CN109133043A - A kind of nano-graphene and preparation method thereof, using and the method for preparing solar energy heat collection pipe - Google Patents
A kind of nano-graphene and preparation method thereof, using and the method for preparing solar energy heat collection pipe Download PDFInfo
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Abstract
The invention discloses a kind of nano-graphene and preparation method thereof, using and the method for preparing solar energy heat collection pipe, using strong acid and potassium permanganate and hydrogen peroxide by graphite oxidation, graphite oxide is made, then graphite oxide is ultrasonically treated and graphene oxide is made, it is restored finally by trisodium citrate, obtain graphene, surfacing, there are a small amount of folds for lamella, and lamella transparency is very high, through being analyzed with the adsorption experiment of methylene blue solution it is found that graphene prepared by the present invention can be used as optical absorbing agent and apply on solar energy heat collection pipe with preferable light absorptive.
Description
Technical field
The invention belongs to the application and preparation technical fields of nano-graphene, and in particular to a kind of nano-graphene and its preparation
Method, using and the method for preparing solar energy heat collection pipe.
Background technique
Coating for selective absorption of sunlight spectrum is one of the core material technology in solar energy heat utilization field.Firstly, sharp
Solar energy thermal conversion efficiency can be effectively improved with the excellent photothermal conversion performance of nano material.Addition vulcanization in silica
Copper can make the photothermal conversion performance of composite phase-change material be significantly improved.Variety classes and different quality are added in conduction oil
The solid particle of score helps to improve its photothermal conversion characteristic, and graphite-oil and copper foil-oil show good photothermal conversion
Energy.Vulcanized lead/attapulgite composite material photothermal conversion ability is better than body phase PbS；To the sun of wavelength 300-2 500nm
Light has absorptivity more higher than body phase PbS；PbS in composite material is more wider than the electron transition energy band of body phase PbS；Density of material
Far below body phase PbS, bigger area can be covered under condition of equivalent thickness.However, nano material absorptance is to solar energy heating
The research of pipe photothermal conversion effect rarely has open report.
Summary of the invention
The purpose of the present invention is to provide a kind of nano-graphene and preparation method thereof, using and prepare solar energy heat collection pipe
Method, the nano-graphene of preparation has good photo absorption performance, can be used as optical absorbing agent and apply on solar energy heat collection pipe.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of nano-graphene, comprising the following steps:
1) under conditions of ice-water bath, sulfuric acid and phosphoric acid are mixed in such a way that glass bar drains with graphite powder, control is anti-
It answers temperature at 0~4 DEG C, is persistently stirred to react 1~2h；Wherein, the mass ratio of sulfuric acid and phosphoric acid is 9:1；
2) potassium permanganate being added to mixed solution made from step 1), control reaction temperature is stirring while adding at 0~7 DEG C,
Persistently stir 1~2h, after be warming up to 35~40 DEG C, persistently stir 0.5~1h；Wherein, the mass ratio of graphite powder and potassium permanganate
For 1:3；
3) deionized water is instilled into mixed solution made from step 2), and temperature is risen to 85~98 DEG C, sustained response 1~
After 2h, hydrogen peroxide is added, golden yellow appearance, as graphite oxide solution are at this moment had in beaker；
4) washing centrifugation is carried out to graphite oxide solution made from step 3), until solution is in neutrality, after sediment is taken
Out, evaporation drying obtains graphite oxide powder；
5) graphite oxide powder obtained is made graphite oxide solution, after ultrasonic treatment, obtains graphene oxide solution；
6) trisodium citrate is added into graphene oxide solution, is warming up to 80~90 DEG C, is stirred to react 5~6.5h, it will
Obtained product washing centrifugation, until the supernatant pH that centrifugation obtains reaches neutral；Finally sediment is taken out, evaporation drying,
Obtain the graphene thin layer of bright silver, as nano-graphene.
Further, the concentration that hydrogen peroxide is added in step 3) is 10%~30%.
Further, the washing in step 4) uses concentration for 5%~8% salt acid elution, then is washed repeatedly with deionized water
It washs for several times.
