CN109248655A - A kind of method of preparation and use and application of magnetic carbon nano-tube - Google Patents
A kind of method of preparation and use and application of magnetic carbon nano-tube Download PDFInfo
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- CN109248655A CN109248655A CN201811210706.5A CN201811210706A CN109248655A CN 109248655 A CN109248655 A CN 109248655A CN 201811210706 A CN201811210706 A CN 201811210706A CN 109248655 A CN109248655 A CN 109248655A
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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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- B01J20/00—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
- B01J20/28002—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 physical properties
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- B01J20/30—Processes for preparing, regenerating, or reactivating
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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
- 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
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- 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
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- C—CHEMISTRY; METALLURGY
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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Abstract
The invention discloses a kind of method of preparation and use of magnetic carbon nano-tube and applications: preparing a certain amount of aqueous solution containing manganous chloride and ferric trichloride in conical flask；Appropriate carbon nanotube is added, stirs evenly；Under certain mixing speed, warming-in-water adjusts pH to 9-11 to 50-70 DEG C of addition sodium hydroxide solution；4 hours are kept the temperature in water-bath；After cooling, with deionized water repeated flushing, the Magnetic Isolation from aqueous solution is dried for standby；The solution containing humic acid, methylene blue, methyl orange, phosphate radical, tetracycline and copper ion for measuring certain volume respectively, determines the concentration of six kinds of solution；It weighs a certain amount of magnetic carbon nano-tube respectively to be added in six kinds of solution containing humic acid, methylene blue, methyl orange, phosphate radical, tetracycline and copper ion, 25 DEG C, separately sampled after adsorbing for 24 hours in 140rpm shaking table, sample distinguishes detectable concentration after membrane filtration.The removal of present invention multiple pollutant suitable for water body.
Description
Technical field
The invention belongs to environment and technical field of chemistry, and more specifically, it relates to a kind of preparations of magnetic carbon nano-tube
And application method and application.
Background technique
Adsorption technology is considered the water treatment technology of most practical value by U.S. EPA, the carbon with excellent absorption property
Nanotube is applied to removal environmental contaminants, however carbon nanotube nanometer poisonous effect that may be present causes that scholar's is extensive
Concern, therefore, it is that cannot be neglected critical issue that carbon nanotube is efficiently separated from medium.
Conventional centrifugation and filtering can not effectively realize good separation of solid and liquid, and magnetic separation technique is efficient, fast because of it
The characteristics such as speed, economy receive more and more attention.Nanometer MnFe2O4As a kind of common soft magnetic material, specific surface area and
Saturation magnetization is larger, has excellent chemical stability, the heavy metal being frequently used in Adsorption soil and water and has
Machine object, but its own has that saturated adsorption capacity is small.
It is low with a kind of economic cost accordingly, prepare simple method and synthesize and a kind of there is good magnetic and high-adsorption-capacity
MnFe2O4/ carbon nano-tube magnetic adsorbent.This magnetic carbon nano-tube adsorbent both can keep desired high-adsorption-capacity also
It can have magnetism, effectively realize and be separated by solid-liquid separation, it is reusable, it is without secondary pollution.The adsorbent is for a variety of pollutions in water
The Adsorption of object provides a kind of economy and facility and extremely promising ways and means for the control of environmental pollution.
Summary of the invention
Purpose of the invention is to overcome the shortcomings in the prior art, is separated by solid-liquid separation for carbon nanotube adsorption agent difficult
The state of the art, propose a kind of method of preparation and use of magnetic carbon nano-tube, and be used for going for multiple pollutant in water
It removes.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of preparation method of magnetic carbon nano-tube, the following steps are included:
Step 1: at room temperature, preparing a certain amount of containing manganous chloride (0.125mol/L) and ferric trichloride (0.25mol/L)
Aqueous solution in conical flask, form stable uniform system；
Step 2: weighing suitable carbon nanotube, it is added in the solution that the first step is prepared, stirs evenly；
Step 3: under certain mixing speed, warming-in-water to 50-70 DEG C of addition 3mol-1The sodium hydroxide solution of L is adjusted
PH to 9-11 keeps the temperature 1 hour, generates MnFe2O4；4 hours are kept the temperature in 100 DEG C of water-baths；After cooling, repeatedly with deionized water
It rinses to remove the Cl introduced in synthesis process-1、Na+1, then the Magnetic Isolation from aqueous solution, is dried standby at 90-150 DEG C
With.
