CN103449414B - There is the preparation method of the Graphene of loose structure - Google Patents
There is the preparation method of the Graphene of loose structure Download PDFInfo
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Abstract
The preparation method of a kind of Graphene with loose structure, comprises the steps: that graphite oxide, reducing agent and pore creating material are added in deionized water by (1), and mix homogeneously obtains mixed liquor；Wherein, the mass ratio of graphite oxide, reducing agent and pore creating material is 1:(0.1 ~ 1): (0.2 ~ 0.5)；(2) mixed liquor is heated to 80 DEG C ~ 100 DEG C, reduction reaction occurs, obtains the mixture of Graphene and pore creating material；(3) after being dried 24 hours ~ 48 hours at 60 DEG C ~ 80 DEG C by mixture, being heated to 300 DEG C ~ 400 DEG C, insulation reaction, after 3 minutes ~ 5 minutes, in protection compression ring border, is cooled to room temperature, obtains the Graphene with loose structure.The preparation method of the above-mentioned Graphene with loose structure is simple, and raw material sources required in preparation process are wide and low cost, and reaction temperature is low, it is easy to control, thus can realize batch production.
Description
Technical field
The present invention relates to the synthesis field of material, particularly to the preparation method of a kind of Graphene with loose structure.
Background technology
Graphene is that peace moral strong K sea nurse (Andre K.Geim) of Univ Manchester UK in 2004 etc. finds
A kind of Two-dimensional Carbon atomic crystal, and obtain physics Nobel Prize in 2010, re-initiation material with carbon element research boom.Owing to it is unique
Structure and photoelectric property become the study hotspot in the fields such as material with carbon element, nanotechnology, Condensed Matter Physics and functional material,
Many scientific workers are attracted.Single-layer graphene has excellent conduction, heat conductivility and low thermal coefficient of expansion, and its
Theoretical specific surface area is up to 2630m2/ g(A Peigney, Ch Laurent, et al.Carbon, 2001,39,507), available
In effect transistor, electrode material, composite, liquid crystal display material, sensor etc..The preparation method of traditional Graphene is still
The place come with some shortcomings, it is difficult to prepare the Graphene with specific morphology.And current, there is researcher to provide porous stone
The preparation method of ink alkene, but its operation is excessively complicated, it is difficult to control.
Summary of the invention
In consideration of it, be necessary to provide the side of the Graphene that preparation that is a kind of simple to operate and that be relatively easy to control has loose structure
Method.
The preparation method of a kind of Graphene with loose structure, comprises the steps:
Step one: graphite oxide, reducing agent and pore creating material are added in deionized water, mix homogeneously, obtain mixed liquor；Its
In, the mass ratio of described graphite oxide, reducing agent and pore creating material is 1:(0.1 ~ 1): (0.2 ~ 0.5)；
, there is reduction reaction in step 2: described mixed liquor is heated to 80 DEG C ~ 100 DEG C, obtains Graphene and described pore-creating
The mixture of agent；And
Step 3: after being dried 24 hours ~ 48 hours at 60 DEG C ~ 80 DEG C by described mixture, be heated to 300 DEG C ~ 400
DEG C, insulation reaction is after 3 minutes ~ 5 minutes, in protection compression ring border, is cooled to room temperature, obtain described in there is the graphite of loose structure
Alkene.
Wherein in an embodiment, in step one, described reducing agent is hydrazine, sodium borohydride, potassium borohydride and citric acid
At least one in sodium.
Wherein in an embodiment, in step one, described pore creating material is sodium bicarbonate or potassium bicarbonate.
Wherein in an embodiment, in step one, described graphite oxide, described reducing agent, described pore creating material and described
The mixed method of deionized water is ultrasonic mixing 30 minutes ~ 60 minutes.
Wherein in an embodiment, after step 2, also include the product after described reduction reaction is carried out filtering and
The step cleaned.
