CN103072968A - Carbon nano composite and preparation method thereof - Google Patents
Carbon nano composite and preparation method thereof Download PDFInfo
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- CN103072968A CN103072968A CN2013100308573A CN201310030857A CN103072968A CN 103072968 A CN103072968 A CN 103072968A CN 2013100308573 A CN2013100308573 A CN 2013100308573A CN 201310030857 A CN201310030857 A CN 201310030857A CN 103072968 A CN103072968 A CN 103072968A
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Abstract
The invention relates to a carbon nano composite and a preparation method thereof. The carbon nano composite comprises a carbon nano material and metal particles, wherein the carbon nano material is subjected to surface functionalization, and the metal particles are formed on the carbon nano material. The carbon nano composite can be used for removing pollutants in waste water, and a removal effect is significantly better than that of the existing nano material.
Description
Technical field
The present invention relates to carbon nano-composite material and preparation method thereof.
Background technology
Carbon nanomaterial has unique structure because of it and excellent electricity, optics, thermodynamic property and mechanical property is widely used in a plurality of fields such as electrode, stored energy, support of the catalyst, filtration unit.When carbon material and metal or metal oxide are combined with each other, can be used as again magneticsubstance, catalyzer and chemical sensor etc.
The method for preparing at present carbon nanomaterial mainly comprises arc discharge method, Laser vaporization, chemical Vapor deposition process.Wherein arc discharge method and Laser vaporization are because of apparatus expensive, consume energy high, the drawbacks limit such as impurity in products is many its application in industrial production, chemical Vapor deposition process in preparation carbon nanotube process, need at first use reducing gas under hot conditions with catalyst reduction out, and easily produce carbon granule in the preparation process, the impurity such as decolorizing carbon and have certain problem.The standby carbon material of solid-state pyrolysis Organometallic precursor legal system prepares simple because of it and the productive rate high becomes in recent years people's study hotspot.The people such as Zhi deliver many pieces of articles and have reported the application of solid-state pyrolysis organometallic complex in preparation carbon nanotube and nanocarbon/metal nano composite material.Such as document small2005,1:210 – 212, small2005,1:798 – 801, Adv.Mater.2008,20:1727 – 1731 etc.Yet the precursor that adopts in the aforesaid method is complicated organometallic complex, and the precursor preparation process is complicated, and the use of organic reagent is harmful to environment, and temperature required height in the pyrolytic process, time are long.
In addition, because the consistency of carbon nanotube extreme difference and dispersiveness easily produce from winding or agglomeration it, thereby limited its practical application.For this reason, people are by direct fluoridation, acidification reaction, free radical reaction, the several different methods such as electrochemical reaction are carried out modification to carbon nano tube surface, but aforesaid method all exists reactions steps loaded down with trivial details in various degree, and reaction time is long, cost is high, environmental-protecting performance is poor, the functionalization degree is low, the carbon nanotube inherent structure is destroyed large and is not suitable for the problem such as scale operation.
Layered double hydroxide (Layered Double Hydroxide is referred to as hydrotalcite), general formula is [M
2+ 1-xM
3+ x(OH)
2]
X+A
N- X/nMH
2O, wherein M
2+, M
3+Represent respectively divalence and trivalent metal cation, A
N-Represent the commutative negatively charged ion of interlayer.Such material is a kind of metal catalyst for preparing, effective precursor of support of the catalyst.The people such as Sun take dodecyl sodium sulfonate root intercalation cobalt aluminum hydrotalcite as precursor one the step pyrolysis prepared carbon nano ring (Adv.Mater.2012, DOI:10.1002/adma.201203108).The people such as Xu take terephthalic acid intercalation cobalt magnesium aluminum-hydrotalcite as precursor one the step pyrolysis prepared carbon nano-particles/metal oxide nano composite material (Nano Lett., 2001,1:703-706).Contain transition metal with laminate, interlayer is that the organic anion intercalated houghite is that precursor prepares the concern that carbon material has caused people.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or provides at least a kind of useful commerce to select.
