CN105329883A - Porous graphene preparation method - Google Patents
Porous graphene preparation method Download PDFInfo
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- CN105329883A CN105329883A CN201510661921.7A CN201510661921A CN105329883A CN 105329883 A CN105329883 A CN 105329883A CN 201510661921 A CN201510661921 A CN 201510661921A CN 105329883 A CN105329883 A CN 105329883A
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Abstract
The present invention belongs to the technical field of nanometer materials, and discloses a novel porous graphene preparation method, which specifically comprises: (1) respectively weighing a proper amount of a carbon-hydrogen-oxygen-containing organic matter and an inorganic salt; (2) uniformly mixing the carbon-hydrogen-oxygen-containing organic matter and the inorganic salt to obtain a mixture; and (3) heating the mixture under an inert gas atmosphere to achieve a temperature of 900-1600 DEG C so as to finally prepare the porous graphene. According to the present invention, the obtained graphene material having the porous structure has characteristics of uniform pore size distribution and controllable pore size, and is widely used in the fields of catalysis, adsorption, ultracapacitors and the like; the carbon-hydrogen-oxygen-containing organic matter and the inorganic salt are adopted as the raw materials to prepare the graphene, such that the variety of the raw materials is rich, the sources are wide, the cost is low, and the method is suitable for mass production; and the high temperature firing process is used, the process is simple and is easy to operate, no substance harm on the environment is introduced or generated, and the advantages of safety and environmental protection are provided.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to a kind of novel method preparing porous graphene based on carbohydrate and ammonium class inorganic salt, described prepare porous graphene facilitate Simple energy-saving.
Background technology
Graphene is because of its excellent optics, and electricity, mechanics, the characteristic such as biological and become the novel material of people's common concern, mono-layer graphite has large specific surface area, excellent conduction, heat conductivility and low thermal expansivity.Especially the textural property of its high connductivity character, large specific surface character and its unimolecular layer two-dimensional nanoscale, can be used as electrode materials in ultracapacitor and lithium ion battery.Theoretical Calculation shows that Graphene has the specific surface area (Science2009,323,610) up to 2630cm2/g.The grapheme material with vesicular structure is used for gas delivery by the people such as Jiang, proves that porous graphene is the mould material of a kind of high-level efficiency, highly selective.The preparation method of current Graphene comprises mechanically peel method, chemical stripping method, chemical synthesis, catalytic growth method and electrochemical stripping method etc.Current, the grapheme material preparation great majority about vesicular structure adopt the metals such as carrier loaded Fe, Co to be catalyzer, in certain temperature range, use the gas of inertia and carbon containing hydro carbons to carry out chemical vapor deposition to prepare the Graphene of vesicular structure.The advantage of this method is: can produce porous graphene low-costly and in high volume, shortcoming is: preparation method is complicated and in preparation process, have heavy metal to participate in reaction (the open patent application CN102115069A of China).In addition, the presoma of porous metal oxide template and carbon dissolves in organic solvent by the people such as Fan Zhuanjun, and vacuum is heat-treated under being placed in rare gas element, finally obtained the porous graphene with layer columnar structure after removing solvent.This porous graphene can reduce the resistance to mass transfer of graphene film interlayer, but preparation method is complicated and in preparation process, need the organic solvent adding contaminate environment.As can be seen here, in prior art Graphene preparation method's complicated operation and easily cause environmental pollution.
In view of the special structure of porous graphene, excellent performance, and the huge applications in fields such as catalysis, gas delivery, absorption and ultracapacitors, we need the preparation method finding a kind of simple, safety and environmental protection badly.The invention provides so a kind of synthetic route, using the organism of the carbon containing hydrogen-oxygen of cheapness as starting material, be aided with inorganic salt, made by high-temperature firing the carbon in the organism of carbon containing hydrogen-oxygen form vesicular Graphene.
Summary of the invention
In view of there is above-mentioned technical problem in prior art, the invention provides a kind of preparation method of novel porous graphene, the organism of the carbon containing hydrogen-oxygen that the method use is cheap and inorganic salt are as starting material, the starting material of synthesizing graphite alkene are developed, cost reduces rapidly, and adopt high-temperature firing technique, the porous graphene meeting different demand can be prepared quickly and easily, preparation technology is simplified greatly.The method of the invention has with low cost, and starting material are extensive, and the advantages such as technique is simple can be used for large batch of suitability for industrialized production, have greatly promoted the commercial applications of Graphene.
The novel method preparing porous graphene of the present invention, its concrete steps are: (1) takes organism, the inorganic salt of appropriate carbon containing hydrogen-oxygen respectively; (2) organism of carbon containing hydrogen-oxygen and inorganic salt are mixed, obtain mixture; (3) said mixture is heated to 900-1600 DEG C in an inert atmosphere, finally obtained porous graphene.
Above-mentionedly prepare in the method for porous graphene, in step (1), the organism of described carbon containing hydrogen-oxygen can be carbohydrate or other contain one or more mixture in the organism (as graphene oxide GO) of hydrocarbon oxygen element, described carbohydrate can be glucose, sucrose, white sugar or maltose.
