CN112023876A - Preparation of magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material and application of adsorption material in removal of phosphorus in wastewater - Google Patents
Preparation of magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material and application of adsorption material in removal of phosphorus in wastewater Download PDFInfo
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- 235000013162 Cocos nucifera Nutrition 0.000 title claims abstract description 70
- 244000060011 Cocos nucifera Species 0.000 title claims abstract description 70
- 239000002028 Biomass Substances 0.000 title claims abstract description 51
- 239000000463 material Substances 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 42
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000003610 charcoal Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002351 wastewater Substances 0.000 title claims abstract description 18
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title abstract description 38
- 229910052698 phosphorus Inorganic materials 0.000 title abstract description 38
- 239000011574 phosphorus Substances 0.000 title abstract description 38
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- 239000000835 fiber Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 22
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 20
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 10
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 15
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 12
- 229960002218 sodium chlorite Drugs 0.000 claims description 12
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 238000004042 decolorization Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 229910003023 Mg-Al Inorganic materials 0.000 abstract description 21
- 239000002699 waste material Substances 0.000 abstract description 9
- 238000004140 cleaning Methods 0.000 abstract 2
- 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 abstract 1
- 239000003513 alkali Substances 0.000 abstract 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 abstract 1
- 229940077239 chlorous acid Drugs 0.000 abstract 1
- 239000003463 adsorbent Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 description 7
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000010170 biological method Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 150000003018 phosphorus compounds Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010457 zeolite 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
- B01J20/20—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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic 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)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention belongs to the technical field of composite materials, relates to a preparation method of a modified biomass charcoal material, and particularly relates to a preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material, which comprises the following steps: soaking the crushed coconut shells in alkali liquor to remove impurities, cleaning, adding acetic acid acidified chlorous acid to decolor, cleaning and drying to obtain coconut shell fibers; continuously soaking in an aluminum nitrate solution, filtering, drying, and calcining at 200-800 ℃ in a nitrogen atmosphere to obtain Al2O3(ii) CSF; magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 0.3-1.8 g, 0.1-0.9 g, 0.05-1.0 g and 50-200 mL2O3CSF, hexamethylenetetramine solutionReacting in deionized water at 60-180 ℃ for 6-48 h, filtering, washing and calcining at high temperature to obtain Mg-Al/CSF. The invention utilizes common waste coconut shells as biomass resources, is prepared by a hydrothermal and calcining method, can realize the high-efficiency removal of phosphorus in wastewater, can recycle materials, reduces the preparation cost to the maximum extent, and improves the adsorption performance.
Description
Technical Field
The invention belongs to the technical field of composite materials, relates to a preparation method of a modified biomass charcoal material, and particularly relates to preparation of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material and application of the adsorption material in removal of phosphorus in wastewater.
Background
In recent years, with the economic development and the modernization of social industry, the discharge amount of various environmental pollutants is increasing day by day, and particularly, the discharge amount of phosphorus is increasing sharply, so that the natural water environment is seriously damaged. At present, the commonly used sewage dephosphorization techniques include a chemical precipitation method, an adsorption method, an ion exchange method, a biological method and the like. The simple precipitation method is difficult to remove a large amount of phosphorus compounds in the sewage; the biological method has limited dephosphorization treatment effect; the ion exchange method has a series of defects of high resin preparation price, low exchange capacity, poor selectivity and the like. The adsorption method has the advantages of high efficiency, low cost, simple operation, reproducibility, sustainability and the like, and the key point of removing phosphorus by utilizing the adsorption method lies in the selection of the adsorbent. The conventional adsorbents comprise active carbon, zeolite and the like, and a large amount of sludge is generated in the using process, so that the application effect is poor. Therefore, the search for an environment-friendly adsorbent capable of efficiently removing phosphorus from wastewater is urgent. Meanwhile, the biomass material is utilized to prepare the composite material which can be used as the adsorbent, so that the composite material is widely concerned in the aspect of environmental improvement.
Biomass-based carbon materials are generally obtained by discarding agricultural and forestry crops, have the characteristics of easy availability, good adsorption performance and the like, and are widely concerned, but the preparation of biomass materials for adsorbing phosphorus in water by using agricultural and forestry wastes as precursors is rarely reported. The agricultural and forestry wastes are used as the precursor of the biomass composite material, so that the agricultural and forestry wastes are fully utilized, the wastes can be treated by the wastes, and the aim of protecting the environment is fulfilled. The biomass carbon material has adsorption capacity and is an effective method for removing phosphorus. The biomass charcoal material is doped with metal or metal oxide, so that the adsorption capacity of the adsorbent can be improved, and the composite material has catalytic performance and can remove pollutants in multiple ways.
