CN1792432A - Method for preparing carbon nanometer material carried with noble metal(S) - Google Patents
Method for preparing carbon nanometer material carried with noble metal(S) Download PDFInfo
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Abstract
A process for preparing the nano-carbon material carrying noble metal includes such steps as adding nano-carbon material, compound of noble metal and surfactant to water and/or organic solvent, stirring, centrifugal separation, and drying. It has unique catalytic, optical, electric, thermal and mechanical performance.
Description
Technical field: the preparation method who the present invention relates to the carbon nanomaterial of a kind of Preparation Method of carbon nanomaterial of modification, particularly carried noble metal.
Background technology: nano science is often referred at nano-scale (10
-10-10
-7M) knowledge of natural environment, nature remodeling and create the science and technology (" carbon nanomaterial " of novel substance, new construction, new material, new unit and new system in the scope, Liu Jiping, Sun Hongqiang write, Science Press, 2004, chapter 1, book number: ISBN7-03-010612-1).Owing to have small-size effect, quantum size effect, skin effect and macro quanta tunnel effect, nano material shows physics, the chemical property of many uniquenesses, make it wide application prospect be arranged, and may in the next-generation technology innovation, play central role in fields such as electronics, machinery, medicine, the energy, environmental protection.In addition, be that the organic matter of main skeleton has not only been constructed life itself with carbon, and also suitable that this world is colourful.For this reason, the research of carbon nanomaterial and further using seems and is even more important.Discovered in recent years or the main carbon nanomaterial that grows up have fullerene, CNT, carbon nano-fiber, Nano diamond, Nano carbon balls, onion shape and taper carbon nanometer body.Wherein the appearance of CNT makes that especially the research of nano science is in the ascendant.CNT can be thought a kind of curling graphite flake structure.The sheet number of plies according to its composition, generally be divided into SWCN (singlewalled carbon nanotubes, SWCNTs), double-walled carbon nano-tube (doublewalled carbon nanotubes, DWCNTs) and multi-walled carbon nano-tubes (Multiwalled carbonnanotubes, MWCNTs).
Precious metal element refers to gold, silver, palladium, platinum, rhodium, ruthenium, iridium, eight kinds of elements of osmium.Form and the conduction conductivity of heat owing to have chemical stability and specific electron energy level, precious metal material is widely applied already in fields such as catalysis, electrode, ornament craft product.Generally there are two kinds of methods from precious metal chemical complex, to prepare corresponding precious metal material.The one, chemical method, promptly by chemical reducing agent or electrochemical reduction, chemical combination attitude noble metal is reduced to simple substance attitude metal, and (JACS 127 (30): 10639-10647).The 2nd, the physics method promptly by x ray irradiation x, ultrasonic or ultraviolet lighting processing, obtains simple substance attitude metal material (Nano Letters, 2003,3 (3): 279-282) from chemical combination attitude noble metal.The present invention will provide another kind of method, promptly directly prepare noble metal with nano-carbon material.Cost is low, and step is few, and is easy to operate, easy to control.Therefore, the present invention is with its called after " carbon method ".
Compound or hydridization can be prepared new material or improve the combination property of original material with two kinds of materials.In view of unique premium properties of carbon nanomaterial and noble metal, two kinds of materials are combined the interest that the carbon nanomaterial for preparing carried noble metal has caused science and industrial quarters.This hybrid material is general to adopt two kinds of strategies to prepare.The one, physisorphtion promptly by Electrostatic Absorption, is adsorbed onto carbon surface with the noble metal granule that has prepared.Utilize this method, gold colloid particles is adsorbed onto carbon nano tube surface, obtained CNT (Nano Letters, 2003,3 (3): 279-282) of golden load.The 2nd, chemical reduction method, promptly with the surface active groups in-situ reducing of chemical reducing agent or modification material with carbon element, with noble metal granule " growth " in carbon surface.Obviously, these two kinds of methods all exist shortcoming and defect.The former must at first prepare the noble metal granule of surface charging lotus; The latter then must use additional reducing agent, cost height, complex process.
Summary of the invention: the present invention seeks to need not any additional reducing agent or the situation of special sound, light, electric treatment under, carbon nanomaterial is mixed with noble metal compound solution, directly prepare the carbon nanomaterial of carried noble metal.
The carbon nanomaterial of carried noble metal of the present invention is made up of carbon nanomaterial and noble metal granule, and wherein the noble metal granule size accounts for 0.5-98wt% in 1 nanometer to 5 micron in the carbon nanomaterial of carried noble metal.
The carbon nanomaterial of carried noble metal of the present invention is to be raw material with carbon nanomaterial or its surface modification body and precious metal chemical complex, directly prepares the nano-carbon material of a series of carried noble metals.