Further, the washing in step 6) is successively alternately to be washed with dehydrated alcohol and deionized water.
Nano-graphene made from preparation method of the invention, there are fold, lamella is transparent on surface.
Application of the nano-graphene prepared by the present invention as optical absorbing agent.
Nano-graphene prepared by the present invention prepares the application of solar energy heat collection pipe as optical absorbing agent.
For nano-graphene of the invention when preparing solar energy heat collection pipe, specific preparation method is by nano-graphene system
As fine and close nano coating, it is coated in solar energy heating pipe surface.
Further, by nano-graphene acidification, the pH of nano-graphene is adjusted to 4.
Compared with prior art, the invention has the following beneficial technical effects:
The preparation method of nano-graphene disclosed by the invention will be strong by the way of drainage under conditions of ice-water bath
Acid mix with graphite powder, it is possible to reduce be vigorously mixed it is caused slop over reaction temperature it is excessively high caused by personal injury, be one kind
Very safe method；Strong acid molecule is inserted into graphite powder interlayer, modifies its surface oxygen functional group, increases graphite powder interlamellar spacing
Greatly, it prepares for addition strong oxidizer oxidation；Using the strong oxidizing property graphite oxide powder of potassium permanganate and the concentrated sulfuric acid, modification is wherein
Hydroxyl and carboxyl etc. change its intermolecular force, increase the Qinshui property of graphite powder, more convenient can be dissolved in water
In, the purpose of ice-water bath is mainly the reaction speed of the safety and Control experiment process that guarantee that experiment carries out；Use lemon
Reducing agent of the sour trisodium as graphene oxide, safe and non-toxic, environmentally protective, solubility property is good in water, can be with water temperature liter
It is high and increase, facilitate the progress of reduction reaction.
Further, use concentration for 5%~8% salt acid elution graphite oxide solution, keep graphite oxide expansion and
Hydrophily, concentration is too high to occur kickback, destroy the structure of nano-graphene.
Further, it is washed with deionized to pH and reaches neutral, sulfate ion and/or phosphorus when being to make sample detection
Acid ion does not occur, and main purpose is in order not to damage to drying box.
Nano-graphene prepared by the present invention, through scanning electron microscope analysis, it is seen that the graphene surface of preparation is smooth, and lamella is deposited
In fold, and lamella transparency is very high.
There are folds for nano-graphene prepared by the present invention, have preferable light absorptive, can be used as optical absorbing agent use, especially
It is that can apply on solar energy heat collection pipe.
Nano-graphene is made as densification by the method that nano-graphene disclosed by the invention prepares solar energy heat collection pipe
Nano coating is coated in solar energy heating pipe surface, using the light absorptive of nano-graphene, improves solar energy heat collection pipe
Collecting efficiency.
Further, by nano-graphene acidification, the pH of nano-graphene is adjusted to 4, improves the extinction of graphene
Rate, and then greatly improve the collecting efficiency of solar energy heat collection pipe.
Detailed description of the invention
Fig. 1 is by the graphite oxide solution photo after hydrogen peroxide oxidation；
Fig. 2 is the supernatant that centrifugation obtains and diluted graphite oxide precipitating photo；
Fig. 3 is the graphene photo of lamelliform；
Fig. 4 is that the SEM of graphene schemes；Fig. 4 a is the SEM figure of the graphene in the case where multiple is 7.13KX, and Fig. 4 b is to be in multiple
The SEM figure of graphene under 5.56KX；
Fig. 5 is the adsorbance of graphene and graphite with methylene blue solution initial concentration change curve；
Fig. 6 be graphene and graphite to solution adsorbance with the change curve of its dosage；
Fig. 7 be graphene and graphite to methylene blue solution adsorbance with the change curve of pH value.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The laboratory apparatus that the present invention uses has beaker, magnetic stirring apparatus, ultrasonic washing instrument, electronic balance, visible light point
Light photometer, vacuum oven etc., there is used various reagents in preparation process: graphite powder, potassium permanganate, hydrogen peroxide,
Phosphoric acid, dehydrated alcohol, sulfuric acid, hydrochloric acid, deionized water, trisodium citrate etc..