In one aspect of the invention, it comprises to the present invention proposes a kind of carbon nano-composite material: carbon nanomaterial, and described carbon nanomaterial is by surface-functionalized; And metallic particles, described metallic particles is formed on the described carbon nanomaterial.This carbon nano-composite material can be used for removing the pollutent of waste water, the removal Congo red such as azoic dyestuff, and removal effect is significantly higher than existing nano material.The contriver finds, 30mg is joined 50ml according to the carbon nano-composite material of the embodiment of the invention, in the Congo red solution of 100ppm, 10min be adsorbable fully, this moment, adsorptive capacity was 167mg/g, and the adsorptive capacity that can obtain maximum by increasing Congo red strength of solution is 880mg/g.
According to embodiments of the invention, above-mentioned carbon nano-composite material can also have following additional technical feature one of at least:
According to embodiments of the invention, the surface of described carbon nanomaterial carries-OH and-COO-functional group.
According to embodiments of the invention, described metallic particles be selected from Co, Ni, Fe, Cu metal simple-substance or consisting of group that alloy forms at least a, and be selected from least a of Mg, Zn, Al group that oxide compound forms.
According to embodiments of the invention, described carbon nanomaterial is the form of multi-walled carbon nano-tubes, described metal simple-substance or alloying pellet be formed in the pipe of described multi-walled carbon nano-tubes and tube head one of at least.
According to embodiments of the invention, described carbon nanomaterial is the form of carbon nanometer layer, and described metal simple-substance or alloying pellet are coated on described carbon nanometer layer.According to embodiments of the invention, when adopting this clad structure, this carbon-clad metal simple substance or alloying pellet randomly are scattered among metal oxide.
In a second aspect of the present invention, the present invention proposes a kind of method for preparing carbon nano-composite material.According to embodiments of the invention, the method comprises: a) form the salicylate intercalation layered metal hydroxides precursor that laminate contains transition metal; And b) described precursor is carried out roasting, in order to obtain described carbon nano-composite material, wherein, described carbon nano-composite material comprises: carbon nanomaterial, and described carbon nanomaterial is by surface-functionalized; And metallic particles, described metallic particles is formed on the described carbon nanomaterial.Utilize the method can effectively prepare foregoing carbon nano-composite material.
According to embodiments of the invention, the above-mentioned method for preparing carbon nano-composite material can also have following additional technical feature one of at least:
According to embodiments of the invention, at least a preparation in the described salicylate intercalation of step a) layered metal hydroxides precursor employing coprecipitation method, hydrothermal method, roasting restoring method, the ion exchange method.Wherein, reaction pH scope is 6.5-8.5 in coprecipitation method and the hydrothermal method, and the crystallization temperature scope is room temperature-100 ℃.According to a concrete example of the present invention, with metal salt solution, alkaline solution and Whitfield's ointment salt solution mix, and be lower than under 100 degrees centigrade the temperature, carry out crystallization and process, in order to obtain the salicylate intercalation layered metal hydroxides precursor that this laminate contains metallic element.
According to embodiments of the invention, described metal-salt is be selected from metal nitrate, metal sulfate and metal chloride at least a, described salicylate preferably water poplar acid sodium and potassium salicylate.
According to embodiments of the invention, described alkaline solution is be selected from NaOH, KOH, urea at least a.
According to embodiments of the invention, described precursor is carried out roasting comprises:
Described precursor is placed tube-type atmosphere furnace, in nonoxidizing atmosphere, behind 500 ℃～1000 ℃ roasting 0.2h～10h, naturally be cooled to room temperature.Preferably, contain the Co element system for laminate, maturing temperature is 600-1000 degree centigrade, and roasting time is 1h-10h, and laminate contains the Ni element system, and maturing temperature is 500-1000 degree centigrade, and roasting time is 0.2h-10h.
According to embodiments of the invention, described nonoxidizing atmosphere is made of at least a of hydrogen, rare gas element.
According to embodiments of the invention, described rare gas element is for being selected from N
2, He or Ar at least a.
In a third aspect of the present invention, the present invention also proposes the purposes of above-mentioned carbon nano-composite material.
