CN115228434A - Surface-wrapped gamma-Al 2 O 3 : carbon nanotube adsorbent with Dy & lt 3+ & gt particles and preparation method thereof - Google Patents

Surface-wrapped gamma-Al 2 O 3 : carbon nanotube adsorbent with Dy & lt 3+ & gt particles and preparation method thereof Download PDF

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CN115228434A
CN115228434A CN202210865645.6A CN202210865645A CN115228434A CN 115228434 A CN115228434 A CN 115228434A CN 202210865645 A CN202210865645 A CN 202210865645A CN 115228434 A CN115228434 A CN 115228434A
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nano tube
carbon nano
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adsorbent
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CN115228434B (en
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姚义俊
陈学肖
陈雍昊
季志祥
李凯
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Nanjing University of Information Science and Technology
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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
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0207—Compounds of Sc, Y or Lanthanides
    • 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
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

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Abstract

The invention discloses a surface-coated gamma-Al 2 O 3 ：Dy 3+ A granular carbon nano tube adsorbent and a preparation method thereof belong to the field of wastewater treatment. Surface-wrapped gamma-Al 2 O 3 ：Dy 3+ The preparation method of the granular carbon nanotube adsorbent comprises the following steps: stirring aluminium isopropoxide and water in a reflux device fully to hydrolyze aluminium isopropoxide completely to generate boehmite precipitate, stirring the hydrolyzed mixture, and evaporating until (CH) is not existed any more 3 ) 2 CHOH, adding HNO 3 Continuously stirring to obtain boehmite sol; dy (NO) is added into the boehmite sol 3 ) 3 ·5H 2 Stirring the O solution to obtain Dy doped solution 3+ Boehmite sol; oxidizing a carbon nano tube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, filtering and drying, then placing the carbon nano tube into a glass bottle, adding deionized water and Triton X-100 nonionic surfactant, and stirring in a constant-temperature water bath; then adding the doped Dy 3+ Mixing boehmite sol by ultrasonic, and drying in a vacuum drying oven; calcining to obtain the surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of particles.

