CN102615290B - A kind of preparation method of Ag/ graphene nanocomposite material - Google Patents
A kind of preparation method of Ag/ graphene nanocomposite material Download PDFInfo
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- CN102615290B CN102615290B CN201110434334.6A CN201110434334A CN102615290B CN 102615290 B CN102615290 B CN 102615290B CN 201110434334 A CN201110434334 A CN 201110434334A CN 102615290 B CN102615290 B CN 102615290B
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Abstract
The invention discloses a kind of preparation method of silver/graphite alkene nano composite material, comprising: (1) is by photochemical catalyst nanometer WO
3particle, silver nitrate and graphene oxide ultrasonic disperse in deionized water, obtain dispersion liquid: (2) add the agent of reproducibility alcohol and obtain dual-solvent system in dispersion liquid, logical N
2dissolved oxygen in solution is drained, photo catalytic reduction reaction under simulated solar irradiation; (3) sodium borohydride reaction removing nanometer WO is added in dual-solvent system
3particle; (4) suction filtration, washing, drying and grinding obtain silver/graphite alkene nano composite material.The present invention can obtain a kind of composite of Graphene high uniform load silver nano-grain by photo catalytic reduction method, for the graphene-supported nano composition of graphene oxide reduction preparation provides a kind of green, environment-friendly new method.
Description
Technical field
The invention belongs to technical field of new material preparation, relate to a kind of preparation method of Ag/ graphene nanocomposite material.
Technical background
Since the people such as Univ Manchester UK Geim in 2004 find and obtain stable Graphene (graphene), Graphene is because of excellent physicochemical properties and wide application prospect, and the research work relevant with Graphene becomes the current study hotspot of related discipline.
Nanometer-level silver particle has quantum size effect, small-size effect, skin effect and macro quanta tunnel effect, thus shows much distinctive character, has broad application prospects in catalysis, antibacterial, conduction and new material etc.But easily there is local and reunite and affect its performance in nanometer-level silver particle.
Graphene is the carbonaceous new material of monoatomic thickness the thinnest in the world at present, has the former molecular two-dimensional nanostructure of monolayer carbon, becomes the new support of fabrication of new materials.Graphene after oxidation, its surface is containing a large amount of oxy radical, and the combination for other particle provides effective site.In addition, the π-πconjugation being rich in electronics in the middle of Graphene, is had again, for the Electrostatic Absorption of metallic silver corpuscle provides possibility.When nanometer-level silver particle and Graphene compound tense, these sites and this energy of adsorption effectively stop the reunion of nanometer-level silver particle.But because the inertia of graphenic surface and slickness make directly graphenic surface obtain higher density and comparatively equally loaded Nano silver grain be very difficult.Research shows to obtain Graphene with electronation graphite oxide, and it can be used as the carrier of Nano silver grain, thus fixing Nano silver grain.But the graphenic surface that this method obtains contains more group and the defect of not reducing, and the randomness of these groups and defect distribution makes the Nano silver grain load quality of the composite obtained be restricted.
In recent years, photo catalytic reduction graphite oxide is prepared Graphene and is received extensive concern as a kind of green, environment-friendly new method.The object of present patent application is to provide a kind of preparation method of Ag/ graphene nanocomposite material.The method not only can realize the high uniform load of silver, but also significantly can reduce graphenic surface and do not reduce the quantity of group and defect, improves the performance of nano composite material.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Ag/ graphene nanocomposite material, it is characterized by: by photochemical catalyst nanometer WO
3particle, silver nitrate and graphene oxide ultrasonic disperse are in the solvent pairs of deionized water and the agent of reproducibility alcohol, and adopt photo-reduction to prepare a kind of silver/graphite alkene nano composite material, its processing step comprises:
(1) dispersion liquid is prepared: under ultrasonication, photochemical catalyst nanometer WO
3granular composite in deionized water, then adds graphene oxide and silver nitrate successively, and ultrasonic disperse 1-5 hour obtains dispersion liquid;
(2) photo catalytic reduction: add the agent of reproducibility alcohol in the dispersion liquid that step (1) is obtained, obtain dual-solvent system, logical N
2dissolved oxygen in solution is drained, is transferred in photo catalysis reactor afterwards, photo catalytic reduction reaction 1 ~ 5 hour under simulated solar irradiation;
(3) photochemical catalyst is removed: the dual-solvent system that step (2) is obtained is poured in round-bottomed flask, adds sodium borohydride powder, reaction removing nanometer WO at 80 DEG C
3particle, the reaction time is 0.5-~ 1 hour;
(4) suction filtration, washing and collection: reacted dual-solvent system poured into while hot in Vacuum filtration device and carry out suction filtration, spend deionized water, vacuum drying, grinding obtain silver/graphite alkene nano composite material.
