CN111298760A - Preparation method of flower-like aluminum oxide-magnesium oxide composite adsorbent, product and application thereof - Google Patents
Preparation method of flower-like aluminum oxide-magnesium oxide composite adsorbent, product and application thereof Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- CNGGOAOYPQGTLH-UHFFFAOYSA-N [O-2].[O-2].[Mg+2].[Al+3] Chemical compound [O-2].[O-2].[Mg+2].[Al+3] CNGGOAOYPQGTLH-UHFFFAOYSA-N 0.000 title claims abstract description 17
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 35
- 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 34
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 30
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000005470 impregnation Methods 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims description 16
- 239000011777 magnesium Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 239000004202 carbamide Substances 0.000 claims description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 4
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 36
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 20
- 150000002500 ions Chemical class 0.000 abstract description 11
- 229920006395 saturated elastomer Polymers 0.000 abstract description 6
- 239000002156 adsorbate Substances 0.000 abstract description 5
- 238000009792 diffusion process Methods 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of a flower-shaped aluminum oxide-magnesium oxide composite adsorbent, and a product and application thereof2O3And using it as carrier to prepare load type Al by adopting impregnation method2O3-MgO composite adsorbent for effective control of Al2O3The morphology of the substrate fully utilizes the three-dimensional large specific surface area and the surface high-density adsorption sites to load more MgO particles. And using betweenThe synergistic effect further improves the diffusion of adsorbate in the adsorbent, greatly improves the adsorption rate of heavy metal ions, and in addition, the flower-shaped Al2O3the-MgO composite adsorbent has high response speed to pollutants and large saturated adsorption capacity, is easy to separate from water after treatment, effectively reduces the operation cost of water treatment, and has a wide application prospect.
Description
Technical Field
The invention relates to a preparation method of a flower-shaped aluminum oxide-magnesium oxide composite adsorbent, a product and application thereof, and belongs to the field of heavy metal wastewater treatment.
Background
The heavy metal ion pollution in water is a generation source of heavy metal ion pollution to water environment. Even trace heavy metal pollution can bring risks to human beings. Therefore, how to effectively remove these hazardous heavy metals from water deeply is a very challenging task. At present, methods for effectively removing heavy metal pollution in water mainly comprise a chemical precipitation method, an ion exchange method, a membrane separation method, an electrolysis method, an adsorption method and the like, and among the technologies, the adsorption method is simple to operate, efficient and energy-saving, most of adsorption processes have reversibility, and an adsorbent can be recycled for multiple times through a desorption process, so that the adsorption method is a recognized technology for removing heavy metal with the highest application value. Among the numerous adsorbents, nano-metal oxides, including nano-iron oxides, manganese oxides, cerium oxides, are commonly used to remove heavy metal ions from water due to their high specific surface area and special surface interface characteristics and reactivity. The nano metal oxide provides effective and specific adsorption for heavy metal ions, however, the problems of agglomeration, difficult separation, excessive pressure drop, poor mechanical properties and the like are generally caused by too small size and shape difference, so that the adsorption performance is influenced, and the applicability of the nano metal oxide in actual wastewater treatment is limited. How to effectively synthesize a metal oxide with a controllable shape and high stability is the focus of attention of researchers in recent years.
Magnesium oxide is the only solid which is discovered so far and has strong ionic characteristics, simple stoichiometric formula and complete crystal structure, and has good adsorption performance due to the fact that the surface of the solid has a large number of edges and structural defects, and the specific surface area and the porosity are large. Alumina is a traditional heavy metal adsorbent, is low in price and low in removal efficiency, but the specific surface area and the adsorption capacity of the alumina are still a big problem limiting the application of the alumina, and a large amount of alumina adsorbent needs to be consumed in the adsorption process, so that the phase change is caused, and the treatment cost is increased. However, the difficult problem of separating and recycling the powder adsorbent is a technical bottleneck in water pollution treatment engineering, so that the powder adsorbent can be recycled while developing the efficient adsorption material, the recycling rate of the powder adsorbent is improved, and the treatment cost is saved, which has important significance for industrial practical application.
The patent utilizes the surfactant as the structure directing agent to effectively control Al2O3The shape of the substrate and the self-assembly of the flower-shaped Al2O3And the carrier is used as a carrier, and three-dimensional large specific surface area and surface high-density adsorption sites are fully utilized to load more MgO particles. The synergistic effect between the two is utilized to further improve the diffusion of the adsorbate in the adsorbent, and the adsorption rate of heavy metal ions is greatly improved. The process is simple and convenient to operate, has large saturated adsorption capacity, is easy to separate from water after treatment, and has a wide application prospect.