Description

Surface-wrapped gamma-Al 2 O 3 ：Dy 3+ Granular carbon nanotube adsorbent and preparation method thereof
Technical Field
The invention relates to the field of wastewater treatment, in particular to a surface-coated gamma-Al 2 O 3 ：Dy 3+ A granular carbon nanotube adsorbent and a method for preparing the same.
Background
The current industrial development is accompanied by environmental problems caused by industrial solid waste, sewage and waste gas emission, industries such as agriculture, printing material industry, metallurgical industry, paper industry and the like are main sources of industrial sewage emission, cost loss in the aspects of manpower and financial resources can be caused by improper treatment, the heavy metal pollution, organic solvent pollution, antibiotic pollution and the like mainly cause, the current treatment method for the heavy metal pollution of water resources is mainly an adsorption method, cadmium in the waste water is adsorbed by utilizing an adsorbent through chemical chelation, electrostatic action and the like, and development of the adsorbent with low cost, green and high efficiency becomes a research trend.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a surface-coated gamma-Al 2 O 3 ：Dy 3+ A particulate carbon nanotube adsorbent and a method for preparing the same.
The purpose of the invention can be realized by the following technical scheme:
surface-wrapped gamma-Al 2 O 3 ：Dy 3+ The preparation method of the granular carbon nanotube adsorbent comprises the following steps:
stirring aluminium isopropoxide and water in a reflux device fully to hydrolyze aluminium isopropoxide completely to generate boehmite precipitate, stirring the hydrolyzed mixture, and evaporating until (CH) is not existed any more 3 ) 2 CHOH, adding HNO 3 Is followed byStirring to obtain boehmite sol;
dy (NO) is added into the boehmite sol 3 ) 3 ·5H 2 Stirring the O solution to obtain Dy doped solution 3+ Boehmite sol;
oxidizing a carbon nano tube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, filtering and drying the carbon nano tube, putting the carbon nano tube into a glass bottle, adding deionized water and Triton X-100 nonionic surfactant, and stirring in a constant-temperature water bath; then adding the doped Dy 3+ Mixing boehmite sol by ultrasonic, and drying in a vacuum drying oven; calcining to obtain the surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of particles.
In another aspect, the invention also relates to the carbon nano tube adsorbent prepared by the method and application of the adsorbent in wastewater treatment.
The invention has the beneficial effects that:
compared with the prior art, the invention utilizes sol-gel chemical reaction to coat gamma-Al on the surface of the carbon nano tube 2 O 3 ：Dy 3+ Granules, adding HNO to boehmite (AlOOH) precipitate 3 Forming a sol, adding highly active Dy 3+ Rare earth ion Dy calcined at 150-200 deg.C 3+ Is eccentrically polymerized in Al 2 O 3 The surface of the particles can block the migration of Al ions and reduce Al 2 O 3 The surface formation energy of the particles is obtained, and high-activity and small-size gamma-Al is obtained 2 O 3 ：Dy 3+ The particles are uniformly adsorbed on the surface of the carbon nano tube, so that the adsorption of the carbon nano tube is improved, the adsorption amount of heavy metals such as cadmium in industrial wastewater is improved, and a process flow chart is shown in figure 1. The preparation process is simple and environment-friendly, and the prepared carbon nano tube is an ideal environment-friendly material for adsorbing heavy metals in industrial wastewater.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a flow chart of a surface treatment process for carbon nanotubes in the preparation method of the present application;
FIG. 2 shows the effect of carbon nanotubes on cadmium ion removal rate before and after treatment.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
as further described below, the present invention provides a surface-coated gamma-Al 2 O 3 ：Dy 3+ A granular carbon nanotube adsorbent and a method for preparing the same, comprising:
step 1, oxidizing a carbon nanotube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid for 2-8 hours, wherein the volume ratio of the concentrated sulfuric acid to the peroxytrifluoroacetic acid is 3;
step 2, adding aluminum isopropoxide (Al (OC) 3 H 7 ) 3 ) The molar ratio of the water to the water is 1: stirring at 90 deg.C for 2 hr to hydrolyze aluminum isopropoxide completely to obtain precipitate of boehmite (AlOOH), stirring at 90 deg.C, and evaporating to remove (CH) 3 ) 2 CHOH according to HNO 3 And Al (OC) 3 H 7 ) 3 In a molar ratio of 0.07 3 Continuously stirring for 2h at 60 ℃ to enable the solution to be colloidal for later use;
step 3, according to Dy (NO) 3 ) 3 ·5H 2 O∶Al(OC 3 H 7 ) 3 In a molar ratio of 0.2: 1, dy (NO) is added to the boehmite sol 3 ) 3 ·5H 2 Stirring the O solution for 10 hours to obtain stable Dy doped solution with different concentrations 3+ Boehmite sol;
and 4, putting 10g of carbon nano tube into a glass bottle, adding 500ml of deionized water, adding 2ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 500r.min-1, and maintaining the temperature of the system at 51 ℃. Slowly adding the sol into a system according to the volume ratio of 1. Finally calcining for 1h in the atmosphere at 200 ℃ to obtain the surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of particles.
Example 2:
the invention is further described below by providing a surface-coated gamma-Al 2 O 3 ：Dy 3+ A particulate carbon nanotube adsorbent and a method of making the same, comprising:
step 1, oxidizing a carbon nanotube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid for 6 hours, wherein the volume ratio of the concentrated sulfuric acid to the peroxytrifluoroacetic acid is 3;
step 2, adding aluminum isopropoxide (Al (OC) 3 H 7 ) 3 ) The molar ratio of the water to the water is 1:100 placing in a reflux device, stirring at 80 deg.C for 2 hr to completely hydrolyze aluminum isopropoxide to obtain boehmite (AlOOH) precipitate, stirring the hydrolyzed mixture at 90 deg.C, and evaporating until no (CH) is obtained 3 ) 2 CHOH according to HNO 3 And Al (OC) 3 H 7 ) 3 In a molar ratio of 0.05 3 Continuously stirring for 2h at 60 ℃ to enable the solution to be colloidal for later use;
step 3, according to Dy (NO) 3 ) 3 ·5H 2 O∶Al(OC 3 H 7 ) 3 In a molar ratio of 0.3: 1, dy (NO) is added into the sol 3 ) 3 ·5H 2 O solution, stirringAfter 10 hours, stable Dy-doped crystals with different concentrations can be obtained 3+ Sol;
and 4, putting 10g of carbon nano tube into a glass bottle, adding 500ml of deionized water, adding 3ml of Triton X-100 nonionic surfactant, stirring in a constant-temperature water bath, keeping the rotating speed at 350r.min < -1 >, and maintaining the temperature of the system at 50 ℃. Slowly adding the sol into a system according to the volume ratio of 1. Finally calcining for 1h in atmosphere at 150 ℃ to obtain the surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of particles.
Surface coating of gamma-Al prepared in example 1 2 O 3 ：Dy 3+ The adsorption performance of the carbon nano tube of the particles is researched, 25mL of 50mg/L cadmium ion solution is respectively added into a group of 100mL iodine flasks, then a certain amount of the carbon nano tube sample 1 prepared in the example 1 and a comparative untreated carbon nano tube sample are respectively added, the mixture is oscillated for a certain time at a set temperature and at 150r/min, the supernatant is taken after centrifugation for 10min, the residual amount of cadmium ions in the supernatant is determined (the analysis of the cadmium ions adopts an atomic absorption spectrophotometry), and the adsorption removal rate of the cadmium ions by the carbon nano tubes is calculated. As can be seen from fig. 2, the unpurified carbon nanotubes have a low removal rate of cadmium ions, and the removal rate is only 39.2% when the amount of the carbon nanotubes is 8.0g/L, while the carbon nanotubes subjected to surface treatment have a significantly improved removal rate of cadmium ions, and after purification, on one hand, a large number of functional groups are generated on the surface of the carbon nanotubes, and on the other hand, the surface adsorption treatment increases the surface area of the CNTs, which are all beneficial to improving the adsorption performance of the CNTs. When the dosage of the treated carbon nano tube is 4.0g/L, the removal rate reaches 89.3 percent, the dosage is continuously increased, and the adsorption removal rate is slowly increased, which is mainly caused by the balance of adsorption.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.

