CN110508279A - Cuprous oxide embeds graphene superfine composite ball and its preparation method and application - Google Patents
Cuprous oxide embeds graphene superfine composite ball and its preparation method and application Download PDFInfo
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- CN110508279A CN110508279A CN201910783107.0A CN201910783107A CN110508279A CN 110508279 A CN110508279 A CN 110508279A CN 201910783107 A CN201910783107 A CN 201910783107A CN 110508279 A CN110508279 A CN 110508279A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 57
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 46
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 108010010803 Gelatin Proteins 0.000 claims abstract description 15
- 229920000159 gelatin Polymers 0.000 claims abstract description 15
- 239000008273 gelatin Substances 0.000 claims abstract description 15
- 235000019322 gelatine Nutrition 0.000 claims abstract description 15
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 8
- 239000008103 glucose Substances 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 6
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000011941 photocatalyst Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 3
- 229940012189 methyl orange Drugs 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000002604 ultrasonography Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- 238000007146 photocatalysis Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013066 combination product Substances 0.000 description 1
- 229940127555 combination product Drugs 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- -1 zinc oxide Compound Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B01J35/39—
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a kind of cuprous oxide to embed graphene superfine composite ball, and the crystal grain of superfine composite ball is 200-500nm, and the mass percent for being embedded in graphene of cuprous oxide can reach 1-25%.It also discloses that preparation method includes the following steps: step 1: gelatin and graphene oxide is dissolved in deionized water, be placed in ultrasonic device ultrasound, to obtain gelatin graphene mixed liquor；Step 2: cupric sulfate pentahydrate and polyethylene glycol are dissolved in deionized water；Step 3: the solution that step 2 is obtained is added drop-wise in the gelatin graphene mixed liquor of step 1；Step 4: glucose solution is added dropwise in the mixed liquor that step 3 obtains；Step 5: sodium hydroxide solution is added dropwise in the mixed liquor that step 4 obtains, is centrifuged, washed, dried after fully reacting.The present invention not only has the advantages that distribution is equal, and spherical shape is excellent and very high activity, and preparation method is at low cost, pollution-free.
Description
Technical field
The invention belongs to the preparation fields of nanometer visible light catalytic material, and in particular to a kind of embedded graphene of cuprous oxide
The preparation method and applications of superfine composite ball.
Background technique
In recent years, the attention due to various countries to environmental protection makes people to the concern of photocatalysis field and studies increasingly
It is more, current one of research hotspot is become using photocatalyst treatment water pollution problems.It is partly led as a kind of p-type narrow band gap
The forbidden bandwidth of body, cuprous oxide is lower, and band gap magnitude is 2.17ev or so, relative to some traditional catalysis materials, such as
ZnO and TiO2, cuprous oxide can more efficiently utilize visible light, therefore have in terms of the photocatalysis of visible light extensively.Meanwhile
Cuprous oxide have hypotoxicity, low cost and can by it is wide variety of be prepared under visible light water decomposition and dye discoloration
The ideal semiconductor of the degradation of object.But since the light induced electron and hole that generate inside cuprous oxide are easily compound, so that it
Photo-catalysis capability also need further to be promoted, photocatalytic degradation efficiency will further increase.It is anti-in experiment by changing
Condition and process are answered, people have made intensive studies the different-shape of cuprous oxide.L.J.Fu etc. is in Applied Surface
Science 256 (2010) 7335-7338 reports wet chemistry method and is prepared for hollow cuprous oxide microballoon；Matthew etc. is in J
Am Chem Soc 128 (2006) 10357, which is reported, has synthesized the octahedral bodily form, cube blocky oxidation Asia with the method for electrochemistry
Copper；Song Ji-Mei etc. is reported in Chinese J Appl.Chem.27 (2010) 1328-1333 with reduction in aqueous solution at room temperature method
It is prepared for cubic and spherical cuprous oxide with hydrothermal reaction at low temperature, result of study shows that spherical cuprous oxide has higher catalysis to live
Property.
Graphene is the two-dimension nano materials that a kind of carbon atom is constituted, conductive capability with super strength, high electron transfer
Rate and high surface area, and it is regarded as zero band gap material in the ideal case, make graphene and semiconductors coupling for light
Catalysis aspect has carried out a large amount of research.These semiconductor materials mainly include the metal oxygens such as titanium dioxide, tin oxide, zinc oxide
Compound.Graphene can significantly improve the photocatalysis performance of semiconductor due to adsorption capacity with higher and electron conductivity.
Therefore judge that graphene improves the photocatalysis efficiency of cuprous oxide with the recombination energy of cuprous oxide, especially there is spherical oxidation
Cuprous is compound, can significantly improve the degradation rate to organic dye pollutant.
