CN105776200A - Device and method for continuously preparing graphene by photocatalytic reduction - Google Patents
Device and method for continuously preparing graphene by photocatalytic reduction Download PDFInfo
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Abstract
The invention discloses a device for continuously preparing graphene by photocatalytic reduction. The device comprises a reactor, a peristaltic pump, a precursor liquid storage bottle and a graphene storage bottle, wherein the reactor is a transparent spiral glass tube; one end of the transparent spiral glass tube is a feeding hole; the other end of the transparent spiral glass tube is a discharge hole; the peristaltic pump is arranged between the feeding hole and a first storage bottle; the feeding hole is communicated with the first storage bottle through a peristaltic pump hose of the peristaltic pump; the outlet hole is communicated with the graphene storage bottle through a discharge tube; the transparent spiral glass tube is formed by a transparent glass tube which is wound from top to bottom in a spiral manner so as to form an inner spiral body and then is wound from bottom to top around the inner spiral body in the spiral manner; and the reactor is wrapped by a reflecting membrane. In addition, the invention further discloses a method for continuously preparing graphene by photocatalytic reduction. By adopting the device, continuous controllability of the photocatalytic reduction process is achieved, the preparation efficiency of graphene is greatly improved, the cost is sufficiently lowered, and industrial on-scale preparation can be easily achieved.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of photo catalytic reduction and prepare the device and method of Graphene continuously.
Background technology
Graphene is a kind of Two-dimensional structural carbon nanomaterial with monoatomic layer thickness.It has the crystal structure of a kind of bi-dimensional cellular shape, and its internal each hydbridized carbon atoms constitutes stable hexagon with the carbon atom of surrounding.Graphene is two-dimensional material the thinnest in the world, and hydbridized carbon atoms can form the big π key of delocalization, and electronics can move freely therein, and this special structure makes Graphene have much excellent physics and chemical property.Graphene has outstanding mechanics, optics, calorifics and electrical properties so that it is have wide application prospect in all many-sides such as energy and material, super capacitor, composite, micro-nano electronic devices.
The preparation method of Graphene has a lot, including mechanical stripping method, oxidation-reduction method, chemical vapour deposition technique, crystal epitaxy method, electrochemical process, arc process, cutting carbon nanotubes etc..Wherein, Graphene size difficulty prepared by mechanical stripping method controls and productivity is low, is only applicable to laboratory and carries out basic research；Although the methods such as arc discharge method, epitaxial growth method, electrochemical process can prepare high-quality Graphene, but condition is just carved, productivity is low, it is impossible to meet the demand of actual large-scale application.Comparing with said method, its preparation process of chemistry redox method is relatively easy, and it is developing direction prepared by industrial mass.
Current traditional chemical method of reducing process is generally adopted there is toxicity or corrosive reducing agent (hydrazine hydrate, highly basic etc.), it is easy to contaminated environment；Reduction process is generally adopted and reacts in quantitative vessel in heating stirring simultaneously, and the response time is longer, and efficiency is low, it is impossible to realize serialization reduction preparation.
Summary of the invention
The technical problem to be solved is in that for above-mentioned the deficiencies in the prior art, it is provided that a kind of photo catalytic reduction prepares the device of Graphene continuously.This apparatus structure is simple, reasonable in design, adopt the transparent spiral glass tubing made further around described internal spiral spiral winding from bottom to up after being formed internal spiral by transparent glass tube spiral winding from top to bottom as reactor, it is capable of photo catalytic reduction process controlled continuously, greatly improves the preparation efficiency of Graphene.