Claims (9)

1. Surface-wrapped gamma-Al 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized by comprising the following steps:
stirring aluminium isopropoxide and water in reflux device to hydrolyze aluminium isopropoxide completely to generate boehmite precipitate, stirring hydrolyzed mixture, and evaporating until no (CH) exists 3 ) 2 CHOH, adding HNO 3 Stirring continuously to obtain boehmite sol;
dy (NO) is added into the boehmite sol 3 ) 3 ·5H 2 Stirring the O solution to obtain Dy doped solution 3+ Boehmite sol;
oxidizing a carbon nano tube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, filtering and drying the carbon nano tube, putting the carbon nano tube into a glass bottle, adding deionized water and Triton X-100 nonionic surfactant, and stirring in a constant-temperature water bath; then adding the doped Dy 3+ Mixing the boehmite sol and the ultrasonic wave, and drying the mixture in a vacuum drying oven; calcining to obtain the surface-wrapped gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of particles.
2. The surface-coated γ -Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that Dy doped is added 3+ Adding ammonia water dropwise after the boehmite sol, and adjusting the pH value to 9-10.
3. The surface-coated γ -Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that after constant-temperature water bath, the granular carbon nano tube adsorbent is kept stand and aged at the temperature of 60 ℃, cooled to room temperature and washed by deionized water.
4. The surface-coated γ -Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that the Triton X-100 nonionic surfactant is added, and after constant-temperature water bath, the temperature of a reaction system is maintained at 50-55 ℃.
5. The surface-coated γ -Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that HNO is added 3 And Al (OC) in solution 3 H 7 ) 3 In a molar ratio of 0.05 to 0.07.
6. The surface-coated γ -Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that the calcining temperature is 150-200 ℃.
7. The surface-coated γ -Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nanotube adsorbent is characterized in that in the step of oxidizing the carbon nanotube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, the volume ratio of the concentrated sulfuric acid to the peroxytrifluoroacetic acid is 3And (3) adding the filtered carbon nano tube into 200-400ml of hydrogen peroxide until the pH value is 6-8, and drying in a drying oven at 70-80 ℃ until the weight is constant for later use.
8. A carbon nanotube adsorbent prepared by the method of any one of claims 1 to 7.
9. Use of the adsorbent of claim 8 in the treatment of wastewater.
CN202210865645.6A 2022-07-21 2022-07-21 gamma-Al coated on surface 2 O 3 : dy3+ particle carbon nanotube adsorbent and preparation method thereof Active CN115228434B (en)

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