CN109174074A - A kind of preparation method and applications with defect state carbon nanotube - Google Patents
A kind of preparation method and applications with defect state carbon nanotube Download PDFInfo
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- CN109174074A CN109174074A CN201811185479.5A CN201811185479A CN109174074A CN 109174074 A CN109174074 A CN 109174074A CN 201811185479 A CN201811185479 A CN 201811185479A CN 109174074 A CN109174074 A CN 109174074A
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- carbon nanotube
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
Abstract
A kind of preparation method and applications with defect state carbon nanotube, it is related to a kind of preparation method and applications of carbon nanotube.The present invention is to solve existing carbon nanotube activity points cannot be fully utilized, the weaker technical problem of the catalytic capability of itself.The present invention: one, oxide/carbon nanometer tube is prepared；Two, it is heat-treated.Defect state carbon nanotube prepared by the present invention is applied to the organic pollutant in catalysis potassium peroxymonopersulfate degradation water body.The present invention is prepared for a kind of with defect state carbon nanotube, and it is used as the catalyst of potassium peroxymonopersulfate (PMS) activation degradation water phase organic pollutant, it is smaller by the organic interference with inorganic matter of background, and the efficient oxidation makes target contaminant mineralising.Importantly, the oxidation system that electric charge transfer mediates shows excellent performance and its degradation selectivity in renovation of organic pollution object space face in practical water body compared with traditional oxidation system based on free radical.
Description
Technical field
The present invention relates to a kind of preparation method and applications of carbon nanotube.
Background technique
In recent decades, the organic pollutant in aquatic environment has become serious problems generally existing in global range.
For the advanced technology for developing organic pollutant reparation, many researchers have paid great efforts.In these techniques,
Propose effective ways of the advanced oxidation processes based on persulfate as decomposing organic compounds.A variety of plans are developed
Slightly activate persulfate to generate active oxygen (ROS), such as UV radiation plus thermal and electrochemical process.However, these activation skills
Art needs high-energy to input, this does not have cost-effectiveness.Metal_based material (such as Co3O4, MnO2, CuOFe3O4) it is persulfate
The effective catalyst of activation.But toxic metals leaching inevitably occurs for metal-based catalyst, will lead to the two of water body
Secondary pollution.
In order to overcome this disadvantage, no metal carbon nanomaterial promises to be common metal base activation of catalyst persulfuric acid
The substitute of salt.In these nano-sized carbons, carbon nanotube is as green catalyst, due to its excellent biocompatibility and relatively
Cheap cost can be realized the reparation of organic pollutant.But unmodified nano-carbon material, active point cannot obtain
It makes full use of, the catalytic capability of itself is weaker, needs to be optimized preparation.Defect sturcture is one of the active site of catalysis,
Edge defect is limited in the pi-electron on nano-carbon material on carbon atom, results in very high chemical activity.
Summary of the invention
The present invention is to solve existing carbon nanotube activity points cannot be fully utilized, itself catalytic capability compared with
Weak technical problem, and a kind of preparation method and applications with defect state carbon nanotube are provided.
A kind of preparation method with defect state carbon nanotube of the invention carries out according to the following steps:
One, it prepares oxide/carbon nanometer tube: the concentrated sulfuric acid being uniformly mixed with concentrated nitric acid, obtains mixed acid；By carbon nanotube plus
Enter into mixed acid, be placed in thermostat water bath, 3h~9h is reacted under conditions of 75 DEG C~80 DEG C, then with deionized water and
Dehydrated alcohol is washed to cleaning solution repeatedly and is in neutrality, and is finally dried under conditions of temperature is 60 DEG C~65 DEG C, is obtained carbonoxide
Nanotube；The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3:1；The volume of the mixed acid and the mass ratio of carbon nanotube
For 1L:(15g~17g)；
Two, it is heat-treated: oxide/carbon nanometer tube prepared by step 1 being placed in tube furnace, with 150mL/min~160mL/
The flow velocity of min leads to inert gas 20min to drain air, then with 3 DEG C/min~5 DEG C/min heating rate and inert gas
Protection under so that the temperature of tube furnace is risen to 600 DEG C~1100 DEG C from room temperature, and be 600 DEG C~1100 DEG C and inertia in temperature
Anneal 2h~4h under the protection of gas, finally cooled to room temperature under inert gas protection, obtains defect state carbon nanotube.