Embodiment 1
The preparation method of nano-graphene of the invention, comprising the following steps:
(1) sulfuric acid of 82.8mL, the phosphoric acid of 9.2mL, the hydrogen peroxide of 40mL, the graphite powder of 4g and the Gao Meng of 12g are measured
Sour potassium；
(2) dried 250mL beaker is placed in ice-water bath, and be put into magnetic stirring apparatus, by load weighted sulfuric acid
It is added in beaker in a manner of glass bar drainage with phosphoric acid, system temperature is controlled at 1 DEG C, it is allowed to stir, is uniformly mixed；
(3) 4g graphite powder is slowly added into beaker, persistently stirs 1h；
(4) temperature is controlled at 2 DEG C, is slowly added to potassium permanganate by several times in beaker, the time of addition is 2h, is persistently stirred
Mix 2h；Next system is transferred in 35 DEG C of water-baths, is persistently stirred to react 30min；
(5) it is slowly dropped into deionized water in beaker, system temperature is slowly increased to 85 DEG C, sustained response 1h；
(6) 10% hydrogen peroxide is added in beaker for aoxidizing remaining graphite, at this moment has golden yellow in beaker and goes out
Show, as graphite oxide solution；
(7) it is centrifuged while hot, takes out upper layer filtrate with centrifuge tube, upper layer filtrate is poured into waste liquid barrel, then with 5%
HCL washing to be centrifuged remaining graphite oxide solution multiple, centrifugation persistently wash with deionized water repeatedly, up to upper layer filtrate pH
Until reaching neutrality；
(8) sediment is taken out, is put into evaporating dish, then dry, the acquisition graphite oxide in drying box；
(9) the ground graphite oxide of 300mg is put into beaker, deionized water is then added dropwise and is stirred using magnetic force
It mixes device to be stirred, Color development goes out coffee color；
(10) progress ultrasound is stirred evenly, stable dispersion liquid, i.e. graphene oxide solution are obtained；Beaker is put into magnetic
In power blender, ice bath 30min is first carried out；
(11) system temperature then risen to 90 DEG C, is slowly added to 4g trisodium citrate by several times, at being 90 DEG C in temperature into
Row is sufficiently stirred and reacts 6h, will obtain reaction product deionized water and dehydrated alcohol alternately washs, until what centrifugation obtained
Until supernatant pH reaches neutrality；
(12) taking-up of obtained sediment is put into evaporating dish, is placed in drying box dry 20h, obtains the stone of bright silver
Black alkene thin layer, finally shreds thin graphene, grind into powder, as nano-graphene powder.
Embodiment 2
The preparation method of nano-graphene of the invention, comprising the following steps:
(1) sulfuric acid of 31.5mL, the phosphoric acid of 3.5mL, the hydrogen peroxide of 10mL, the graphite powder of 1.5g and the height of 4.5g are measured
Potassium manganate；
(2) dried beaker is placed in ice-water bath, now sulfuric acid is added in beaker in a manner of glass bar drainage, then
Phosphoric acid is added in beaker in a manner of glass bar drainage, control system temperature is at 2 DEG C；
(3) continue that 1.5g graphite powder is added into beaker, continue to stir, react 1h；
(4) it is slowly added to 4.5g potassium permanganate by several times in beaker, the time that potassium permanganate is added is 1h, maintenance system temperature
Degree reacts 2h, is next transferred to system in 38 DEG C of water-bath and is persistently stirred to react 30min at 5 DEG C；Wherein, potassium permanganate
It has to slowly, prevent sulfuric acid from splashing out beaker when addition；
(5) it is slowly dropped into deionized water into beaker, system is diluted, system temperature is slowly increased to 90 DEG C, instead
Answer 1h；
(6) hydrogen peroxide of 30% concentration of 10mL is added, reacts 10min, mixture becomes golden yellow, as oxidation stone
Ink；
(7) it is centrifuged while hot, takes out upper layer filtrate with centrifuge tube, upper layer filtrate is poured into waste liquid barrel, then with 7%
HCL washing to be centrifuged remaining graphite oxide solution multiple, centrifugation persistently wash with deionized water repeatedly, up to upper layer filtrate pH
Until reaching neutrality；
