CN106694039A - Preparation method and application of carbon sphere/Au nanometer composite material - Google Patents
Preparation method and application of carbon sphere/Au nanometer composite material Download PDFInfo
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- CN106694039A CN106694039A CN201610831254.7A CN201610831254A CN106694039A CN 106694039 A CN106694039 A CN 106694039A CN 201610831254 A CN201610831254 A CN 201610831254A CN 106694039 A CN106694039 A CN 106694039A
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
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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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
- B01J2231/64—Reductions in general of organic substrates, e.g. hydride reductions or hydrogenations
Abstract
The invention discloses a preparation method and application of a carbon sphere/Au (copper) nanometer composite material. The preparation method comprises the following steps of firstly, preparing a carbon sphere, modifying the surface of the carbon sphere by PDDA (poly diallyldimethylammonium chloride), enabling the surface of the carbon sphere to carry positive charges, and utilizing electrostatic attraction to uniformly and quickly adsorb AuC14<-> onto the surface of the carbon sphere in the heating and stirring process with an H2O and DMF mixed solvent; finally, under the protection action of PVP (polyvinylpyrrolidone), using N,N-DMF (N,N-dimethylformamide) as a reduction agent, enabling Au to grow along a particular crystal face, and further reducing in situ in one step, so as to obtain the uniformly loaded carbon sphere/Au nanometer composite material. Compared with the prior art, the preparation method has the advantages that a gold nanoparticle is loaded by using the green, low-price and easily-synthetic carbon sphere as a substrate, the reaction time is short, the operation is simple and convenient, and the repeatability is high; by changing the adding amount of HAuC14, the carbon sphere/Au nanometer composite material with controllable loading amount is obtained; the carbon sphere/Au nanometer composite material has catalyzing property, and especially has excellent catalyzing property on the reduction of 4-nitrophenol.
Description
Technical field
The present invention relates to the preparation method of nano composite material, and in particular to a kind of system of carbon ball/Au nano composite materials
Preparation Method and its application.
Background technology
Noble metal nanometer material have the electronic structure that size relies on, surface characteristic, controllable composition, good conductivity, can be with
The advantages of easily synthesizing in the liquid phase and process so that it is received in catalysis and based on the field of biosensors that catalysis builds
The extensive concern of researcher is arrived.But due to the wilderness demand to catalyst, the high cost of noble metal but hinders its reality
Application.When the timing of amount one of noble metal, the size of noble metal nano particles are smaller, just there is bigger electro-chemical activity surface
Product and more accessible metal surfaces.Average-size it is therefore desirable to remove reduction noble metal nano particles as much as possible.So
And, when noble metal nano particles are below 10nm sizes, due to its surface can it is higher it is easy occur reunite or surface reconstruction, in order to
Preventing nanostructured from reuniting generally needs stabilizer to be coated on its surface.But then, these stabilizers such as surfactant,
Polymer etc. can reduce accessible metallic atom surface, so as to have influence on the catalytic performance and service life of material.To understand
Certainly this problem is, it is necessary to find the base material of various suitable carried noble metals to stablize noble metal nano particles, while increasing
Plus accessible nano grain surface.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of preparation method of carbon ball/Au nano composite materials, passing through
Novel nano composite material is built in carbon ball area load Au, synthetic method is simply controllable.
Present invention also offers the application of this carbon ball/Au nano composite materials.