Carbon nanotube described in second step is single wall, double-walled or multi-walled carbon nanotube, and the carbon nanotube is carbon nanotube
Primary sample, the carbon nanotube primary sample can be former for the carbon nanotube of arc process or the preparation of chemical vapour deposition technique or laser method
Beginning sample.
The MnFe that carbon nanotube mass and third step generate in second step2O4Mass ratio is 1:1-1:5.
Mixing speed is in 100-250r/min in third step.
A kind of application method of the magnetic carbon nano-tube of the method preparation, comprising the following steps:
Step 1: respectively measure certain volume containing humic acid, methylene blue, methyl orange, phosphate radical, tetracycline and copper from
The solution of son, determines the concentration of six kinds of solution；
It is added in six kinds of solution of the first step step 2: weighing a certain amount of magnetic carbon nano-tube respectively, 25 DEG C, 140rpm
Separately sampled after adsorbing in shaking table for 24 hours, sample distinguishes detectable concentration after 0.45um membrane filtration.
The density determination method of six kinds of solution in the first step: using direct spectrophotometry to humic acid, methylene blue, first
The base orange concentration different with tetracycline carries out absorbance measurement, standard curve is established, so that it is molten to measure each pollutant in water
Degree；Phosphate radical and copper ion use molybdenum-antimony anti-spectrophotometric method and double acetaldehyde oxalyl dihydrazone spectrophotometry measurements respectively.
A kind of application of the magnetic carbon nano-tube of the method preparation, magnetic carbon nano-tube pollute in the water for removal
It is any in object, including humic acid, methylene blue, tetracycline, methyl orange, phosphate radical and copper ion.
Compared with prior art, the beneficial effects brought by the technical solution of the present invention are as follows:
(1) magnetic carbon nano-tube prepared by the present invention avoids use directly with the carbon nanotube primary sample of preparation synthesis
The complex process of strong acid purifying surface metal catalyst.The characteristic for making full use of carbon nano tube surface to be easy to modify, is prepared for having
There is the magnetic adsorbent of good chemical stability and mechanical strength.
(2) compared with original carbon nanotubes, magnetic carbon nano-tube prepared by the present invention is not only provided with good Magneto separate
Performance also keeps or largely improves its absorption property.The magnetic carbon nano-tube of preparation has big specific surface area,
Adsorption capacity is big, can Reusability number up to 5 times or more, avoid secondary pollution.
(3) condition for crossing range request that the present invention synthesizes is easy to control, and low energy consumption, easy to operate, and does not have to have in the process
Solvent belongs to process for cleanly preparing, easy to industrialized production.
Detailed description of the invention
Fig. 1 is the projection microscopic comparison of multi-walled carbon nanotube before and after 1 carried magnetic carbon nano-particle of embodiment；
Fig. 2 is 3 magnetic carbon nano-tube regenerated outcome figure of embodiment.
Specific embodiment
The invention will be further described with reference to the accompanying drawing.
The preparation method of magnetic carbon nano-tube of the invention, the following steps are included:
Step 1: at room temperature, preparing a certain amount of containing manganous chloride (0.125mol/L) and ferric trichloride (0.25mol/L)
Aqueous solution in conical flask, form stable uniform system (wherein molar ratio Mn:Fe=1:2).
Step 2: weighing suitable carbon nanotube, it is added in the solution that the first step is prepared, stirs evenly.