nullFor solving above-mentioned technical problem，The technical solution used in the present invention is: a kind of photo catalytic reduction prepares the device of Graphene continuously，It is characterized in that，Including reactor、Peristaltic pump、Precursor liquid storage bottle and Graphene storage bottle，Described reactor is transparent spiral glass tubing，One end of transparent spiral glass tubing is charging aperture，The other end is discharging opening，Described peristaltic pump is arranged between charging aperture and the first storage bottle，And be connected by the peristaltic pump flexible pipe of peristaltic pump between charging aperture and the first storage bottle，It is connected by discharge nozzle between described discharging opening with Graphene storage bottle，Described transparent spiral glass tubing is made further around described internal spiral spiral winding from bottom to up after being formed internal spiral by transparent glass tube spiral winding from top to bottom，The structure formed around described internal spiral spiral winding from bottom to up is external spiral body，Described charging aperture is positioned at the transparent glass tube opening forming internal spiral，Discharging opening is positioned at the transparent glass tube opening forming external spiral body，And charging aperture and discharging opening are respectively positioned on the top of transparent spiral glass tubing，It is enclosed with reflective membrane outside described reactor.
Above-mentioned a kind of photo catalytic reduction prepares the device of Graphene continuously, it is characterised in that on described reflective membrane and be positioned at the middle part of reactor and bottom all offers observation port.
Above-mentioned a kind of photo catalytic reduction prepares the device of Graphene continuously, it is characterised in that the number of plies of described internal spiral is 12～14 layers, and the number of plies of external spiral body is 14～16 layers.
Above-mentioned a kind of photo catalytic reduction prepares the device of Graphene continuously, it is characterised in that be provided with Ultraviolet Detector on described discharge nozzle and between discharging opening and Graphene storage bottle.
It addition, present invention also offers a kind of method adopting said apparatus to prepare Graphene, it is characterised in that comprise the following steps:
Step one, by reducing agent and graphene oxide according to 1:(0.5～2) mass ratio mixing, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulates pH value to 7～10 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 0.1mg/mL～10mg/mL；
Step 2, light source is placed in the middle part of the internal spiral of reactor and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle, by peristaltic pump, the precursor liquid in precursor liquid storage bottle is continuously pumped in reactor, and to control the precursor liquid time of staying in the reactor be 0.5h～1h, pump into the precursor liquid in reactor and flow in Graphene storage bottle through discharge nozzle after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is iodine-tungsten lamp, electric filament lamp or uviol lamp；
Step 3, by the material filtering collected in Graphene storage bottle or centrifugal segregation solvent, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Above-mentioned method, it is characterised in that reducing agent described in step one is ascorbic acid, formic acid, glucose, citric acid, oxalic acid, ammonium carbonate or ammonium hydrogen carbonate.
Above-mentioned method, it is characterised in that in step 2, the power of iodine-tungsten lamp, electric filament lamp and uviol lamp is 20W～3000W.
The present invention compared with prior art has the advantage that
1, assembly of the invention simple in construction, reasonable in design, adopt the transparent spiral glass tubing made further around described internal spiral spiral winding from bottom to up after being formed internal spiral by transparent glass tube spiral winding from top to bottom as reactor, it is capable of photo catalytic reduction process controlled continuously, greatly improves the preparation efficiency of Graphene.
2, the present invention is preferably on reflective membrane and be positioned at the middle part of reactor and bottom all offers observation port, can by the color of in the middle part of perusal transparent spiral glass tubing and bottom in tandem reaction sequence, it is achieved the monitor in real time of course of reaction.
3, the present invention is provided with Ultraviolet Detector preferably on discharge nozzle and between discharging opening and Graphene storage bottle, it may be achieved the real-time detection of product in tandem reaction sequence, it is achieved photo catalytic reduction process is controlled continuously.
4, the present invention is by introducing photoirradiation catalysis redox graphene, it is possible to is obviously promoted reduction reaction and carries out, it is achieved reduction process is controlled continuously, greatly improves preparation efficiency, fully reduces cost, it is easy to accomplish prepared by industrial mass.
5, the present invention is by adopting avirulence, gentle reducing agent to react, it is possible to achieve prepared by environmental protection, do not introduce metal ion, it is to avoid contaminated environment simultaneously.
6, the graphene powder size uniform that prepared by the present invention, has 1～10 layer of monoatomic layer, and minimum thickness is up to 0.4nm, and Graphene has good dispersibility simultaneously.
Below in conjunction with drawings and Examples, technical scheme is described in further detail.
Figure of description
Fig. 1 is the structural representation after apparatus of the present invention remove reflective membrane.