Defect state carbon nanotube prepared by the present invention is applied to organic in catalysis potassium peroxymonopersulfate degradation water body
Pollutant.
Carbon nanotube described in step one of the invention is bought from Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences,
OD:10nm~20nm, Length:10 μm~30 μm, Purith:>95wt%, Ash:<1.5wt%.
The present invention, which is prepared for one kind, has defect state carbon nanotube, and it is living to be used as potassium peroxymonopersulfate (PMS)
Change the catalyst of degradation water phase organic pollutant.It is different from free radical involved in conventional PMS base oxidation system, in defect state carbon
The defect level of carbon nanotube is larger in nanotube/PMS system, causes cloud density larger, during making organic matter degradation
Electric charge transfer number is more, so that the excellent oxidative degradation effect of organic pollutant is obtained, by the organic interference with inorganic matter of background
It is smaller, and the efficient oxidation and make target contaminant mineralising.Importantly, with traditional oxidation system phase based on free radical
Than the oxidation system that electric charge transfer mediates shows excellent performance and its choosing in renovation of organic pollution object space face in practical water body
The degradation of selecting property, the 4- chlorophenol that 92% is up in actual water body can be by defect state carbon nanotube@PMS system oxidative degradation.
Detailed description of the invention
Fig. 1 is the TEM figure for testing the carbon nanotube in one in step 1；
Fig. 2 is the TEM figure for the defect state carbon nanotube for testing a preparation；
Fig. 3 is the TEM figure for testing the carbon nanotube in one in step 1；
Fig. 4 is the TEM figure for the defect state carbon nanotube for testing a preparation；
Fig. 5 is XRD diagram；
Fig. 6 is Raman figure；
Fig. 7 is the defect state carbon nanotube selective oxidation degradation figure for testing three；
Fig. 8 is the degradation efficiency figure of organic pollutant.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of preparation method with defect state carbon nanotube, specifically press
What following steps carried out:
One, it prepares oxide/carbon nanometer tube: the concentrated sulfuric acid being uniformly mixed with concentrated nitric acid, obtains mixed acid；By carbon nanotube plus
Enter into mixed acid, be placed in thermostat water bath, 3h~9h is reacted under conditions of 75 DEG C~80 DEG C, then with deionized water and
Dehydrated alcohol is washed to cleaning solution repeatedly and is in neutrality, and is finally dried under conditions of temperature is 60 DEG C~65 DEG C, is obtained carbonoxide
Nanotube；The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3:1；The volume of the mixed acid and the mass ratio of carbon nanotube
For 1L:(15g~17g)；
Two, it is heat-treated: oxide/carbon nanometer tube prepared by step 1 being placed in tube furnace, with 150mL/min~160mL/
The flow velocity of min leads to inert gas 20min to drain air, then with 3 DEG C/min~5 DEG C/min heating rate and inert gas
Protection under so that the temperature of tube furnace is risen to 600 DEG C~1100 DEG C from room temperature, and be 600 DEG C~1100 DEG C and inertia in temperature
Anneal 2h~4h under the protection of gas, finally cooled to room temperature under inert gas protection, obtains defect state carbon nanotube.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: dense sulphur described in step 1
The mass percent of acid is 95%~98%.Other are same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: it is described in step 1
The mass percent of concentrated nitric acid is 65%~68%.Other are the same as one or two specific embodiments.
Specific embodiment 4: present embodiment is answering for the defect state carbon nanotube prepared in specific embodiment one
With the organic pollutant being specially applied in catalysis potassium peroxymonopersulfate degradation water body.
Specific embodiment 5: present embodiment is unlike specific embodiment four: the organic pollutant is
Chlorophenols organic pollutant or sulfamido organic pollutant.Other are identical as specific embodiment four.