Currently, having some researchs for the report of the synthesis of this composite material, but the combination product reported is mainly
Pattern is undesirable, the Cu of mineral carbon load2O mostly occurs with octahedra, irregular spherical, cube and porous structure；On the other hand
Be then complicated cumbersome, the hydro-thermal reaction of high temperature, especially some reducing agents used of preparation method it is toxic, is to environment
Non- close friend.Therefore, there is an urgent need to develop a kind of simple, low cost, environmentally friendly preparation method, and it is excellent to obtain pattern
It is good, be evenly distributed and the optic catalytic composite material of performance boost, thus this case generates.
Summary of the invention
It is an object of the present invention to provide a kind of cuprous oxide to embed graphene superfine composite ball, not only has distribution
Equal advantage, and spherical shape is excellent and very high activity.
The second purpose of the present invention is to provide the preparation method that a kind of cuprous oxide embeds graphene superfine composite ball, preparations
It is at low cost, pollution-free, meet environmentally protective purpose.
The three of the object of the invention are to provide a kind of application of embedded graphene superfine composite ball of cuprous oxide.
In order to solve the above technical problems, the technical solution of the invention is as follows:
Cuprous oxide embeds the preparation method of graphene superfine composite ball, comprising the following steps:
Step 1: gelatin and graphene oxide are dissolved in deionized water, are placed in ultrasonic device and are ultrasonically treated, with
To finely dispersed gelatin graphene mixed liquor；
Step 2: cupric sulfate pentahydrate and polyethylene glycol are dissolved in deionized water, are stirred at room temperature；
Step 3: in the state of heating, the solution that step 2 is obtained is added drop-wise to the gelatin graphene mixing of step 1
In liquid, and it is stirred continuously；
Step 4: in the state of heating, glucose solution is added dropwise in the mixed liquor that step 3 obtains, and constantly stir
It mixes；
Step 5: in the state of heating, sodium hydroxide solution is added dropwise in the mixed liquor that step 4 obtains, and constantly stir
It mixes, is centrifuged, is washed after fully reacting, dried to get the embedded graphene superfine composite ball of the cuprous oxide is arrived.
Further, in step 1, ultrasonic time is 0.5-1 hours, and in step 2, the Polyethylene glycol is
0.8-2.4mg/ml, mixing time is 3-5 minutes, and in step 4, glucose solution 100ml, concentration 0.05- is added dropwise
0.2mol/l, in step 5, the concentration of sodium hydroxide solution is 0.5-3mol/l, and hydrogen has been slowly added dropwise in additional amount 100ml
Continue stirring 1-2 hours after sodium oxide molybdena.
Further, the graphene oxide is the concentration 0.1-0.3mg/ as made from improved Hummers method
Ml, number of plies 1-7.
Further, Step 3: the dropwise addition mode is slowly to be added dropwise dropwise, in step in step 4 and step 5
Three, temperature when heated condition described in step 4 and step 5 is 40-70 degree.
Further, in step 5, the revolving speed of the centrifugation is 6000-8000 revs/min；The washing is deionized water
With dehydrated alcohol alternately washing 4-6 times；The drying mode be 60 degree vacuum drying 6-8 hours.
Cuprous oxide embeds graphene superfine composite ball, and the crystal grain of superfine composite ball is 200-500nm, cuprous oxide
The mass percent for being embedded in graphene is 1-25%.
Cuprous oxide embeds application of the graphene superfine composite ball as photocatalyst material.
Further, the photochemical catalyst is used for degradating organic dye methyl orange.
After adopting the above scheme, compared with prior art, the invention has the following advantages: simple process and low cost,
It easily promotes, is convenient for high-volume industrial production；Obtained composite material pattern is good, and is spherical shape, good dispersion, photocatalysis efficiency
Height has good application prospect in terms of environmental improvement.
Detailed description of the invention
Fig. 1 is the scanning electron that the cuprous oxide that a preferred embodiment of the invention obtains embeds graphene superfine composite ball
Microscope photo.
Specific embodiment
The invention will be further described in the following with reference to the drawings and specific embodiments.Disclosed is cuprous oxide
The preparation method and application of embedded graphene superfine composite ball,
A kind of cuprous oxide embeds the preparation method of graphene superfine composite ball, comprising the following steps:
Step 1: gelatin and graphene oxide are dissolved in deionized water, are placed in ultrasound a period of time in ultrasonic device ultrasound,
To obtain finely dispersed gelatin graphene mixed liquor；It adsorbs the functional group of gelatin on the surface of graphene, and prevents graphene
Reunite, and gelatin provides basis for the formation of subsequent spherical cuprous oxide.
