CN115228434B - gamma-Al coated on surface 2 O 3 : dy3+ particle carbon nanotube adsorbent and preparation method thereof - Google Patents
gamma-Al coated on surface 2 O 3 : dy3+ particle carbon nanotube adsorbent and preparation method thereof Download PDFInfo
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- 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
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- 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
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- 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
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- 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
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Abstract
The application 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. gamma-Al coated on surface 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent comprises the following steps: the aluminum isopropoxide and water are fully stirred in a reflux device to completely hydrolyze the aluminum isopropoxide to form boehmite precipitate, the hydrolyzed mixture is stirred and evaporated until no more (CH) 3 ) 2 CHOH, adding HNO 3 Continuously stirring to obtain boehmite sol; dy (NO) is added into boehmite sol 3 ) 3 ·5H 2 O solution is stirred to obtain Dy doped solution 3+ A boehmite sol; oxidizing the carbon nano tube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, filtering, drying, 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; adding Dy doped 3+ Mixing with boehmite sol, ultrasonic mixing, and drying in a vacuum drying oven; calcining to obtain surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of the particles.
Description
Technical Field
The application relates to the field of wastewater treatmentIn particular to a gamma-Al coated surface 2 O 3 ：Dy 3+ A granular carbon nanotube adsorbent and a preparation method thereof.
Background
The current industrial development is accompanied by environmental problems caused by industrial solid waste, sewage and waste gas discharge, industries such as agriculture, printing material industry, metallurgical industry, paper industry and the like are main sources of industrial sewage discharge, improper treatment can cause cost loss in terms of manpower and financial resources, the cost loss is mainly caused by heavy metal pollution, organic solvent pollution, antibiotic pollution and the like, the current treatment method for the heavy metal pollution of water resources is mainly an adsorption method, and cadmium in wastewater is adsorbed by utilizing an adsorbent through chemical chelation, electrostatic action and other modes, so that the adsorbent with low development cost, green and high efficiency becomes a research trend.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a surface-coated gamma-Al 2 O 3 ：Dy 3+ A granular carbon nanotube adsorbent and a preparation method thereof.
The aim of the application can be achieved by the following technical scheme:
gamma-Al coated on surface 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent comprises the following steps:
the aluminum isopropoxide and water are fully stirred in a reflux device to completely hydrolyze the aluminum isopropoxide to form boehmite precipitate, the hydrolyzed mixture is stirred and evaporated until no more (CH) 3 ) 2 CHOH, adding HNO 3 Continuously stirring to obtain boehmite sol;
dy (NO) is added into boehmite sol 3 ) 3 ·5H 2 O solution is stirred to obtain Dy doped solution 3+ A boehmite sol;
oxidizing the carbon nano tube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, filtering, drying, 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; adding Dy doped 3+ The ratio of boehmite sol and superMixing with sound, and drying in vacuum drying oven; calcining to obtain surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of the particles.
On the other hand, the application also relates to the carbon nano tube adsorbent prepared by the method and application of the adsorbent in wastewater treatment.