Concrete preparation method is as follows for the carbon nanomaterial of carried noble metal of the present invention:
The carbon nanomaterial of 1 weight portion or its surface modification body and 0.1-10000 weight portion precious metal chemical complex mix in the mixed solvent of 0.1～50 weight parts water, organic solvent or water and organic solvent, after stirring 5 minutes to 120 hours under 0-150 ℃, through centrifugation, drying, obtain the carbon nanomaterial of carried noble metal, wherein water is 1/0.1-1/1000 with the volume of organic solvent ratio in the mixed solvent.
The used carbon nanomaterial of the present invention is selected from and is nano level carbon particulate, carbon ball, carbon-point, carbon pipe, SWCN, double-walled carbon nano-tube, multi-walled carbon nano-tubes, carbon film, carbon fiber, taper material with carbon element, block carbon material, arc material with carbon element, onion shape material with carbon element, polyhedron material with carbon element, reticulated carbon material, porous carbon materials or fullerene at least one dimension.
The surface modification body of the carbon nanomaterial that the present invention is used is selected from through chemistry, ultrasonicly involve plasma treated carbon nanomaterial, wherein the carbon nanomaterial of chemical treatment comprises with oxidant such as nitric acid, sulfuric acid, potassium permanganate, the carbon nanomaterial that hydrogen peroxide and composition thereof was handled, organic molecule, metal complex, the carbon nanomaterial that the surfactant valency connects or adsorbs, the carbon nanomaterial of polymer macromolecule grafting or absorption, polypeptide, protein, DNA, RNA, polysaccharide, carbon nanomaterial or its mixture that cellulosic molecule connects or adsorbs.
The used precious metal chemical complex of the present invention is selected from gold trichloride, tetra chlorauric acid, gold hydroxide, potassium chloroaurate, ammonium chloraurate, sodium chloraurate, potassium auricyanide, silver nitrate, silver acetate, chloroplatinic acid, ammonium chloroplatinate, potassium chloroplatinate, dinitroso diammonia platinum, potassium chloroplatinite, ammonium chloroplatinite, platinum nitrate, cis-platinum, platinic sodium chloride, dintrile phenyl platinous chloride, the triphenylphosphine platinum chloride, rhodium chloride, the acid of chlorine rhodium, rhodium sulfate, dimerization acetic acid rhodium, the acetic acid rhodium, rhodium nitrate, chlorine rhodium acid potassium, chlorine rhodium acid ammonium, the triphenylphosphine radium chloride, triphenylphosphine bromination rhodium, triphenylphosphine carbonyl radium chloride, ruthenium trichloride, the triphenylphosphine ruthenic chloride, the carbonyl ruthenic chloride, ruthenium hydrochloride potassium, ruthenium hydrochloride sodium, the ruthenium hydrochloride ammonium, chloro-iridic acid, iridous chloride, acetic acid iridium, ammonium chloroiridate, potassium hexachloroiridate, iridium sodium chloride, palladium nitrate, palladium, palladium bichloride, palladium sulfate or its mixture.
The used organic solvent of the present invention is selected from methyl alcohol, ethanol, propyl alcohol, butanols, dimethyl sulfoxide (DMSO), N, dinethylformamide, N, N-dimethylacetylamide, N-N-methyl-2-2-pyrrolidone N-, oxolane, acetate, acetone, butanone, acetonitrile, chloroform, triethylamine, pyridine, dimethylamino pyridine or its mixture.
The structure of the carbon nanomaterial of the carried noble metal of gained of the present invention and pattern disperse analyses signs such as spectrum (EDS), electronic diffraction (ED), X-ray diffraction, Raman spectrum, infrared spectrum, heat analysis to obtain conclusive evidence through transmission electron microscope (TEM), SEM (SEM), scanning transmission electron microscope (STEM), energy.
Prepare the carbon nanomaterial of carried noble metal according to the present invention, need not additional reducing agent, cost is low, the reaction condition gentleness, and processing step is few, and controllability is good, and is simple to operate, is fit to prepared in laboratory and production in enormous quantities.Prepared hybrid nano-material has unique catalysis, optics, electricity, calorifics and mechanical property, the suitable efficient catalytic material of doing, the body or the additive of high-strength special type material, high performance membrane material, high tensile strength fibrous material, absorbing material, at nano-catalytic, electrode, battery, fields such as special optical, electricity, mechanics and the energy absorbing material value that has a wide range of applications.