Disclosure of Invention
Aiming at the problems of small adsorption capacity, difficult separation and recovery of the adsorbent and the like commonly existing in the conventional heavy metal adsorbent, the invention aims to provide a preparation method of a flower-shaped aluminum oxide-magnesium oxide composite adsorbent.
Yet another object of the present invention is to: provides a product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a flower-shaped aluminum oxide-magnesium oxide composite adsorbent is characterized in that a surfactant is used as a structure directing agent, and Al with a flower-shaped structure is synthesized by a simple hydrothermal method2O3And using it as carrier to prepare load type Al by adopting impregnation method2O3-a MgO composite adsorbent comprising the steps of:
(1) preparation ofFlower-like Al2O3Under magnetic stirring, Al (NO) is added3)3·9H2Dissolving O and surfactant in deionized water, mixing, adding urea solution dropwise within 15min, and adding Al (NO) to obtain mixture3)3·9H2The mass ratio of the O, the urea and the surfactant is 1: 3.125: (0.01 to 0.2); transferring the mixture into a polytetrafluoroethylene-lined stainless steel high-pressure reaction kettle, carrying out hydrothermal reaction at 120-200 ℃ for 24 hours, taking out, repeatedly cleaning the product with ethanol and deionized water, drying at 100 ℃ for 12 hours, and roasting in a 600 ℃ muffle furnace for 4-6 hours to obtain flower-shaped Al2O3；
(2) Preparation of Al2O3-MgO composite adsorbent: according to Al2O3And Mg (NO)3)2·9H2Flower-shaped Al with the mass ratio of O being 1:202O3Immersion in Mg (NO)3)2·9H2Soaking in O solution, removing excessive soaking solution, drying at 120 deg.C for 12 hr, and roasting in muffle furnace for 4 hr to obtain supported flower-like Al2O3-MgO composite adsorbent.
The surfactant is any one of Cetyl Trimethyl Ammonium Bromide (CTAB), cetyl trimethyl ammonium chloride and triton 100.
In the step (2), the roasting temperature is the same as or different from that in the step (1).
The Al is2O3And Mg (NO)3)2·9H2The mass ratio of O is 1:20, and the dipping time is 6-12 h.
The invention also provides a flower-shaped aluminum oxide-magnesium oxide composite adsorbent prepared by any one of the methods.
The invention also provides application of the flower-shaped aluminum oxide-magnesium oxide composite adsorbent in preparation of the adsorbent for removing lead or nickel. Can effectively improve the adsorption capacity to heavy metal ions and is used in the field of heavy metal wastewater treatment.
The invention utilizes the surfactant as the structure directing agent, and adopts the simple processThe hydrothermal method synthesizes Al with flower-shaped structure2O3And using it as carrier to prepare load type Al by adopting impregnation method2O3-MgO composite adsorbent.
By synthesizing supported flower-like Al2O3-MgO composite adsorbent, exposing more highly active adsorption sites, using Al2O3The three-dimensional flower-shaped structure promotes the improvement of the load rate and the specific surface area of the MgO adsorbent, and the synergistic effect between the two is utilized, thereby being beneficial to the diffusion of adsorbate in the adsorbent and improving the saturated adsorption capacity of heavy metal ions in water. Effective control of Al2O3The morphology of the substrate fully utilizes the three-dimensional large specific surface area and the surface high-density adsorption sites to load more MgO particles. And the synergistic effect between the two is utilized to further improve the diffusion of adsorbate in the adsorbent, greatly improve the adsorption rate of heavy metal ions, and in addition, the flower-shaped Al2O3the-MgO composite adsorbent has high response speed to pollutants and large saturated adsorption capacity, is easy to separate from water after treatment, effectively reduces the operation cost of water treatment, and has a wide application prospect. Can effectively promote the adsorption of heavy metal ions in water, improve the removal rate of heavy metal pollutants, and simultaneously can effectively avoid the problems of loss, difficult recovery and the like of the adsorbent,
flower-like Al2O3Evaluation of adsorption Performance of-MgO composite adsorbent was carried out in a beaker to which 20mLPb (NO) was added3)2Or Ni (NO)3)2Solution, adding prepared Al2O3Subjecting to water bath oscillation adsorption for 60min with MgO adsorbent, centrifuging, collecting supernatant, vacuum filtering, collecting filtrate, and measuring Pb before and after adsorption with atomic absorption spectrophotometer2+Or Ni2+And calculating the adsorption efficiency.