Technological method of the present invention can have following advantages one of at least:
1, according to embodiments of the invention; the used layered hydroxide precursor of preparation carbon nano-composite material has even structure; but form modulation; preparation process is simple, can be applicable to the characteristics such as industrial scale production, and the salicylate that carbon source is provided is organic molecule; degradation production is single; be conducive to prepare the high purity carbon material, and raw material is easy to get environmentally safe.
2, according to embodiments of the invention, because what adopt is the layered hydroxide presoma, the dispersion of its laminate metallic element atomic level makes that metal has higher catalytic activity in its product of roasting, thereby effectively reduce the temperature of carbon nano-tube matrix material in the pyrolytic process, and greatly shortened roasting time.
3, according to embodiments of the invention, the carbon nanotube for preparing/metal nanometer composite material even structure, purity is high, can be mass-produced, and has realized that it is surface-functionalized without one step of any chemically modified.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the X ray crystalline diffraction spectrogram of cobalt aluminium lamination shape oxyhydroxide precursor of the salicylate intercalation of the embodiment of the invention 1 preparation;
Fig. 2 is the stereoscan photograph of the carbon nanotube/metal nanometer composite material of the embodiment of the invention 1 preparation;
Fig. 3 is the XRD spectra of the carbon nanotube/metal nanometer composite material of the embodiment of the invention 1 preparation;
Fig. 4 is the fourier-transform infrared data of the carbon nanotube/metal nanometer composite material of the embodiment of the invention 1 preparation.
Embodiment
The below describes embodiments of the invention in detail, and these embodiment are exemplary, is intended to for explanation the present invention, and can not be interpreted as limitation of the present invention.In addition, unless stated otherwise, below the starting material and the equipment that adopt be commercially available.
Embodiment 1:
Steps A: the Co (NO that takes by weighing 11.64g
3)
26H
2Al (the NO of O and 7.5g
3)
39H
2O adds deionized water and is configured to the 50ml mixing solutions, and the sodium salicylate that other takes by weighing 12.81g is dissolved in the 100mL deionized water, takes by weighing 8g NaOH adding deionized water and is configured to the alkaline solution that 100mL concentration is 2M.Under mechanical stirring mixing salt solution and NaOH solution are added drop-wise in the sodium salicylate solution simultaneously, it is 7 that the dropping process keeps pH value of solution, the gained slurries are transferred in the autoclave, and at 100 ℃, crystallization 24 hours.After crystallization finishes, treat that temperature drops to room temperature, with deionized water wash, centrifugal 4 times, in 60 ℃ lower dry 12 hours, obtain the cobalt aluminum hydrotalcite presoma of salicylate intercalation.
Step B: take by weighing 1.5g hydrotalcite precursor after the grinding, evenly divide in porcelain boat and place tube furnace, at N
2In the atmosphere, gas cross section flow 40ml/cm
2Be warming up to 600 ℃ with 5 ℃/min under the condition of min, be incubated 2 hours.Detect through SEM and TEM, the gained pyrolysis product is the matrix material of multi-walled carbon nano-tubes and cobalt, wherein length of carbon nanotube is about 1 μ m, diameter is about 24nm, cobalt metal mainly is arranged in tube head and the caliber of carbon nanotube, characterize discovery through FT-IR, this composite material surface is with the carboxyl of hydroxyl and deprotonation.It the results are shown among Fig. 1-4.
Wherein, Fig. 1 is the X ray crystalline diffraction spectrogram of cobalt aluminium lamination shape oxyhydroxide precursor of the salicylate intercalation of the present embodiment preparation; Fig. 2 is the stereoscan photograph of the carbon nanotube/metal nanometer composite material of the present embodiment preparation, shows that the product pattern that obtains is the carbon nanotube of even structure; Fig. 3 is the XRD spectra of the carbon nanotube/metal nanometer composite material of the present embodiment preparation, shows that the product that obtains is the nano composite material of carbon nanotube and metal Co; Fig. 4 is the fourier-transform infrared data of the carbon nanotube/metal nanometer composite material of the present embodiment preparation, shows that the carbon nano tube surface that obtains with a large amount of hydroxyls and carboxyl, is functionalized carbon nano-tube.