On the basis of such scheme, control WO in described step (1)
3, graphene oxide and silver nitrate mass ratio be 1: (0-01-0.3): (0.01-0.1);
On the basis of such scheme, the reproducibility alcohol agent described in step (2) is at least as methyl alcohol, one of ethanol or ethylene glycol;
On the basis of such scheme, quality or the volume of the reproducibility alcohol agent quality added in step (2) or volume and the required graphene oxide that simultaneously reduces and silver ion match.
On the basis of such scheme, the simulated solar irradiation described in step (2) is xenon lamp, and power is the one of 100W, 150W, 200W or 500W.
On the basis of such scheme, the sodium borohydride quality added in step (3) and required removing nanometer WO
3the quality of particle matches.
The present invention relates to a kind of preparation method of Ag/ graphene nanocomposite material, by the optical excitation WO when there being hole trapping agents to exist
3nano particle produces light induced electron, is reduced into Nano silver grain and Graphene respectively after the silver ion that graphite oxide surface uniform is adsorbed and oxy radical catch light induced electron, finally by adding sodium borohydride reaction removing photochemical catalyst nanometer WO
3particle, obtain a kind of silver/graphite alkene nano composite material, silver particles is high is evenly distributed on graphenic surface.The advantage of the method is the composite that can be obtained a kind of graphene-supported silver nano-grain by photo catalytic reduction method, course of reaction is simple, for the graphene-supported nano composition of graphene oxide reduction preparation provides a kind of green, environment-friendly new method.
Accompanying drawing explanation
Fig. 1 is the XRD image of graphite oxide in embodiment 1;
Fig. 2 is the XRD image of product in embodiment 1;
Fig. 3 is the TEM image of product in embodiment 1;
Detailed description of the invention
Embodiment one:
(1) graphite oxide is prepared.2g graphite powder is joined the potassium peroxydisulfate (1g) of 80 DEG C, in the concentrated sulfuric acid solution (15mL) of phosphorus pentoxide (1g), pre-oxidation 6 hours, is cooled to room temperature, suction filtration afterwards, and washing is to neutral.The graphite powder (2g) of pre-oxidation is joined in the 50mL concentrated sulfuric acid solution of 0 DEG C, slowly add 6g potassium permanganate afterwards, afterwards in 35 DEG C of reactions 2 hours, the hydrogen peroxide slowly adding 100mL deionized water and 20mL30% in the most backward reactant liquor makes reaction terminating, suction filtration, washing, dialysis, obtained graphite oxide, Fig. 1 is shown in by its XRD collection of illustrative plates;
(2) dispersion liquid is prepared: 5g photochemical catalyst nanometer WO
3granular composite, in 100mL deionized water, then adds 0.5g graphene oxide and 0.05g silver nitrate successively, and ultrasonic disperse obtains dispersion liquid in 2 hours;
(3) photo catalytic reduction: add 10mL absolute ethyl alcohol in the dispersion liquid that step (2) is obtained, obtain dual-solvent system, logical N in dual-solvent system
21 hour, be transferred to afterwards in photo catalysis reactor, under simulated solar irradiation, photo catalytic reduction reacts 2 hours;
(4) remove photochemical catalyst: the dual-solvent system that step (3) is obtained is poured in round-bottomed flask, adds 10g sodium borohydride powder, react 0.5 hour at 80 DEG C;
(5) suction filtration, washing and collection: reacted dual-solvent system poured into while hot in Vacuum filtration device and carry out suction filtration, spend deionized water 5 times, in 80 DEG C of vacuum drying 12 hours, grinding obtained silver/graphite alkene nano composite material.Fig. 2 is shown in by the XRD collection of illustrative plates of product, and TEM figure is shown in Fig. 3.
