CN110252372A - A kind of two dimension rGO/R-CeO2The preparation method of/CNNS hierarchical structure composite photo-catalyst - Google Patents
A kind of two dimension rGO/R-CeO2The preparation method of/CNNS hierarchical structure composite photo-catalyst Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 84
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 73
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 77
- 238000006243 chemical reaction Methods 0.000 claims abstract description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- 239000011218 binary composite Substances 0.000 claims abstract description 21
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 74
- 239000000243 solution Substances 0.000 claims description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- 239000011259 mixed solution Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229910001220 stainless steel Inorganic materials 0.000 claims description 19
- 239000010935 stainless steel Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 11
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 24
- 229910002092 carbon dioxide Inorganic materials 0.000 description 18
- 238000009210 therapy by ultrasound Methods 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 description 9
- 238000010531 catalytic reduction reaction Methods 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 5
- 230000001476 alcoholic effect Effects 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 5
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229960004424 carbon dioxide Drugs 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000549556 Nanos Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
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- 238000010792 warming Methods 0.000 description 1
Classifications
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B01J35/61—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
Abstract
The invention belongs to energy conversion technical field of material, and one kind is for restoring CO2Two-dimentional rGO/R-CeO2The preparation method of/CNNS hierarchical structure composite photo-catalyst.The present invention includes the preparation of (1) graphene oxide (GO): using the Hummers method preparation of improvement.(2) CNNS and rodlike CeO2Preparation by Muffle furnace calcine cyanuric acid obtain CNNS；With Ce (NO3)3·6H2O and NaOH is raw material, takes hydro-thermal method, obtains rodlike CeO2(R‑CeO2)。(3)R‑CeO2The preparation of/CNNS binary composite photo-catalyst, and (4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst.The two-dimentional rGO/R-CeO obtained by multistep processes2/ CNNS hierarchical structure composite photo-catalyst is used to restore CO under ultraviolet light2Purposes；The formation that preparation method of the present invention is simple, will not result in waste of resources with secondary pollution, provides a kind of technology for alleviating energy crisis.
Description
Technical field
The invention belongs to energy conversion technical field of material, are related to a kind of two dimension rGO/R-CeO2/ CNNS level knot
The preparation method and applications of structure composite photo-catalyst.
Background technique
Global carbon dioxide (CO2) discharge caused extensive concern, CO2Caused greenhouse effects cause seriously
Weather and environmental problem, however CO2It is also a kind of potential carbon resource, more and more scientific research persons are carrying out positive exploitation
And utilization.With the development of science and technology more and more methods are used for CO2Energy conversion, such as electro-catalysis, photocatalysis, photoelectricity are urged
Change, the methods of biology conversion, CO2Gas synthesis chemical products create new condition and may.Currently, a kind of ideal solution
CO2The method of problem is to restore CO under the action of photoreduction using solar energy2Generate hydrocarbon.For example, from CO2Out
Hair can be reduced directly the useful chemical products such as synthesizing methane, methanol, formic acid, formic acid, low-carbon hydro carbons and carbonic acid, develop CO2Benefit
With technology, the fossil resources such as petroleum, natural gas and coal can be not only saved, but also are changed harmful to treasure, CO is reduced2Caused by environment it is dirty
Dye, has obvious economic and environmental benefits.
However, photocatalysis CO2Reduction remains following problems: photochemical catalyst is not sufficiently stable, and efficiency of light absorption is low, light
The disadvantages of raw electron-hole is easily compound, poor selectivity.These problems are to hinder CO2The main reason for recycling.It designs and develops
With preparation there is high stability, high adsorption and highly selective catalysis material to have become current CO2Study on the transformation direction
One of.
Summary of the invention
Present invention discover that CeO2It is nontoxic with chemical stability, the characteristics of easily preparation, it is widely used in Photocatalyzed Hydrogen Production,
CO2The fields such as absorption, reduction and toluene catalytic combustion, and due to CeO2With suitable reduction potential.By controlling hydro-thermal temperature
Degree and reaction time synthesize rodlike cerium oxide (R-CeO2).But R-CeO2Monomer is easy to reunite, and present invention introduces azotized carbon nanos
Piece (CNNS) Lai Tigao R-CeO2Dispersibility introduce the biggish GO of specific surface area in order to improve the stability of catalyst and carry out structure
It builds a kind of for CO2The two-dimentional rGO/R-CeO of reduction2/ CNNS hierarchical structure composite photo-catalyst.