The present invention solves the technical scheme taken of above-mentioned technical problem：A kind of system of carbon ball/Au nano composite materials
Preparation Method, including carbon ball preparation process, the modifying process of carbon ball, the loading process of Au nano-particles, preparation method tool
Body step is as follows：
A, weigh cetyl trimethylammonium bromide (CTAB) and be dissolved in distilled water, Portugal is added during magnetic agitation
Grape sugar, after after all dissolvings, stops stirring, and above-mentioned solution is poured into reactor, is put into baking oven, is warming up to 160-180 DEG C,
Reaction 10-12h, is cooled to room temperature, and sediment is centrifuged to obtain, and with deionized water and absolute ethyl alcohol, respectively washing for several times, is being vacuum dried
60-80 DEG C of drying obtains carbon ball to constant weight in case；Wherein, glucose concentration in aqueous is 100g/L, cetyl front three
Base ammonium bromide is 1 with the mass ratio of glucose：40；
B, weigh step a preparation carbon ball be dissolved in distilled water, sequentially add NaCl and diallyl dimethyl chlorine
Change ammonium (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, is washed with deionized for several times, obtains modified carbon ball；Its
In, NaCl concentration in aqueous is 1mol/L, and diallyl dimethyl ammoniumchloride, carbon ball and NaCl are in aqueous
Mass ratio is (34.67-104)：1：116.88；
C, the modified carbon ball that step b is obtained is transferred to flask, and is dispersed in DMF and H2In the mixed solvent of O, add
PVP and HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 130-150 DEG C, is refluxed 2h, is cooled to room temperature, and being centrifuged to sink
Starch, is respectively washed for several times with deionized water and absolute ethyl alcohol, and 60-80 DEG C of drying obtains carbon ball/Au to constant weight in vacuum drying chamber
Nano composite material；Wherein, HAuCl4The mass ratio of solution, modified carbon ball and PVP is (0.33-1)：1：(1.33-10).
Described DMF is reducing agent, and DMF is 630 with the mass ratio of modified carbon ball:1.
Described DMF and H2In the mixed solvent of O, DMF and H2The volume ratio of O is 1：1.
The centrifugal rotational speed is 6000-9000r/min, and the time is 1-4min.
Application of this carbon ball/Au nano composite materials that the present invention is also provided in catalysis 4- nitrophenol reduction.
The appearance of carbon nano-structured support materials such as CNT, carbon nano-fiber, Graphene, carbon ball etc., it is new to prepare
The carried noble metal nano composite material of type is provided may.In these support materials, carbon ball has carbon nanomaterial carrier
The general advantage being had, such as high stability under acid and alkalescence condition, it is easy to carry out surface modification etc..Additionally, comparing
In the nano material of other carbon families, carbon ball also have it is easily prepared, with the nanometer spherical morphology for being conducive to catalytic applications, and
And be easy to reclaim noble metal by decarburization of burning after catalyst is inactivated.If noble metal and carbon ball can be carried out uniformly and effectively multiple
Close, can either effectively reduce the load capacity of noble metal, improve the catalytic performance and stability of noble metal catalyst, again can be in turn
The biocompatibility of carbon ball is improved, so as to obtain difunctional or multi-functional composite, promotes it in every field
Using.
Beneficial effects of the present invention：The present invention is repaiied by diallyl dimethyl ammoniumchloride (PDDA) on carbon ball surface
Decorations so that carbon ball surface carries positive charge, using electrostatic attraction, with H2During O and DMF is for the heating stirring of mixed solvent
Allow AuCl4 -Uniform quick adsorption is to carbon ball surface；Then under the protection of PVP with N,N-dimethylformamide (DMF) for reduction
Agent, so that a step in-situ reducing obtains the carbon ball/Au nano composite materials of Load Balanced.Compared with the prior art, the present invention is anti-
Should be easy to operate, reproducible, Load Balanced；By changing HAuCl4Concentration, the carbon ball/Au that can obtain different loads amount receives
Nano composite material.Gained composite has catalytic performance, especially has superior catalysis to catalysis reduction 4- nitrophenols
Performance.
Brief description of the drawings
Fig. 1 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 1；
Fig. 1 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 1；
Fig. 2 is the X-ray powder diffraction figure of carbon ball/Au composites prepared by embodiment 1；
Fig. 3 is the catalytic effect figure of carbon ball/Au composites catalysis reduction 4- nitrophenols prepared by embodiment 1；
Fig. 4 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 2；
Fig. 4 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 2；
Fig. 5 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 3；
Fig. 5 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 3；
Fig. 6 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 4；
Fig. 6 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 4；
Fig. 7 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 5；
Fig. 7 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 5；
Fig. 8 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 6；
Fig. 8 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 6；
Fig. 9 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 7；
Fig. 9 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 7；
Figure 10 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 8；
Figure 10 (b) is the high power scanning electron microscope (SEM) photograph of carbon ball/Au composites prepared by embodiment 8.