Fig. 2 is x diffraction θ-2 θ scanning figure of the Graphene of the embodiment of the present invention 2 preparation.
Fig. 3 is the scanning electron microscope (SEM) photograph of the Graphene pattern of the embodiment of the present invention 2 preparation.
Fig. 4 is the atomic force scanning figure of the Graphene of the embodiment of the present invention 2 preparation.
Description of reference numerals:
1 precursor liquid storage bottle；2 peristaltic pumps；3 peristaltic pump flexible pipes；
4 charging apertures；5 discharging openings；6 reactors；
7 discharge nozzles；8 Ultraviolet Detectors；9 Graphene storage bottles.
Detailed description of the invention
Embodiment 1
nullAs shown in Figure 1，The photo catalytic reduction of the present embodiment prepares the device of Graphene continuously，Including reactor 6、Peristaltic pump 2、Precursor liquid storage bottle 1 and Graphene storage bottle 9，Described reactor 6 is transparent spiral glass tubing，One end of transparent spiral glass tubing is charging aperture 4，The other end is discharging opening 5，Described peristaltic pump 2 is arranged between charging aperture 4 and the first storage bottle 1，And be connected by the peristaltic pump flexible pipe 3 of peristaltic pump 2 between charging aperture 4 with the first storage bottle 1，It is connected by discharge nozzle 7 between described discharging opening 5 and Graphene storage bottle 9，Described transparent spiral glass tubing is made further around described internal spiral spiral winding from bottom to up after being formed internal spiral by transparent glass tube spiral winding from top to bottom，The structure formed around described internal spiral spiral winding from bottom to up is external spiral body，Described charging aperture 4 is positioned at the transparent glass tube opening forming internal spiral，Discharging opening 5 is positioned at the transparent glass tube opening forming external spiral body，And charging aperture 4 and discharging opening 5 are respectively positioned on the top of transparent spiral glass tubing，It is enclosed with reflective membrane outside described reactor 6.
In the present embodiment, on described reflective membrane and be positioned at the middle part of reactor 6 and bottom all offers observation port.
In the present embodiment, the number of plies of described internal spiral preferably 12～14 layers, the number of plies of external spiral body preferably 14～16 layers.
In the present embodiment, on described discharge nozzle 7 and between discharging opening 5 and Graphene storage bottle 9, it is provided with Ultraviolet Detector 8.
Embodiment 2
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 12 layers, and the number of plies of external spiral body is 14 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:1, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 10 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 0.1mg/mL；Described reducing agent is ascorbic acid；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 0.5h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is iodine-tungsten lamp, and power is 1000W；
Step 3, the material filtering removal solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Fig. 2 is x diffraction θ-2 θ scanning figure of Graphene prepared by the present embodiment, and as can be seen from the figure Graphene has CeO2(002) peak, and there is no the dephasign peak of graphene oxide, display is fully reduced.Fig. 3 is scanning electron microscope (SEM) figure of Graphene prepared by the present embodiment, and as can be seen from the figure Graphene is monolayer lamellar, has good uniformity and dispersibility, and in figure, light plication region is the natural shrinking of reduction process.Fig. 4 is atomic force scanning (AFM) figure of Graphene prepared by the present embodiment, it can be seen that the thickness of Graphene is 0.4nm, it was shown that Graphene is monolayer.Graphene film footpath prepared by the present embodiment is of a size of 1.5 microns, and thickness is 0.4nm, and Graphene is monolayer, has good uniform dispersibility.
Embodiment 3
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 13 layers, and the number of plies of external spiral body is 15 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:2, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 8 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 1mg/mL；Described reducing agent is ammonium hydrogen carbonate；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 0.8h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is uviol lamp, and power is 3000W；
Step 3, the material centrifugal segregation solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath prepared by the present embodiment is of a size of 0.5～3 micron, and thickness is 1nm, and Graphene is 3 layers, has good uniform dispersibility.
