CN106115664A - A kind of preparation method of platinum/graphen lamella composite - Google Patents
A kind of preparation method of platinum/graphen lamella composite Download PDFInfo
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- CN106115664A CN106115664A CN201610413872.XA CN201610413872A CN106115664A CN 106115664 A CN106115664 A CN 106115664A CN 201610413872 A CN201610413872 A CN 201610413872A CN 106115664 A CN106115664 A CN 106115664A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention is the preparation method of a kind of platinum/graphen lamella composite, concretely comprises the following steps: the preparation of (1) graphite oxide；(2) preparation of graphene sheet layer；(3) preparation of platinum/graphen lamella composite: by graphene sheet layer and dimethyl (1,5 cyclo-octadiene) platinum mixing, add in high pressure stainless steel reactor, reactor seals, it is filled with carbon dioxide, gets rid of air in still, stirring, heating compressive reaction, presoma is sufficiently mixed with graphene sheet layer；Again sample is added high pressure stainless steel reactor, use N2Wash away air in still, be slowly introducing N2, reacting by heating, after being cooled to room temperature, gas slowly is got rid of, collect sample；With a large amount of ethanol purge, filtration, the removal of impurity, product vacuum is gone to be dried.The present invention is a kind of supercritical process effective, convenient and eco-friendly, and the platinum/graphen lamella composite prepared shows higher electro catalytic activity and stability for the oxidation of methanol point.
Description
Technical field
The present invention relates to Graphene metallic composite production field, particularly relate to a kind of platinum/graphen lamella composite wood
The preparation method of material.
Background technology
The current transparency conductive electrode in intelligent light modulation film product mainly uses tin indium oxide (ITO) material, has
The advantages such as photosensitiveness is good, surface resistance is low, technical maturity.But ITO is weak to bending, it is susceptible to during producing, transporting and use
Fracture and scrap, and indium ore reserves is rare and disperse, and exploits and reclaim difficulty, along with the continuous consumption of resource, the cost of ITO
To constantly rise.Due to above reason, people are constantly looking for the succedaneum of ITO.With traditional transparent conductive material phase
Ratio, Graphene has the advantage of flexibility, it is easy to applies in the flexible substrates such as polyester (PET), expands products application scope；Soft
Property formed material be suitable for and volume to volume process integration, it is possible to omnidistance continuous prodution, reduce process costs, and grapheme material this
The Material Cost of body is the lowest, has great cost advantage.Metal platinum has good decay resistance in strong acidic environment
And chemical stability, platinum and Graphene are combined with each other, there is high-specific surface area, excellent chemical stability, unique electricity
Learn and mechanical property.But can add environmentally harmful volatile organic molten during generally platinum and Graphene being combined
Agent, constrains the preparation of material.
Summary of the invention
Present invention seek to address that the deficiencies in the prior art, and the preparation side of a kind of platinum/graphen lamella composite is provided
Method.
The present invention for achieving the above object, by the following technical solutions:
The preparation method of a kind of platinum/graphen lamella composite, concretely comprises the following steps:
(1) preparation of graphite oxide:
Low-temp reaction: under stirring condition, in the concentrated sulphuric acid of ice-water bath cooling, is slowly added into graphite powder and anhydrous nitric acid
Sodium, after question response thing is mixed thoroughly, then is slowly added into potassium permanganate, concentrated sulphuric acid, graphite powder, anhydrous nitric acid sodium and Gao Meng
The mass fraction of acid potassium is more than 1h than respectively 16:1:115:45, the time controlling charging, reacts 1.5h after having fed；
Middle temperature is reacted: after low-temp reaction, removes ice-water bath, and controlling temperature is 30 DEG C of stirring reactions 6 days, obtains brown
Color product；
Pyroreaction: be slowly added to the sulphuric acid dilute solution of 5%, the temperature of mixed liquor raises rapidly, treats that dilute sulfuric acid is complete
After addition, it is warming up to 90 DEG C of reaction 2.5h；Natural cooling afterwards, treats that temperature drops to 60 DEG C, and the hydrogen peroxide of addition 30% neutralizes not
The potassium permanganate of reaction, reacts 2h；
Post processing: the mixed liquor filtration under diminished pressure obtained after reaction, finally, cleans repeatedly with deionized water, and reduce pressure sucking filtration, directly
It is neutral to pH value；By 50 DEG C of forced air dryings of filter membrane of obtaining 1 day, then 60 DEG C were vacuum dried 2 days, and product seals and preserves；
