CN101066758A - High nitrogen doped corrugated carbon nanotube material and its synthesis process - Google Patents
High nitrogen doped corrugated carbon nanotube material and its synthesis process Download PDFInfo
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Abstract
The present invention relates to high nitrogen doped corrugated carbon nanotube material and its synthesis process. The synthesis process includes the following steps: mixing Fe source and proper amount of distilled water, soaking porous molecular sieve to carry ferric oxide or ferrous oxide, stoving and roasting at 300-1000 deg.c for 0.5-24 hr to obtain catalyst; setting the catalyst inside a pipe furnace, leading organic amine into the furnace under the protection of Ar or N2 and reacting at 650-1000 deg.c for 0.2-4.0 hr to obtain high nitrogen doped corrugated carbon nanotube mixture containing the catalyst; soaking the mixture in proper amount of or excessive hydrofluoric acid, sulfuric acid, nitric acid or acid for 0.5-24 hr; and washing in distilled water, suction filtering and drying to obtain high nitrogen doped corrugated carbon nanotube material. The material has nitrogen content of 10-40 %, reinforced surface polarity, etc, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of high nitrogen doped corrugated carbon nanotube material and synthetic method.
Background technology
CNT (carbon nano-tube) is found a kind of carbon structure in 1991.Desirable CNT (carbon nano-tube) is seamless, the hollow tube body that is rolled into by the Graphene lamella that carbon atom forms.The lamella of Graphene generally can be from one deck to layers up to a hundred.What contain one deck Graphene lamella is called Single Walled Carbon Nanotube (SWNT), then is called multiple-wall carbon nanotube (MWNT) more than one deck.The diameter of SWNT is generally 1～6nm, and minimum diameter is approximately 0.5nm, but the diameter of SWNT is unstable especially later on greater than 6nm, and subsiding of SWNT pipe can be taken place, and length then can reach the hundreds of nanometer to several microns.The interlamellar spacing of MWNT is about 0.34 nanometer, and to tens nanometers, length is generally in micron dimension in several nanometers for diameter, and elder can reach several millimeters.Because CNT (carbon nano-tube) has bigger length-to-diameter ratio, is quasi-one-dimensional nanometer material so can regard it as.
The main preparation method method of CNT (carbon nano-tube) has arc process, pyrolysis method and laser evaporation method.Wherein arc process is in inert gas atmosphere, and two root graphite electrode direct-current discharges produce CNT (carbon nano-tube) on the negative electrode.Pyrolysis method adopts transition metal to make catalyzer exactly, and under the condition of 700～1600K, the decomposition by hydrocarbon polymer obtains CNT (carbon nano-tube).The laser ablation method adopts the graphite target in the laser ablation High Temperature Furnaces Heating Apparatus, and CNT (carbon nano-tube) just is present in the graphite evaporate that rare gas element carries secretly.The main drawback of above-mentioned three kinds of methods is: what obtain is the pure nano-carbon tube material, wetting ability extreme difference, load and bad dispersibility.
The Theoretical Calculation work of research nitrogen-doped carbon material both at home and abroad appears in the newspapers; Synthetic nitrogen modification carbon material is a film like, and the purpose of research is to be used for improving its hardness and to obtain Electronic Performance preferably, and synthetic method is carbon material electrion or laser ablation under nitrogen atmosphere; This method complicated operation, the cost height, and material is a film like.
It is a kind of nitrating bamboo-like carbon nano tubes of raw material with the metal phthalocyanine that patent CN1401560A discloses, and its nitrogen content is low, generally between 0.5～9%, and the nitrating bamboo-like carbon nano tubes cost height that produces, be not suitable for large-scale industrial production.The raising itrogen content of getter with nitrogen doped is the important channel with introducing to the market of carbon nanotube, the itrogen content of getter with nitrogen doped height can improve even obtain many new material behaviors, can effectively improve the surface charge density of carbon nanotube, strengthen surface polarity and surface alkalinty, other material of load or better with the mutual dispersing property of other material also has more important role at bioelectrode with aspect solid basic catalyst.Not seeing as yet at present both at home and abroad with simple organic amine molecule is that raw material obtains nitrogen content and is higher than high nitrogen doped corrugated carbon nanotube material of 10% and preparation method thereof.
