CN107619040B - 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 methods that partial combustion method quickly prepares porous graphene, specific steps are as follows: zinc nitrate is added in graphene oxide water slurry, ultrasonic 2-30 min, then quantitative filter paper rapid filtration under suction is used, 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 lighting on alcolhol burner, after black graphene completely burned, the compound of Zinc oxide nanoparticle and porous graphene can be obtained, porous graphene can be obtained after being cleaned 1-8 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, to considerably reduce the preparation cost of porous graphene, improves utilization efficiency.
Description
Technical field
The present invention relates to the methods that partial combustion method quickly prepares porous graphene.
Background technique
The porous graphene defect more because of its surface has mass-transfer efficiency more higher than graphene, therefore in energy electricity
The fields such as pond, the storage of gas, biomedicine, separation analysis play an important role.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.However these methods are required to higher cost, the equipment requirement of longer generated time and complexity, to seriously restrict
The prepare with scale of porous graphene and its production application in industrial circle.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that graphene oxide partial combustion method quickly prepares porous graphene.
The neatly layer that the present invention uses zinc nitrate to spontaneously form on the surface of graphene passes through control nitre as fire retardant
The additional amount of sour zinc, can form the neatly layer of different degree of imperfections on the surface of graphene, when 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 the high temperature for generation of burning will not
The oxygen-containing group of combustion parts surface of graphene oxide removes, and is then washed away the metal oxide on surface with salt, to prepare
Porous graphene material out.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, simplifies synthesis step, improves production efficiency.
The method that partial combustion method quickly prepares porous graphene, it is characterised in that specific steps are as follows: zinc nitrate is added
In graphene oxide water slurry, then ultrasonic 2-30 min uses 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
It lights, after black graphene completely burned, the compound of Zinc oxide nanoparticle and porous graphene can be obtained, it is clear with strong acid
Wash 1-8 times, washing after porous graphene can be obtained.
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, obtain being dispersed with a large amount of nanoscale holes (10 ~
100 nm) porous graphene material, porous graphene surface have super large specific surface area (~ 800 m2/ g), there is amplification
The potentiality of production and very extensive application prospect.
The invention has the following advantages that
1) this method does not need starvation or air, does not need high temperature, therefore reaction process is easy, economical, quick.
2) this method prepares porous graphene material by partial combustion method, and the by-product of burning is tractable gas
(carbon dioxide and nitrogen dioxide), thus it is more environmentally protective.
3) this method does not need complicated reaction process and advanced reaction vessel, at low cost, with large-scale application
Potentiality.
Detailed description of the invention
Fig. 1 is the preparation 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 picture；B is XPS characterization；C is Raman spectral characterization；d
For pore analysis.
Specific embodiment
The preparation of 1 porous graphene of embodiment
Operating procedure:
1. configuring 2 mL of graphene oxide suspension of 1 g/L first, 10 min of room temperature ultrasound.
2. weighing 50 mg zinc nitrates, it is dissolved in above-mentioned suspension, 2 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 35 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.01 mol/L hydrochloric acid 4 times washings.
The preparation of 2 porous graphene of embodiment
Operating procedure:
1. configuring 2 mL of graphene oxide suspension of 1 g/L first, 10 min of room temperature ultrasound.
2. weighing 100 mg zinc nitrates, it is dissolved in above-mentioned suspension, 2 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 35 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.01 mol/L hydrochloric acid 4 times washings.
The preparation of 3 porous graphene of embodiment
Operating procedure:
1. configuring 2 mL of graphene oxide suspension of 1 g/L first, 10 min of room temperature ultrasound.
2. weighing 200 mg zinc nitrates, it is dissolved in above-mentioned suspension, 4 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 35 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.01 mol/L hydrochloric acid 4 times washings.
The preparation of 4 porous graphene of embodiment
Operating procedure:
1. configuring 2 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 500 mg zinc nitrates, it is dissolved in above-mentioned suspension, 5 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 35 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. washing using 0.05 mol/L hydrochloric acid 5, porous graphene can be obtained after washing 3 times.
The preparation of 5 porous graphene of embodiment
Operating procedure:
1. configuring 5 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 1 g zinc nitrate, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 40 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.01mol/L nitric acid 5 times washings.
The preparation of 6 porous graphene of embodiment
Operating procedure:
1. configuring 10 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 1.5 g zinc nitrates, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 45 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.01mol/L nitric acid 5 times washings.
The preparation of 7 porous graphene of embodiment
Operating procedure:
1. configuring 10 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 2 g zinc nitrates, it is dissolved in above-mentioned suspension, 30 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 50 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.01mol/L hydrochloric acid 8 times washings.
The preparation of 8 porous graphene of embodiment
Operating procedure:
1. configuring 10 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 4 g zinc nitrates, it is dissolved in above-mentioned suspension, 30 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 55 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. washing using 0.05mol/L nitric acid 10, porous graphene can be obtained after washing 3 times.
The preparation of 9 porous graphene of embodiment
Operating procedure:
1. configuring 20 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 5g zinc nitrate, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 55 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.1 mol/L hydrochloric acid 4 times washings.
The preparation of 10 porous graphene of embodiment
Operating procedure:
1. configuring 20 mL of graphene oxide suspension of 2 g/L first, 10 min of room temperature ultrasound.