(2) preparation of graphene sheet layer:
Graphite oxide is placed in the quartz ampoule of sealing, under nitrogen atmosphere, is brought rapidly up 1100 DEG C, high-temperature process one
The section time, high-temperature process afterproduct is become the Graphene of black by tan graphene oxide lamella, and volume occurs the most swollen
Swollen, obtain graphene sheet layer；
(3) preparation of platinum/graphen lamella composite:
Be mixed grinding by graphene sheet layer and dimethyl (1,5-cyclo-octadiene) platinum, the dimethyl of graphene sheet layer sum
The mass fraction of (1,5-cyclo-octadiene) platinum is than for 1:1.5-1.9；The sample mixed is added in high pressure stainless steel reactor,
Reactor seals, and is filled with carbon dioxide, gets rid of air in still, opens magnetic agitation, be heated to 80 DEG C, is forced into 25MPa reaction
After 5.5h, presoma is sufficiently mixed with graphene sheet layer, takes out samples weighing；The most again sample is added high pressure rustless steel anti-
Answer device, use N2Wash away air in still, be slowly introducing N2, it is heated to 200 DEG C, reacts 5h, after being cooled to room temperature, gas slowly is arranged
Remove, collect sample；With a large amount of ethanol purge, filtration, going the removal of impurity, product is 60 DEG C of vacuum drying 7h in vacuum drying oven,
To platinum/graphen lamella composite.
The carbon dioxide being filled with in the preparation process of described platinum/graphen lamella composite be volume fraction be 99.9%
The supercritical carbon dioxide that produces after temperature and pressure regulate of high-purity carbon dioxide.
The platinum/graphen lamella composite prepared be platinum grain the densest be deposited on graphene sheet layer surface.
The invention has the beneficial effects as follows: the present invention is a kind of supercritical process effective, convenient and eco-friendly, supercritical
Carbon dioxide has that viscosity is low, good dispersion, surface tension are the advantages such as zero-sum density is controlled, and it is nontoxic, cheap, be difficult to
Combustion, wide material sources, those harmful volatile organic solvents alternative.The platinum/graphen lamella that this method is prepared is multiple
Condensation material shows higher electro catalytic activity and stability for the oxidation of methanol point.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
The preparation method of a kind of platinum/graphen lamella composite, concretely comprises the following steps:
(1) preparation of graphite oxide:
Low-temp reaction: under stirring condition, 16kg ice-water bath cooling concentrated sulphuric acid in, be slowly added into 1kg graphite powder and
115kg anhydrous nitric acid sodium, after question response thing is mixed thoroughly, then is slowly added into 45kg potassium permanganate, control charging time
Between be 1.5h, after having fed react 1.5h；
Middle temperature is reacted: after low-temp reaction, removes ice-water bath, and controlling temperature is 30 DEG C of stirring reactions 6 days, obtains brown
Color product；
Pyroreaction: be slowly added to the sulphuric acid dilute solution of 5%, the temperature of mixed liquor raises rapidly, treats that dilute sulfuric acid is complete
After addition, it is warming up to 90 DEG C of reaction 2.5h；Natural cooling afterwards, treats that temperature drops to 60 DEG C, and the hydrogen peroxide of addition 30% neutralizes not
The potassium permanganate of reaction, reacts 2h；
Post processing: the mixed liquor filtration under diminished pressure obtained after reaction, finally, cleans repeatedly with deionized water, and reduce pressure sucking filtration, directly
It is neutral to pH value；By 50 DEG C of forced air dryings of filter membrane of obtaining 1 day, then 60 DEG C were vacuum dried 2 days, and product seals and preserves；
(2) preparation of graphene sheet layer:
Graphite oxide is placed in the quartz ampoule of sealing, under nitrogen atmosphere, is brought rapidly up 1100 DEG C, high-temperature process one
The section time, high-temperature process afterproduct is become the Graphene of black by tan graphene oxide lamella, and volume occurs the most swollen
Swollen, obtain graphene sheet layer；
(3) preparation of platinum/graphen lamella composite:
Be mixed grinding by 1kg graphene sheet layer and 1.5kg dimethyl (1,5-cyclo-octadiene) platinum；The sample that will mix
Product add in high pressure stainless steel reactor, and reactor seals, and are filled with carbon dioxide, get rid of air in still, open magnetic agitation, heating
To 80 DEG C, after being forced into 25MPa reaction 5.5h, presoma is sufficiently mixed with graphene sheet layer, takes out samples weighing；The most again
Sample is added high pressure stainless steel reactor, uses N2Wash away air in still, be slowly introducing N2, it is heated to 200 DEG C, reacts 5h, cooling
To room temperature, gas slowly is got rid of, collect sample；With a large amount of ethanol purge, filtration, going the removal of impurity, product is in vacuum drying
In case, 60 DEG C of vacuum drying 7h, obtain platinum/graphen lamella composite.