Summary of the invention
Low in order to overcome existing nitrating bamboo-like carbon nano tubes nitrogen content, the working method complexity, shortcomings such as cost height, the present invention proposes a kind of high nitrogen doped corrugated carbon nanotube material and synthetic method, employing supports the sieve peg-raking catalyst of iron, simultaneously as carbon source and nitrogenous source, control reaction temperature obtains high nitrogen doped carbon nanotube with the higher organic amine of nitrogen content.Compared with the prior art, the present invention has adopted the mixture of single organic amine such as hexamethylenetetramine, methylamine or multiple organic amine as starting raw material, use on the molecular sieve and support moderate iron amount, can obtain itrogen content of getter with nitrogen doped under the suitable temperature greater than 10% high nitrogen doped carbon nanotube as better catalyst.The raw materials used wide material sources of the present invention, production technique is simple, is easy to large-scale production, and can adjust itrogen content of getter with nitrogen doped in the product according to the variant production needs.
High nitrogen doped corrugated carbon nanotube material and synthetic method is characterized in that: implementation step is as follows:
A) Preparation of Catalyst: source of iron is mixed with an amount of distilled water, porous molecular screen is supported ferric oxide or iron protoxide with dipping method; The oven dry back was 300～1000 ℃ of following roastings 0.5～24 hour;
B) synthetic method of high nitrogen doped corrugated carbon nanotube material: catalyzer is placed tube furnace, under argon or nitrogen protection, carry organic amine and import tube furnace, in 650～1000 ℃ of reactions 0.2～4.0 hour, obtain containing the high nitrogen doped corrugated carbon nanotube material of catalyzer;
C) remove catalyzer: with an amount of or excessive HF acid, sulfuric acid, nitric acid or hydrochloric acid soln, dipping 0.5～24h; Use suction filtration then, again with a large amount of distilled water cleanings, suction filtration; To obtain black solid at last and place 120 ℃ of baking ovens to remove moisture, do not contained the high nitrogen doped corrugated carbon nanotube novel material of catalyzer.
Described high nitrogen doped corrugated carbon nanotube material, before removing catalyzer, the mass ratio of high nitrogen doped corrugated carbon nanotube material and catalyzer is 0.10～5.0; After removing catalyzer, nitrogen content is 10～40% in the high nitrogen doped corrugated carbon nanotube material.
Described high nitrogen doped corrugated carbon nanotube material, the nitrogen carbon source that provides are following any or their mixture: hexamethylenetetramine, methylamine, ethamine, propylamine, quadrol, diethylamine, triethylamine, dipropyl amine, tripropyl amine, butylamine, hexylamine, hexahydroaniline, hexanediamine.
Porous molecular screen of the present invention be the micro porous molecular sieve that generally adopts in the prior art, mesoporous molecular sieve and in-micro porous molecular sieve; Source of iron comprises iron nitrate, ironic oxalate, Ferrox, freshly prepd ironic hydroxide or ferrous hydroxide precipitation.
Said high nitrogen doped corrugated carbon nanotube material is that its mole of removing in acid after catalyzer, the 120 ℃ of oven dry consists of xC:yN in the high nitrogen doped corrugated carbon nanotube novel material that catalysis method provided by the invention obtains; The value of x is 0.60～0.90, and the value of y is 0.10～0.40.X, y value are more preferably: x is 0.75～0.85, and y is 0.15～0.25.When above-mentioned materials contained catalyzer, the mass ratio of itself and catalyzer was 0.10～5.0.
The present invention has adopted catalysis method to synthesize high nitrogen doped corrugated carbon nanotube material, and its advantage is: (1) has strengthened the electric density and the polarity of carbon nanotube; (2) specific surface and interlamellar spacing have been significantly improved; (3) this material tentatively shows the new capability of super large charge/discharge capacity and efficient, considerably beyond the carbon nano-tube material of general method preparation, is suitable for being used as the raw material or the high-power electrode materials that discharges and recharges power supply of ultracapacitor; (4) catalysis process synthesis condition gentleness, raw material is cheap, be easy to get, and production technique is simple, is suitable for scale operation.
Description of drawings
Fig. 1 is TEM (transmission electron microscope) figure of many high nitrogen doped corrugated carbon nanotubes;
Fig. 2 is TEM (transmission electron microscope) figure of single high nitrogen doped corrugated carbon nanotube.
Fig. 1 synthetic material is the ring shape, caliber 30～60nm, joint length 30～50nm.
Fig. 2 synthetic material is the ring shape, and thickness of pipe 20nm, tube wall are the graphite linings that certain distortion is arranged.