The invention takes waste coconut shells as a biomass carbon precursor, selects the magnesium-aluminum bimetal composite oxide, prepares the magnesium-aluminum bimetal composite oxide/biomass carbon composite material with a hierarchical structure by an in-situ growth method, and applies the magnesium-aluminum bimetal composite oxide/biomass carbon composite material to the removal of phosphorus in wastewater. In addition, the agricultural and forestry waste is used as a precursor of the adsorbent, so that the waste agricultural and forestry crops generated in the natural environment are fully utilized, and a good adsorbent is provided for removing phosphorus in water.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to disclose a preparation method of a biomass charcoal adsorbing material of coconut shells modified by magnesium-aluminum composite oxides.
Technical scheme
A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material comprises the following steps:
a) soaking crushed coconut shells in a sodium hydroxide solution, stirring for 1-8 h, preferably 1M at 60-150 ℃, stirring for 3h at 80 ℃, removing impurities, washing with deionized water, adding into an acetic acid acidified sodium chlorite solution for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) according to the method, 1-20 g of aluminum nitrate nonahydrate is dissolved in per 100mL of deionized water, the obtained coconut shell fiber is soaked for 5-20 h, then is filtered, preferably 5g is soaked for 10h, the dried sample is calcined for 2-8 h at 200-800 ℃ in a nitrogen atmosphere, preferably 4h at 400 ℃, and the coconut shell fiber (Al) coated with alumina is obtained2O3/CSF)；
c) Magnesium nitrate hexahydrate and Al are mixed according to a solid-to-liquid ratio of 0.3-1.8 g, 0.1-0.9 g, 0.05-1.0 g, 50-200 mL, preferably 0.9g, 0.3g, 0.5g, 75mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, stirring, and mixingTransferring the substance into a stainless steel reaction kettle, reacting for 6-48 h at 60-180 ℃, preferably reacting for 12h at 120 ℃, filtering, washing, calcining the dried product for 2-8 h at 200-800 ℃ in a nitrogen atmosphere, preferably calcining for 4h at 500 ℃ to obtain the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorbing material (Mg-Al/CSF).
In the preferred embodiment of the invention, the concentration of the sodium hydroxide solution is 0.2-1.5M, and the sodium chlorite solution acidified by acetic acid is prepared by dissolving sodium chlorite in water according to the mass fraction of 5% and then adjusting the pH value to 4 by using acetic acid.
According to the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF) prepared by the method, the original coconut shell fiber structure is still maintained in the shape, and the hierarchical structure nanosheet growing on the surface effectively improves the specific surface area of the Mg-Al/CSF material, so that more adsorption sites are exposed, and the Mg-Al/CSF material can be used for removing phosphorus elements in wastewater.
The invention also aims to apply the prepared magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorbing material (Mg-Al/CSF) to the dephosphorization of wastewater.
The invention discloses a method for removing phosphorus element in wastewater, which comprises the following steps:
adding 10-40 Mg of Mg-Al/CSF into every 10mL of 100Mg/L potassium dihydrogen phosphate solution, adjusting the pH of the solution to 3-10 at the temperature of 25-45 ℃, adsorbing for 2h, detecting the phosphorus concentration at the position of 700nm of wavelength by using a visible spectrophotometer, and calculating to obtain the phosphorus concentration.
Phosphorus removal was calculated from equation (1):
wherein R is the removal rate (%), C0(mg/L) is the initial concentration of the ion before adsorption, CeThe concentration of ions in the solution at the equilibrium adsorption time t is shown.
The invention has the characteristics that:
(1) the prepared magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF) has good biocompatibility, and is convenient in raw material acquisition, simple in preparation process and low in cost;
(2) the prepared magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF) has an obvious hierarchical structure and more adsorption sites on the surface, and has higher adsorption capacity on phosphorus in wastewater; the adsorption condition is mild, a small amount of adsorbent can realize higher removal rate, and the material can be recycled.
The sodium hydroxide, acetic acid, hydrochloric acid, sodium chlorite, magnesium nitrate hexahydrate, hexamethylenetetramine, potassium dihydrogen phosphate and aluminum nitrate nonahydrate used in the invention are all from the chemical reagent company Limited of the national medicine group.
Advantageous effects
The invention discloses a preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF) for removing phosphorus elements in environmental wastewater. The method has a good application prospect in the field of efficient wastewater dephosphorization, and has the advantages of energy conservation, environmental protection, convenience in recovery and the like.