Step 2: cupric sulfate pentahydrate and polyethylene glycol are dissolved in deionized water, and polyethylene glycol plays surfactant
Effect, is stirred at room temperature, to obtain finely dispersed solution.
Step 3: in the state of heating, the solution that step 2 is obtained is added drop-wise to the gelatin graphene mixing of step 1
It in liquid, and is stirred continuously, copper ion is complexed fully with the functional group of graphene surface.
Step 4: in the state of heating, glucose solution is added dropwise in the mixed liquor that step 3 obtains, and constantly stir
It mixes；
Step 5: in the state of heating, sodium hydroxide solution is added dropwise in the mixed liquor that step 4 obtains, and constantly stir
It mixes, to achieve the purpose that refine crystal grain, while keeping identical temperature, guarantee crystal grain with suitable growth, reaction
It is centrifuged, washed after completely, being dried to get the embedded graphene superfine composite ball of the cuprous oxide is arrived.
Further, in step 1, ultrasonic time is 0.5-1 hours, and in step 2, the Polyethylene glycol is
0.8-2.4mg/ml, mixing time is 3-5 minutes, in step 4, glucose solution 100ml is slowly added dropwise dropwise, concentration is
0.05-0.2mol/l, in step 5, the concentration of sodium hydroxide solution is 0.5-3mol/l, additional amount 100ml, slowly by
Continue stirring 1-2 hours after dripping sodium hydroxide.
Further, the graphene oxide is the concentration 0.1-0.3mg/ as made from improved Hummers method
Ml, number of plies 1-7.
Further, Step 3: the dropwise addition mode is slowly to be added dropwise dropwise, in step 4 and step 5 to allow it
Slowly nucleation is grain growth Step 3: temperature when heated condition described in step 4 and step 5 is 40-70 degree
Preference temperature.
Further, in step 5, the revolving speed of the centrifugation is 6000-8000 revs/min；The washing is deionized water
With dehydrated alcohol alternately washing 4-6 times；The drying mode be 60 degree vacuum drying 6-8 hours.
The invention also discloses a kind of cuprous oxide to embed graphene superfine composite ball, and the crystal grain of superfine composite ball is
200-500nm, the mass percent that cuprous oxide is embedded in graphene can reach 1-25%.
The invention also discloses a kind of cuprous oxide to embed application of the graphene superfine composite ball as photocatalyst material.
Further, the photochemical catalyst is used for degradating organic dye methyl orange.
Embodiment 1
Step 1: 1g gelatin and 10mg graphene oxide are added in 100ml deionized water, surpass in the ultrasonic device of 500W
Sound 1h keeps its evenly dispersed.
Step 2: 2.5g cupric sulfate pentahydrate and 0.16g polyethylene glycol are added in 100ml deionized water, stir at room temperature
It mixes, until being completely dissolved.
Step 3: in the resulting solution of step 1 under 50 degree magnetic agitation, slowly dropwise the resulting solution of step 2
It is added drop-wise in the resulting solution of step 1, and is stirred continuously.
Step 4: the glucose solution of 100ml 0.1mol/l is slowly dripped dropwise in the resulting mixed liquor of step 3
It is added in above-mentioned mixed liquor, and the magnetic agitation in 50 degree of water-bath；
Step 5: in the resulting mixed liquor of step 4, slowly dropwise by the sodium hydroxide solution of 100ml 0.5mol/l
It is added drop-wise in above-mentioned mixed liquor, and the magnetic agitation in 50 degree of water-bath；Continue the magnetic agitation 2h under 50 degree after dripping, it will
Obtained suspension is centrifuged with 8000 revs/min of revolving speed, dry in vacuum with deionized water and dehydrated alcohol alternately washing 5 times
In dry case graphene ultrathin composite powder is embedded up to cuprous oxide within vacuum drying 6 hours for 60 degree.
Fig. 1 is the stereoscan photograph that the cuprous oxide that embodiment 1 obtains embeds graphene superfine composite ball material, is shown
In the composite material that the present invention obtains, cuprous oxide pattern is spherical shape, and size uniformity, crystallinity is high, and cuprous oxide is equably
It is embedded in graphene.
The present invention obtains the compound ball material of graphene cuprous oxide, simple process, cost by simple solution reduction
It is low, it is practical, it is convenient for high-volume industrial production；Obtained composite material spherical shape is good, and is evenly distributed, photocatalysis efficiency
Height, environmental improvement and in terms of have good application prospect.
