CN111097381A - Renewable modified activated carbon adsorbent and preparation method and application thereof - Google Patents
Renewable modified activated carbon adsorbent and preparation method and application thereof Download PDFInfo
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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
- 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
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- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention discloses a reproducible modified activated carbon adsorbent and a preparation method thereof. The regenerable modified activated carbon adsorbent comprises the following components: 4-8% of molybdenum disulfide/carbon nanotube composite material, 3-5% of magnetic nanoparticles, 5-15% of diatom ooze, 6-12% of bentonite and the balance of activated carbon. The preparation method comprises the following steps: modifying the modified carbon nano tube, adding the modified carbon nano tube into water to form a dispersion solution, then adding soluble molybdenum salt, thiourea and a surfactant, magnetically stirring, carrying out vacuum heat preservation at 160-190 ℃ for 18-20 h, cooling, filtering, washing and drying to obtain a molybdenum disulfide/carbon nano tube composite material; the composite material is uniformly mixed with other raw materials, ball-milled, washed and dried, and then vacuum-calcined at 200-250 ℃ for 1-2 hours. The adsorption capacity of the regenerable modified activated carbon adsorbent on heavy metal ions in industrial wastewater is greatly higher than that of the current commercial activated carbon.
Description
Technical Field
The invention relates to the field of nano materials and environment-friendly materials, in particular to a renewable modified activated carbon adsorbent and a preparation method and application thereof.
Background
With the rapid development of national economy and science and technology, the material life of people is greatly enriched, and the environmental pollution and energy crisis become the main hot problems of the current society. The reduction and purification of the discharge of various pollutants in air and water has been effective for environmental protection, and among them, physical adsorption is considered as the most effective method for solving air pollution and industrial wastewater treatment in a wide range, but the poor separability and regenerability of the adsorbent in the aqueous phase limits its application in water treatment or air purification processes. In addition, the application of the photocatalytic technology in the treatment of industrial wastewater has been emerging in recent years, and has a wide application prospect, however, the application of the photocatalytic technology in the field of wastewater treatment is limited due to the high treatment cost and the inapplicability of the photocatalytic technology to a wide range of practical applications. The existing activated carbon has low adsorption efficiency on heavy metal ions in industrial wastewater, and limits the application of the activated carbon in the field of wastewater treatment.
Disclosure of Invention
One of the purposes of the invention is to provide a regenerable modified activated carbon adsorbent. The specific technical scheme is as follows:
a reproducible modified activated carbon adsorbent comprises the following components in percentage by mass: 4-8% of molybdenum disulfide/carbon nanotube composite material, 3-5% of magnetic nanoparticles, 5-15% of diatom ooze, 6-12% of bentonite and the balance of activated carbon.
Preferably, the mass percent of the carbon nanotubes in the molybdenum disulfide/carbon nanotube composite material is 5% -10%, and the balance is molybdenum disulfide.
More preferably, the molybdenum disulfide is spherical with a diameter of 100-200 nm; the inner diameter of the carbon nano tube is 5-10nm, the outer diameter is 10-20nm, and the length is 0.5-2 μm; and the molybdenum disulfide grows on the outer wall of the carbon nanotube in situ.
Preferably, the magnetic nanoparticles are Co3O4、Fe3O4Or NiFe2O4The particle size is 50-300 nm.