Used carbon nanotube is single wall, double-walled or multi-walled carbon nanotube, and the carbon nanotube is that carbon nanotube is original
Sample, the carbon nanotube primary sample can be arc process or the original sample of carbon nanotube of chemical vapour deposition technique or laser method preparation
Product.The MnFe that used carbon nanotube mass and third step generate2O4Mass ratio is 1:1-1:5.
Step 3: under certain mixing speed, warming-in-water to 50-70 DEG C of addition 3mol-1The sodium hydroxide solution of L is adjusted
PH to 9-11 keeps the temperature 1 hour, generates MnFe2O4；4 hours are kept the temperature in 100 DEG C of water-baths；After cooling, repeatedly with deionized water
It rinses to remove the Cl introduced in synthesis process-1、Na+1Deng then the Magnetic Isolation from aqueous solution, is dried at 90-150 DEG C
It is spare.Wherein, mixing speed is in 100-250r/min.
Water pollutant of the magnetic carbon nano-tube prepared by the present invention for removal, including humic acid, methylene blue, four
It is any in ring element (TC), methyl orange, phosphate radical and copper ion.
The application method of magnetic carbon nano-tube prepared by the present invention, comprising the following steps:
Step 1: respectively measure certain volume containing humic acid, methylene blue, methyl orange, phosphate radical, tetracycline and copper from
The solution of son, determines the concentration of six kinds of solution.
Wherein, the density determination method of six kinds of solution: using direct spectrophotometry to humic acid, methylene blue, methyl
The orange concentration different with tetracycline carries out absorbance measurement, standard curve is established, to measure each pollutant solubility in water；
Phosphate radical and copper ion use molybdenum-antimony anti-spectrophotometric method and double acetaldehyde oxalyl dihydrazone spectrophotometry measurements respectively.
It is added in six kinds of solution of the first step step 2: weighing a certain amount of magnetic carbon nano-tube respectively, 25 DEG C, 140rpm
Separately sampled after adsorbing in shaking table for 24 hours, sample distinguishes detectable concentration after 0.45um membrane filtration.
Embodiment 1: magnetic carbon nano-tube preparation
A kind of load MnFe2O4The preparation method of the carbon nanotube adsorption agent of magnetic nano-particle, the specific steps are as follows:
1. magnetic kind prepares: at room temperature, preparing 200ml and contain manganous chloride (0.025mol) and ferric trichloride (0.05mol)
Aqueous solution in the conical flask of 250ml, form stable uniform system, be denoted as solution A.
2. carbon nanotube prepares: weighing 5.7735g multi-walled carbon nanotube with a ten thousandth balance, be added in solution A and stir
It mixes uniformly, obtains mixed liquid B.
3. prepared by magnetic carbon nano-tube: under constant stirring, by mixed liquid B warming-in-water to 60 DEG C, being added dropwise 3mol/L's
Sodium hydroxide solution adjusts pH to 11, keeps the temperature 1 hour.Finally, keeping the temperature 4 hours in 100 DEG C of water-baths.After cooling, spend from
Sub- water repeated flushing is to remove the Cl introduced in synthesis process-1、Na+1Deng the then Magnetic Isolation from aqueous solution, at 110 DEG C
It is dried for standby.Projection Electronic Speculum (TEM) characterization result of multi-walled carbon nanotube is as shown in Figure 1 before and after carried magnetic nano particle.
By Fig. 1 (a) it is found that multi-walled carbon nanotube hollow structure in a tubular form before modified, tube wall is smooth, and other phase does not go out
It is existing.Since magnetic multi-walled carbon nanotube synthesizes the washing and Magnetic Isolation of laggard mistake repeatedly, to remove unreacted impurity.By scheming
1 (b) can be clearly apparent, and magnetic-particle, which has consolidated, to be loaded on multi-wall carbon nano-tube tube wall, and dispersion is relatively uniform, synthesized
Magnetic-particle should be nano particle, and size is about 10nm, have biggish surface energy.After before modified, the shape of multi-walled carbon nanotube
Looks have almost no change, and illustrate that the magnetism multi-walled carbon nano-tubes adsorbent has preferable mechanical stability.