The invention has the following advantages:
(1) the invention provides flower-shaped Al2O3Preparation method of-MgO composite adsorbent, using surfactant as structure directing agent to effectively control Al2O3The morphology of the substrate is sufficientThe three-dimensional large specific surface area and high-density adsorption sites on the surface are utilized, and the MgO adsorbent with high specific surface area and porosity is combined, so that the diffusion of adsorbate in the adsorbent is facilitated, and the saturated adsorption capacity of heavy metal ions in water is greatly improved.
(2) Flower-shaped Al provided by the invention2O3the-MgO composite adsorbent has high response speed to pollutants and large saturated adsorption capacity, is easy to separate from water after treatment, effectively reduces the operation cost of water treatment, and has a wide application prospect.
(3) The invention provides flower-shaped Al2O3The preparation method of the-MgO composite adsorbent is simple and controllable, has mild process conditions and high adsorption efficiency, and is suitable for large-scale application.
Detailed Description
The present invention is further illustrated by examples.
Example 1:
a flower-like aluminum oxide-magnesium oxide composite adsorbent is characterized in that a surfactant is used as a structure directing agent, and Al with a flower-like structure is synthesized by a simple hydrothermal method2O3And using it as carrier to prepare load type Al by adopting impregnation method2O3-a MgO composite adsorbent, prepared as follows:
(1) preparation of flower-like Al2O3Under magnetic stirring, pressing Al (NO)3)3·9H2The mass ratio of O to the surfactant is 1: 0.2 adding Al (NO)3)3·9H2Dissolving O and a CTAB surfactant in deionized water, uniformly mixing, and then mixing in a mass ratio of 1: 3.125 urea solution is dripped; after the dropwise addition is finished, transferring the mixture into a polytetrafluoroethylene-lined stainless steel high-pressure reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 24 hours, taking out, repeatedly cleaning the product with ethanol and deionized water, drying at 100 ℃ for 12 hours, and then roasting in a 600 ℃ muffle furnace for 6 hours to obtain flower-shaped Al2O3；
(2) Preparation of Al2O3-MgO composite adsorbent: according to Al2O3And Mg (NO)3)2·9H2Flower-shaped Al with the mass ratio of O being 1:202O3Immersion in Mg (NO)3)2·9H2Soaking in O solution for 6 hr, removing excessive soaking solution, drying at 120 deg.C for 12 hr, and roasting in muffle furnace at 600 deg.C for 4 hr to obtain supported flower-like Al2O3-MgO composite adsorbent.
The prepared flower-shaped Al2O3-MgO composite adsorbent for Pb2+The adsorption rate of the solution was 91.7%.
Example 2:
similar to example 1, the flower-shaped aluminum oxide-magnesium oxide composite adsorbent is prepared by the following steps:
(1) preparation of flower-like Al2O3Under the magnetic stirring, the mass ratio of 1: 0.01 mixing Al (NO)3)3·9H2Dissolving O in CTAB deionized water as surfactant, mixing, and adding Al (NO) within 15min3)3·9H2The mass ratio of O to urea is 1: 3.125 dropwise adding a urea solution, transferring the obtained mixture into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining after the dropwise adding is finished, taking out after 24 hours of hydrothermal reaction at 150 ℃, repeatedly cleaning the product with ethanol and deionized water, drying the product at 100 ℃ for 12 hours, and then roasting the product in a muffle furnace at 600 ℃ for 4 hours to obtain the flower-shaped Al2O3；
(2) Preparation of Al2O3-MgO composite adsorbent: according to Al2O3And Mg (NO)3)2·9H2Flower-shaped Al with the mass ratio of O being 1:202O3Immersion in Mg (NO)3)2·9H2Soaking in O solution for 12h, removing excessive soaking solution, drying at 120 deg.C for 12h, and roasting in muffle furnace for 4h to obtain supported flower-like Al2O3-MgO composite adsorbent.
The prepared flower-shaped Al2O3-MgO composite adsorbent for Pb2+The adsorption rate of the solution was 87.9%.
Example 3:
similar to example 1, the flower-shaped aluminum oxide-magnesium oxide composite adsorbent is prepared by the following steps:
(1) preparation of flower-like Al2O3Under magnetic stirring, pressing Al (NO)3)3·9H2The mass ratio of O to CTAB is 1: 0.1 adding Al (NO)3)3·9H2Dissolving O in CTAB deionized water, mixing, and adding Al (NO) within 15min3)3·9H2The mass ratio of O to urea is 1: 3.125 adding urea solution, transferring the mixture into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining after the dropwise addition is finished, performing hydrothermal treatment at 200 ℃ for 24 hours, and taking out. Repeatedly cleaning the product with ethanol and deionized water, drying at 100 deg.C for 12 hr, and calcining in 600 deg.C muffle furnace for 4 hr to obtain flower-like Al2O3；
(2) Preparation of Al2O3-MgO composite adsorbent: according to Al2O3And Mg (NO)3)2·9H2Flower-shaped Al with the mass ratio of O being 1:202O3Immersion in Mg (NO)3)2·9H2Soaking in O solution for 12h, removing excessive soaking solution, drying at 120 deg.C for 12h, and roasting in muffle furnace for 4h to obtain supported flower-like Al2O3-MgO composite adsorbent.