The carbon dioxide being filled with in the preparation process of described platinum/graphen lamella composite be volume fraction be 99.9%
The supercritical carbon dioxide that produces after temperature and pressure regulate of high-purity carbon dioxide.
The platinum/graphen lamella composite prepared be platinum grain the densest be deposited on graphene sheet layer surface.
Embodiment 2:
The preparation method of a kind of platinum/graphen lamella composite, concretely comprises the following steps:
(1) preparation of graphite oxide:
Low-temp reaction: under stirring condition, 16kg ice-water bath cooling concentrated sulphuric acid in, add lentamente 1kg enter graphite powder and
115kg anhydrous nitric acid sodium, after question response thing is mixed thoroughly, then is slowly added into 45kg potassium permanganate, control charging time
Between be 2h, after having fed react 1.5h；
Middle temperature is reacted: after low-temp reaction, removes ice-water bath, and controlling temperature is 30 DEG C of stirring reactions 6 days, obtains brown
Color product；
Pyroreaction: be slowly added to the sulphuric acid dilute solution of 5%, the temperature of mixed liquor raises rapidly, treats that dilute sulfuric acid is complete
After addition, it is warming up to 90 DEG C of reaction 2.5h；Natural cooling afterwards, treats that temperature drops to 60 DEG C, and the hydrogen peroxide of addition 30% neutralizes not
The potassium permanganate of reaction, reacts 2h；
Post processing: the mixed liquor filtration under diminished pressure obtained after reaction, finally, cleans repeatedly with deionized water, and reduce pressure sucking filtration, directly
It is neutral to pH value；By 50 DEG C of forced air dryings of filter membrane of obtaining 1 day, then 60 DEG C were vacuum dried 2 days, and product seals and preserves；
(2) preparation of graphene sheet layer:
Graphite oxide is placed in the quartz ampoule of sealing, under nitrogen atmosphere, is brought rapidly up 1100 DEG C, high-temperature process one
The section time, high-temperature process afterproduct is become the Graphene of black by tan graphene oxide lamella, and volume occurs the most swollen
Swollen, obtain graphene sheet layer；
(3) preparation of platinum/graphen lamella composite:
Be mixed grinding by 1kg graphene sheet layer and 1.9kg dimethyl (1,5-cyclo-octadiene) platinum；The sample that will mix
Product add in high pressure stainless steel reactor, and reactor seals, and are filled with carbon dioxide, get rid of air in still, open magnetic agitation, heating
To 80 DEG C, after being forced into 25MPa reaction 5.5h, presoma is sufficiently mixed with graphene sheet layer, takes out samples weighing；The most again
Sample is added high pressure stainless steel reactor, uses N2Wash away air in still, be slowly introducing N2, it is heated to 200 DEG C, reacts 5h, cooling
To room temperature, gas slowly is got rid of, collect sample；With a large amount of ethanol purge, filtration, going the removal of impurity, product is in vacuum drying
In case, 60 DEG C of vacuum drying 7h, obtain platinum/graphen lamella composite.
The carbon dioxide being filled with in the preparation process of described platinum/graphen lamella composite be volume fraction be 99.9%
The supercritical carbon dioxide that produces after temperature and pressure regulate of high-purity carbon dioxide.
The platinum/graphen lamella composite prepared be platinum grain the densest be deposited on graphene sheet layer surface.
