and excellent adsorption performance to Cr (VI). The obtained material can continuously detoxify Cr (VI) without using other activators, has abundant micropores and large specific surface area, and can realize excellent adsorption on chromium ions. Therefore, the invention has excellent adsorption effect on hexavalent chromium ions in the water body, and has high adsorption speed and removal rate.
Drawings
FIG. 1 shows Cr removal for materials synthesized with different alumina loadings;
FIG. 2 scanning electron micrograph of materials synthesized at different alumina loadings, (a) 5 wt.% Al2O3/C; (b) 20 wt.%Al2O3/C; (c) 50 wt.%Al2O3/C。
Detailed Description
Example 1:
the application of the alumina/carbon nano-sheet with controllable thickness in heavy metal adsorption comprises the following steps:
(1) adding 20% phenolic resin (20 g) ethanol solution into F127 (1 g) ethanol solution (0.2 g/mL) at 35%oC and stirring for 10 min at the rotating speed of 600 rpm. 0.95 g of an ethanol solution of aluminum nitrate (0.2 g/mL) was slowly dropped into the above mixed solution, and then 0.77 mL of an acetylacetone solution was added thereto, followed by stirring for another 40 min.
(2) Dropwise adding an ammonia water solution with the concentration of 4 mol/mL into the solution, adjusting the pH value to 12, and continuously stirring for 1 h; filtering and washing to neutrality.
(3) Placing the mixture into a container 100oC, placing the mixture in an oven for 24 hours, and then performing a nitrogen atmosphere 600oC heat treatment to get 20 wt.% Al2O3a/C nano-sheet. The thickness of the nano-sheet is as follows: and (5) 25 nm.
(4) In a 30 mL glass bottle, 20 mL of 1mg/L Cr (VI) solution was added, and then 40 mg of Al prepared in step (2) was weighed2O3the/C is added as an adsorbent. At the time of 10 min, 30 min, 1 h, 3 h and 6 h, respectively, 3 mL of filtrate was obtained by filtration with a disposable syringe and a 0.45 μm filter, 60 μ L of phosphoric acid solution was added, 120 μ L of diphenylcarbodihydrazide indicator was added after shaking, and shaking was performed again. Standing for 8 min, and measuring absorbance of the dibenzoyl dihydrazide solution (indicator) at the maximum absorption wavelength of 540 nm by spectrophotometry with water as reference. According to the absorbance and the standard curve, the Cr (VI) removal rate is calculated, and under the condition of adsorbing for 3 hours at room temperature, the material and the Cr (VI) removal rate can reach 100 percent.
Example 2:
the application of the thickness-controllable alumina/carbon nanosheet in heavy metal adsorption comprises the following steps:
(1) adding 20% phenolic resin (30 g) ethanol solution into F127 (0.5 g) ethanol solution (0.2 g/mL) at 35%oC, stirring for 10 min at the rotating speed of 600 rpm. 0.38 g of an aluminum nitrate ethanol solution (0.2 g/mL) was slowly dropped into the above mixed solution, and then 0.31 mL of an acetylacetone solution was added thereto, followed by further addition ofStirring for 40 min.
(2) Dropwise adding an ammonia water solution with the concentration of 4 mol/mL into the solution, adjusting the pH value to 10, and continuously stirring for 1 h; filtering and washing to be neutral.
(3) Placing the mixture into a container 100oC, placing the mixture in an oven for 24 hours, and then performing a nitrogen atmosphere 600oC heat treatment to get 10 wt.% Al2O3a/C nano-sheet. The thickness of the nano-sheet is as follows: and 10 nm.