Drawings
FIG. 1 coconut husk fiber (A, B) prepared in example 3, Al2O3SEM of coconut shell fiber (C, D) and magnesium aluminum bimetal oxide/coconut shell carbon fiber (E, F);
FIG. 2 CSF, Al prepared in example 32O3XRD of/CSF and Mg-Al/CSF.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Unless otherwise defined, terms (including technical and scientific terms) used herein should be construed to have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art, and should not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material comprises the following steps:
a) soaking crushed coconut shells in 0.2M sodium hydroxide solution, stirring for 1h at 60 ℃, removing impurities, washing with deionized water, adding acetic acid acidified sodium chlorite solution (mass fraction is 5%) for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) according to the method, 1g of aluminum nitrate nonahydrate is dissolved in 100mL of deionized water, the obtained coconut shell fiber is soaked for 5h and then filtered, and a sample obtained by drying is calcined for 2h at 200 ℃ under the nitrogen condition to obtain the coconut shell fiber (Al) coated with aluminum oxide2O3/CSF)；
c) Magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 0.3g to 0.1g to 0.05g to 50mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, fully stirring, transferring the mixture into a stainless steel reaction kettle, reacting for 6 hours at 60 ℃, filtering, washing, calcining the dried product for 2 hours at 200 ℃ in a nitrogen atmosphere to obtain the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF).
Removing phosphorus in the wastewater:
after 10Mg of Mg-Al/CSF was added to 100Mg/L of 10mL of 100Mg/L potassium dihydrogen phosphate solution and the pH of the solution was adjusted to 3 and the solution was adsorbed at 25 ℃ for 2 hours, the phosphorus concentration was measured at a wavelength of 700nm using a visible spectrophotometer, and the phosphorus concentration was calculated.
The removal rate of the prepared adsorbent to phosphorus reaches 58%.
Example 2
A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material comprises the following steps:
a) soaking crushed coconut shells in 0.5M sodium hydroxide solution, stirring for 4h at 90 ℃, removing impurities, washing with deionized water, adding acetic acid acidified sodium chlorite solution (mass fraction is 5%) for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) according to the weight of 10g of aluminum nitrate nonahydrate dissolved in per 100mL of deionized water, the obtained coconut shell fiber is soaked for 8h, filtered, dried to obtain a sample, and calcined for 6h at 450 ℃ under the nitrogen condition to obtain the coconut shell fiber (Al) coated with aluminum oxide2O3/CSF)；
c) Magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 0.6g to 0.25g to 0.2g to 90mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, fully stirring, transferring the mixture into a stainless steel reaction kettle, reacting for 18 hours at 90 ℃, filtering, washing, calcining the dried product for 6 hours at 500 ℃ in a nitrogen atmosphere to obtain the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF).
Removing phosphorus in the wastewater:
after 15Mg of Mg-Al/CSF was added to 100Mg/L of 10mL of a potassium dihydrogen phosphate solution and the solution was adjusted to pH 7 and adsorbed at 30 ℃ for 2 hours, the phosphorus concentration was measured at a wavelength of 700nm using a visible spectrophotometer, and the phosphorus concentration was calculated.
The removal rate of the prepared adsorbent to phosphorus reaches 66%.
Example 3
A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material comprises the following steps:
a) soaking crushed coconut shells in 1M sodium hydroxide solution, stirring for 3h at 80 ℃, removing impurities, washing with deionized water, adding acetic acid acidified sodium chlorite solution (mass fraction is 5%) for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) calculated as 5g of aluminum nitrate nonahydrate dissolved in 100mL of deionized waterSoaking the obtained coconut shell fiber for 10h, filtering, drying to obtain a sample, calcining the sample at 400 ℃ for 4h under the nitrogen condition to obtain the coconut shell fiber (Al) coated by aluminum oxide2O3/CSF)；
c) Magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 0.9g to 0.3g to 0.5g to 75mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, fully stirring, transferring the mixture into a stainless steel reaction kettle, reacting for 12 hours at 120 ℃, filtering, washing, calcining the dried product for 4 hours at 500 ℃ in a nitrogen atmosphere to obtain the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF).
Removing phosphorus in the wastewater:
after adding 25Mg of Mg-Al/CSF per 10mL of 100Mg/L potassium dihydrogen phosphate solution and adjusting the pH of the solution to 6 and adsorbing at 45 ℃ for 2 hours, the phosphorus concentration is detected by a visible spectrophotometer at a wavelength lambda of 700nm, and the phosphorus concentration is calculated.
The removal rate of the prepared adsorbent to phosphorus reaches 94.5 percent.
Example 4
A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material comprises the following steps:
a) soaking crushed coconut shells in 1.2M sodium hydroxide solution, stirring for 4h at 150 ℃, removing impurities, washing with deionized water, adding acetic acid acidified sodium chlorite solution (mass fraction is 5%) for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) according to the method, 15g of aluminum nitrate nonahydrate is dissolved in 100mL of deionized water, the obtained coconut shell fiber is soaked for 16h and then filtered, and a sample obtained by drying is calcined for 8h at 350 ℃ under the nitrogen condition to obtain the coconut shell fiber (Al) coated with aluminum oxide2O3/CSF)；
c) Magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 1.2g to 0.6g to 0.8g to 100mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, stirring, transferring the mixture to a stainless steel reaction kettle, reacting at 120 deg.C for 24 hr, and filteringFiltering, washing, and calcining the dried product for 6 hours at 600 ℃ in a nitrogen atmosphere to obtain the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorbing material (Mg-Al/CSF).