The present invention prepares two-dimentional rGO/R-CeO using multistep processes2/ CNNS hierarchical structure composite photo-catalyst.
The present invention is to realize above-mentioned technical purpose by following technological means.
A kind of two dimension rGO/R-CeO2The preparation method of/CNNS hierarchical structure composite photo-catalyst, includes the following steps
(1) prepared by graphene oxide (GO):
Pass through prior art preparation graphene oxide (GO).
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
A certain amount of cyanuric acid is put into crucible with cover, then crucible is put into Muffle furnace and is calcined, wait drop to
After room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；
Cerium nitrate hexahydrate (Ce (NO is weighed respectively3)3·6H2O it) is dissolved in deionized water, surpasses with sodium hydroxide (NaOH)
Sonication is then transferred into polytetrafluoroethyllining lining stainless steel cauldron, and reaction kettle is put into baking oven and is reacted, wait react knot
Reaction kettle cooled to room temperature is taken out after beam, it is then multiple with deionized water and ethanol washing, it is dried to obtain rodlike CeO2(R-
CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
The CNNS and R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in methanol solution respectively, at ultrasound
Reason obtains suspension, then by R-CeO2Methanol solution be added drop-wise in the methanol solution of CNNS dropwise, mixed solution room temperature is stirred
It mixes, drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst disperses in deionized water, then to take step
Suddenly the GO solution of (1) preparation is added in above-mentioned solution, is stirred at room temperature for 24 hours, mixed solution is put into baking oven after reaction
Middle drying to get arrive two dimension rGO/R-CeO2/ CNNS hierarchical structure composite photo-catalyst.
In step (1), the preparation of the graphene oxide (GO) is prepared using the Hummers method of improvement: in ice-water bath
In be put into three-necked flask, 1g graphite powder and 2.5g sodium nitrate is added, the 30mL concentrated sulfuric acid is then added, magnetic agitation is uniformly mixed；
Then 4g potassium permanganate is added in three-necked flask several times, after having added, continues magnetic agitation under conditions of ice-water bath
2h；35 DEG C are then heated to, after stirring 30min at such a temperature, 40mL deionized water is slowly added into three-necked flask；So
After be warming up to 98 DEG C, at such a temperature react 40min after, stirring continue, close heating；Temperature to water-bath is down to 70 DEG C
When, it is 30% hydrogen peroxide (H by 10mL volume fraction2O2) be added in three-necked flask, after dropping to room temperature, by three-necked flask
In mixed solution be transferred in beaker, and with 5%HCl solution wash three times, remove foreign ion, be finally washed with deionized water
The pH of GO is washed, washing to pH value is 6 or so, and freeze-drying, collection obtain GO powder；Then the GO solution of 1mg/mL is prepared, it is spare.
In step (2), 500-600 DEG C of temperature of the cyanuric acid calcining, calcination time 2-4h.
In step (2), the Ce (NO3)3·6H2O, NaOH and the amount ratio of deionized water are 1g:(5.64-16.93) g:
70mL。
In step (2), the hydrothermal temperature is 100-140 DEG C, and the hydro-thermal time is 24-72h.
In step (3), the amount ratio of the rodlike cerium oxide, azotized carbon nano piece and methanol solution is 1g:(2-10) g:
40mL。
In step (3), the mixing time is 24-48h.
In step (4), the R-CeO2The mass ratio of/CNNS and GO is 1:(0.002-0.014).
Two dimension rGO/R-CeO of the present invention2The pattern of/CNNS hierarchical structure composite photo-catalyst is two-dimentional level knot
Structure, rodlike CeO2It is dispersed between rGO and CNNS.
By two dimension rGO/R-CeO prepared by the present invention2/ CNNS hierarchical structure composite photo-catalyst is used for light under ultraviolet light and urges
Change CO2Convert purposes.
Deionized water dosage is that soluble solids can be made to be completely dissolved in above-mentioned technical proposal.
CO2For high-purity gas, it is purchased from Shanghai Pujiang Specialty Gases Co., Ltd..
Beneficial effects of the present invention:
(1) the biggish azotized carbon nano piece of specific surface area is prepared by calcination method, then by rodlike cerium oxide (R-CeO2)
Its surface is dispersed in improve the dispersibility of rodlike cerium oxide.