(4) In a 30 mL glass bottle, 20 mL of a 1mg/L Cr (VI) solution was added, and then 40 mg of Al prepared in step (3) was weighed2O3the/C is added as an adsorbent. At the time of 10 min, 30 min, 1 h, 3 h and 6 h respectively, 3 mL of filtrate was obtained by filtration with a disposable syringe and a 0.45 μm filter, 60 μ L of phosphoric acid solution was added, 120 μ L of dibenzoyl dihydrazide indicator was added after shaking, and shaking was performed again. Standing for 8 min, and measuring absorbance of the dibenzoyl dihydrazide solution (indicator) at the maximum absorption wavelength of 540 nm by spectrophotometry with water as reference. According to the absorbance and the standard curve, the Cr (VI) removal rate is calculated, and under the condition of room-temperature adsorption for 3 hours, the Cr (VI) removal rate of the material and the Cr (VI) removal rate can reach 82%. Under the condition of room temperature adsorption for 6 hours, the removal rate of the material and Cr (VI) can reach 99 percent.
Example 3:
the application of the thickness-controllable alumina/carbon nanosheet in heavy metal adsorption comprises the following steps:
(1) adding 20% phenolic resin (10 g) ethanol solution into F127 (2 g) ethanol solution (0.2 g/mL) at 35%oC, stirring for 10 min at the rotating speed of 600 rpm. 0.75 g of an ethanol solution of aluminum nitrate (0.2 g/mL) was slowly added dropwise to the mixed solution, and then 0.61 mL of an acetylacetone solution was added thereto, followed by stirring for another 40 min.
(2) Dropwise adding an ammonia water solution with the concentration of 4 mol/mL into the solution, adjusting the pH value to 12, and continuously stirring for 1 h; filtering and washing to neutrality.
(3) Placing the mixture into a container 100oC, placing the mixture in an oven for 24 hours, and then performing nitrogen atmosphere600 oC heat treatment to give 15 wt.% Al2O3a/C nano-sheet. The thickness of the nano-sheet is as follows: and (5) 20 nm.
(4) In a 30 mL glass bottle, 20 mL of 1mg/L Cr (VI) solution was added, and then 40 mg of Al prepared in step (3) was weighed2O3the/C is added as an adsorbent. At the time of 10 min, 30 min, 1 h, 3 h and 6 h respectively, 3 mL of filtrate was obtained by filtration with a disposable syringe and a 0.45 μm filter, 60 μ L of phosphoric acid solution was added, 120 μ L of dibenzoyl dihydrazide indicator was added after shaking, and shaking was performed again. Standing for 8 min, and measuring absorbance of the dibenzoyl dihydrazide solution (indicator) at the maximum absorption wavelength of 540 nm by spectrophotometry with water as reference. According to the absorbance and the standard curve, the Cr (VI) removal rate is calculated, and under the condition of adsorbing for 3 hours at room temperature, the Cr (VI) removal rate of the material and the Cr (VI) removal rate can reach 86%. Under the condition of adsorbing for 6 hours at room temperature, the removal rate of the material and Cr (VI) can reach 98 percent.
Example 4:
the application of the thickness-controllable alumina/carbon nanosheet in heavy metal adsorption comprises the following steps:
(1) adding 20% phenolic resin (10 g) ethanol solution into F127 (1 g) ethanol solution (0.2 g/mL) at 35%oC, stirring for 10 min at the rotating speed of 600 rpm. To the mixed solution, 1.14 g of an ethanol solution of aluminum nitrate (0.2 g/mL) was slowly dropped, and then 0.93 mL of an acetylacetone solution was added thereto, followed by stirring for 40 minutes.
(2) Dropwise adding an ammonia water solution with the concentration of 4 mol/mL into the solution, adjusting the pH value to 12, and continuously stirring for 1 h; filtering and washing to be neutral.
(3) Placing the mixture in an oven at 100 deg.C for 24 hr, and introducing into nitrogen atmosphere 600oC heat treatment to get 30 wt.% Al2O3a/C nano sheet. The thickness of the nano-sheet is as follows: and 35 nm.