The present invention is verified with following tests:
Test one: this test is a kind of preparation method with defect state carbon nanotube, is specifically carried out according to the following steps
:
One, it prepares oxide/carbon nanometer tube: the concentrated sulfuric acid being uniformly mixed with concentrated nitric acid, obtains mixed acid；By carbon nanotube plus
Enter into mixed acid, be placed in thermostat water bath, reacts 6h under conditions of 75 DEG C, it is then anti-with deionized water and dehydrated alcohol
After backwashing is washed to cleaning solution and is in neutrality, and is finally dried under conditions of temperature is 60 DEG C, is obtained oxide/carbon nanometer tube；The dense sulphur
The volume ratio of acid and concentrated nitric acid is 3:1；The volume of the mixed acid and the mass ratio of carbon nanotube are 1L:16.67g；
Two, it is heat-treated: oxide/carbon nanometer tube prepared by step 1 is placed in tube furnace, it is logical with the flow velocity of 150mL/min
Argon gas 20min is to drain air, then to make the temperature of tube furnace from room temperature under the protection of the heating rate of 5 DEG C/min and argon gas
1000 DEG C are risen to, and the 2h that anneals under being 1000 DEG C and the protection of argon gas in temperature, finally naturally cooled under protection of argon gas
Room temperature obtains defect state carbon nanotube；
The mass percent of the concentrated sulfuric acid described in step 1 is 98%；The quality percentage of concentrated nitric acid described in step 1
Than being 35%~37%.
Test two: this test is comparative test, and carbon nanotube is added separately to 10 equipped with organic pollutant to be processed
In the beaker of aqueous solution, the organic pollutant in 10 beakers is respectively phenol, 4- chlorophenol, 2,4- Dichlorophenol, 4- sylvan, 4-
Amino phenols, resorcinol, hydroquinone, benzoic acid, Pyrogentisinic Acid's formic acid and 4- nitrophenols；Organic pollutant is dense in 10 beakers
Degree is 0.16mM, and the concentration of carbon nanotube is 0.1g/L, 10 beakers ultrasound 5min in 10 beakers；By 10 beakers
It is placed on magnetic stirring apparatus and is stirred respectively, it is water-soluble that the PMS that 500 μ L concentration are 50mmol/L is respectively added into 10 beakers
Liquid；It is sampled respectively in 10 jar agitation 1min, 3min, 5min, 10min, 25min, 40min and 60min, sample passes through respectively
0.22 μm of glass fiber filter filtering is crossed, post-filtration samples 1mL is taken to be placed in liquid phase bottle, is separately added into the quenching of 0.5mL methanol,
(4 DEG C) of sample low temperature are saved；Using the concentration of organic pollutant in high performance liquid chromatography (HPLC) analysis sample.
Carbon nanotube described in test two is identical as the carbon nanotube in one step 1 of test, is purchased from Chinese science
Chengdu organic chemistry Co., Ltd of institute, OD:10nm~20nm, Length:10 μm~30 μm, Purith:>95wt%, Ash:<
1.5wt%.
Test three: defect state carbon nanotube prepared by test one is added separately to 10 unlike test two by this test
In a beaker equipped with organic pollutant to be processed.It is other identical as test two.
Test four: this test is Gan Jiangshui from the solvent unlike test three in beaker.It is other identical as test three.
Fig. 1 and Fig. 3 is the TEM figure for testing the carbon nanotube in one in step 1, and Fig. 2 and Fig. 4 are to test lacking for a preparation
The TEM figure of state carbon nanotube is fallen into, as can be seen from the figure carbon nanotube is through sulfuric acid and nitric acid oxidation, then under argon atmosphere,
By oxygen barrier its microscopic appearance of the carbon nanotube being mildly heat-treated there is no apparent variation occurs, this illustrates that carbon nanotube has
Stable " carbon nanotube-amorphous carbon " structure, calcining make carbon nanotube become defect state carbon nanotube.
Fig. 5 is XRD diagram, and curve 1 is the carbon nanotube tested in one in step 1, and curve 2 is the defect for testing a preparation
State carbon nanotube, as can be seen from the figure the strong diffraction maximum at 25.9 ° and the weak peak at 43.0 ° are respectively six sides of carbon nanotube
(002) and (111) of graphite-structure is reflected.It is heat-treated no significant change XRD diagram at 1000 DEG C, shows that stablizing for CNT is brilliant
Body structure.