Wherein in an embodiment, in step 3, described protection gas is at least one in hydrogen, argon and nitrogen.
Wherein in an embodiment, in step 3, the product after described insulation reaction is in described protection compression ring border
The speed of cooling is 30 DEG C/min～50 DEG C/min.
The preparation method of the above-mentioned Graphene with loose structure, graphite oxide is reduced into Graphene, pore-creating by reducing agent
The Graphene with loose structure is prepared in agent by high temperature decomposing, and its preparation method is simple, and institute in preparation process
The raw material sources needed are wide and low cost, and reaction temperature is low, it is easy to control, thus can realize batch production.
Accompanying drawing explanation
Fig. 1 is the preparation method flow chart of the Graphene with loose structure of an embodiment；
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) of the Graphene with loose structure of embodiment 1 preparation.
Detailed description of the invention
Preparation method mainly in combination with the drawings and the specific embodiments Graphene to having loose structure is made further below
Detailed description.
As it is shown in figure 1, the preparation method of the Graphene with loose structure of an embodiment, including such as step:
Step S1: graphite oxide, reducing agent and pore creating material are added in deionized water, mix homogeneously, obtain mixed liquor.Its
In, the mass ratio of graphite oxide, reducing agent and pore creating material is 1:(0.1 ~ 1): (0.2 ~ 0.5).
Wherein, graphite oxide is conventional graphite oxide.
Wherein, the mixed method of graphite oxide, reducing agent, pore creating material and deionized water is ultrasonic mixing 30 minutes ~ 60 points
Clock.
Wherein, reducing agent is reducing agent commonly used in the art, preferably hydrazine, sodium borohydride, potassium borohydride and sodium citrate
In at least one.Graphite oxide is reduced into Graphene by reducing agent.
Wherein, pore creating material is pore creating material commonly used in the art, preferably sodium bicarbonate or potassium bicarbonate.Pore creating material can be
Decomposing under high temperature, discharge carbon dioxide, thus leave abundant hole on Graphene, reaction equation is as follows:
The chemical equation of sodium bicarbonate pyrolytic:
The chemical equation of potassium bicarbonate pyrolytic:
, there is reduction reaction, obtain the mixing of Graphene and pore creating material in step S2: mixed liquor is heated to 80 DEG C ~ 100 DEG C
Thing.
In the present embodiment, after step S2, also include the step that the product after reduction reaction is filtered and cleaned.
By filtering and cleaning, obtain the mixture of purer Graphene and pore creating material.
Step S3: after being dried 24 hours ~ 48 hours at 60 DEG C～80 DEG C by mixture, be heated to 300 DEG C ~ 400 DEG C, protects
After temperature reaction 3 minutes ~ 5 minutes, in protection compression ring border, it is cooled to room temperature, obtains the Graphene with loose structure.Insulation is anti-
Answering 3 minutes ~ 5 minutes makes pore creating material decompose more complete.In the present embodiment, the product after insulation reaction is at protection compression ring
The speed of the cooling in border is 30 DEG C/min～50 DEG C/min, by cooling rapidly, thus at stone after keeping pore creating material to decompose
The hole stayed on ink alkene is not closed so that Graphene has the structure of porous.Wherein, protection gas is hydrogen, argon and nitrogen
In at least one.When using sodium bicarbonate or potassium bicarbonate as pore creating material, the step after step S3, to the cleaning of Graphene
Rapid: in Graphene, to add deionized water, filter, until filtrate is neutrality.By cleaning Graphene, remove sodium ion therein
Or potassium ion.
The preparation method of the above-mentioned Graphene with loose structure, graphite oxide is reduced into Graphene, pore-creating by reducing agent
The Graphene with loose structure is prepared in agent by high temperature decomposing, and its preparation method is simple, and institute in preparation process
The raw material sources needed are wide and low cost, and reaction temperature is low, it is easy to control, thus can realize batch production.And above-mentioned preparation method
The Graphene prepared has abundant hole, and oxygen content is low, can be applicable to noise reduction, deadener, gas absorption etc..