(8) it takes out precipitating to be put into evaporating dish, places it in drying box and be dried for 24 hours, then by the object after drying
Matter is ground, and graphite oxide is obtained；
(9) the graphite oxide 250mg after being ground with electronic balance weighing is put into dry 500mL beaker, is slowly added to
250mL deionized water is stirred, and obtains graphite oxide solution, and Color development goes out coffee color；
(10) next graphite oxide solution is ultrasonically treated, obtains finely dispersed graphene oxide solution；
(11) then the beaker for holding graphene oxide solution is put into magnetic stirring apparatus, carries out stirring in water bath
Then 30min is slowly added to 5g trisodium citrate by several times into beaker, the addition time is 2h, and temperature is raised slowly to 80 DEG C,
It is sufficiently stirred at being 80 DEG C in temperature and reacts 5h；Obtained product is successively alternately washed with dehydrated alcohol and deionized water
It washs, until the supernatant pH that centrifugation obtains reaches neutrality；
(12) obtained precipitating is put into vessel, dries 20h in a vacuum drying oven, setting temperature is no more than 57
DEG C, the thin graphene of bright silver is obtained after dry, is finally shredded thin graphene, grind into powder, as nano-graphite
Alkene powder.
Embodiment 3
The preparation method of nano-graphene of the invention, comprising the following steps:
(1) sulfuric acid of 54.9mL, the phosphoric acid of 6.1mL, the hydrogen peroxide of 20mL, the graphite powder of 2.8g and the height of 8.4g are measured
Potassium manganate；
(2) dried beaker is placed in ice-water bath, now sulfuric acid is added in beaker in a manner of glass bar drainage, then
Phosphoric acid is added in beaker in a manner of glass bar drainage, control system temperature is at 4 DEG C；
(3) continue that 2.8g graphite powder is added into beaker, continue to stir, react 2h；
(4) it is slowly added to 8.4g potassium permanganate by several times in beaker, the time that potassium permanganate is added is 2h, maintenance system temperature
Degree stirs in addition at 7 DEG C, is next transferred to system in 40 DEG C of water-bath and is persistently stirred to react 1h；Wherein, permanganic acid
Potassium has to slowly, prevent sulfuric acid from splashing out beaker when addition；
(5) it is slowly dropped into deionized water into beaker, system is diluted, system temperature is slowly increased to 98 DEG C, instead
Answer 2h；
(6) hydrogen peroxide of 20% concentration of 20mL is added, reacts 10min, mixture becomes golden yellow, as oxidation stone
Ink；
(7) it is centrifuged while hot, takes out upper layer filtrate with centrifuge tube, upper layer filtrate is poured into waste liquid barrel, then with 8%
HCL washing to be centrifuged remaining graphite oxide solution multiple, centrifugation persistently wash with deionized water repeatedly, up to upper layer filtrate pH
Until reaching neutrality；
(8) it takes out precipitating to be put into evaporating dish, places it in drying box and be dried for 24 hours, then by the object after drying
Matter is ground, and graphite oxide is obtained；
(9) the graphite oxide 250mg after being ground with electronic balance weighing is put into dry 500mL beaker, is slowly added to
250mL deionized water is stirred, and obtains graphite oxide solution, and Color development goes out coffee color；
(10) next graphite oxide solution is ultrasonically treated, obtains finely dispersed graphene oxide solution；
(11) then the beaker for holding graphene oxide solution is put into magnetic stirring apparatus, carries out stirring in water bath
Then 30min is slowly added to 5g trisodium citrate by several times into beaker, the addition time is 2h, and temperature is raised slowly to 85 DEG C,
It is sufficiently stirred at being 85 DEG C in temperature and reacts 5h；Obtained product is successively alternately washed with dehydrated alcohol and deionized water
It washs, until the supernatant pH that centrifugation obtains reaches neutrality；
(12) obtained precipitating is put into vessel, dries 20h in a vacuum drying oven, setting temperature is no more than 57
DEG C, the thin graphene of bright silver is obtained after dry, is finally shredded thin graphene, grind into powder, as nano-graphite
Alkene powder.