Removing phosphorus in the wastewater:
after 30Mg of Mg-Al/CSF was added to 100Mg/L of 10mL of potassium dihydrogen phosphate solution and the solution was adjusted to pH 8 and adsorbed at 40 ℃ for 2 hours, the concentration of phosphorus was measured at a wavelength of 700nm using a visible spectrophotometer, and the concentration of phosphorus was calculated.
The removal rate of the prepared adsorbent to phosphorus reaches 78.5 percent.
Example 5
A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material comprises the following steps:
a) soaking crushed coconut shells in 1.5M sodium hydroxide solution, stirring for 8h at 150 ℃, removing impurities, washing with deionized water, adding acetic acid acidified sodium chlorite solution (mass fraction is 5%) for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) according to the weight of 20g of aluminum nitrate nonahydrate dissolved in 100mL of deionized water, the obtained coconut shell fiber is soaked for 20h and then filtered, and a sample obtained by drying is calcined for 8h at 800 ℃ under the nitrogen condition to obtain the coconut shell fiber (Al) coated with aluminum oxide2O3/CSF)；
c) Magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 1.8g to 0.9g to 1.0g to 200mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, fully stirring, transferring the mixture into a stainless steel reaction kettle, reacting for 48 hours at 180 ℃, filtering, washing, calcining the dried product for 8 hours at 800 ℃ in a nitrogen atmosphere to obtain the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material (Mg-Al/CSF).
Removing phosphorus in the wastewater:
after adding 40Mg of Mg-Al/CSF per 10mL of 100Mg/L potassium dihydrogen phosphate solution and adjusting the pH of the solution to 10 and adsorbing at 45 ℃ for 2h, the phosphorus concentration is detected by a visible spectrophotometer at a wavelength lambda of 700nm, and the phosphorus concentration is calculated.
The removal rate of the prepared adsorbent to phosphorus reaches 83 percent.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (10)
1. A preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material is characterized by comprising the following steps:
a) soaking the crushed coconut shells in a sodium hydroxide solution, stirring for 1-8 h at 60-150 ℃, removing impurities, washing with deionized water, adding into a sodium chlorite solution acidified by acetic acid for decolorization, washing the decolorized biomass with deionized water, and drying to obtain coconut shell fibers;
b) according to the method, 1-20 g of aluminum nitrate nonahydrate is dissolved in per 100mL of deionized water, the obtained coconut shell fiber is soaked for 5-20 h and then filtered, and a dried sample is calcined for 2-8 h at 200-800 ℃ in a nitrogen atmosphere to obtain the aluminum oxide coated coconut shell fiber Al2O3/CSF；
c) Magnesium nitrate hexahydrate and Al are mixed according to the solid-liquid ratio of 0.3-1.8 g, 0.1-0.9 g, 0.05-1.0 g and 50-200 mL2O3dissolving/CSF and hexamethylenetetramine in deionized water, fully stirring, transferring the mixture to a stainless steel reaction kettle, reacting for 6-48 h at 60-180 ℃, filtering, washing, and calcining the dried product for 2-8 h at 200-800 ℃ in a nitrogen atmosphere to obtain the catalyst.
2. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: in the step a), the concentration of the sodium hydroxide solution is 0.2-1.5M, and the sodium chlorite solution acidified by acetic acid is prepared by dissolving sodium chlorite in water according to the mass fraction of 5% and then adjusting the pH value to 4 by using acetic acid.
3. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: the crushed coconut shells are soaked in 1M sodium hydroxide solution and stirred for 3h at 80 ℃ in the step a).
4. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: soaking the coconut shell fiber obtained in the step b) for 10 hours according to the amount of 5g of aluminum nitrate nonahydrate dissolved in 100mL of deionized water, and filtering.
5. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: calcining the dried sample obtained in the step b) for 4 hours at 400 ℃ in a nitrogen atmosphere.
6. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: magnesium nitrate hexahydrate and Al are mixed according to the solid-to-liquid ratio of 0.9g to 0.3g to 0.5g to 75mL in the step c)2O3the/CSF and the hexamethylenetetramine are dissolved in the deionized water.
7. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: transferring the mixture into a stainless steel reaction kettle in the step c), and reacting for 12h at 120 ℃.
8. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material according to claim 1, characterized by comprising the following steps: calcining the dried product in the step c) for 4 hours at 500 ℃ in a nitrogen atmosphere.
9. The magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorbing material prepared by the method of any one of claims 1 to 8.
10. The application of the magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorbing material as claimed in claim 9, is characterized in that: the method is applied to the dephosphorization of the wastewater.
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