It is below specific embodiment part:
Embodiment 1
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.1g in beaker
Hydrazine and 0.2g sodium bicarbonate add in deionized water, and ultrasonic mixing 30 minutes obtains mixed liquor.
(2) mixed liquor is heated to 100 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and sodium bicarbonate
Compound.
(3), after mixture being dried 24 hours at 60 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 300 DEG C,
After insulation reaction 5 minutes, in the hydrogen gas atmosphere, being cooled to room temperature, cooldown rate is 30 DEG C/min, opens reacting furnace, collects solid
Body product, adds deionized water in solid product, filters, repeatedly add deionized water, filtration, until filtrate is neutrality, obtain
There is the Graphene of loose structure.Fig. 2 is the scanning electron microscope (SEM) photograph of the Graphene with loose structure prepared by the present embodiment
(SEM), it can be seen that the Graphene with loose structure prepared by the present embodiment has abundant hole, hole
Size is about 1nm～3nm from 1nm～500nm, lamellar spacing so that the specific surface area of Graphene is 1270m2/g。
Embodiment 2
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 1g boron in beaker
Sodium hydride and 0.4g sodium bicarbonate add in deionized water, and ultrasonic mixing 60 minutes obtains mixed liquor.
(2) mixed liquor is heated to 90 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and sodium bicarbonate
Compound.
(3), after mixture being dried 36 hours at 80 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 400 DEG C,
After insulation reaction 3 minutes, in ar gas environment, being cooled to room temperature, cooldown rate is 50 DEG C/min, opens reacting furnace, collects solid
Body product, adds deionized water in solid product, filters, repeatedly add deionized water, filtration, until filtrate is neutrality, obtain
There is the Graphene of loose structure.
Embodiment 3
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.8g in beaker
Potassium borohydride and 0.3g potassium bicarbonate add in deionized water, and ultrasonic mixing 40 minutes obtains mixed liquor.
(2) mixed liquor is heated to 95 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and potassium bicarbonate
Compound.
(3), after mixture being dried 30 hours at 70 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 400 DEG C,
After insulation reaction 4 minutes, in nitrogen environment, being cooled to room temperature, cooldown rate is 40 DEG C/min, opens reacting furnace, collects solid
Body product, adds deionized water in solid product, filters, repeatedly add deionized water, filtration, until filtrate is neutrality, obtain
There is the Graphene of loose structure.
Embodiment 4
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.5g in beaker
Sodium citrate and 0.5g potassium bicarbonate add in deionized water, and ultrasonic mixing 50 minutes obtains mixed liquor.
(2) mixed liquor is heated to 80 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and potassium bicarbonate
Compound.
(3), after mixture being dried 48 hours at 65 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 350 DEG C,
After insulation reaction 5 minutes, in the gaseous mixture environment of hydrogen and argon, being cooled to room temperature, cooldown rate is 45 DEG C/min, opens
Reacting furnace, collects solid product, adds deionized water, filter, repeatedly add deionized water, filtration in solid product, until filter
Liquid is neutrality, obtains the Graphene with loose structure.
Embodiment 5
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.2g in beaker
Hydrazine and 0.2g potassium bicarbonate add in deionized water, and ultrasonic mixing 60 minutes obtains mixed liquor.
(2) mixed liquor is heated to 95 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and potassium bicarbonate
Compound.
(3), after mixture being dried 35 hours at 70 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 320 DEG C,
After insulation reaction 5 minutes, in the gaseous mixture environment of hydrogen, argon and nitrogen, it being cooled to room temperature, cooldown rate is 35 DEG C/
Min, opens reacting furnace, collects solid product, adds deionized water, filter, repeatedly add deionized water, mistake in solid product
Filter, until filtrate is neutrality, obtains the Graphene with loose structure.