Measuring graphene partial size prepared by Examples 1 to 3 is 100~500nm.All processes of Examples 1 to 3 must be
Stirring is lower to be carried out, and entire reaction process of testing almost needs 8h, and washing process probably needs 2-3h, than existing Hummers
Method reaction speed is fast, saves the time, high-efficient.Step (6) operation is completed, and finally obtains golden yellow solution, then with hydrochloric acid with
During deionized water washing centrifugation, solution becomes more and more sticky, and golden yellow of the color by becomes brown color, acid
Slowly become smaller, precipitating has the tendency that blackening.Graphite oxide does not occur hydrophobic phenomenon during washing centrifugation, this is because
Graphite oxide functional group is all hydrophilic mostly.
The function analysis of experimental procedure
The effect of (1) step is to start to be ready for experiment and get out ice-water bath.The effect of (2), (3) step be by
Strong acid molecule is inserted into graphite powder interlayer, modifies its surface oxygen functional group, increases graphite powder interlamellar spacing, to add Strong oxdiative
Agent oxidation is prepared.The effect of (4) step is the strong oxidizing property graphite oxide powder using potassium permanganate and the concentrated sulfuric acid, and modification is wherein
Hydroxyl and carboxyl etc. change its intermolecular force, increase the Qinshui property of graphite powder, enable graphite powder is more convenient can be dissolved in
In water, control temperature here is required by Hummers method, effect is that graphite powder is in ice-water bath, can make oxidant
It is more dissolved into wherein, the purpose of ice-water bath is mainly the reaction of the safety and Control experiment process that guarantee that experiment carries out
Speed.The purpose that deionized water is added in (5) step is to reduce acidity, reduces pH, prepares for next step experimental work.(6)
It is to remove remaining oxidant that hydrogen peroxide, which is added, in step.The effect of (7), (8) step is to carry out the graphite oxide prepared
It extracts, the hydrochloric acid of addition 5%~8% is the expansion and hydrophily in order to keep graphite oxide, is washed with deionized to pH and reaches
To neutrality, sulfate ion and/or phosphate anion do not occur when being to make sample detection, and main purpose is in order not to dry
Dry case damages.
During preparing graphite oxide, to H is added in mixture at being 85~98 DEG C in temperature2O2, lead to solution colour
Glassy yellow is become from brown, as shown in Figure 1.The graphite oxide solution hydrochloric acid and deionized water of acquisition are alternately washed to centrifugation number
It is secondary, then with deionized water solution washed into centrifugation until pH reaches neutral, the supernatant of acquisition is centrifuged in faint yellow, uses deionization
Graphite oxide after water dilution centrifugation is precipitated as brown color, as shown in Figure 2.Graphene oxide after washing reduction with dehydrated alcohol
When, sample is presented unqualified shape and does not dissolve in dehydrated alcohol, need to be sufficiently stirred and just not will form precipitating, turn to when being washed with deionized
Solution, the precipitating that supernatant and sticky shape are obtained after centrifugation is all bright black.After the precipitated filter cakes that centrifugation is obtained are dry, obtain
Graphene thin layer be bright silver, as shown in Figure 3.
Scanning electron microscope analysis has been done to the nano-graphene prepared to detect its surface property.Using scanning electron microscope
It before instrument, needs to be applied to graphene powder in sample disc and carries out sample preparation, carrying out metal spraying processing to sample can be such that sample sees
That examines is more careful, reaches desired vacuum when being full of nitrogen in sealing room to completely cut off air, avoids the suspended matter in air
Matter pollutes sample, and sample disc is then put into sample stage.It is learnt by Fig. 4 a, in the case where multiple is 7.13KX, graphene surface is flat
It is whole, it is clear that it is observed that there are pleated structures for redox graphene.And in the case where amplification factor is 5.56KX, it can be more straight
The fold that redox graphene is seen in sight is layered as single layer structure.In especially Fig. 4 b, it can be seen that lamella is than more complete, piece
Layer transparency is very high, and reducing condition is highly desirable, and under the conditions of micron, there are folds for lamella, it may be said that bright graphene oxide is
It is reduced agent and is reduced to graphene.The lamellar structure of graphene surface is significant, and gauffer is more on surface, its photo absorption performance
Also more significant.