Specific embodiment
Specific embodiment of the invention is described in detail below.It should be appreciated that described herein specific
Implementation method is merely to illustrate and explain the present invention, and is not intended to limit the invention.In embodiment, CTAB, glucose, PDDA,
PVP, NaCl and DMF are the commercially available product of Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and 1mL
Diallyl dimethyl ammoniumchloride (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and number is washed with deionized
It is secondary, obtain modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 100mg PVP and 1mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cooling
To room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are to perseverance in vacuum drying chamber
Weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 8000r/min, and the time is 2min.
The testing result of embodiment 1 is as follows：
Fig. 1 (a) is the low power scanning electron microscope (SEM) photograph of carbon ball/Au nano composite materials prepared by embodiment 1, and Fig. 1 (b) is implementation
The high power scanning electron microscope (SEM) photograph of carbon ball/Au nano composite materials prepared by example 1, as can be seen from Figure, Au nano-particles are uniform
Carbon ball surface is supported on, the size of Au nano-particles is 30-50nm.
Fig. 2 is the X-ray powder diffraction figure of carbon ball/Au nano composite materials prepared by embodiment 1, all diffraction in spectrogram
Peak is all consistent with Emission in Cubic Au (JCPDS No.04-0784).
Fig. 3 is the carbon ball/Au nano-complex particles in the preparation of embodiment 1 in 0.04M NaBH4Under solution be catalyzed reduction 1 ×
10-4The catalytic effect figure of the 4- nitrophenols of M.As shown in figure 3, the carbon ball of 30mg/L/Au nano composite materials can after 10min
The conversion ratio of 4- nitrophenols is set to reach 94.4%.It can be seen that Au nano composite materials and the equal table of Au nano-particles
Reveal catalysis activity, but under same catalyst concentration the carbon ball/Au nano composite materials of Load Balanced catalysis activity ratio
Single Au nano-particles are more superior.
Embodiment 2：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and
0.5mL diallyl dimethyl ammoniumchlorides (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and uses deionized water
Washing for several times, obtains modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 100mg PVP and 1mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cooling
To room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are to perseverance in vacuum drying chamber
Weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 9000r/min, and the time is 1min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 2 have carried out ESEM detection, and Fig. 4 (a) is real
The low power scanning electron microscope (SEM) photograph of the carbon ball/Au nano composite materials of the preparation of example 2 is applied, Fig. 4 (b) is that carbon ball/Au prepared by embodiment 2 receives
The high power scanning electron microscope (SEM) photograph of nano composite material；As can be seen from Figure, Au nano-particles are more uniform is supported on carbon ball surface, Au
The size of nano-particle is 20-40nm.
Embodiment 3：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and
1.5mL diallyl dimethyl ammoniumchlorides (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and uses deionized water
Washing for several times, obtains modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 100mg PVP and 1mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cooling
To room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are to perseverance in vacuum drying chamber
Weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 7000r/min, and the time is 3min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 3 have carried out ESEM detection, and Fig. 5 (a) is real
The low power scanning electron microscope (SEM) photograph of the carbon ball/Au nano composite materials of the preparation of example 3 is applied, Fig. 5 (b) is that carbon ball/Au prepared by embodiment 3 receives
The high power scanning electron microscope (SEM) photograph of nano composite material；As can be seen from Figure, Au nano-particles are more uniform is supported on carbon ball surface, Au
The size of nano-particle is 20-50nm.