Embodiment 6
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.8g in beaker
Sodium borohydride and 0.3g potassium bicarbonate add in deionized water, and ultrasonic mixing 50 minutes obtains mixed liquor.
(2) mixed liquor is heated to 85 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and potassium bicarbonate
Compound.
(3), after mixture being dried 45 hours at 65 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 400 DEG C,
After insulation reaction 3 minutes, in the gaseous mixture environment of hydrogen and nitrogen, being cooled to room temperature, cooldown rate is 40 DEG C/min, opens
Reacting furnace, collects solid product, adds deionized water, filter, repeatedly add deionized water, filtration in solid product, until filter
Liquid is neutrality, obtains the Graphene with loose structure.
Embodiment 7
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 1g boron in beaker
Hydrofining and 0.5g sodium bicarbonate add in deionized water, and ultrasonic mixing 40 minutes obtains mixed liquor.
(2) mixed liquor is heated to 100 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and sodium bicarbonate
Compound.
(3), after mixture being dried 24 hours at 80 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 380 DEG C,
After insulation reaction 5 minutes, in the gaseous mixture environment of argon and nitrogen, being cooled to room temperature, cooldown rate is 45 DEG C/min, opens
Reacting furnace, collects solid product, adds deionized water, filter, repeatedly add deionized water, filtration in solid product, until filter
Liquid is neutrality, obtains the Graphene with loose structure.
Embodiment 8
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.3g in beaker
Sodium citrate and 0.4g potassium bicarbonate add in deionized water, and ultrasonic mixing 30 minutes obtains mixed liquor.
(2) mixed liquor is heated to 80 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and potassium bicarbonate
Compound.
(3), after mixture being dried 48 hours at 75 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 330 DEG C,
After insulation reaction 3 minutes, in the hydrogen gas atmosphere, being cooled to room temperature, cooldown rate is 50 DEG C/min, opens reacting furnace, collects solid
Body product, adds deionized water in solid product, filters, repeatedly add deionized water, filtration, until filtrate is neutrality, obtain
There is the Graphene of loose structure.
Embodiment 9
(1) selecting capacity is the beaker of 1L, adds the deionized water of 1L, then by 1g graphite oxide, 0.5g in beaker
Hydrazine, 0.2g sodium borohydride and 0.2g potassium bicarbonate add in deionized water, and ultrasonic mixing 60 minutes obtains mixed liquor.
(2) mixed liquor is heated to 95 DEG C, reduction reaction occurs, filter and clean, obtain the mixed of Graphene and potassium bicarbonate
Compound.
(3), after mixture being dried 45 hours at 60 DEG C, it is placed on quartz boat, and in reacting furnace, is heated to 300 DEG C,
After insulation reaction 5 minutes, in nitrogen environment, being cooled to room temperature, cooldown rate is 30 DEG C/min, opens reacting furnace, collects solid
Body product, adds deionized water in solid product, filters, repeatedly add deionized water, filtration, until filtrate is neutrality, obtain
There is the Graphene of loose structure.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (6)
1. the preparation method of a Graphene with loose structure, it is characterised in that comprise the steps:
Step one: graphite oxide, reducing agent and pore creating material are added in deionized water, mix homogeneously, obtain mixed liquor；Wherein,
The mass ratio of described graphite oxide, reducing agent and pore creating material is 1:(0.1～1): (0.2～0.5)；
, there is reduction reaction in step 2: described mixed liquor is heated to 80 DEG C～100 DEG C, obtains Graphene and described pore creating material
Mixture；And
Step 3: after being dried 24 hours～48 hours at 60 DEG C～80 DEG C by described mixture, be heated to 300 DEG C～400 DEG C,
After insulation reaction 3 minutes～5 minutes, in protection compression ring border, be cooled to room temperature, obtain described in there is the graphite of loose structure
Alkene；
In step one, described pore creating material is sodium bicarbonate or potassium bicarbonate.