The invention also aims to provide a preparation method of the regenerable modified activated carbon adsorbent. The specific technical scheme is as follows:
the preparation method of the regenerable modified activated carbon adsorbent comprises the following steps:
(1) modification of carbon nanotubes
Adding the carbon nano tube into a concentrated nitric acid solution, performing ultrasonic treatment for more than 0.5h, keeping the temperature of 80-120 ℃ for 0.5-2 h, naturally cooling to room temperature, repeatedly washing a product with deionized water and ethanol until the product is clean, and performing vacuum drying to obtain a modified carbon nano tube;
(2) preparation of molybdenum disulfide/carbon nanotube composite material
Adding the modified carbon nano tube obtained in the step (1) into water to form a dispersion liquid, then adding soluble molybdenum salt, thiourea and a surfactant into the dispersion liquid, magnetically stirring for more than 10 minutes, then carrying out vacuum heat preservation for 18-20 hours at 160-190 ℃, naturally cooling to room temperature, filtering, washing and drying to obtain a molybdenum disulfide/carbon nano tube composite material; the mass ratios, namely the concentrations, of the modified carbon nanotube, the soluble molybdenum salt, the thiourea, the surfactant and the water are respectively as follows: 0.5-1 g/L, 5-30 g/L, 30-120 g/L, 15-75 g/L;
(3) preparation of renewable modified activated carbon adsorbent
And (3) mixing the molybdenum disulfide/carbon nanotube composite material obtained in the step (2), magnetic nanoparticles, diatom ooze, bentonite and activated carbon according to mass percent, magnetically stirring until the mixture is uniform, adding ethanol accounting for 3-8% of the total mass of the components as a ball milling aid, performing ball milling for 2-4 h, washing, drying, and performing vacuum calcination at 200-250 ℃ for 1-2h to obtain the renewable modified activated carbon adsorbent.
Preferably, the soluble molybdenum salt is ammonium molybdate or sodium molybdate.
Preferably, the surfactant is polyvinylpyrrolidone, sodium cetyl bromide, calcium dodecylbenzenesulfonate or triethanolamine soap.
The invention also aims to provide application of the regenerable modified activated carbon adsorbent. The specific technical scheme is as follows:
the regenerable modified activated carbon adsorbent is applied to adsorption of heavy metals in industrial wastewater.
Preferably, an externally applied magnetic field is used for recovery and regeneration.
Preferably, the step of recovering and regenerating is: firstly, the reproducible modified activated carbon adsorbent which reaches the adsorption balance is kept at a constant temperature for 0.5-1h at the temperature of 50-80 ℃, and then vacuum desorption is carried out for 1-2h at the temperature of 300-400 ℃.
The invention has the beneficial effects that:
the regenerable modified activated carbon adsorbent prepared by the embodiment of the invention can be used for treating rhodamine B, methylene blue and Pb in wastewater2+、Cd2+The adsorption capacity of (2) exceeds that of commercial activated carbon, and is particularly represented by shorter adsorption equilibrium time and larger maximum adsorption amount (wherein the specific adsorption amount of heavy metal ions is increased by 1 time). The method has the advantages of low cost, simple and easily-controlled production process and high product yield, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is a schematic diagram of the synthesis of the molybdenum disulfide/carbon nanotube composite material of the present invention.
Fig. 2(a), 2(b) and 2(c) are XRD, Raman and infrared spectra of the molybdenum disulfide/carbon nanotube composite material of the present invention, respectively.
Fig. 3 is a TEM image of the molybdenum disulfide/carbon nanotube composite of the present invention, wherein the magnifications of fig. 3(a), fig. 3(b) and fig. 3(c) are 1000, 2000, 25000 in this order.
Detailed Description
The present invention will be further described below by way of specific embodiments, and it is apparent from the technical knowledge that the present invention can be described by other means without departing from the technical features of the present invention, and therefore all changes within the scope of the present invention or the equivalent scope of the present invention are encompassed by the present invention.
Example 1
Preparation of renewable modified activated carbon adsorbent
(1) Modification of carbon nanotubes
0.3g of multi-wall carbon nano-tube (the inner diameter is 5-10nm, the outer diameter is 10-20nm, and the length is 0.5-2 μm) is added into 30mLHNO3 (69%) solution, ultrasonic treatment is carried out for 0.5h, then the mixture is transferred into a 50mL stainless steel reaction kettle, and heat preservation is carried out for 1h at the temperature of 100 ℃. And naturally cooling to room temperature, repeatedly washing the product to be clean by deionized water and ethanol, and drying in vacuum to obtain the modified carbon nano tube.