2. weighing 6 g zinc nitrates, it is dissolved in above-mentioned suspension, 20 min of ultrasound.
3. filtering above-mentioned solution using quantitative filter paper.
4. filter paper and residue are dried in 55 DEG C.
5. the filter paper with residue is lighted, sinters to white zinc oxide covering porous graphene and occur.
6. porous graphene can be obtained after washing 3 times using 0.1 mol/L nitric acid 4 times washings.
Most of experiment parameter in fixed embodiment 1 can pass through transmission electricity using the additional amount of zinc nitrate as dependent variable
Mirror (TEM) investigates the surface topography of the porous graphene of this method preparation.The experimental result table of the porous graphene wherein prepared
Sign is as shown in Figure 2.
Surface topography and crystal characterization: it for porous graphene, needs using transmission electron microscope observing pattern, gained TEM shines
Piece is as shown in Figure 2 a, and porous graphene surface includes the hole of many whites.Fig. 2 b is that XPS is composed entirely, and porous graphene is main
It is made of carbon and oxygen.In addition, Fig. 2 c is shown as the Raman spectral characterization of Raman porous graphene, the porous graphite of different pore size
Alkene all has the characteristic strip (D1 and G band) of graphene, wherein characteristic strip D1/G(integral area ratio) it gradually decreases, show porous stone
The defect sites sp of black alkene3Carbon gradually decreases, and quality is gradually increased.Fig. 2 d shows the pore-size distribution of porous graphene: with nitre
The change of sour zinc additional amount, obtained aperture are respectively as follows: 8-12,12-25,20-40 and 20-30 nm.These statistics indicate that,
The process can successfully prepare the porous graphene of different pore size distribution.
Claims (3)
1. the method that partial combustion method quickly prepares porous graphene, it is characterised in that specific steps are as follows: oxygen is added in zinc nitrate
In graphite alkene water slurry, then ultrasonic 2-30 min uses 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 be obtained the compound of Zinc oxide nanoparticle and porous graphene, is cleaned with strong acid
1-8 times, washing after porous graphene can be obtained；
The mass ratio of the zinc nitrate and graphene oxide is 25:1- 200:1.
2. 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.
3. the method as described in claim 1, it is characterised in that the strong acid of the cleaning is hydrochloric acid or nitric acid, and concentration is
0.01-0.1 mol/L, centrifuge washing 3-6 times.
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| CN112079349A (en) * | 2020-08-25 | 2020-12-15 | 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 |
| CN113018503A (en) * | 2021-03-25 | 2021-06-25 | 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 |
Families Citing this family (2)
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| CN108872204B (en) * | 2018-04-27 | 2020-12-01 | 中国科学院兰州化学物理研究所 | Preparation and application of two-dimensional porous graphene/cuprous oxide composite material |
| 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849734A (en) * | 2012-09-28 | 2013-01-02 | 中国科学院宁波材料技术与工程研究所 | Preparation method of porous graphene |
| CN103137957A (en) * | 2013-02-27 | 2013-06-05 | 中国石油大学(北京) | Porous graphene-metal oxide composite material and its preparation method |
| CN104743548A (en) * | 2015-03-16 | 2015-07-01 | 浙江大学 | Porous graphene as well as preparation method and application thereof |
| CN105621406A (en) * | 2016-02-29 | 2016-06-01 | 上海交通大学 | Nitrogen-doped porous graphite and preparation method thereof |
| CN106045552A (en) * | 2016-05-25 | 2016-10-26 | 全球能源互联网研究院 | Three-dimensional graphene macroscopic body preparation method |
| CN106395753A (en) * | 2016-09-12 | 2017-02-15 | 中国科学院兰州化学物理研究所 | Method for preparing metal elementary substance or metal oxide nano material through quick reduction caused by graphene combustion |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140205796A1 (en) * | 2013-01-18 | 2014-07-24 | International Business Machines Corporation | Method of forming graphene nanomesh |
-
2017
- 2017-11-01 CN CN201711053922.9A patent/CN107619040B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849734A (en) * | 2012-09-28 | 2013-01-02 | 中国科学院宁波材料技术与工程研究所 | Preparation method of porous graphene |
| CN103137957A (en) * | 2013-02-27 | 2013-06-05 | 中国石油大学(北京) | Porous graphene-metal oxide composite material and its preparation method |
| CN104743548A (en) * | 2015-03-16 | 2015-07-01 | 浙江大学 | Porous graphene as well as preparation method and application thereof |
| CN105621406A (en) * | 2016-02-29 | 2016-06-01 | 上海交通大学 | Nitrogen-doped porous graphite and preparation method thereof |
| CN106045552A (en) * | 2016-05-25 | 2016-10-26 | 全球能源互联网研究院 | Three-dimensional graphene macroscopic body preparation method |
| CN106395753A (en) * | 2016-09-12 | 2017-02-15 | 中国科学院兰州化学物理研究所 | Method for preparing metal elementary substance or metal oxide nano material through quick reduction caused by graphene combustion |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112079349A (en) * | 2020-08-25 | 2020-12-15 | 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 |
| CN113018503A (en) * | 2021-03-25 | 2021-06-25 | 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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