Embodiment 4：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and 1mL
Diallyl dimethyl ammoniumchloride (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and number is washed with deionized
It is secondary, obtain modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 20mg PVP and 1mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cooling
To room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are to perseverance in vacuum drying chamber
Weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 9000r/min, and the time is 1min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 4 have carried out ESEM detection, and Fig. 6 (a) is real
The low power scanning electron microscope (SEM) photograph of the carbon ball/Au nano composite materials of the preparation of example 4 is applied, Fig. 6 (b) is that carbon ball/Au prepared by embodiment 4 receives
The high power scanning electron microscope (SEM) photograph of nano composite material；As can be seen from Figure, Au nano-particles are more uniform is supported on carbon ball surface, Au
The size of nano-particle is 20-60nm.
Embodiment 5：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and 1mL
Diallyl dimethyl ammoniumchloride (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and number is washed with deionized
It is secondary, obtain modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 50mg PVP and 1mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cooling
To room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are to perseverance in vacuum drying chamber
Weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 9000r/min, and the time is 1min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 5 have carried out ESEM detection, and Fig. 7 (a) is real
The low power scanning electron microscope (SEM) photograph of the carbon ball/Au nano composite materials of the preparation of example 5 is applied, Fig. 7 (b) is that carbon ball/Au prepared by embodiment 5 receives
The high power scanning electron microscope (SEM) photograph of nano composite material；As can be seen from Figure, Au nano-particles are uniformly supported on carbon ball surface, and Au receives
The size of rice corpuscles is 20-50nm.
Embodiment 6：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and 1mL
Diallyl dimethyl ammoniumchloride (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and number is washed with deionized
It is secondary, obtain modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 150mg PVP and 1mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cooling
To room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are to perseverance in vacuum drying chamber
Weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 8000r/min, and the time is 2min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 6 have carried out ESEM detection, and Fig. 8 (a) is real
The low power scanning electron microscope (SEM) photograph of the carbon ball/Au nano composite materials of the preparation of example 6 is applied, Fig. 8 (b) is that carbon ball/Au prepared by embodiment 6 receives
The high power scanning electron microscope (SEM) photograph of nano composite material；As can be seen from Figure, Au nano-particles are uniformly supported on carbon ball surface, and Au receives
The size of rice corpuscles is 20-50nm.
Embodiment 7：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and 1mL
Diallyl dimethyl ammoniumchloride (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and number is washed with deionized
It is secondary, obtain modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 100mg PVP and 0.5mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cold
But to room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are extremely in vacuum drying chamber
Constant weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 6000r/min, and the time is 4min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 7 have carried out ESEM detection, and Fig. 9 (a) is real
The low power scanning electron microscope (SEM) photograph of the carbon ball/Au nano composite materials of the preparation of example 7 is applied, Fig. 9 (b) is that carbon ball/Au prepared by embodiment 7 receives
The high power scanning electron microscope (SEM) photograph of nano composite material；As can be seen from Figure, Au nano-particles are uniformly supported on carbon ball surface, and Au receives
The size of rice corpuscles is 20-40nm.
Embodiment 8：
A kind of preparation method of carbon ball/Au nano composite materials, including the preparation process of carbon ball, the modifying process of carbon ball,
The loading process of Au nano-particles, the preparation method is comprised the following steps that：
A, weigh 0.05g cetyl trimethylammonium bromides (CTAB) and be dissolved in 20mL distilled water, in the mistake of magnetic agitation
2g glucose is added in journey, after after all dissolvings, stops stirring, above-mentioned solution is poured into the reactor of 25mL, be put into baking oven
In, 170 DEG C are warming up to, 12h is reacted, room temperature is cooled to, sediment is centrifuged to obtain, respectively wash number with deionized water and absolute ethyl alcohol
Secondary, 60 DEG C of dryings obtain carbon ball to constant weight in vacuum drying chamber；
B, weigh step a preparation carbon ball 15mg be dissolved in 30mL distilled water, sequentially add 1.7532g NaCl and 1mL
Diallyl dimethyl ammoniumchloride (PDDA), magnetic agitation 1h stops standing and sediment is centrifuged to obtain, and number is washed with deionized
It is secondary, obtain modified carbon ball；
C, the modified carbon ball that step b is obtained is transferred to flask, and be dispersed in DMF and H2O respectively accounts for the mixed solvent of 10mL
In, add 100mg PVP and 1.5mL HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 140 DEG C, is refluxed 2h, cold
But to room temperature, sediment is centrifuged to obtain, with deionized water and absolute ethyl alcohol respectively washing for several times, 60 DEG C of dryings are extremely in vacuum drying chamber
Constant weight, obtains carbon ball/Au nano composite materials.