Above-mentionedly prepare in the method for porous graphene, in step (1), described inorganic salt also can be one or more the mixtures in ammonium chloride, volatile salt, bicarbonate of ammonia, calcium carbonate, sodium bicarbonate or ammonium sulfate.
Above-mentionedly prepare in the method for porous graphene, in step (2), the organism of starting material carbon containing hydrogen-oxygen and inorganic salt in mass ratio routine 1:0.1-1:10 mix, and also can be that between them, multiple different substances mixes at random.
Above-mentionedly prepare in the method for porous graphene, in step (2), the organism of described starting material carbon containing hydrogen-oxygen can mix with inorganic salt under solution state, also can grind in the solid state and mix.
Above-mentionedly prepare in the method for porous graphene, in step (3), described rare gas element can be nitrogen or argon gas.
Above-mentionedly prepare in the method for porous graphene, in step (3), adopt mixture described in diamond heating, in described tube furnace, baking temperature range is 900 DEG C-1600 DEG C, heat-up rate is 4 DEG C/and min-8 DEG C/min.
Above-mentionedly prepare in the method for porous graphene, the starting material adopted, raw-material blending ratio, the temperature and time etc. fired can have an impact to the pore size of obtained porous graphene, can change the porous graphene of above-mentioned processing condition for the preparation of different pore size.
For 300nm-3um aperture, technical scheme of the present invention is described below.Glucose and ammonium chloride first mix by we, 1400 DEG C are heated in a nitrogen environment by tube furnace, Graphene under making the carbon in glucose form porous state, can regulate and control pore size and distribution on Graphene by the amount of regulating and controlling temperature and ammonium chloride in technique scheme.
The novel method preparing porous graphene of the present invention has following beneficial effect:
1, the method for the invention, the grapheme material with vesicular structure of acquisition, its even aperture distribution, and pore size is controlled, and in catalysis, absorption, the fields such as ultracapacitor have a wide range of applications;
What 2, the method for the invention used the organism of carbon containing hydrogen-oxygen and inorganic salt prepares Graphene for starting material, and raw material types is enriched, wide material sources, with low cost, is convenient to large-scale production.
3, the method for the invention adopts high-temperature firing technique, and technique is simple, convenient operation, does not have to introduce or produce the material being unfavorable for environment, safety and environmental protection.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) picture of the porous graphene that embodiment 1 obtains.
Fig. 2 is scanning electron microscope (SEM) picture after the porous graphene mesoporous obtained to embodiment 1 amplifies.
Embodiment
Below in conjunction with specific embodiment, the novel method preparing porous graphene of the present invention is described.
(1) organism and the inorganic salt of appropriate carbon containing hydrogen-oxygen are taken respectively; (2) organism of carbon containing hydrogen-oxygen and inorganic salt are mixed, obtain mixture; (3) said mixture is heated to 900-1600 DEG C in an inert atmosphere, finally obtained porous graphene.
Embodiment 1
(1) glucose of 5g and the ammonium chloride of 0.5g is taken respectively;
(2) glucose and ammonium chloride are poured in the beaker cleaned in advance, and mix, obtain both mixtures;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace in a nitrogen atmosphere with the ramp to 1400 DEG C of 4 DEG C/min, finally obtained porous graphene.
The analysis of SEM electron microscope scanning is carried out to obtained porous graphene, its result as depicted in figs. 1 and 2, can find out that from Fig. 1 (a) and (b) the porous graphene cavernous structure that this programme obtains is obvious, be evenly distributed, and pore size is homogeneous, by further amplifying observation, as Fig. 2 more obviously can find out that its aperture is between 2-4 μm.
Embodiment 2
(1) glucose of 5g, the calcium chloride of 5g and 4.4g volatile salt is taken respectively
(2) glucose, calcium chloride and volatile salt are mixed, obtain mixture;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace under an argon atmosphere with the ramp to 900 DEG C of 4 DEG C/min, finally obtained porous graphene.
Embodiment 3
(1) glucose of 1g, the ammonium chloride of 10g is taken respectively;
(2) glucose, graphene oxide and calcium carbonate are mixed, obtain mixture;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace in a nitrogen atmosphere with the ramp to 1400 DEG C of 4 DEG C/min, finally obtained porous graphene.
Embodiment 4
(1) graphene oxide (GO) of 1g, the ammonium chloride of 5g is taken respectively;
(2) graphene oxide (GO) and ammonium chloride are mixed, obtain mixture;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace in a nitrogen atmosphere with the ramp to 1600 DEG C of 6 DEG C/min, finally obtained porous graphene.
Embodiment 5
(1) white sugar of 5g and the bicarbonate of ammonia of 5g is taken respectively;
(2) white sugar and bicarbonate of ammonia are mixed, obtain mixture;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace in a nitrogen atmosphere with the ramp to 1000 DEG C of 8 DEG C/min, finally obtained porous graphene.