Embodiment 4
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 14 layers, and the number of plies of external spiral body is 16 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:0.5, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 7 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 10mg/mL；Described reducing agent is glucose；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 1h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is iodine-tungsten lamp, and power is 20W；
Step 3, the material filtering removal solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath size prepared by the present embodiment reaches 2 microns, and thickness is 2nm, and Graphene is 6 layers, has good uniform dispersibility.
Embodiment 5
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 14 layers, and the number of plies of external spiral body is 14 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:1.5, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 9 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 5mg/mL；Described reducing agent is formic acid；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 1h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is electric filament lamp, and power is 20W；
Step 3, the material centrifugal segregation solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath prepared by the present embodiment is of a size of 0.5～3 micron, and thickness is 3nm, and Graphene is 10 layers, has good uniform dispersibility.
Embodiment 6
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 14 layers, and the number of plies of external spiral body is 16 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:2, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 10 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 6mg/mL；Described reducing agent is citric acid；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 0.5h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is uviol lamp, and power is 2000W；
Step 3, the material filtering removal solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath prepared by the present embodiment is of a size of 0.5～3 micron, and thickness is 2nm, and Graphene is 6 layers, has good uniform dispersibility.
Embodiment 7
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 14 layers, and the number of plies of external spiral body is 16 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:1, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 7 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 2mg/mL；Described reducing agent is oxalic acid；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 1h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is uviol lamp, and power is 20W；
Step 3, the material filtering removal solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath prepared by the present embodiment is of a size of 0.5～3 micron, and thickness is 3nm, and Graphene is 10 layers, has good uniform dispersibility.
Embodiment 8
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 14 layers, and the number of plies of external spiral body is 16 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:1, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 10 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 5mg/mL；Described reducing agent is ammonium carbonate；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 1h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is iodine-tungsten lamp, and power is 3000W；
Step 3, the material filtering removal solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath prepared by the present embodiment is of a size of 0.5～3 micron, and thickness is 2nm, and Graphene is 5 layers, has good uniform dispersibility.
Embodiment 9
The present embodiment adopts the device of embodiment 1 to prepare Graphene, and in device, the number of plies of internal spiral is 14 layers, and the number of plies of external spiral body is 16 layers, and concrete preparation method comprises the following steps:
Step one, reducing agent and graphene oxide are mixed according to the mass ratio of 1:1, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulate pH value to 10 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 5mg/mL；Described reducing agent is ascorbic acid；
Step 2, light source is placed in the middle part of the internal spiral of reactor 6 and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle 1, by peristaltic pump 2, the precursor liquid in precursor liquid storage bottle 1 is continuously pumped in reactor 6, and to control the precursor liquid time of staying in reactor 6 be 1h, the precursor liquid pumped in reactor 6 flows in Graphene storage bottle 9 through discharge nozzle 7 after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is electric filament lamp, and power is 2000W；
Step 3, the material filtering removal solvent will collected in Graphene storage bottle 9, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
Graphene film footpath prepared by the present embodiment is of a size of 0.5～3 micron, and thickness is 1nm, and Graphene is 3 layers, has good uniform dispersibility.
The above; it it is only presently preferred embodiments of the present invention; not the present invention is done any restriction, every any simple modification, change and equivalent structure change above example made according to inventive technique essence, all still falls within the protection domain of technical solution of the present invention.
Claims (7)
- null1. a photo catalytic reduction prepares the device of Graphene continuously，It is characterized in that，Including reactor (6)、Peristaltic pump (2)、Precursor liquid storage bottle (1) and Graphene storage bottle (9)，Described reactor (6) is transparent spiral glass tubing，One end of transparent spiral glass tubing is charging aperture (4)，The other end is discharging opening (5)，Described peristaltic pump (2) is arranged between charging aperture (4) and the first storage bottle (1)，And be connected by the peristaltic pump flexible pipe (3) of peristaltic pump (2) between charging aperture (4) with the first storage bottle (1)，It is connected by discharge nozzle (7) between described discharging opening (5) with Graphene storage bottle (9)，Described transparent spiral glass tubing is made further around described internal spiral spiral winding from bottom to up after being formed internal spiral by transparent glass tube spiral winding from top to bottom，The structure formed around described internal spiral spiral winding from bottom to up is external spiral body，Described charging aperture (4) is positioned at the transparent glass tube opening forming internal spiral，Discharging opening (5) is positioned at the transparent glass tube opening forming external spiral body，And charging aperture (4) and discharging opening (5) are respectively positioned on the top of transparent spiral glass tubing，Described reactor (6) outside is enclosed with reflective membrane.