Embodiment 2:
Steps A: the Ni (NO that takes by weighing 11.63g
3)
26H
2Al (the NO of O and 7.5g
3)
39H
2O adds deionized water and is configured to the 50ml mixing solutions, and the sodium salicylate that other takes by weighing 12.81g is dissolved in the 100mL deionized water, takes by weighing 8g NaOH adding deionized water and is configured to the alkaline solution that 100mL concentration is 2M.Under mechanical stirring mixing salt solution and NaOH solution are added drop-wise in the sodium salicylate solution simultaneously, it is 7 that the dropping process keeps pH value of solution, the gained slurries are transferred in the autoclave, and at 100 ℃, crystallization 24 hours.After crystallization finishes, treat that temperature drops to room temperature, with deionized water wash, centrifugal 4 times, in 60 ℃ lower dry 12 hours, obtain the nickel aluminum hydrotalcite presoma of salicylate intercalation.
Step B: take by weighing 1.5g hydrotalcite precursor after the grinding, evenly divide in porcelain boat and place tube furnace, at N
2In the atmosphere, flow area flow 60ml/cm
2Be warming up to 500 ℃ with 5 ℃/min under the condition of min, be incubated 2 hours.Detect through SEM and TEM, the gained pyrolysis product is the nanocarbon/metal nano composite material that surface coverage has a large amount of multi-walled carbon nano-tubes, and wherein length of carbon nanotube is about 400nm, and caliber is about 25nm, characterize discovery through FT-IR, this composite material surface is with the carboxyl of hydroxyl and deprotonation.
Embodiment 3:
Steps A: the Co (NO that takes by weighing 11.64g
3) 26H
2Al (the NO of O and 7.5g
3)
39H
2O adds deionized water and is configured to the 50ml mixing solutions, and the sodium salicylate that other takes by weighing 12.81g is dissolved in the 100mL deionized water, takes by weighing 8g NaOH adding deionized water and is configured to the alkaline solution that 100mL concentration is 2M.Under mechanical stirring mixing salt solution and NaOH solution are added drop-wise in the sodium salicylate solution simultaneously, it is 7 that the dropping process keeps pH value of solution, the gained slurries are transferred in the autoclave, and at 100 ℃, crystallization 24 hours.After crystallization finishes, treat that temperature drops to room temperature, with deionized water wash, centrifugal 4 times, in 60 ℃ lower dry 12 hours, obtain the cobalt aluminum hydrotalcite presoma of salicylate intercalation.
Step B: take by weighing 1.5g hydrotalcite precursor after the grinding, evenly divide in porcelain boat and place tube furnace, at N
2/ H
2In the atmosphere, flow area flow 60ml/cm
2Be warming up to 600 ℃ with 5 ℃/min under the condition of min, be incubated 2 hours.Detect through SEM and TEM, the gained pyrolysis product is the matrix material of multi-walled carbon nano-tubes and cobalt, wherein length of carbon nanotube is about 2 μ m, diameter is about 27nm, cobalt metal mainly is arranged in tube head and the caliber of carbon nanotube, characterize discovery through FT-IR, this composite material surface is with the carboxyl of hydroxyl and deprotonation.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or the example in conjunction with specific features, structure, material or the characteristics of this embodiment or example description.In this manual, the schematic statement of above-mentioned term not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or characteristics can be with suitable mode combinations in any one or more embodiment or example.
Although the above has illustrated and has described embodiments of the invention, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art is not in the situation that break away from principle of the present invention and aim can change above-described embodiment within the scope of the invention, modification, replacement and modification.
Claims (8)
1. a carbon nano-composite material is characterized in that, comprises:
Carbon nanomaterial, described carbon nanomaterial is by surface-functionalized; And
Metallic particles, described metallic particles is formed on the described carbon nanomaterial.
2. carbon nano-composite material according to claim 1 is characterized in that, the surface of described carbon nanomaterial carries-OH and-COO-functional group.
3. carbon nano-composite material according to claim 1, it is characterized in that, described metallic particles be selected from Co, Ni, Fe, Cu metal simple-substance or consisting of group that alloy forms at least a, and randomly be selected from least a of Mg, Zn, Al group that oxide compound forms.