Embodiment two:
(1) with the step (1) in embodiment 1;
(2) dispersion liquid is prepared: 5g photochemical catalyst nanometer WO
3granular composite, in 100mL deionized water, then adds 0.1g graphene oxide and 0.05g silver nitrate successively, and ultrasonic disperse obtains dispersion liquid in 1.5 hours;
(3) photo catalytic reduction: add 8mL absolute ethyl alcohol in the dispersion liquid that step (2) is obtained, obtain dual-solvent system, logical N in dual-solvent system
21 hour, be transferred to afterwards in photo catalysis reactor, under simulated solar irradiation, photo catalytic reduction reacts 1 hour;
(4) with the step (4) in embodiment 1;
(5) with the step (5) in embodiment 1.
Embodiment three:
(1) with the step (1) in embodiment 1;
(2) dispersion liquid is prepared: 5g photochemical catalyst nanometer WO
3granular composite, in 100mL deionized water, then adds 1g graphene oxide and 0.05g silver nitrate successively, and ultrasonic disperse obtains dispersion liquid in 3 hours;
(3) photo catalytic reduction: add 50mL absolute ethyl alcohol in the dispersion liquid that step (2) is obtained, obtain dual-solvent system, logical N in dual-solvent system
21 hour, be transferred to afterwards in photo catalysis reactor, under simulated solar irradiation, photo catalytic reduction reacts 5 hours;
(4) with the step (4) in embodiment 1;
(5) with the step (5) in embodiment 1.
Embodiment four:
(1) with the step (1) in embodiment 1;
(2) dispersion liquid is prepared: 5g photochemical catalyst nanometer WO
3granular composite, in 100mL deionized water, then adds 0.5g graphene oxide and 0.1g silver nitrate successively, and ultrasonic disperse obtains dispersion liquid in 2 hours;
(3) photo catalytic reduction: add 15mL absolute ethyl alcohol in the dispersion liquid that step (2) is obtained, obtain dual-solvent system, logical N in dual-solvent system
21 hour, be transferred to afterwards in photo catalysis reactor, under simulated solar irradiation, photo catalytic reduction reacts 2 hours;
(4) with the step (4) in embodiment 1;
(5) with the step (5) in embodiment 1.
Embodiment five:
(1) with the step (1) in embodiment 1;
(2) dispersion liquid is prepared: 5g photochemical catalyst nanometer WO
3granular composite, in 100mL deionized water, then adds 0.5g graphene oxide and 0.3g silver nitrate successively, and ultrasonic disperse obtains dispersion liquid in 2 hours;
(3) photo catalytic reduction: add 40mL absolute ethyl alcohol in the dispersion liquid that step (2) is obtained, obtain dual-solvent system, logical N in dual-solvent system
21 hour, be transferred to afterwards in photo catalysis reactor, under simulated solar irradiation, photo catalytic reduction reacts 3 hours;
(4) with the step (4) in embodiment 1;
(5) with the step (5) in embodiment 1.
Embodiment six:
(1) with the step (1) in embodiment 1;
(2) dispersion liquid is prepared: 10g photochemical catalyst nanometer WO
3granular composite, in 100mL deionized water, then adds 0.5g graphene oxide and 0.05g silver nitrate successively, and ultrasonic disperse obtains dispersion liquid in 2 hours;
(3) with the step (3) in embodiment 1;
(4) remove photochemical catalyst: the dual-solvent system that step (3) is obtained is poured in round-bottomed flask, adds 20g sodium borohydride powder, react 1 hour at 80 DEG C;
(5) with the step (5) in embodiment 1.
It should be noted that: above embodiment is only and embodies technical characteristic of the present invention and provide, and not limits the scope of patent protection of Patent request of the present invention with this.