(4) In a 30 mL glass bottle, 20 mL of 1mg/L Cr (VI) solution was added, and then 40 mg of Al prepared in step (3) was weighed2O3C as suctionAn adjuvant is added thereto. At the time of 10 min, 30 min, 1 h, 3 h and 6 h, respectively, 3 mL of filtrate was obtained by filtration with a disposable syringe and a 0.45 μm filter, 60 μ L of phosphoric acid solution was added, 120 μ L of diphenylcarbodihydrazide indicator was added after shaking, and shaking was performed again. Standing for 8 min, and measuring absorbance of the dibenzoyl dihydrazide solution (indicator) at the maximum absorption wavelength of 540 nm by spectrophotometry with water as reference. According to the absorbance and the standard curve, the Cr (VI) removal rate is calculated, and under the condition of adsorbing for 3 hours at room temperature, the material and the Cr (VI) removal rate can reach 57 percent. Under the condition of adsorbing for 6 hours at room temperature, the removal rate of the material and Cr (VI) can reach 99 percent.
Example 5:
the application of the alumina/carbon nano-sheet with controllable thickness in heavy metal adsorption comprises the following steps:
(1) adding 20% phenolic resin ethanol solution into F127 ethanol solution (0.2 g/mL) at 35%oC and stirring for 10 min at the rotating speed of 600 rpm. To the mixed solution, 1.90 g of an ethanol solution of aluminum nitrate (0.2 g/mL) was slowly dropped, and then 1.5 mL of an acetylacetone solution was added thereto, followed by stirring for another 40 min.
(2) Dropwise adding an ammonia water solution with the concentration of 4 mol/mL into the solution, adjusting the pH value to 12, and continuously stirring for 1 h; filtering and washing to be neutral.
(3) Placing the mixture into a container 100oC, placing the mixture in an oven for 24 hours, and then performing nitrogen atmosphere 600oC heat treatment to give 50 wt.% Al2O3a/C nano-sheet. The thickness of the nano-sheet is as follows: the sheet structure collapses to a thickness of about 10 nm.
(4) Preparation of 0.1g of Pb2+The lead nitrate solution of/L is added with 10 percent of HNO dropwise3The pH was adjusted to 6.0. And (3) putting 300mL into a 1000mL conical flask, adding 0.01 g of the nanosheet in the step (3), and shaking at room temperature at 100 rpm. Samples were taken every 0.5 min and the Pb in the solution was determined according to GB/T7475-19872+And (4) concentration. Calculation of Pb2+Removal rate, Pb of the material adsorbed at room temperature for 3 hours2+The removal rate can reach 67 percent. Adsorbing at room temperature for 6 hrPb of the material2+The removal rate can reach 87%.
Claims (3)
1. The application of the thickness-controllable alumina/carbon nanosheet in heavy metal adsorption is characterized in that the preparation method of the thickness-controllable alumina/carbon nanosheet comprises the following steps:
(1) adding poloxamer F127 ethanol solution into the phenolic resin ethanol solution, and uniformly stirring; slowly dripping an aluminum nitrate ethanol solution; then adding acetylacetone solution and stirring;
(2) after the reaction is finished, adding ammonia water to adjust the pH value to 12, and continuing stirring;
(3) filtering and washing to be neutral; after drying, performing heat treatment at the temperature of 500 ℃ and 800 ℃ in a nitrogen atmosphere;
the phenolic resin, poloxamer F127 and aluminum nitrate are added in a mass ratio of: 10-30: 0.5-1: 0.1-10; the molar ratio of the addition amount of the acetylacetone to the aluminum nitrate is 1-10: 1.
2. The use according to claim 1, wherein the thickness of the alumina/carbon nanoplatelets ranges from 5 to 50 nm.
3. Use according to claim 1, for the adsorption of the heavy metal Cr (VI).
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2009068117A1 (en) * | 2007-11-30 | 2009-06-04 | Nanologica Ab | Method for manufacturing a nanoporous alumina based materials with controlled textural and particle size and nanoporous alumina obtained by said method |
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