The application has the beneficial effects that:
compared with the prior art, the application utilizes the sol-gel chemical reaction to wrap the gamma-Al on the surface of the carbon nano tube 2 O 3 ：Dy 3+ Particles, HNO is added in boehmite (AlOOH) precipitation 3 Forming sol, adding high-activity Dy 3+ Rare earth ion, dy in calcination at 150-200 DEG C 3+ Segregation at Al 2 O 3 The surface of the particles can obstruct migration of Al ions and reduce Al 2 O 3 The surface forming energy of the particles is high, and the gamma-Al with small size 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, and the adsorption amount of heavy metals such as cadmium in industrial wastewater is improved, and the 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 application is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of a surface-treated carbon nanotube in the preparation method of the present application;
FIG. 2 shows the effect of carbon nanotubes on cadmium ion removal before and after treatment.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1:
the present application is further described below, and provides 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 nano tube 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 3:1, the mass ratio of the carbon nano tube to the concentrated acid solution is 1:400, the oxidation temperature is 90 ℃, the oxidation time is 3 hours, washing a product until the pH value is 8 after the oxidation is finished, adding the filtered carbon nano tube into 400ml of hydrogen peroxide, and drying the mixture in a 70 ℃ drying box until the weight is constant for later use;
step 2, aluminum isopropoxide (Al (OC) 3 H 7 ) 3 ) The molar ratio of the water to the water is 1:90 are placed in a reflux device and fully stirred for 2 hours at 90 ℃ to lead aluminum isopropoxide to be completely hydrolyzed to generate boehmite (AlOOH) sediment, the hydrolyzed mixture is stirred at 90 ℃ and evaporated until no more (CH) 3 ) 2 CHOH according to HNO 3 And Al (OC) 3 H 7 ) 3 HNO is added in a molar ratio of 0.07:1 3 Stirring at 60deg.C for 2 hr to give colloidal solution;
step 3, according to Dy (NO) 3 ) 3 ·5H 2 O∶Al(OC 3 H 7 ) 3 Dy (NO) was added to the boehmite sol at a molar ratio of 0.2:1 3 ) 3 ·5H 2 O solution, stirring for 10h to obtain stable Dy-doped solution with different concentrations 3+ A boehmite sol;
and 4, placing 10g of carbon nano tubes into a glass bottle, then 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 keeping the system temperature at 51 ℃. Slowly adding sol into the system according to the volume ratio of 1:2, dropwise adding ammonia water, regulating the pH of the system to 9, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature, washing with deionized water for 5 times, and drying in a vacuum drying oven at 80 ℃ for 24 hours. Finally, the mixture is in the atmosphere at 200 DEG CCalcining for 1h to obtain the surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of the particles.
Example 2:
the present application is further described below, and provides 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 nano tube 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 3:1, the mass ratio of the carbon nano tube to the concentrated acid solution is 1:300, the oxidation temperature is 80 ℃, the oxidation time is 2 hours, washing a product until the pH value is 7 after the oxidation is finished, adding the filtered carbon nano tube into 300ml of hydrogen peroxide, and drying in a drying box at 80 ℃ until the weight is constant for standby;
step 2, aluminum isopropoxide (Al (OC) 3 H 7 ) 3 ) The molar ratio of the water to the water is 1:100 is placed in a reflux device and fully stirred for 2 hours at 80 ℃ to lead aluminum isopropoxide to be fully hydrolyzed to generate boehmite (AlOOH) sediment, the hydrolyzed mixture is stirred at 90 ℃ and evaporated until no more (CH) 3 ) 2 CHOH according to HNO 3 And Al (OC) 3 H 7 ) 3 HNO is added in a molar ratio of 0.05:1 3 Stirring at 60deg.C for 2 hr to give colloidal solution;
step 3, according to Dy (NO) 3 ) 3 ·5H 2 O∶Al(OC 3 H 7 ) 3 Dy (NO) was added to the sol at a molar ratio of 0.3:1 3 ) 3 ·5H 2 O solution, stirring for 10h to obtain stable Dy-doped solution with different concentrations 3+ Sol;