(2) Preparation of molybdenum disulfide/carbon nanotube composite material
And (2) dispersing 20mg of the modified carbon nano tube obtained in the step (1) into 30mL of deionized water to form a suspension, then adding 0.8g of ammonium molybdate tetrahydrate, 3.6g of thiourea and 2.2g of polyvinylpyrrolidone into the suspension, magnetically stirring for 30min, transferring the mixture into a 50mL stainless steel reaction kettle, placing the stainless steel reaction kettle in a vacuum drying oven, preserving the temperature for 18h at 160 ℃, naturally cooling to room temperature, filtering, washing and drying to obtain the molybdenum disulfide/carbon nano tube composite material.
(3) Preparation of renewable modified activated carbon adsorbent
By mass percentage, the molybdenum disulfide/carbon nanotube composite material is 4%, and the magnetic nanoparticle Co3O43 percent (granularity is 50-300nm), 5 percent of diatom ooze, 6 percent of bentonite and 82 percent of active carbon, the components are stirred by magnetic force for 1 hour to be uniformly mixed, ethanol solution is taken as an auxiliary agent, the mass of the ethanol solution is 5 percent of the total mass of other raw materials, the materials are washed, dried and calcined for 1 hour under vacuum low temperature at 200 ℃ after being ball-milled for 2 hours, and the reproducible modified active carbon adsorbent is prepared.
Example 2
Preparation of renewable modified activated carbon adsorbent
(1) Modification of carbon nanotubes
0.3g of multi-wall carbon nano-tube (the inner diameter is 5-10nm, the outer diameter is 10-20nm, and the length is 0.5-2 μm) is added into 30mLHNO3 (69%) solution, ultrasonic treatment is carried out for 0.5h, then the mixture is transferred into a 50mL stainless steel reaction kettle, and heat preservation is carried out for 1h at the temperature of 100 ℃. And naturally cooling to room temperature, repeatedly washing the product to be clean by deionized water and ethanol, and drying in vacuum to obtain the modified carbon nano tube.
(2) Preparation of molybdenum disulfide/carbon nanotube composite material
And (2) dispersing 20mg of the modified carbon nano tube obtained in the step (1) into 30mL of deionized water to form a suspension, then adding 0.4g of ammonium molybdate tetrahydrate, 1.8g of thiourea and 1.1g of polyvinylpyrrolidone into the suspension, magnetically stirring for 30min, transferring the mixture into a 50mL stainless steel reaction kettle, placing the stainless steel reaction kettle in a vacuum drying oven, preserving the temperature for 20h at 190 ℃, naturally cooling to room temperature, filtering, washing and drying to obtain the molybdenum disulfide/carbon nano tube composite material.
(3) Preparation of renewable modified activated carbon adsorbent
By mass percentage, the molybdenum disulfide/carbon nanotube composite material accounts for 8 percent, and the magnetic nanoparticles are Fe3O45% (granularity is 50-300nm), 15% of diatom ooze, 12% of bentonite and 60% of activated carbon, the above magnetic stirring is carried out for 0.5h to ensure that the diatom ooze and the activated carbon are uniformly mixed, ethanol solution is taken as an auxiliary agent, the mass of the ethanol solution is 5% of the total mass of other raw materials, the ethanol solution is washed and dried after being ball-milled for 4h, and then the mixture is calcined for 2h under vacuum low temperature at 200 ℃, so as to obtain the renewable modified activated carbon adsorbent.
Example 3
Preparation of renewable modified activated carbon adsorbent
(1) Modification of carbon nanotubes
0.3g of multi-wall carbon nano-tube (the inner diameter is 5-10nm, the outer diameter is 10-20nm, and the length is 0.5-2 μm) is added into 30mLHNO3 (69%) solution, ultrasonic treatment is carried out for 0.5h, then the mixture is transferred into a 50mL stainless steel reaction kettle, and heat preservation is carried out for 1h at the temperature of 100 ℃. And naturally cooling to room temperature, repeatedly washing the product to be clean by deionized water and ethanol, and drying in vacuum to obtain the modified carbon nano tube.