Embodiment 3:
The preparation method of a kind of platinum/graphen lamella composite, concretely comprises the following steps:
(1) preparation of graphite oxide:
Low-temp reaction: under stirring condition, 16kg ice-water bath cooling concentrated sulphuric acid in, be slowly added into 1kg graphite powder and
115kg anhydrous nitric acid sodium, after question response thing is mixed thoroughly, then is slowly added into 45kg potassium permanganate, control charging time
Between be 1.5h, after having fed react 1.5h；
Middle temperature is reacted: after low-temp reaction, removes ice-water bath, and controlling temperature is 30 DEG C of stirring reactions 6 days, obtains brown
Color product；
Pyroreaction: be slowly added to the sulphuric acid dilute solution of 5%, the temperature of mixed liquor raises rapidly, treats that dilute sulfuric acid is complete
After addition, it is warming up to 90 DEG C of reaction 2.5h；Natural cooling afterwards, treats that temperature drops to 60 DEG C, and the hydrogen peroxide of addition 30% neutralizes not
The potassium permanganate of reaction, reacts 2h；
Post processing: the mixed liquor filtration under diminished pressure obtained after reaction, finally, cleans repeatedly with deionized water, and reduce pressure sucking filtration, directly
It is neutral to pH value；By 50 DEG C of forced air dryings of filter membrane of obtaining 1 day, then 60 DEG C were vacuum dried 2 days, and product seals and preserves；
(2) preparation of graphene sheet layer:
Graphite oxide is placed in the quartz ampoule of sealing, under nitrogen atmosphere, is brought rapidly up 1100 DEG C, high-temperature process one
The section time, high-temperature process afterproduct is become the Graphene of black by tan graphene oxide lamella, and volume occurs the most swollen
Swollen, obtain graphene sheet layer；
(3) preparation of platinum/graphen lamella composite:
Be mixed grinding by 1kg graphene sheet layer and 1.7kg dimethyl (1,5-cyclo-octadiene) platinum；The sample that will mix
Product add in high pressure stainless steel reactor, and reactor seals, and are filled with carbon dioxide, get rid of air in still, open magnetic agitation, heating
To 80 DEG C, after being forced into 25MPa reaction 5.5h, presoma is sufficiently mixed with graphene sheet layer, takes out samples weighing；The most again
Sample is added high pressure stainless steel reactor, uses N2Wash away air in still, be slowly introducing N2, it is heated to 200 DEG C, reacts 5h, cooling
To room temperature, gas slowly is got rid of, collect sample；With a large amount of ethanol purge, filtration, going the removal of impurity, product is in vacuum drying
In case, 60 DEG C of vacuum drying 7h, obtain platinum/graphen lamella composite.
The carbon dioxide being filled with in the preparation process of described platinum/graphen lamella composite be volume fraction be 99.9%
The supercritical carbon dioxide that produces after temperature and pressure regulate of high-purity carbon dioxide.
The platinum/graphen lamella composite prepared be platinum grain the densest be deposited on graphene sheet layer surface.
Above the present invention is exemplarily described, it is clear that the present invention implements and is not subject to the restrictions described above,
As long as have employed method design and the various improvement that carry out of technical scheme of the present invention, or the most improved directly apply to other
Close, all within protection scope of the present invention.