Description of drawings:
Fig. 1: the TEM figure of the SWCN of gold particle load
Fig. 2: the TEM figure of the multi-walled carbon nano-tubes of gold particle load
Fig. 3: the TEM figure of the multi-walled carbon nano-tubes of silver particles load
Fig. 4: the STEM figure of the multi-walled carbon nano-tubes of silver particles load
Fig. 5: the TEM figure of the SWCN of silver particles load
The specific embodiment: the following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the 0.1g SWCN, and 100mL water, after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 150mL, (20-25 ℃) stirred 5 minutes under the room temperature.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the SWCN of golden nanometer particle load.The size of golden nanometer particle is 3-20nm.
Embodiment 2: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the 0.1g SWCN, and 100mL water, after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 150mL, (20-25 ℃) stirred 50 hours under the room temperature.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the SWCN of gold particle load.The size of gold particle is 50nm-800nm.
Embodiment 3: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the 0.1g SWCN, and 100mL water, after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 150mL, (20-25 ℃) stirred 120 hours under the room temperature.Repeatedly centrifugation, remove solution after, the solid that obtains obtains the SWCN of bulky grain gold particle load through vacuum drying.The size of gold particle is 100nm-5 μ m.
Embodiment 4: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the 0.1g multi-walled carbon nano-tubes, and 100mL water, after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 150mL, (20-25 ℃) stirred 24 hours under the room temperature.Repeatedly centrifugation, remove solution after, obtain solid through vacuum drying, obtain the multi-walled carbon nano-tubes of gold particle load.The size of gold particle is 30nm-200nm.Fig. 1 is the TEM photo of the multi-walled carbon nano-tubes of the gold particle load that obtains of present embodiment.
Embodiment 5: in the 500mL round-bottomed flask, adds the 6g multi-walled carbon nano-tubes, adds 60% red fuming nitric acid (RFNA) 60mL, and concentrated sulfuric acid 180mL, the strong agitation reaction is 100 minutes under the 90-135 ℃ of oil bath.Through washing, suction filtration repeatedly, centrifugation obtains the multi-walled carbon nano-tubes 3.5g of oxidation.
In the 500mL boiling flask that the magnetic agitation rotor is housed, add the multi-walled carbon nano-tubes of 0.1g oxidation, 100mL water, after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 150mL, (20-25 ℃) stirred 30 hours under the room temperature.Repeatedly centrifugation, remove solution after, solid obtains the multi-walled carbon nano-tubes of gold particle load through vacuum drying.The size of gold particle is 40nm-300nm.
Embodiment 6: in the 500mL round-bottomed flask, adds the 2g SWCN, adds 60% red fuming nitric acid (RFNA) 20mL, and 98% concentrated sulfuric acid 60mL, the strong agitation reaction is 100 minutes under the 90-135 ℃ of oil bath.Through washing, suction filtration repeatedly, centrifugation obtains the SWCN 1.1g of oxidation.
In the 500mL boiling flask that the magnetic agitation rotor is housed, add the SWCN of 35mg oxidation, 100mL water, after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 80mL, (20-25 ℃) stirred 24 hours under the room temperature.Repeatedly centrifugation, remove solution after, solid obtains the SWCN of gold particle load through vacuum drying.The size of gold particle is 50nm-800nm.Fig. 2 is the corresponding TEM photo of the multi-walled carbon nano-tubes of the gold particle load that obtains of present embodiment.
Embodiment 7: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the 30mg SWCN, 50mL water, 100mL N, the N-dimethylacetylamide is after the dispersed with stirring, dripping concentration is 0.02mol/L tetra chlorauric acid aqueous solution 80mL, and 0-5 ℃ was stirred 50 hours down.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the SWCN of gold particle load.The size of gold particle is 40nm-2 μ m.
Embodiment 8: implementation process is with embodiment 7, and reaction temperature rises to 50-60 ℃, stirs 30 hours.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the SWCN of gold particle load.The size of gold particle is 30nm-3 μ m.
Embodiment 9: implementation process is with embodiment 7, and reaction temperature rises to 140-150 ℃, stirs 20 hours.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the SWCN of gold particle load.The size of gold particle is 50nm-5 μ m.
Embodiment 10: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the multi-walled carbon nano-tubes of 35mg oxidation, and 100mL water, after the dispersed with stirring, dripping concentration is 0.01mol/L silver nitrate aqueous solution 150mL, (20-25 ℃) stirred 20 hours under the room temperature.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the multi-walled carbon nano-tubes of Nano silver grain load.The size of Nano silver grain is 1-3nm.Fig. 3,4 is respectively corresponding TEM, the STEM figure of the multi-walled carbon nano-tubes of the silver particles load that obtains of present embodiment.
Embodiment 11: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the SWCN of 35mg oxidation, and 100mL water, after the dispersed with stirring, dripping concentration is 0.01mol/L silver nitrate aqueous solution 150mL, (20-25 ℃) stirred 20 hours under the room temperature.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the SWCN of Nano silver grain load.The size of Nano silver grain is 5nm-30nm.Fig. 5 is the corresponding TEM photo of the multi-walled carbon nano-tubes of the silver particles load that obtains of present embodiment.