(2) Preparation of molybdenum disulfide/carbon nanotube composite material
And (2) dispersing 20mg of the modified carbon nano tube obtained in the step (1) into 30mL of deionized water to form a suspension, then adding 0.2g of ammonium molybdate tetrahydrate, 0.9g of thiourea and 0.55g of polyvinylpyrrolidone into the suspension, magnetically stirring for 30min, transferring the mixture into a 50mL stainless steel reaction kettle, placing the stainless steel reaction kettle in a vacuum drying oven, preserving the temperature for 20h at 190 ℃, naturally cooling to room temperature, filtering, washing and drying to obtain the molybdenum disulfide/carbon nano tube composite material.
(3) Preparation of renewable modified activated carbon adsorbent
By mass percentage, the molybdenum disulfide/carbon nanotube composite material accounts for 6 percent, and the magnetic nano-particle NiFe2O44% (granularity is 50-300nm), 10% of diatom ooze, 10% of bentonite and 70% of activated carbon, the components are stirred by magnetic force for 1 hour to be uniformly mixed, ethanol solution is used as an auxiliary agent, the mass of the ethanol solution is 5% of the total mass of other raw materials, the materials are washed, dried and calcined at low temperature and vacuum of 250 ℃ for 1.5 hours after being ball-milled for 3 hours, and the renewable modified activated carbon adsorbent is obtained.
Example 4 Performance testing
Fig. 1 is a schematic diagram of the synthesis of the molybdenum disulfide/carbon nanotube composite material of the present invention, which schematically illustrates the process of in-situ growth of molybdenum disulfide on the outer wall of a carbon nanotube.
Fig. 2(a), 2(b) and 2(c) are XRD, Raman and infrared spectra of the molybdenum disulfide/carbon nanotube composite material of the present invention, respectively. FIG. 2(a) shows CNTs and MoS2The coexistence of XRD characteristic peaks proves that MoS2Nanospheres readily couple to CNTs during hydrothermal processing. FIG. 2(c) shows MoS2CNTs and CNTs/MoS2FTIR spectra of the nanocomposites revealed that the characteristic absorption peaks at 3436cm-1 and 1624cm-1 were due to O-H and C ═ C stretching vibrations at the surface of CNT and MoS2@ CNTs. Meanwhile, a distinct band caused by Mo-S vibration was observed at 601 cm-1. Furthermore, Raman spectra in FIG. 2(b) further indicate CNTs/MoS2Two characteristic peaks of C, 1320 and 1582cm-1, were present in the complex, with MoS2Characteristic peaks e12g and a1g of (A) were observed at 361.2 and 402.6 cm-1. MoS based on XRD, Raman and infrared spectrum verification2And CNTs are subjected to hydrothermal conditions to form the molybdenum disulfide/carbon nanotube composite material.
Fig. 3 is a TEM image of the molybdenum disulfide/carbon nanotube composite of the present invention, wherein the magnifications of fig. 3(a), fig. 3(b) and fig. 3(c) are 1000, 2000, 25000 in this order. From FIGS. 3(a) and 3(b), it was confirmed that flower-like MoS2The nanospheres are uniformly grown onSurface of CNTs, MoS2The size of the nano-sphere crystal grain is 100-200nm, and the outer diameter of the CNTs is about 20 nm. As shown in FIG. 3(c) (HRTEM), MoS2The lattice spacing of the catalyst is increased to 0.97nm due to the introduction of the CNTs, so that the catalytic performance of the catalyst is improved.
Adsorption test for industrial wastewater pollutants
The Shimadzu atomic absorption spectrophotometer (AA-7000) measures the content of heavy metal ions in the waste liquid. Specifically, a heavy metal ion solution with a certain concentration is prepared, then the regenerable modified activated carbon adsorbent is added, the pH value is 7, the magnetic stirring rotating speed is 200r/min, an atomic absorption spectrophotometer is adopted to test the amount of different heavy metal ions, after adsorption is balanced, the adsorption saturation time is recorded, and the maximum adsorption amount of the heavy metal ions is measured and calculated. Specific data are shown in table 1:
table 1 adsorption performance of the regenerable modified activated carbon adsorbent obtained in example on different pollutants
As can be seen from table 1, the adsorption capacity of the regenerable modified activated carbon adsorbent obtained in the embodiment of the present invention for rhodamine B, methylene blue, Pb2+, and Cd2+ in wastewater exceeds that of commercial activated carbon, and specifically shows that the adsorption equilibrium time is shorter, and the maximum adsorption capacity is larger (where the specific adsorption capacity of heavy metal ions is increased by 1 time).