Claims (3)
1. the preparation method of a platinum/graphen lamella composite, it is characterised in that concretely comprise the following steps:
(1) preparation of graphite oxide:
Low-temp reaction: under stirring condition, in the concentrated sulphuric acid of ice-water bath cooling, is slowly added into graphite powder and anhydrous nitric acid sodium,
After question response thing is mixed thoroughly, then it is slowly added into potassium permanganate, concentrated sulphuric acid, graphite powder, anhydrous nitric acid sodium and permanganic acid
The mass fraction of potassium is more than 1h than respectively 16:1:115:45, the time controlling charging, reacts 1.5h after having fed；
Middle temperature is reacted: after low-temp reaction, removes ice-water bath, and controlling temperature is 30 DEG C of stirring reactions 6 days, obtains sepia and produces
Thing；
Pyroreaction: be slowly added to the sulphuric acid dilute solution of 5%, the temperature of mixed liquor raises rapidly, treats that dilute sulfuric acid is added completely into
After, it is warming up to 90 DEG C of reaction 2.5h；Natural cooling afterwards, treats that temperature drops to 60 DEG C, adds in the hydrogen peroxide of 30% and unreacted
Potassium permanganate, react 2h；
Post processing: the mixed liquor filtration under diminished pressure obtained after reaction, finally, cleans repeatedly with deionized water, and reduce pressure sucking filtration, until PH
Value is neutrality；By 50 DEG C of forced air dryings of filter membrane of obtaining 1 day, then 60 DEG C were vacuum dried 2 days, and product seals and preserves；
(2) preparation of graphene sheet layer:
Graphite oxide is placed in the quartz ampoule of sealing, under nitrogen atmosphere, is brought rapidly up 1100 DEG C, during high-temperature process one section
Between, high-temperature process afterproduct is become the Graphene of black by tan graphene oxide lamella, and volume occurs substantially to expand,
To graphene sheet layer；
(3) preparation of platinum/graphen lamella composite:
Be mixed grinding by graphene sheet layer and dimethyl (1,5-cyclo-octadiene) platinum, the dimethyl of graphene sheet layer sum (1,
5-cyclo-octadiene) mass fraction of platinum is than for 1:1.5-1.9；The sample mixed is added in high pressure stainless steel reactor, instead
Answer device to seal, be filled with carbon dioxide, get rid of air in still, open magnetic agitation, be heated to 80 DEG C, be forced into 25MPa and react 5.5h
After, presoma is sufficiently mixed with graphene sheet layer, takes out samples weighing；The most again sample is added high pressure stainless steel reaction
Device, uses N2Wash away air in still, be slowly introducing N2, it is heated to 200 DEG C, reacts 5h, after being cooled to room temperature, gas slowly is got rid of,
Collect sample；With a large amount of ethanol purge, filtration, going the removal of impurity, product is 60 DEG C of vacuum drying 7h in vacuum drying oven, obtain
Platinum/graphen lamella composite.
The preparation method of a kind of platinum/graphen lamella composite the most according to claim 1, it is characterised in that described
The carbon dioxide being filled with in the preparation process of platinum/graphen lamella composite be volume fraction be high-purity titanium dioxide of 99.9%
The supercritical carbon dioxide that carbon produces after temperature and pressure regulate.
The preparation method of a kind of platinum/graphen lamella composite the most according to claim 2, it is characterised in that preparation
The platinum/graphen lamella composite gone out be platinum grain the densest be deposited on graphene sheet layer surface.
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| CN201610413872.XA CN106115664A (en) | 2016-06-13 | 2016-06-13 | A kind of preparation method of platinum/graphen lamella composite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107096926A (en) * | 2017-04-20 | 2017-08-29 | 华南理工大学 | A kind of supercritical CO2The method that original position prepares Au/ graphene nanocomposite materials |
| CN107539984A (en) * | 2017-10-19 | 2018-01-05 | 苏州方卓材料科技有限公司 | The preparation method of graphite material |
| CN111743192A (en) * | 2020-07-10 | 2020-10-09 | 湖北中烟工业有限责任公司 | Preparation method of geraniol-graphene oxide slow-release heat-conducting composite material for cigarettes |
-
2016
- 2016-06-13 CN CN201610413872.XA patent/CN106115664A/en not_active Withdrawn
Non-Patent Citations (1)
| Title |
|---|
| JIAN ZHAO等: "Supercritical Deposition Route of Preparing Pt/Graphene Composites and Their Catalytic Performance toward Methanol Electrooxidation", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107096926A (en) * | 2017-04-20 | 2017-08-29 | 华南理工大学 | A kind of supercritical CO2The method that original position prepares Au/ graphene nanocomposite materials |
| CN107539984A (en) * | 2017-10-19 | 2018-01-05 | 苏州方卓材料科技有限公司 | The preparation method of graphite material |
| CN111743192A (en) * | 2020-07-10 | 2020-10-09 | 湖北中烟工业有限责任公司 | Preparation method of geraniol-graphene oxide slow-release heat-conducting composite material for cigarettes |
| CN111743192B (en) * | 2020-07-10 | 2022-05-17 | 湖北中烟工业有限责任公司 | Preparation method of geraniol-graphene oxide slow-release heat-conducting composite material for cigarettes |
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Application publication date: 20161116 |