Claims (6)
1. a preparation method for silver/graphite alkene nano composite material, is characterized by: by photochemical catalyst nanometer WO
3particle, silver nitrate and graphene oxide ultrasonic disperse are in the solvent pairs of deionized water and the agent of reproducibility alcohol, and adopt photo-reduction to prepare a kind of silver/graphite alkene nano composite material, its processing step comprises:
(1) dispersion liquid is prepared: under ultrasonication, photochemical catalyst nanometer WO
3granular composite in deionized water, then adds graphene oxide and silver nitrate successively, and ultrasonic disperse 1-5 hour obtains dispersion liquid;
(2) photo catalytic reduction: add the agent of reproducibility alcohol in the dispersion liquid that step (1) is obtained, obtain dual-solvent system, logical N
2dissolved oxygen in solution is drained, is transferred in photo catalysis reactor afterwards, photo catalytic reduction reaction 1-5 hour under simulated solar irradiation;
(3) photochemical catalyst is removed: the dual-solvent system that step (2) is obtained is poured in round-bottomed flask, adds sodium borohydride powder, reaction removing nanometer WO at 80 DEG C
3particle, the reaction time is 0.5-1 hour;
(4) suction filtration, washing and collection: reacted dual-solvent system poured into while hot in Vacuum filtration device and carry out suction filtration, spend deionized water, vacuum drying, grinding obtain silver/graphite alkene nano composite material.
2. the preparation method of a kind of silver/graphite alkene nano composite material according to claim 1, is characterized in that: control WO in step (1)
3, graphene oxide and silver nitrate mass ratio be: 1: (0.01-0.3): (0.01-0.1).
3. the preparation method of a kind of silver/graphite alkene nano composite material according to claim 1, is characterized in that: the reproducibility alcohol agent described in step (2) is the one in methyl alcohol, ethanol or ethylene glycol.
4. the preparation method of a kind of silver/graphite alkene nano composite material according to claim 1, is characterized in that: quality or the volume of the reproducibility alcohol agent quality added in step (2) or volume and the required graphene oxide that simultaneously reduces and silver ion match.
5. the preparation method of a kind of silver/graphite alkene nano composite material according to claim 1, it is characterized in that: the simulated solar irradiation described in step (2) is xenon lamp, power is the one in 100W, 150W, 200W or 500W.
6. the preparation method of a kind of silver/graphite alkene nano composite material according to claim 1, is characterized in that: the sodium borohydride quality added in step (3) and required removing nanometer WO
3the quality of particle matches.
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| CN104308184B (en) * | 2014-10-24 | 2016-08-24 | 武汉理工大学 | A kind of visible ray prepares the method for Au-Ag core-shell nano |
| CN106480434B (en) * | 2015-08-26 | 2019-01-15 | 中国科学院宁波材料技术与工程研究所 | A kind of chemical plating graphene and preparation method thereof and a kind of metal-base composites |
| CN105397103A (en) * | 2015-11-01 | 2016-03-16 | 华南理工大学 | Nano-silver/graphene composite material and preparation method thereof |
| CN105562707B (en) * | 2015-12-23 | 2018-12-11 | 陈添乾 | The preparation method of silver-graphene composite material and its application method for being used to prepare silver-graphene alloy wire |
| CN105833865B (en) * | 2016-04-11 | 2017-12-26 | 河南科技学院 | A kind of preparation method of the graphene-supported Ag photochemical catalysts with concave surface cube pattern |
| CN106179315B (en) * | 2016-07-10 | 2018-09-28 | 上海博栋化学科技有限公司 | A kind of preparation method of the graphene-supported Bi photochemical catalysts with 40 shape of octahedron |
| CN106268803A (en) * | 2016-07-20 | 2017-01-04 | 武夷学院 | A kind of preparation method of the graphene-supported Ag Bi photocatalyst with 40 shape of octahedron |
| CN109434098A (en) * | 2018-12-25 | 2019-03-08 | 广西大学 | A kind of method that photocatalysis lignin reduction silver nitrate prepares silver nano-grain |
| CN110776786A (en) * | 2019-12-18 | 2020-02-11 | 武汉华知智能科技有限公司 | Graphene nano-silver composite conductive ink and preparation method thereof |
| CN110862716A (en) * | 2019-12-18 | 2020-03-06 | 九江纳维新材料科技有限公司 | Graphene composite conductive ink and preparation method thereof |
| CN111995836B (en) * | 2020-08-11 | 2022-11-08 | 五邑大学 | Polymer dispersed liquid crystal, preparation method and application |
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