- 2. a kind of photo catalytic reduction according to claim 1 prepares the device of Graphene continuously, it is characterised in that on described reflective membrane and be positioned at the middle part of reactor (6) and bottom all offers observation port.
- 3. a kind of photo catalytic reduction according to claim 1 prepares the device of Graphene continuously, it is characterised in that the number of plies of described internal spiral is 12～14 layers, and the number of plies of external spiral body is 14～16 layers.
- 4. a kind of photo catalytic reduction according to claim 1 prepares the device of Graphene continuously, it is characterized in that, described discharge nozzle (7) is upper and is positioned between discharging opening (5) and Graphene storage bottle (9) and is provided with Ultraviolet Detector (8).
- 5. one kind adopts the method that device as described in any claim prepares Graphene in Claims 1-4, it is characterised in that comprise the following steps:Step one, by reducing agent and graphene oxide according to 1:(0.5～2) mass ratio mixing, then the mixture ultrasonic disperse of reducing agent and graphene oxide is dissolved in deionized water, regulates pH value to 7～10 with ammonia, obtain precursor liquid；In described precursor liquid, the concentration of graphene oxide is 0.1mg/mL～10mg/mL；Step 2, light source is placed in the middle part of the internal spiral of reactor (6) and opens light source, then precursor liquid described in step one is placed in precursor liquid storage bottle (1), by peristaltic pump (2), the precursor liquid in precursor liquid storage bottle (1) is continuously pumped in reactor (6), and to control the precursor liquid time of staying in reactor (6) be 0.5h～1h, pump into the precursor liquid in reactor (6) and flow in Graphene storage bottle (9) through discharge nozzle (7) after illumination condition issues third contact of a total solar or lunar eclipse catalytic reaction；Described light source is iodine-tungsten lamp, electric filament lamp or uviol lamp；Step 3, by the material filtering collected in Graphene storage bottle (9) or centrifugal segregation solvent, obtain Graphene, the Graphene that washing obtains, obtain graphene powder after drying.
- 6. method according to claim 5, it is characterised in that reducing agent described in step one is ascorbic acid, formic acid, glucose, citric acid, oxalic acid, ammonium carbonate or ammonium hydrogen carbonate.
- 7. method according to claim 5, it is characterised in that in step 2, the power of iodine-tungsten lamp, electric filament lamp and uviol lamp is 20W～3000W.
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| CN108083263A (en) * | 2018-02-24 | 2018-05-29 | 张静娟 | A kind of UV degradation method for preparing high-quality graphene material |
| CN108363129A (en) * | 2018-04-20 | 2018-08-03 | 南开大学 | More structure combinatorial artificial resistance electromagnetic surfaces |
| CN110562965A (en) * | 2019-10-30 | 2019-12-13 | 武汉低维材料研究院有限公司 | Preparation method of graphene powder |
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| CN102126720A (en) * | 2011-04-14 | 2011-07-20 | 中国科学院理化技术研究所 | Method for synthesizing graphene |
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| CN103964424A (en) * | 2014-05-13 | 2014-08-06 | 桂林理工大学 | Method for preparing photoreduction graphene oxide thin film |
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| CN108083263A (en) * | 2018-02-24 | 2018-05-29 | 张静娟 | A kind of UV degradation method for preparing high-quality graphene material |
| CN108363129A (en) * | 2018-04-20 | 2018-08-03 | 南开大学 | More structure combinatorial artificial resistance electromagnetic surfaces |
| CN110562965A (en) * | 2019-10-30 | 2019-12-13 | 武汉低维材料研究院有限公司 | Preparation method of graphene powder |
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