Embodiment 12: in the 500mL boiling flask that the magnetic agitation rotor is housed, add the multi-walled carbon nano-tubes of carbon containing 3mmol (36mg) oxidation, 150mL water after the dispersed with stirring, adds the 0.003mmol silver nitrate, and (20-25 ℃) stirred 50 hours under the room temperature.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the multi-walled carbon nano-tubes of Nano silver grain load.Silver content is 0.5%, and the size of Nano silver grain is 1-3nm.
Embodiment 13: in the 1000mL boiling flask that the magnetic agitation rotor is housed, add the multi-walled carbon nano-tubes of carbon containing 0.05mmol (0.6mg) oxidation, 500mL water after the dispersed with stirring, adds the 25mmol silver nitrate, and (20-25 ℃) stirred 2 hours under the room temperature.Repeatedly centrifugation, remove the aqueous solution after, obtain black solid, through vacuum drying, obtain the multi-walled carbon nano-tubes of Nano silver grain load.The size of Nano silver grain is 1-10nm.
Claims (4)
1. the preparation method of the carbon nanomaterial of carried noble metal is characterized in that concrete preparation method is as follows:
The carbon nanomaterial of 1 weight portion or its surface modification body and 0.1-10000 weight portion precious metal chemical complex mix in the mixed solvent of 0.1～50 weight parts water, organic solvent or water and organic solvent, after stirring 5 minutes to 120 hours under 0-150 ℃, through centrifugation, drying, obtain the carbon nanomaterial of carried noble metal, wherein water is 1/0.1-1/1000 with the volume of organic solvent ratio in the mixed solvent.
2. the preparation method of the carbon nanomaterial of carried noble metal according to claim 1 is characterized in that it is the surface modification thing of nano level carbon particulate, carbon ball, carbon-point, SWCN, double-walled carbon nano-tube, multi-walled carbon nano-tubes, carbon film, carbon fiber, tubulose material with carbon element, taper material with carbon element, block carbon material, arc material with carbon element, ring-type material with carbon element, onion shape material with carbon element, polyhedron material with carbon element, reticulated carbon material, porous carbon materials, fullerene and these nano-carbon materials that carbon nanomaterial or its surface modification body are selected from least one dimension.
3. the preparation method of the carbon nanomaterial of carried noble metal according to claim 1 is characterized in that used precious metal chemical complex is selected from gold trichloride, tetra chlorauric acid, gold hydroxide, potassium chloroaurate, ammonium chloraurate, sodium chloraurate, potassium auricyanide, silver nitrate, silver acetate, chloroplatinic acid, ammonium chloroplatinate, potassium chloroplatinate, dinitroso diammonia platinum, potassium chloroplatinite, ammonium chloroplatinite, platinum nitrate, cis-platinum, platinic sodium chloride, dintrile phenyl platinous chloride, the triphenylphosphine platinum chloride, rhodium chloride, the acid of chlorine rhodium, rhodium sulfate, dimerization acetic acid rhodium, the acetic acid rhodium, rhodium nitrate, chlorine rhodium acid potassium, chlorine rhodium acid ammonium, the triphenylphosphine radium chloride, triphenylphosphine bromination rhodium, triphenylphosphine carbonyl radium chloride, ruthenium trichloride, the triphenylphosphine ruthenic chloride, the carbonyl ruthenic chloride, ruthenium hydrochloride potassium, ruthenium hydrochloride sodium, the ruthenium hydrochloride ammonium, chloro-iridic acid, iridous chloride, acetic acid iridium, ammonium chloroiridate, potassium hexachloroiridate, iridium sodium chloride, palladium nitrate, palladium, palladium bichloride, palladium sulfate or its mixture.
4. the preparation method of the carbon nanomaterial of carried noble metal according to claim 1, it is characterized in that organic solvent is selected from methyl alcohol, ethanol, propyl alcohol, butanols, dimethyl sulfoxide (DMSO), N, dinethylformamide, N, N-dimethylacetylamide, N-N-methyl-2-2-pyrrolidone N-, oxolane, acetate, acetone, butanone, acetonitrile, chloroform, triethylamine, pyridine, dimethylamino pyridine or its mixture.
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| CN113894288B (en) * | 2020-07-06 | 2023-11-10 | 中国科学院青岛生物能源与过程研究所 | Preparation method of ultra-small and high-dispersion metal nano particles |
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| CN115888699A (en) * | 2022-11-30 | 2023-04-04 | 安徽科技学院 | Preparation method of carbon nanotube composite material loaded with noble metal |
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