Fig. 6 is Raman figure, and curve 1 is the carbon nanotube tested in one in step 1, and curve 2 is to test lacking for a preparation
State carbon nanotube is fallen into, as can be seen from the figure feature D band (1319cm-1) and G band (1580cm-1), the intensity ratio of D band and G band
(ID/IG) it can be used for assessing the defect level of carbon material.The defect of one preparation of carbon nanotube and test in test one in step 1
The I of state carbon nanotubeD/IGValue is respectively 0.8285,1.3707.It can be found that the defect level of carbon nanotube is in low-level.And
And pre-oxidation and heat treatment can increase the defect in carbon nano tube surface.
Fig. 7 is the defect state carbon nanotube selective oxidation degradation figure for testing three, the organic pollutant of abscissa from a left side to
The right side is followed successively by phenol, 4- chlorophenol, 2,4- Dichlorophenol, 4- sylvan, 4- amino phenols, resorcinol, hydroquinone, benzoic acid, right
Phenol formic acid and 4- nitrophenols, as can be seen from the figure each organic pollutant declines in the system of defect state carbon nanotube@PMS
The effect of solution has very big difference, and pseudo- First order kinetic constant is respectively 0.0706min-1, 0.1263min-1, 0.1629min-1, 0.1276min-1, 0.1466min-1, 0.0282min-1, 0.0294min-1, 0.0065min-1, 0.0071min-1With
0.0098min-1.Obviously, the aromatic compound of the system degradation different substituents of defect state carbon nanotube@PMS has difference
Degradation effect, this selective catalytic oxidation is heavily dependent on ionization potential (IP), the electron with substituent group
Ability/electron-withdrawing ability is strongly related.Aromatic compound with electron donating group, as methyl and amide groups usually have compared with
Low IP value and tend to be oxidized；And the aromatic hydrocarbons with electron-withdrawing group, as nitro and carboxyl are shown significantly reversely
Performance.
Test five: defect state carbon nanotube, cobalt nitrate and ferrous sulfate prepared by test one are added separately to 3 and are equipped with
In the beaker of organic pollutant solution to be processed, the organic pollutant in 3 beakers is 4- chlorophenol, and solvent is Gan Jiangshui；3
The concentration of organic pollutant is 0.16mM in a beaker, defect state carbon nanotube in 3 beakers, cobalt nitrate and ferrous sulfate
Concentration is 8.33mmol/L, 3 beakers ultrasound 5min；3 beakers are placed on magnetic stirring apparatus and are stirred respectively, it is past
The PMS aqueous solution that 500 μ L concentration are 50mmol/L is respectively added in 3 beakers；Respectively 3 jar agitation 1min, 3min,
It is sampled when 5min, 10min, 25min, 40min and 60min, sample passes through 0.22 μm of glass fiber filter filtering respectively, takes filtering
Sample 1mL is placed in liquid phase bottle afterwards, is separately added into the quenching of 0.5mL methanol, (4 DEG C) of sample low temperature are saved；Using efficient liquid
Phase chromatography (HPLC) analyzes the concentration of 4- chlorophenol in sample.
Test six: defect state carbon nanotube prepared by test one, MnO, Fe2O3And Co3O44 are added separately to be equipped with
In the beaker of organic pollutant solution to be processed, the organic pollutant in 4 beakers is 4- chlorophenol, and solvent is Gan Jiangshui；4
The concentration of organic pollutant is 0.16mM, defect state carbon nanotube, MnO, Fe in 4 beakers in a beaker2O3And Co3O4's
Concentration is 0.1g/L, 4 beakers ultrasound 5min；4 beakers are placed on magnetic stirring apparatus and are stirred respectively, toward 4
The PMS aqueous solution that 500 μ L concentration are 50mmol/L is respectively added in beaker；Respectively 4 jar agitation 1min, 3min, 5min,
It is sampled when 10min, 25min, 40min and 60min, sample passes through 0.22 μm of glass fiber filter filtering respectively, takes sample after filtering
Product 1mL is placed in liquid phase bottle, is separately added into the quenching of 0.5mL methanol, (4 DEG C) of sample low temperature are saved；Using high-efficient liquid phase color
Compose the concentration of 4- chlorophenol in (HPLC) analysis sample.