The prepared flower-shaped Al2O3-MgO composite adsorbent pair Ni2+The adsorption rate of the solution was 93.5%.
Example 4:
similar to example 1, the flower-shaped aluminum oxide-magnesium oxide composite adsorbent is prepared by the following steps:
(1) preparation of flower-like Al2O3Under magnetic stirring, pressing Al (NO)3)3·9H2The mass ratio of O to the surfactant triton 100 is 1: 0.2 dissolving in deionized water of Triton 100, mixing, and adding Al (NO) within 15min3)3·9H2The mass ratio of O to urea is 1: 3.125 adding urea solution, transferring the mixture into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining after the dropwise addition is finished, performing hydrothermal treatment at 180 ℃ for 24 hours, and taking out.Repeatedly cleaning the product with ethanol and deionized water, drying at 100 deg.C for 12 hr, and calcining in 600 deg.C muffle furnace for 4 hr to obtain flower-like Al2O3；
(2) Preparation of Al2O3-MgO composite adsorbent: according to Al2O3And Mg (NO)3)2·9H2Flower-shaped Al with the mass ratio of O being 1:202O3Immersion in Mg (NO)3)2·9H2Soaking in O solution for 4 hr, removing excessive soaking solution, drying at 120 deg.C for 12 hr, and roasting in muffle furnace for 4 hr to obtain supported flower-like Al2O3-MgO composite adsorbent.
The prepared flower-shaped Al2O3-MgO composite adsorbent pair Ni2+The adsorption rate of the solution was 85.3%.
Claims (6)
1. A preparation method of a flower-shaped aluminum oxide-magnesium oxide composite adsorbent is characterized in that a surfactant is used as a structure directing agent, and Al with a flower-shaped structure is synthesized by a simple hydrothermal method2O3And using it as carrier to prepare load type Al by adopting impregnation method2O3-a MgO composite adsorbent comprising the steps of:
(1) preparation of flower-like Al2O3Under magnetic stirring, Al (NO) is added3)3·9H2Dissolving O and surfactant in deionized water, mixing, adding urea solution dropwise within 15min, and adding Al (NO) to obtain mixture3)3·9H2The mass ratio of the O, the urea and the surfactant is 1: 3.125: (0.01 to 0.2); transferring the mixture into a polytetrafluoroethylene-lined stainless steel high-pressure reaction kettle, carrying out hydrothermal reaction at 120-200 ℃ for 24 hours, taking out, repeatedly cleaning the product with ethanol and deionized water, drying at 100 ℃ for 12 hours, and roasting in a 600 ℃ muffle furnace for 4-6 hours to obtain flower-shaped Al2O3；
(2) Preparation of Al2O3-MgO composite adsorbent: according to Al2O3And Mg (NO)3)2·9H2Flower-shaped Al with the mass ratio of O being 1:202O3Immersion in Mg (NO)3)2·9H2Soaking in O solution, removing excessive soaking solution, drying at 120 deg.C for 12 hr, and roasting in muffle furnace for 4 hr to obtain supported flower-like Al2O3-MgO composite adsorbent.
2. The method for preparing the flower-like aluminum oxide-magnesium oxide composite adsorbent according to claim 1, wherein the surfactant is any one of cetyltrimethyl ammonium bromide, cetyltrimethyl ammonium chloride and triton 100.
3. The method for preparing the flower-shaped aluminum oxide-magnesium oxide composite adsorbent according to claim 1, wherein in the step (2), the flower-shaped Al is prepared2O3Immersion in Mg (NO)3)2·9H2The dipping time of the O solution is 6-12 h.
4. The method for preparing the flower-shaped aluminum oxide-magnesium oxide composite adsorbent according to claim 1 or 3, wherein in the step (2), the roasting temperature is the same as or different from that in the step (1).
5. A flower-like alumina-magnesia composite adsorbent, characterized by being prepared according to the method of any one of claims 1 to 4.
6. The application of the flower-shaped aluminum oxide-magnesium oxide composite adsorbent according to claim 5 in preparation of an adsorbent for removing lead or nickel.
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