CN107619040A - The method that partial combustion method quickly prepares porous graphene - Google Patents
The method that partial combustion method quickly prepares porous graphene Download PDFInfo
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Abstract
The invention discloses the method that partial combustion method quickly prepares porous graphene, concretely comprise the following steps：Zinc nitrate is added in graphene oxide water slurry, 2 30 min of ultrasound, then with quantitative filter paper rapid filtration under suction, the graphene oxide compound of the endless all standing of zinc nitrate neatly layer is obtained on filter paper；By the filter paper with compound after 35 55 DEG C of drying, in being lighted on alcolhol burner, after black graphene completely burned, the compound of Zinc oxide nanoparticle and porous graphene is can obtain, porous graphene is can obtain after being cleaned 18 times with strong acid, washed.Burning synthesis method is used in the preparation of porous graphene by the present invention, realizes the low temperature of porous graphene, simple and quick preparation process, so as to considerably reduce the preparation cost of porous graphene, improves utilization ratio.
Description
Technical field
The present invention relates to the method that partial combustion method quickly prepares porous graphene.
Background technology
Porous graphene because its surface it is more the defects of, there is the mass-transfer efficiency higher than graphene, therefore in energy electricity
The field such as pond, the storing of gas, biomedical, separation analysis has the function that important.The preparation method of porous graphene at present
Have：Ion beam bombardment method, highly basic etching method, metal thermal etching process, high temperature carbothermic method, aryl-aryl coupling reaction method
Deng.But these methods are required to the equipment requirement of higher cost, longer generated time and complexity, so as to seriously restrict
The prepare with scale of porous graphene and its production application in industrial circle.
The content of the invention
It is an object of the invention to provide a kind of method that graphene oxide partial combustion method quickly prepares porous graphene.
The present invention uses the neatly layer that zinc nitrate is spontaneously formed in graphenic surface as fire retardant, while by controlling nitre
The addition of sour zinc, can form the neatly layer of different degree of imperfections in graphenic surface, during burning, without the graphite of neatly layer covering
Alkene exposed part will be carbon dioxide by direct oxidation, and the part covered will be retained, while high temperature caused by burning will not
The oxy radical of combustion parts surface of graphene oxide removes, and is then washed away the metal oxide on surface with salt, so as to prepare
Go out porous graphene material.Combustion synthesis method is applied in the preparation of porous graphene by the present invention, significantly reduces porous stone
The preparation cost of black alkene, has saved generated time, has simplified synthesis step, improved production efficiency.
The method that partial combustion method quickly prepares porous graphene, it is characterised in that concretely comprise the following steps：Zinc nitrate is added
In graphene oxide water slurry, ultrasonic 2-30 min, then with quantitative filter paper rapid filtration under suction, zinc nitrate water is obtained on filter paper
The graphene oxide compound of the endless all standing of slip layer；By the filter paper with compound after 35-55 DEG C of drying, on alcolhol burner
Light, after black graphene completely burned, can obtain the compound of Zinc oxide nanoparticle and porous graphene, it is clear with strong acid
Wash 1-8 times, washing after can obtain porous graphene.
The mass ratio of the zinc nitrate and graphene oxide is 25:1- 200:1.
The concentration of the graphene oxide water slurry is 1-2 g/L.
The strong acid of the washing is hydrochloric acid or nitric acid, and concentration is 0.01-0.1 mol/L, centrifuge washing 3-6 times.
The present invention can be with endless all standing surface of graphene oxide, by unlapped graphite oxide using zinc nitrate neatly layer
The conflagration of alkene part, the step for realizing porous graphene are quickly prepared, and obtain being dispersed with a large amount of nano level holes（10~
100 nm）Porous graphene material, porous graphene surface has the specific surface area of super large（~800 m2/g）, there is amplification
The potentiality of production and very extensive application prospect.
The present invention has advantages below：
1）This method does not need starvation or air, it is not necessary to high temperature, therefore course of reaction is easy, economical, quick.
2）This method prepares porous graphene material by partial combustion method, and the accessory substance of burning is tractable gas
（Carbon dioxide and nitrogen dioxide）, therefore it is more green.
3）This method does not need complicated course of reaction and advanced reaction vessel, and cost is low, has large-scale application
Potentiality.
Brief description of the drawings
Fig. 1 is the syntheti c route and preparating mechanism figure of porous graphene of the present invention.
Fig. 2 is the phenogram of porous graphene.Wherein a transmission electron microscope pictures；B characterizes for XPS；C is Raman spectral characterizations；d
For pore analysis.
Embodiment
The preparation of the porous graphene of embodiment 1
Operating procedure：
1. the 1 g/L mL of graphene oxide suspension 2 is configured first, 10 min of normal temperature ultrasound.
2. weighing 50 mg zinc nitrates, it is dissolved in above-mentioned suspension, 2 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 35 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 0.01 mol/L hydrochloric acid, 4 washings, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 2
Operating procedure：
1. the 1 g/L mL of graphene oxide suspension 2 is configured first, 10 min of normal temperature ultrasound.
2. weighing 100 mg zinc nitrates, it is dissolved in above-mentioned suspension, 2 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 35 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 0.01 mol/L hydrochloric acid, 4 washings, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 3
Operating procedure：
1. the 1 g/L mL of graphene oxide suspension 2 is configured first, 10 min of normal temperature ultrasound.