Defect state carbon prepared by the test one of defect state carbon nanotube and 8.33mmol/L prepared by the test one of 0.1g/L
Nanotube is equivalent.
Fig. 8 is the degradation efficiency figure of organic pollutant, and curve 1 is the defect state carbon nanotube for testing a preparation, and curve 2 is
Co3O4, curve 3 is Co2+, curve 4 is Fe2O3, curve 5 is MnO, and curve 6 is Fe2+, as can be seen from the figure electric charge transfer mediates
Oxidation system have it is highly selective, can be by background common in water is organic and inorganic substances are interfered less with.Even if
The 4- chlorophenol that 92% is up in actual water body can be by defect state carbon nanotube@PMS system oxidative degradation.In contrast, it passes through
Allusion quotation Fe2+@PMS system (≈ 10%), Co2+@PMS system (≈ 40%), MnO@PMS system (≈ 15%), Fe2O3@PMS system
(≈ 20%) and Co3O4The free radical that@PMS system (≈ 45%) generates can only obtain very limited 4- chlorophenol degradation.These are enabled
The experimental result of people's excitement highlights defect state carbon nanotube@PMS oxidative system and repairs poisonous organic pollution in actual waste water
The huge efficiency in object space face.
Claims (5)
1. a kind of preparation method with defect state carbon nanotube, it is characterised in that the preparation method with defect state carbon nanotube
It carries out according to the following steps:
One, it prepares oxide/carbon nanometer tube: the concentrated sulfuric acid being uniformly mixed with concentrated nitric acid, obtains mixed acid；Carbon nanotube is added to
It in mixed acid, is placed in thermostat water bath, 3h~9h is reacted under conditions of 75 DEG C~80 DEG C, then with deionized water and anhydrous
Ethyl alcohol is washed to cleaning solution repeatedly and is in neutrality, and is finally dried under conditions of temperature is 60 DEG C~65 DEG C, is obtained carbonoxide nanometer
Pipe；The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3:1；The volume of the mixed acid and the mass ratio of carbon nanotube are
1L:(15g~17g)；
Two, it is heat-treated: oxide/carbon nanometer tube prepared by step 1 being placed in tube furnace, with 150mL/min~160mL/min's
Flow velocity leads to inert gas 20min to drain air, then with the guarantor of 3 DEG C/min~5 DEG C/min heating rate and inert gas
So that the temperature of tube furnace is risen to 600 DEG C~1100 DEG C from room temperature under shield, and is 600 DEG C~1100 DEG C and inert gas in temperature
Protection under anneal 2h~4h, finally cooled to room temperature under inert gas protection, obtains defect state carbon nanotube.
2. a kind of preparation method with defect state carbon nanotube according to claim 1, it is characterised in that in step 1
The mass percent of the concentrated sulfuric acid is 95%~98%.
3. a kind of preparation method with defect state carbon nanotube according to claim 1, it is characterised in that in step 1
The mass percent of the concentrated nitric acid is 65%~68%.
4. a kind of application with defect state carbon nanotube as described in claim 1, it is characterised in that have defect state carbon to receive
The organic pollutant of mitron being applied in catalysis potassium peroxymonopersulfate degradation water body.
5. a kind of application with defect state carbon nanotube according to claim 4, it is characterised in that organic dirt
Contaminating object is chlorophenols organic pollutant or sulfamido organic pollutant.
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| CN113617350A (en) * | 2021-08-11 | 2021-11-09 | 北京林业大学 | Defective carbon material and preparation method and application thereof |
| CN116328751A (en) * | 2023-03-28 | 2023-06-27 | 浙江大学 | Modified carbon catalyst and preparation method and application thereof |
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| CN109174074B (en) | 2021-06-08 |
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