Embodiment 2: magnetic carbon nano-tube absorption property
According to magnetic carbon nano-tube prepared by embodiment 1, carried out to humic acid in water, methylene blue, methyl orange, copper,
The Adsorption effect experiment of tetracycline and phosphate anion.10mg magnetic carbon nano-tube is taken to be added containing above-mentioned all kinds of pollutions respectively
In the 50ml solution of object, 25 DEG C, adsorbs in 140rpm shaking table and sample afterwards for 24 hours, sample detects after 0.45um membrane filtration, as a result
It is as shown in table 1:
Table 1
As shown in Table 1, magnetic carbon nano-tube is to humic acid, methylene blue, methyl orange, copper ion, tetracycline and phosphate radical
Removal rate become 88.0% from original 89.8%, 99.6%, 99.5%, 3.4%, 98.8% and 89.3,99.%,
98.6%, 34.8%, 99.0% and 93.8%, it substantially maintains and the comparable absorption property of carbon nanotube；Magnetic carbon nanometer
Pipe about promotes 10 times to the Adsorption effect of heavy metal copper, and absorption property is promoted significant.It may be since different pollutants exist
Absorption point in carbon nanotube adsorption agent is different, and magnetic nanoparticle of magnetic carbon nano-tube adsorbent itself also has can be with
The adsorption site of the interactions such as pollutant copper makes modified carbon nanotube not only be provided with good Magneto separate characteristic, also
Keep or largely improve its absorption property.
Embodiment 3: magnetic carbon nano-tube regeneration
The magnetic carbon nano-tube adsorbent of 1 preparation according to embodiments of the present invention, its regeneration effect of research effect, specific steps
It is as follows:
1. magnetic carbon nano-tube adsorption experiment: 1000mg magnetic carbon nano-tube being added to 800ml, the TC of 150mg/L is molten
In liquid, 25 DEG C, adsorbed under the conditions of 140rpm for 24 hours to adsorption equilibrium；Then static 5h or more removes supernatant in 60 DEG C of baking ovens
It is dried to obtain sample MWCNTs-A1.
2. magnetic carbon nano-tube regeneration tests: take the MWCNTs-A1 sample of 900mg to be put into the NaOH solution of 0.1M, 25
It is regenerated under the conditions of DEG C for 24 hours, externally-applied magnetic field makes solid-liquid quick separating, and supernatant is gone to be dried to obtain sample in 60 DEG C of baking ovens
MWCNTs-A2。
3. magnetic carbon nano-tube regeneration effect: repeat the above steps 2, successively obtained by same procedure MWCNTs-A3,
MWCNTs-A4, MWCNTs-A5 and MWCNTs-A6.Then above-mentioned six kinds of samples of 10mg are taken, the TC for being put into 50ml 20ppm is molten
In liquid, 25 DEG C, adsorbed under the conditions of 140rpm for 24 hours to adsorption equilibrium.Regeneration tests result is as shown in Figure 2.
As seen from Figure 2, by five regenerated magnetic carbon nano-tubes of alkali to the adsorbance Q of TCeStill up to 59.4mg/
G, regeneration have restored its 73.2% adsorption effect to TC, have illustrated the magnetic carbon nano-tube with good Magneto separate performance
Meanwhile also there is good absorption regeneration ability, this is used for actual water treatment work to it with important economic significance.
Although function and the course of work of the invention are described above in conjunction with attached drawing, the invention is not limited to
Above-mentioned concrete function and the course of work, the above mentioned embodiment is only schematical, rather than restrictive, ability
The those of ordinary skill in domain under the inspiration of the present invention, is not departing from present inventive concept and scope of the claimed protection situation
Under, many forms can also be made, all of these belong to the protection of the present invention.