and 4, placing 10g of carbon nano tubes into a glass bottle, then 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 keeping the temperature of the system at 50 ℃. Slowly adding sol into the system according to the volume ratio of 1:2, dropwise adding ammonia water, regulating the pH of the system to 10, ultrasonically mixing for 30 minutes at 50 ℃, standing and aging for 12 hours at 60 ℃, cooling to room temperature,washing with deionized water for 5 times, and drying in a vacuum drying oven at 80deg.C for 24 hr. Finally calcining in the atmosphere at 150 ℃ for 1h to obtain the surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of the 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 particle is studied, 25mL of 50mg/L cadmium ion solution is respectively added into a group of 100mL iodine measuring bottles, a certain amount of carbon nano tube sample 1 prepared in example 1 and a certain amount of carbon nano tube sample which is not treated by comparison are respectively added, the carbon nano tube sample is oscillated for a certain time at 150r/min at a set temperature, supernatant liquid is taken after centrifugation for 10min, the residual quantity of cadmium ions in the supernatant liquid is measured (an atomic absorption spectrophotometry is adopted for the analysis of the cadmium ions), and the adsorption removal rate of the carbon nano tube on the cadmium ions is calculated. As a result, as shown in FIG. 2, the removal rate of cadmium ions from the unpurified carbon nanotubes was low, and the removal rate was only 39.2% even at the use level of 8.0g/L, whereas the removal rate of cadmium ions from the surface-treated carbon nanotubes was significantly improved, and the carbon nanotubes were purified to produce a large number of functional groups on the surface thereof, and the surface adsorption treatment increased the surface area of CNTs, which is advantageous for improving the adsorption performance thereof. When the dosage of the treated carbon nano tube is 4.0g/L, the removal rate reaches 89.3%, and the adsorption removal rate is slowly increased by continuously increasing the dosage, which is mainly caused by the equilibrium of adsorption.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, 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 present application. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. 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 has shown and described the basic principles, principal features and advantages of the application. It will be understood by those skilled in the art that the present application is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present application, and various changes and modifications may be made without departing from the spirit and scope of the application, which is defined in the appended claims.
Claims (8)
1. gamma-Al coated on surface 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized by comprising the following steps:
the aluminum isopropoxide and water are fully stirred in a reflux device to completely hydrolyze the aluminum isopropoxide to form boehmite precipitate, the hydrolyzed mixture is stirred and evaporated until no more (CH) 3 ) 2 CHOH, adding HNO 3 Continuously stirring to obtain boehmite sol;
dy (NO) is added into boehmite sol 3 ) 3 ·5H 2 O solution is stirred to obtain Dy doped solution 3+ A boehmite sol;
oxidizing the carbon nano tube in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, filtering, drying, placing the carbon nano tube into a glass bottle, adding deionized water and TritonX-100 nonionic surfactant, and stirring in a constant-temperature water bath; adding Dy doped 3+ Mixing with boehmite sol, ultrasonic mixing, and drying in a vacuum drying oven; calcining to obtain surface-coated gamma-Al 2 O 3 ：Dy 3+ Carbon nanotubes of the particles;
the calcining temperature is 150-200 ℃.
2. The surface-coated gamma-Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that the Dy doped carbon nano tube adsorbent is added 3+ After the mixture is mixed with the boehmite sol, ammonia water is added dropwise, and the pH is regulated to 9-10.
3. The surface-coated gamma-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 bathStanding at 60deg.C for aging, cooling to room temperature, and washing with deionized water.
4. The surface-coated gamma-Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nanotube adsorbent is characterized in that the Triton X-100 nonionic surfactant is added, and the temperature of a reaction system is maintained at 50-55 ℃ after constant-temperature water bath is carried out.
5. The surface-coated gamma-Al of claim 1 2 O 3 ：Dy 3+ The preparation method of the granular carbon nano tube adsorbent is characterized in that the added HNO 3 And Al (OC) in solution 3 H 7 ) 3 The molar ratio of (2) is 0.05-0.07:1.
6. The surface-coated gamma-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 nanotubes in a mixed solution of concentrated sulfuric acid and peroxytrifluoroacetic acid, the volume ratio of the concentrated sulfuric acid to the peroxytrifluoroacetic acid is 3:1, the mass ratio of the carbon nanotubes to the concentrated acid solution is 1:200-400, the oxidation temperature is 50-95 ℃, the oxidation time is 1-3 hours, the product is washed to have a pH value of 6-8 after the oxidation is completed, the filtered carbon nanotubes are added into 200-400ml of hydrogen peroxide, and a drying box is used until the weight is constant at 70-80 ℃.
7. A carbon nanotube adsorbent produced by the method of any one of claims 1 to 6.
8. Use of the adsorbent of claim 7 in wastewater treatment.
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