The centrifugal rotational speed is 9000r/min, and the time is 1min.
Carbon ball/Au nano composite materials that the present invention prepares embodiment 8 have carried out ESEM detection, and Figure 10 (a) is
The low power scanning electron microscope (SEM) photograph of carbon ball/Au nano composite materials prepared by embodiment 8, the carbon ball that Figure 10 (b) is prepared for embodiment 8/
The high power scanning electron microscope (SEM) photograph of Au nano composite materials；As can be seen from Figure, Au nano-particles are uniformly supported on carbon ball surface,
The size of Au nano-particles is 20-50nm.
Claims (5)
1. a kind of preparation process of the preparation method of carbon ball/Au nano composite materials, including carbon ball, the modifying process of carbon ball, Au
The loading process of nano-particle, it is characterised in that the preparation method is comprised the following steps that：
A, weigh cetyl trimethylammonium bromide (CTAB) and be dissolved in distilled water, grape is added during magnetic agitation
Sugar, after after all dissolvings, stops stirring, and above-mentioned solution is poured into reactor, is put into baking oven, is warming up to 160-180 DEG C, instead
10-12h is answered, room temperature is cooled to, sediment is centrifuged to obtain, respectively washed for several times, in vacuum drying chamber with deionized water and absolute ethyl alcohol
Middle 60-80 DEG C of drying obtains carbon ball to constant weight；Wherein, glucose concentration in aqueous is 100g/L, cetyl trimethyl
Ammonium bromide is 1 with the mass ratio of glucose：40；
B, weigh step a preparation carbon ball be dissolved in distilled water, sequentially add NaCl and diallyl dimethyl ammoniumchloride
(PDDA), magnetic agitation 1h, stops standing and sediment is centrifuged to obtain, and is washed with deionized for several times, obtains modified carbon ball；Wherein,
NaCl concentration in aqueous is 1mol/L, diallyl dimethyl ammoniumchloride, carbon ball and NaCl matter in aqueous
Amount is than being (34.67-104)：1：116.88；
C, the modified carbon ball that step b is obtained is transferred to flask, and is dispersed in DMF and H2In the mixed solvent of O, add PVP and
HAuCl4Solution, normal temperature magnetic agitation 1h, is warming up to 130-150 DEG C, is refluxed 2h, is cooled to room temperature, and sediment is centrifuged to obtain,
Respectively washed for several times with deionized water and absolute ethyl alcohol, 60-80 DEG C of drying obtains carbon ball/Au nanometers to constant weight in vacuum drying chamber
Composite；Wherein, HAuCl4The mass ratio of solution, modified carbon ball and PVP is (0.33-1)：1：(1.33-10)；HAuCl4It is molten
The concentration of liquid is 10g/L.
2. the preparation method of a kind of carbon ball/Au nano composite materials according to claim 1, it is characterised in that：Described
DMF is reducing agent, and DMF is 630 with the mass ratio of modified carbon ball:1.
3. the preparation method of a kind of carbon ball/Au nano composite materials according to claim 1, it is characterised in that：Described
DMF and H2In the mixed solvent of O, DMF and H2The volume ratio of O is 1：1.
4. the preparation method of a kind of carbon ball/Au nano composite materials according to claim 1, it is characterised in that：It is described from
Heart rotating speed is 6000-9000r/min, and the time is 1-4min.
5. application of the carbon ball described in the claim 1/Au nano composite materials in catalysis 4- nitrophenol reduction.
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