Claims (7)
1. a kind of preparation method of magnetic carbon nano-tube, which comprises the following steps:
Step 1: at room temperature, preparing a certain amount of water containing manganous chloride (0.125mol/L) and ferric trichloride (0.25mol/L)
Solution forms stable uniform system in conical flask；
Step 2: weighing suitable carbon nanotube, it is added in the solution that the first step is prepared, stirs evenly；
Step 3: under certain mixing speed, warming-in-water to 50-70 DEG C of addition 3mol-1The sodium hydroxide solution of L adjusts pH and arrives
9-11 keeps the temperature 1 hour, generates MnFe2O4；4 hours are kept the temperature in 100 DEG C of water-baths；After cooling, with deionized water repeated flushing
To remove the Cl introduced in synthesis process-1、Na+1, then the Magnetic Isolation from aqueous solution, is dried for standby at 90-150 DEG C.
2. the preparation method of magnetic carbon nano-tube according to claim 1, which is characterized in that carbon nanometer described in second step
Pipe is single wall, double-walled or multi-walled carbon nanotube, and the carbon nanotube is carbon nanotube primary sample, the carbon nanotube primary sample
It can be arc process or the carbon nanotube primary sample of chemical vapour deposition technique or laser method preparation.
3. the preparation method of magnetic carbon nano-tube according to claim 1, which is characterized in that carbon nanotube matter in second step
The MnFe that amount is generated with third step2O4Mass ratio is 1:1-1:5.
4. the preparation method of magnetic carbon nano-tube according to claim 1, which is characterized in that mixing speed exists in third step
100-250r/min。
5. a kind of application method of the magnetic carbon nano-tube of claim 1-4 the method preparation, which is characterized in that including following
Step:
Step 1: measure respectively certain volume containing humic acid, methylene blue, methyl orange, phosphate radical, tetracycline and copper ion
Solution determines the concentration of six kinds of solution；
It is added in six kinds of solution of the first step step 2: weighing a certain amount of magnetic carbon nano-tube respectively, 25 DEG C, 140rpm shaking table
Separately sampled after middle absorption for 24 hours, sample distinguishes detectable concentration after 0.45um membrane filtration.
6. the application method of magnetic carbon nano-tube according to claim 5, which is characterized in that six kinds of solution in the first step
Density determination method: the direct spectrophotometry concentration different with tetracycline to humic acid, methylene blue, methyl orange is utilized
Absorbance measurement is carried out, standard curve is established, to measure each pollutant solubility in water；Phosphate radical and copper ion use molybdenum antimony respectively
Anti- spectrophotometry and double acetaldehyde oxalyl dihydrazone spectrophotometry measurements.
7. a kind of application of the magnetic carbon nano-tube of claim 1-4 the method preparation, which is characterized in that magnetic carbon nano-tube
For any in the water pollutant of removal, including humic acid, methylene blue, tetracycline, methyl orange, phosphate radical and copper ion
Kind.
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| CN109759018A (en) * | 2019-03-21 | 2019-05-17 | 湖南农业大学 | The preparation method and application of support type Manganese Ferrite adsorbent |
| CN111135788A (en) * | 2019-09-18 | 2020-05-12 | 青岛农业大学 | Magnetic nitrogen-doped carbon nanotube water treatment adsorbent and preparation method thereof |
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| CN102179229A (en) * | 2011-05-06 | 2011-09-14 | 同济大学 | Method for preparing magnetic carbon nanotube absorbing agent through Fenton reagent method |
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| CN109759018A (en) * | 2019-03-21 | 2019-05-17 | 湖南农业大学 | The preparation method and application of support type Manganese Ferrite adsorbent |
| CN111135788A (en) * | 2019-09-18 | 2020-05-12 | 青岛农业大学 | Magnetic nitrogen-doped carbon nanotube water treatment adsorbent and preparation method thereof |
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Application publication date: 20190122 |