Embodiment
Embodiment 1:10.25g is baked SBA-15 molecular sieve in 850 ℃ of high temperature airs, places the 5mL beaker; Claim 0.1g Fe (NO)
39H
2O is dissolved in the 1.2mL distilled water, then this solution impregnation is stirred to the SBA-15 molecular sieve, leaves standstill 12 hours; Placed 150 ℃ of oven for drying then 12 hours; Place the tube furnace of the band silica tube of Ar protection gas then, be warming up to 850 ℃, the 2mL diethylamine is gone into by catalyzer by the Ar protection band of gas, through finishing this process in 0.5 hour; Stop heating then, continue logical Ar protection gas to dropping to room temperature; Take out the black sample and be high nitrogen doped corrugated carbon nanotube material, C and N mol ratio are 0.85: 0.15.
Embodiment 2:1.0g is baked NaY molecular sieve in 700 ℃ of high temperature airs, places the 5mL beaker; Claim 0.25gFe (NO)
39H
2O is dissolved in the 1.2mL distilled water, then this solution impregnation is stirred to the SAPO-11 molecular sieve, leaves standstill 12 hours; Placed 150 ℃ of oven for drying then 12 hours, 300 ℃ of roastings are 24 hours in the air, reduce to room temperature naturally; Place the tube furnace of the band silica tube of nitrogen protection gas then, be warming up to 700 ℃, 2g hexamethylenetetramine and 0.05mL quadrol are gone into by catalyzer by the nitrogen protection band of gas, through finishing this process in 0.5 hour; Stop heating then, continue logical nitrogen protection gas to dropping to room temperature; Take out the black sample and be the high nitrogen doped corrugated carbon nanotube material that contains catalyzer, C and N mol ratio are 0.62: 0.38.
Embodiment 3:1.0g is baked SBA-15 molecular sieve in 850 ℃ of high temperature airs, places the 5mL beaker; Claim that 0.5g newly prepares Fe (OH)
2Stir with 5mL distilled water, this emulsion is impregnated on the SBA-15 molecular sieve stirs then, left standstill 12 hours; Placed 150 ℃ of oven for drying then 12 hours, 1000 ℃ of roastings are 0.5 hour in the air, reduce to room temperature naturally; Place the tube furnace of the band silica tube of Ar protection gas then, be warming up to 900 ℃, the 2mL diethylamine is gone into by catalyzer by the Ar protection band of gas, through finishing this process in 0.5 hour; Stop heating then, continue logical Ar protection gas to dropping to room temperature; Take out the black sample and be high nitrogen doped corrugated carbon nanotube material, C and N mol ratio are 0.88: 0.12.
Claims (3)
1. high nitrogen doped corrugated carbon nanotube material and synthetic method, it is characterized in that: step is as follows:
A) Preparation of Catalyst: source of iron is mixed with an amount of distilled water, porous molecular screen is supported ferric oxide or iron protoxide with dipping method, the oven dry back was 300～1000 ℃ of following roastings 0.5～24 hour;
B) synthetic method of high nitrogen doped corrugated carbon nanotube material: catalyzer is placed tube furnace, under argon (Ar) or nitrogen atmosphere, carry organic amine and import tube furnace, in 650～1000 ℃ of reactions 0.2～4.0 hour, can obtain containing the high nitrogen doped corrugated carbon nanotube material of catalyzer;
C) remove catalyzer: with an amount of or excessive HF acid, sulfuric acid, nitric acid or hydrochloric acid soln, dipping 0.5～24h; Use suction filtration then, again with a large amount of distilled water cleanings, suction filtration; To obtain black solid at last and place 120 ℃ of baking ovens to remove moisture, do not contained the high nitrogen doped corrugated carbon nanotube novel material of catalyzer.
2. high nitrogen doped corrugated carbon nanotube material according to claim 1 and synthetic method is characterized in that: before removing catalyzer, the mass ratio of high nitrogen doped corrugated carbon nanotube material and catalyzer is 0.10～5.0; After removing catalyzer, nitrogen content is 10～40% in the high nitrogen doped corrugated carbon nanotube material.
3. high nitrogen doped corrugated carbon nanotube material according to claim 1 and synthetic method is characterized in that: the nitrogen carbon source that provides is following any or their mixture: hexamethylenetetramine, methylamine, ethamine, propylamine, quadrol, diethylamine, triethylamine, dipropyl amine, tripropyl amine, butylamine, hexylamine, hexahydroaniline, hexanediamine.
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| CN102247869A (en) * | 2011-06-10 | 2011-11-23 | 广州大学 | Spherical nitrogen-doped carbon-supported non-noble metal oxygen reduction catalyst and preparation method thereof |
| CN102418068A (en) * | 2011-09-19 | 2012-04-18 | 天津师范大学 | Multi-walled carbon nanotube deposited with nano-carbon nitrogen film as well as preparation method and application thereof |
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