Embodiment 6
(1) bicarbonate of ammonia of the glucose of 4g, the white sugar of 4g and 5g is taken respectively;
(2) glucose, white sugar and bicarbonate of ammonia are mixed, obtain mixture;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace in a nitrogen atmosphere with the ramp to 1200 DEG C of 6 DEG C/min, finally obtained porous graphene.
Embodiment 7
(1) white sugar of 5g, the graphene oxide (GO) of 0.2g and the calcium carbonate of 5g is taken respectively;
(2) white sugar, graphene oxide and calcium carbonate are mixed, obtain mixture;
(3) said mixture to be transferred in ceramic cup and to put into tube furnace, tube furnace in a nitrogen atmosphere with the ramp to 1400 DEG C of 4 DEG C/min, finally obtained porous graphene.
Claims (8)
1. prepare a method for porous graphene, it is characterized in that, the concrete steps of described method are:
(1) organism, the inorganic salt of appropriate carbon containing hydrogen-oxygen are taken respectively; (2) organism of carbon containing hydrogen-oxygen and inorganic salt are mixed, obtain mixture; (3) said mixture is heated to 900 DEG C-1600 DEG C in an inert atmosphere, finally obtained porous graphene.
2. method according to claim 1, it is characterized in that, the compound of the carbon containing hydrogen-oxygen described in step (1) be carbohydrate or other contain one or more mixture in the organism of hydrocarbon oxygen, described carbohydrate can be glucose, sucrose, white sugar or maltose.
3. method according to claim 1, is characterized in that, the inorganic salt described in step (1) are one or more the mixtures in ammonium chloride, volatile salt, bicarbonate of ammonia, calcium carbonate, sodium bicarbonate or ammonium sulfate.
4. in accordance with the method for claim 1, it is characterized in that, the organism of carbon containing hydrogen-oxygen described in step (2) and inorganic salt in mass ratio routine 1:0.1-1:10 mix.
5. in accordance with the method for claim 1, it is characterized in that, the organism of carbon containing hydrogen-oxygen described in step (2) can mix with inorganic salt under solution state, also can grind in the solid state and mix.
6. in accordance with the method for claim 1, it is characterized in that, described in step (3), rare gas element is nitrogen or argon gas.
7. in accordance with the method for claim 1, it is characterized in that, adopt mixture described in diamond heating.
8. according to Preparation Method according to claim 7, it is characterized in that, in described tube furnace, baking temperature range is 900 DEG C-1600 DEG C, heat-up rate is 4 DEG C/and min-8 DEG C/min.
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Cited By (6)
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| CN105621406A (en) * | 2016-02-29 | 2016-06-01 | 上海交通大学 | Nitrogen-doped porous graphite and preparation method thereof |
| CN106185890A (en) * | 2016-07-04 | 2016-12-07 | 石河子大学 | A kind of preparation method of porous class Graphene |
| CN106185889A (en) * | 2016-07-04 | 2016-12-07 | 苏州云舒新材料科技有限公司 | A kind of grapheme material and preparation method thereof |
| CN110104641A (en) * | 2019-05-05 | 2019-08-09 | 华北电力大学 | A kind of preparation method and application of foam-like 3 D stereo graphene oxide |
| CN111484002A (en) * | 2020-04-17 | 2020-08-04 | 南京动量材料科技有限公司 | Preparation method and application of porous graphene membrane |
| CN111659346A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Haze collecting, absorbing and converting system based on primary battery principle |
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| CN104966812A (en) * | 2014-12-01 | 2015-10-07 | 天津大学 | Three-dimensional porous quasi-graphene loaded molybdenum disulfide composite and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621406A (en) * | 2016-02-29 | 2016-06-01 | 上海交通大学 | Nitrogen-doped porous graphite and preparation method thereof |
| CN106185890A (en) * | 2016-07-04 | 2016-12-07 | 石河子大学 | A kind of preparation method of porous class Graphene |
| CN106185889A (en) * | 2016-07-04 | 2016-12-07 | 苏州云舒新材料科技有限公司 | A kind of grapheme material and preparation method thereof |
| CN111659346A (en) * | 2019-03-08 | 2020-09-15 | 天津大学 | Haze collecting, absorbing and converting system based on primary battery principle |
| CN110104641A (en) * | 2019-05-05 | 2019-08-09 | 华北电力大学 | A kind of preparation method and application of foam-like 3 D stereo graphene oxide |
| CN110104641B (en) * | 2019-05-05 | 2021-03-16 | 华北电力大学 | Preparation method and application of foamy three-dimensional graphene oxide |
| CN111484002A (en) * | 2020-04-17 | 2020-08-04 | 南京动量材料科技有限公司 | Preparation method and application of porous graphene membrane |
| CN111484002B (en) * | 2020-04-17 | 2023-06-09 | 南京动量材料科技有限公司 | Preparation method and application of porous graphene film |
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Application publication date: 20160217 |