2. according to the preparation method of the Graphene with loose structure described in claim 1, it is characterised in that step one
In, described reducing agent is at least one in hydrazine, sodium borohydride, potassium borohydride and sodium citrate.
3. according to the preparation method of the Graphene with loose structure described in claim 1, it is characterised in that step one
In, the mixed method of described graphite oxide, described reducing agent, described pore creating material and described deionized water is ultrasonic mixing 30 minutes
～60 minutes.
4. according to the preparation method of the Graphene with loose structure described in claim 1, it is characterised in that step 2 it
After, also include the step that the product after described reduction reaction is filtered and cleaned.
5. according to the preparation method of the Graphene with loose structure described in claim 1, it is characterised in that step 3
In, described protection gas is at least one in hydrogen, argon and nitrogen.
6. according to the preparation method of the Graphene with loose structure described in claim 1, it is characterised in that step 3
In, the speed of the cooling in described protection compression ring border of the product after described insulation reaction is 30 DEG C/min～50 DEG C/min.
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| CN105869924B (en) * | 2016-05-06 | 2018-02-23 | 清华大学深圳研究生院 | A kind of preparation method of graphene-based thick cipher telegram pole |
| US10332693B2 (en) | 2016-07-15 | 2019-06-25 | Nanotek Instruments, Inc. | Humic acid-based supercapacitors |
| CN106395802B (en) * | 2016-09-08 | 2020-08-11 | 山东理工大学 | Preparation method of graphene porous membrane |
| CN108584927B (en) * | 2018-05-24 | 2020-03-13 | 浙江农业商贸职业学院 | Preparation method of porous graphene powder for automobile alloy material |
| CN114497513A (en) * | 2022-03-05 | 2022-05-13 | 青岛泰达华润新能源科技有限公司 | Graphene negative electrode material for lithium ion battery and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009029984A1 (en) * | 2007-09-03 | 2009-03-12 | Newsouth Innovations Pty Limited | Graphene |
| CN101454243A (en) * | 2006-05-31 | 2009-06-10 | 促进科学E.V.麦克斯-普朗克公司 | Porous carbon electrode with conductive polymer coating |
| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| CN102239114A (en) * | 2008-12-04 | 2011-11-09 | 泰科电子公司 | Graphene and graphene oxide aerogels |
| CN102408109A (en) * | 2011-08-23 | 2012-04-11 | 中国科学院上海应用物理研究所 | Reduced graphene oxide and preparation method thereof |
| CN102414124A (en) * | 2009-04-24 | 2012-04-11 | 丰田自动车株式会社 | Carbon material and method for producing same |
| WO2012057702A1 (en) * | 2010-10-28 | 2012-05-03 | Nanyang Technological University | Method of preparing a porous graphene film |
| CN102464315A (en) * | 2010-11-18 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
-
2012
- 2012-05-31 CN CN201210176562.2A patent/CN103449414B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101454243A (en) * | 2006-05-31 | 2009-06-10 | 促进科学E.V.麦克斯-普朗克公司 | Porous carbon electrode with conductive polymer coating |
| WO2009029984A1 (en) * | 2007-09-03 | 2009-03-12 | Newsouth Innovations Pty Limited | Graphene |
| CN102239114A (en) * | 2008-12-04 | 2011-11-09 | 泰科电子公司 | Graphene and graphene oxide aerogels |
| CN102414124A (en) * | 2009-04-24 | 2012-04-11 | 丰田自动车株式会社 | Carbon material and method for producing same |
| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
| WO2012057702A1 (en) * | 2010-10-28 | 2012-05-03 | Nanyang Technological University | Method of preparing a porous graphene film |
| CN102464315A (en) * | 2010-11-18 | 2012-05-23 | 海洋王照明科技股份有限公司 | Preparation method of graphene |
| CN102408109A (en) * | 2011-08-23 | 2012-04-11 | 中国科学院上海应用物理研究所 | Reduced graphene oxide and preparation method thereof |
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