The above described is only a preferred embodiment of the present invention, be not intended to limit the scope of the present invention,
Therefore the changes or modifications that claim under this invention and specification are done in every case, it all should belong to the range that the invention patent covers
Within.
Claims (8)
1. the preparation method that cuprous oxide embeds graphene superfine composite ball, it is characterised in that: the following steps are included:
Step 1: gelatin and graphene oxide are dissolved in deionized water, are placed in ultrasonic device and are ultrasonically treated, to be divided
Dissipate uniform gelatin graphene mixed liquor；
Step 2: cupric sulfate pentahydrate and polyethylene glycol are dissolved in deionized water, are stirred at room temperature；
Step 3: in the state of heating, the solution that step 2 is obtained is added drop-wise in the gelatin graphene mixed liquor of step 1,
And it is stirred continuously；
Step 4: in the state of heating, glucose solution is added dropwise in the mixed liquor that step 3 obtains, and be stirred continuously；
Step 5: in the state of heating, being added dropwise sodium hydroxide solution, and be stirred continuously in the mixed liquor that step 4 obtains,
It is centrifuged, washed after fully reacting, being dried to get the embedded graphene superfine composite ball of the cuprous oxide is arrived.
2. the preparation method that cuprous oxide according to claim 1 embeds graphene superfine composite ball, it is characterised in that: In
In step 1, mixing time is 0.5-1 hour, and in step 2, the Polyethylene glycol is 0.8-2.4mg/ml, when stirring
Between be 3-5 minute, in step 4, dropwise addition glucose solution 100ml, concentration 0.05-0.2mol/l, in step 5, hydrogen
The concentration of sodium hydroxide solution is 0.5-3mol/l, additional amount 100ml, be slowly added dropwise after sodium hydroxide continue to stir 1-2 it is small
When.
3. the preparation method that cuprous oxide according to claim 1 embeds graphene superfine composite ball, it is characterised in that: institute
Stating graphene oxide is concentration 0.1-0.3mg/ml, number of plies 1-7 as made from improved Hummers method.
4. the preparation method that cuprous oxide according to claim 1 embeds graphene superfine composite ball, it is characterised in that: In
Step 3: the dropwise addition mode is slowly to be added dropwise dropwise, Step 3: step 4 and step 5 in step 4 and step 5
Described in heated condition when temperature be 40-70 degree.
5. the preparation method that cuprous oxide according to claim 1 embeds graphene superfine composite ball, it is characterised in that: In
In step 5, the revolving speed of the centrifugation is 6000-8000 revs/min；The washing is that deionized water and dehydrated alcohol are alternately washed
It washs 4-6 times；The drying mode be 60 degree vacuum drying 6-8 hours.
6. a kind of cuprous oxide by the preparation of any one of claim 1-5 the method embeds graphene superfine composite ball,
Be characterized in that: the crystal grain of its superfine composite ball is 200-500nm, and the mass percent for being embedded in graphene of cuprous oxide is 1-
25%。
7. a kind of cuprous oxide by the preparation of any one of claim 1-5 the method embeds answering for graphene superfine composite ball
With, it is characterised in that: as photocatalyst material.
8. a kind of cuprous oxide according to claim 7 embeds graphene superfine composite ball answering as photocatalyst material
With, it is characterised in that: the photochemical catalyst is used for degradating organic dye methyl orange.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030170A (en) * | 2013-01-16 | 2013-04-10 | 哈尔滨工业大学 | Preparation method for cuprous oxide/reduced graphene oxide composite functional material |
| CN105664943A (en) * | 2016-01-29 | 2016-06-15 | 上海交通大学 | Preparation method of cubic cuprous oxide/graphene nanocomposite |
| US20190202762A1 (en) * | 2017-12-29 | 2019-07-04 | Uchicago Argonne, Llc | Photocatalytic reduction of carbon dioxide to methanol or carbon monoxide using cuprous oxide |
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2019
- 2019-08-23 CN CN201910783107.0A patent/CN110508279B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030170A (en) * | 2013-01-16 | 2013-04-10 | 哈尔滨工业大学 | Preparation method for cuprous oxide/reduced graphene oxide composite functional material |
| CN105664943A (en) * | 2016-01-29 | 2016-06-15 | 上海交通大学 | Preparation method of cubic cuprous oxide/graphene nanocomposite |
| US20190202762A1 (en) * | 2017-12-29 | 2019-07-04 | Uchicago Argonne, Llc | Photocatalytic reduction of carbon dioxide to methanol or carbon monoxide using cuprous oxide |
Non-Patent Citations (1)
| Title |
|---|
| 王伟: ""铜基内嵌碳纳米管复合颗粒的合成及性能研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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