To the nano-graphene of prepared acquisition, use visible spectrophotometer can with qualitative and quantitative analysis sample at
Point, according to the interaction between the ingredient of absorption spectrum samples can be analyzed of sample, structure and sample material, and absorption spectrum is
Photon in incident light is absorbed the molecule of generation and the result of electron transition by substance.This experiment is using Shanghai essence science and technology
Instrument Ltd. 722N type visible spectrophotometer, can measure wave-length coverage are as follows: 190~1100nm.
Graphene/the graphite for weighing more parts of 20mg respectively is put into the conical flask of 150mL, measures 100mL various concentration
MB solution (1mg/L, 2mg/L, 3mg/L, 4mg/L and 5mg/L) is separately added into the conical flask of the above preparation, and sufficiently shaking up makes stone
Black alkene/graphite dispersion is 6, under conditions of 20 DEG C of temperature in pH, is placed in constant temperature blender with magnetic force and stirs in MB solution, from
The heart takes supernatant, measures its absorbance using visible spectrophotometer, calculates adsorbance, obtain the absorption of graphene and graphite
Amount is with MB initial concentration solution change curve, as shown in Figure 5.As shown in Figure 5, when MB solution concentration is 1~5mg/L, graphite
Alkene increases with initial soln concentration, and adsorbance quicklys increase, and adsorbance curve linearly rises, and the adsorbance of graphite first with
MB solution concentration increases and rises, and break occurs in 3mg/L and gradually tends to balance.It compares and learns, graphene compares graphite
Adsorption effect it is more preferable, this is because the graphene that graphite is prepared by oxidation-reduction method has biggish specific surface
Product, increases adsorption site.
The graphene of different quality is weighed respectively and graphite (10mg, 20mg, 30mg, 40mg and 50mg) is put into 150mL cone
It in shape bottle, measures the MB solution that 100mL concentration is 3mg/L and is separately added into conical flask, the pH for adjusting MB solution is 6, is kept molten
Liquid temperature is 20 DEG C, and conical flask is placed in constant temperature blender with magnetic force and stirs 120min, is centrifuged and takes supernatant, pass through visible light
The absorbance of spectrophotometer measurement graphite and graphene calculates their adsorbance, obtains graphene and graphite and inhales to solution
Attached amount is with the change curve of its dosage, such as Fig. 6.It will be appreciated from fig. 6 that as graphite and graphene dosage increase, their suction
Attached amount fluctuates, and when graphene dosage is 40mg, adsorbance reaches maximum, and then curve is fallen after rise.This be mainly because
For in the timing of MB solution concentration one, when graphene input amount is 40mg, graphene surface can be covered with MB solution, make MB molecule with
It is simple easy that graphene adsorption site combines, and as graphene dosage increases, increases therewith for adsorbing the site of MB molecule,
There is peak value under conditions of MB concentration does not change.Graphite adsorbance increases with dosage and is increased, its increase is more slow
Slowly, it is fallen after rise at 40mg dosage.Through it was found that, graphene is stronger to the adsorption effect of MB solution.Graphene is most
Good input amount is 40mg.