4. carbon nano-composite material according to claim 1 is characterized in that, described carbon nanomaterial is the form of multi-walled carbon nano-tubes, described metal simple-substance or alloying pellet be formed in the pipe of described multi-walled carbon nano-tubes and tube head one of at least; Perhaps
Described carbon nanomaterial is the form of carbon nanometer layer, and described metal simple-substance or alloying pellet are coated on described carbon nanometer layer, and wherein, randomly, carbon-clad metal simple substance or alloying pellet are scattered among the metal oxide.
5. a method for preparing carbon nano-composite material is characterized in that, comprising:
A) form the salicylate intercalation layered metal hydroxides precursor that laminate contains transition metal; And
B) described precursor is carried out roasting, in order to obtain described carbon nano-composite material,
Wherein,
Described carbon nano-composite material comprises:
Carbon nanomaterial, described carbon nanomaterial is by surface-functionalized; And
Metallic particles, described metallic particles is formed on the described carbon nanomaterial.
6. the method for preparing carbon nano-composite material according to claim 5 is characterized in that,
The described salicylate intercalation of step a) layered metal hydroxides precursor is to adopt at least a preparation in coprecipitation method, hydrothermal method, roasting restoring method, the ion exchange method,
Wherein, reaction pH scope is 6.5-8.5 in described coprecipitation method and the hydrothermal method, and the crystallization temperature scope is room temperature-100 ℃,
Randomly, with metal salt solution, alkaline solution and Whitfield's ointment salt solution mix, and be lower than under 100 degrees centigrade the temperature, carrying out crystallization and process, in order to obtain the salicylate intercalation layered metal hydroxides precursor that described laminate contains metallic element.
7. the method for preparing carbon nano-composite material according to claim 6, it is characterized in that, described metal-salt is be selected from metal nitrate, metal sulfate and metal chloride at least a, described salicylate preferably water poplar acid sodium and potassium salicylate, described alkaline solution are be selected from NaOH, KOH, urea at least a.
8. the method for preparing carbon nano-composite material according to claim 6 is characterized in that, described precursor is carried out roasting comprise:
Described precursor is placed tube-type atmosphere furnace, in nonoxidizing atmosphere, behind 500 ℃～1000 ℃ roasting 0.2h～10h, naturally is cooled to room temperature,
Wherein, described nonoxidizing atmosphere is made of at least a of hydrogen, rare gas element.
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| CN103979529A (en) * | 2014-06-04 | 2014-08-13 | 北京化工大学 | Preparation method of porous carbon material and application of porous carbon material as electrode material |
| CN104801303A (en) * | 2015-05-07 | 2015-07-29 | 北京化工大学 | Copper/carbon nano composite catalyst and preparation method thereof |
| CN104860337A (en) * | 2015-05-06 | 2015-08-26 | 北京化工大学 | High pressure intercalation assembly method and application in preparation field of intercalation structure composite material |
| CN104923154A (en) * | 2015-05-07 | 2015-09-23 | 北京化工大学 | Hexagonal sheet magnetic metal/metal oxide/carbon nanocomposite adsorbing material and preparation method therefor |
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| CN105924174A (en) * | 2016-04-26 | 2016-09-07 | 武汉大学 | Preparation method of carbon-based composite material |
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| CN110203904A (en) * | 2019-06-06 | 2019-09-06 | 东北大学 | It is used to prepare the precursor material and method of nanostructured carbon material |
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| CN104860337B (en) * | 2015-05-06 | 2017-02-01 | 北京化工大学 | High pressure intercalation assembly method and application in preparation field of intercalation structure composite material |
| CN104860337A (en) * | 2015-05-06 | 2015-08-26 | 北京化工大学 | High pressure intercalation assembly method and application in preparation field of intercalation structure composite material |
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| CN105772708A (en) * | 2016-03-10 | 2016-07-20 | 合肥工业大学 | Method for using biomass waste for preparing nitrogen-doped carbon nanotube coated metal particle composite material |
| CN105924174A (en) * | 2016-04-26 | 2016-09-07 | 武汉大学 | Preparation method of carbon-based composite material |
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