2. weighing 200 mg zinc nitrates, it is dissolved in above-mentioned suspension, 4 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 35 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 0.01 mol/L hydrochloric acid, 4 washings, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 4
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 2 is configured first, 10 min of normal temperature ultrasound.
2. weighing 500 mg zinc nitrates, it is dissolved in above-mentioned suspension, 5 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 35 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. being washed using 0.05 mol/L hydrochloric acid 5, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 5
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 5 is configured first, 10 min of normal temperature ultrasound.
2. weighing 1 g zinc nitrates, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 40 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 5 washings of 0.01mol/L nitric acid, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 6
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 10 is configured first, 10 min of normal temperature ultrasound.
2. weighing 1.5 g zinc nitrates, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 45 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 5 washings of 0.01mol/L nitric acid, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 7
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 10 is configured first, 10 min of normal temperature ultrasound.
2. weighing 2 g zinc nitrates, it is dissolved in above-mentioned suspension, 30 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 50 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 8 washings of 0.01mol/L hydrochloric acid, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 8
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 10 is configured first, 10 min of normal temperature ultrasound.
2. weighing 4 g zinc nitrates, it is dissolved in above-mentioned suspension, 30 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 55 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. being washed using 0.05mol/L nitric acid 10, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 9
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 20 is configured first, 10 min of normal temperature ultrasound.
2. weighing 5g zinc nitrates, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 55 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 0.1 mol/L hydrochloric acid, 4 washings, porous graphene is can obtain after washing 3 times.
The preparation of the porous graphene of embodiment 10
Operating procedure：
1. the 2 g/L mL of graphene oxide suspension 20 is configured first, 10 min of normal temperature ultrasound.
2. weighing 6 g zinc nitrates, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filter above-mentioned solution using quantitative filter paper.
4. by filter paper and residue in 55 DEG C of drying.
5. the filter paper with residue is lighted, sinter to white zinc oxide covering porous graphene and occur.
6. using 0.1 mol/L nitric acid, 4 washings, porous graphene is can obtain after washing 3 times.
Most of experiment parameter in fixed embodiment 1, can be by transmiting electricity using the addition of zinc nitrate as dependent variable
Mirror（TEM）Investigate the surface topography of porous graphene prepared by this method.The experimental result table of the porous graphene wherein prepared
Sign is as shown in Figure 2.
Surface topography and crystal characterization：For porous graphene, it is necessary to which using transmission electron microscope observing pattern, gained TEM shines
As shown in Figure 2 a, porous graphene surface includes the hole of many whites to piece.Fig. 2 b are that XPS is composed entirely, and porous graphene is main
It is made up of carbon and oxygen.In addition, Fig. 2 c are shown as the Raman spectral characterizations of Raman porous graphenes, the porous graphite of different pore size
Alkene is respectively provided with the characteristic strip of graphene（D1 and G bands）, wherein characteristic strip D1/G（Integral area ratio）Gradually reduce, show porous stone
The defects of black alkene site sp3Carbon gradually decreases, and quality gradually steps up.Fig. 2 d show the pore-size distribution of porous graphene：With nitre
The change of sour zinc addition, resulting aperture are respectively：8-12,12-25,20-40 and 20-30 nm.These as shown by data,
The process can successfully prepare the porous graphene of different pore size distribution.
Claims (4)
1. the method that partial combustion method quickly prepares porous graphene, it is characterised in that concretely comprise the following steps：Zinc nitrate is added into oxygen
In graphite alkene water slurry, ultrasonic 2-30 min, then with quantitative filter paper rapid filtration under suction, zinc nitrate neatly is obtained on filter paper
The graphene oxide compound of the endless all standing of layer；By the filter paper with compound after 35-55 DEG C of drying, in point on alcolhol burner
Combustion, after black graphene completely burned, can obtain the compound of Zinc oxide nanoparticle and porous graphene, is cleaned with strong acid
1-8 times, washing after i.e. can obtain porous graphene.
2. the method as described in claim 1, it is characterised in that the mass ratio of the zinc nitrate and graphene oxide is 25:1-
200:1。
3. the method as described in claim 1, it is characterised in that the concentration of the graphene oxide water slurry is 1-2 g/L.
4. the method as described in claim 1, it is characterised in that the strong acid of the washing is hydrochloric acid or nitric acid, and concentration is
0.01-0.1 mol/L, centrifuge washing 3-6 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108439379A (en) * | 2018-05-28 | 2018-08-24 | 中国科学院兰州化学物理研究所 | A kind of preparation method for the porous graphene nano material that aperture is controllable |
| CN108872204A (en) * | 2018-04-27 | 2018-11-23 | 中国科学院兰州化学物理研究所 | A kind of preparation and application of two dimension porous graphene/cuprous oxide composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112079349B (en) * | 2020-08-25 | 2022-04-22 | 中国科学院兰州化学物理研究所 | Method for preparing nitrogen-doped porous graphene nano material through limited-area combustion and application |
| CN113018503B (en) * | 2021-03-25 | 2022-05-17 | 中国科学院兰州化学物理研究所 | Nano-pore graphene/nitrocellulose membrane with antibacterial and wound healing promoting functions and preparation method thereof |
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