It weighs the graphene of 5 parts of 20mg respectively and graphite is put into 150mL conical flask, measuring 100mL concentration is 3mg/L's
MB solution is separately added into conical flask, and adjusting the pH value of MB solution with dilute HCL and NaOH solution is respectively 2,4,6,8 and 10.It will
Blender, which is put into conical flask, stirs 120min, and supernatant is taken after centrifugation, measures its absorbance with visible spectrophotometer, and
Adsorbance is calculated, the change curve of graphene and graphite to MB solution adsorbance with pH value is provided, sees Fig. 7.As shown in Figure 7, when
Solution ph from 2 increase to 10 when, graphene and graphite are to the adsorbance first increases and then decreases of MB solution, when pH value is 4, stone
There is peak value in the adsorption curve of black alkene and graphite, reaches maximum.When pH value is greater than 4, the adsorption curve of graphene and graphite is first
Slowly decline.This is primarily due to pH value and there is influence to graphene and graphite surface charge, promotes graphene and graphite to MB
Caused by solution effects change.The OH as present in MB solution-Adsorption site is grabbed with MB molecule, causes graphene and stone
Ink reduces the adsorbance of MB molecule.When pH value is 2, there are a large amount of H ions and MB molecule to fight for adsorption site in MB solution,
Reduce graphene and graphite surface to the adsorbance of MB molecule.When pH value is 4, graphene and graphite surface are negatively charged,
And MB solution is the dye of positive ion, graphene and graphite since electrostatic interaction has preferable suction-operated to MB molecule.Therefore, exist
When pH=4, the adsorption effect of graphene and graphite is best.
Show that nano-graphene absorptance with higher prepared by the present invention, can be used as optical absorbing agent makes from the above analysis
With.The nano-graphene of preparation is fabricated to fine and close nano coating, is then coated in solar energy heating pipe surface, improves
Collecting efficiency.It is more preferably that graphene is shifted to an earlier date into acidification, after its pH is adjusted to 4, collecting efficiency is greatly improved.
Claims (9)
1. a kind of preparation method of nano-graphene, which comprises the following steps:
1) under conditions of ice-water bath, sulfuric acid and phosphoric acid are mixed in such a way that glass bar drains with graphite powder, control reaction temperature
Degree is persistently stirred to react 1~2h at 0~4 DEG C；Wherein, the mass ratio of sulfuric acid and phosphoric acid is 9:1；
2) potassium permanganate is added to mixed solution made from step 1), control reaction temperature is stirring while adding at 0~7 DEG C, continues
Stir 1~2h, after be warming up to 35~40 DEG C, persistently stir 0.5~1h；Wherein, the mass ratio of graphite powder and potassium permanganate is 1:
3；
3) deionized water is instilled into mixed solution made from step 2), temperature is risen to 85~98 DEG C, 1~2h of sustained response
Afterwards, hydrogen peroxide is added, golden yellow appearance, as graphite oxide solution are at this moment had in beaker；
4) washing centrifugation is carried out to graphite oxide solution made from step 3), until solution is in neutrality, after sediment is taken out, steam
It is dry dry, obtain graphite oxide powder；
5) graphite oxide powder obtained is made graphite oxide solution, after ultrasonic treatment, obtains graphene oxide solution；
6) trisodium citrate is added into graphene oxide solution, is warming up to 80~90 DEG C, is stirred to react 5~6.5h, will obtain
Product wash centrifugation, until the obtained supernatant pH of centrifugation reaches neutral；Finally sediment is taken out, evaporation drying obtains
The graphene thin layer of bright silver, as nano-graphene.
2. the preparation method of nano-graphene according to claim 1, which is characterized in that hydrogen peroxide is added in step 3)
Concentration is 10%~30%.
3. the preparation method of nano-graphene according to claim 1, which is characterized in that the washing in step 4) is using dense
Degree is 5%~8% salt acid elution, then is washed repeatedly for several times with deionized water.
4. the preparation method of nano-graphene according to claim 1, which is characterized in that the washing in step 6) is successively
It is alternately washed with dehydrated alcohol and deionized water.
5. nano-graphene made from the preparation method as described in Claims 1 to 4 any one, which is characterized in that obtained
There are fold, lamella is transparent on nano-graphene surface.
6. application of the nano-graphene described in claim 5 as optical absorbing agent.
7. the application that nano-graphene described in claim 5 prepares solar energy heat collection pipe as optical absorbing agent.
8. a kind of method that the nano-graphene using described in claim 5 prepares solar energy heat collection pipe, which is characterized in that will receive
Rice graphene is made as fine and close nano coating, is coated in solar energy heating pipe surface.
9. preparation method according to claim 8, which is characterized in that by nano-graphene acidification, by nano-graphite
The pH of alkene is adjusted to 4.
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