Claims (9)
1. The regenerable modified activated carbon adsorbent is characterized by comprising the following components in percentage by mass: 4-8% of molybdenum disulfide/carbon nanotube composite material, 3-5% of magnetic nanoparticles, 5-15% of diatom ooze, 6-12% of bentonite and the balance of activated carbon.
2. The regenerable modified activated carbon sorbent of claim 1, wherein the mass percent content of carbon nanotubes in the molybdenum disulfide/carbon nanotube composite is 5-10%, and the balance is molybdenum disulfide.
3. The regenerable modified activated carbon sorbent of claim 2, wherein the molybdenum disulfide is spherical with a diameter of 100-200 nm; the inner diameter of the carbon nano tube is 5-10nm, the outer diameter is 10-20nm, and the length is 0.5-2 μm; and the molybdenum disulfide grows on the outer wall of the carbon nanotube in situ.
4. The regenerable modified activated carbon sorbent of claim 1, wherein the magnetic nanoparticles are Co3O4、Fe3O4Or NiFe2O4The particle size is 50-300 nm.
5. A method for preparing a regenerable modified activated carbon sorbent as claimed in any one of claims 1 to 4, comprising the steps of:
(1) modification of carbon nanotubes
Adding the carbon nano tube into a concentrated nitric acid solution, performing ultrasonic treatment for more than 0.5h, keeping the temperature of 80-120 ℃ for 0.5-2 h, naturally cooling to room temperature, repeatedly washing a product with deionized water and ethanol until the product is clean, and performing vacuum drying to obtain a modified carbon nano tube;
(2) preparation of molybdenum disulfide/carbon nanotube composite material
Adding the modified carbon nano tube obtained in the step (1) into water to form a dispersion liquid, then adding soluble molybdenum salt, thiourea and a surfactant into the dispersion liquid, magnetically stirring for more than 10 minutes, then carrying out vacuum heat preservation for 18-20 hours at 160-190 ℃, naturally cooling to room temperature, filtering, washing and drying to obtain a molybdenum disulfide/carbon nano tube composite material; the mass ratios, namely the concentrations, of the modified carbon nanotube, the soluble molybdenum salt, the thiourea, the surfactant and the water are respectively as follows: 0.5-1 g/L, 5-30 g/L, 30-120 g/L, 15-75 g/L;
(3) preparation of renewable modified activated carbon adsorbent
And (3) mixing the molybdenum disulfide/carbon nanotube composite material obtained in the step (2), magnetic nanoparticles, diatom ooze, bentonite and activated carbon according to mass percent, magnetically stirring until the mixture is uniform, adding ethanol accounting for 3-8% of the total mass of the components as a ball milling aid, performing ball milling for 2-4 h, washing, drying, and performing vacuum calcination at 200-250 ℃ for 1-2h to obtain the renewable modified activated carbon adsorbent.
6. The method of claim 5, wherein the soluble molybdenum salt is ammonium molybdate or sodium molybdate.
7. The method for preparing the regenerable modified activated carbon sorbent of claim 5, wherein the surfactant is polyvinylpyrrolidone, sodium cetyl bromide, calcium dodecylbenzenesulfonate or triethanolamine soap.
8. The application of the regenerable modified activated carbon sorbent as claimed in any one of claims 1 to 4 in adsorption of heavy metals in industrial wastewater.
9. A method according to claim 8, wherein an externally applied magnetic field is used for recovery and regeneration; the steps of recovering and regenerating are as follows: firstly, the reproducible modified activated carbon adsorbent which reaches the adsorption balance is kept at a constant temperature for 0.5-1h at the temperature of 50-80 ℃, and then vacuum desorption is carried out for 1-2h at the temperature of 300-400 ℃.
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