(2) GO has biggish surface area, good conductivity, the transfer of light induced electron during strong light-catalyzed reaction
And separation, improve the utilization rate of photo-generated carrier.
(3) synergistic effect between semiconductor material improves the electric charge transfer between respective interface, and it is high to improve photocatalysis
Effect reduction conversion CO2Prepare the selectivity of hydrocarbon fuel.
Detailed description of the invention
Fig. 1 is two dimension rGO/R-CeO2The XRD diagram of/CNNS hierarchical structure composite photo-catalyst.
Fig. 2 is two dimension rGO/R-CeO2The UV-vis of/CNNS hierarchical structure composite photo-catalyst schemes.
Fig. 3 is two dimension rGO/R-CeO2The TEM of/CNNS hierarchical structure composite photo-catalyst schemes.
Specific embodiment
With reference to the accompanying drawings of the specification and specific implementation example the present invention will be further described.
The photocatalytic activity evaluation of prepared photochemical catalyst in the present invention: anti-in CY-XD300Q type photochemistry stainless steel
It answers and is carried out in kettle (purchased from Shanghai Lan Yi Industrial Co., Ltd.), irradiated with ultraviolet lamp, the NaOH solution of 100mL 0.1M is added
Enter in reactor, obtained composite photo-catalyst is added, high-purity CO of 30min is then led in reaction kettle2Gas is to exclude
Foreign gas is then shut off air outlet valve, continues logical CO2Gas makes the pressure of reaction kettle in 1.4MPa, is then shut off intake valve.
Lamp source is opened, takes a sample with gas sample needle at interval of 2h, is then detected by FID, is calculated from the formula methane and one
The concentration of carbonoxide, and then calculate the yield of methane and carbon monoxide.
Embodiment 1:
(1) preparation of GO:
It is put into three-necked flask in ice-water bath, 1g graphite powder and 2.5g sodium nitrate is added, the 30mL concentrated sulfuric acid, magnetic is then added
Power is uniformly mixed；Then 4g potassium permanganate is added in three-necked flask several times, after having added, in the condition of ice-water bath
Lower continuation magnetic agitation 2h；35 DEG C are then heated to, after stirring 30min at such a temperature, 40mL deionized water is slowly added to
Into three-necked flask；98 DEG C are then heated to, after reacting 40min at such a temperature, stirring continues, and closes heating；To water-bath
Temperature when being down to 70 DEG C, be 30% hydrogen peroxide (H by 10mL volume fraction2O2) be added in three-necked flask, room temperature to be dropped to
Afterwards, the mixed solution in three-necked flask is transferred in beaker, and is washed three times with 5%HCl solution, remove foreign ion, most
The pH of GO is washed with deionized afterwards, washing to pH value is 6 or so, and freeze-drying, collection obtain GO powder；Then prepare 1mg/mL's
GO solution, it is spare.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 500 DEG C of Muffle furnace and calcines 2h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；
Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·6H2O it) is dissolved in 70mL deionized water with the NaOH of 9.8g,
Ultrasonic treatment, is then transferred into 100mL polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is put into 100 DEG C of baking ovens
Reaction is for 24 hours, then multiple with deionized water and ethanol washing to take out reaction kettle cooled to room temperature after reaction, does
It is dry to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.025g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL respectively
In methanol solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to the methanol of CNNS dropwise
In solution, mixed solution is stirred at room temperature for 24 hours, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 1mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 1.64 μm of ol/ (gh), and the yield of methane is 0.84 μm of ol/ (gh).
Embodiment 2:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 550 DEG C of Muffle furnace and calcines 2h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；
Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·6H2O) and the NaOH of 14.7g is dissolved in 70mL deionized water
In, ultrasonic treatment is then transferred into 100mL polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is put into 110 DEG C of baking ovens
Middle reaction is for 24 hours, then multiple with deionized water and ethanol washing to take out reaction kettle cooled to room temperature after reaction,
It is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.05g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL first respectively
In alcoholic solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to dropwise CNNS methanol it is molten
In liquid, mixed solution is stirred at room temperature for 24 hours, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 3mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 1.81 μm of ol/ (gh), and the yield of methane is 0.92 μm of ol/ (gh).
Embodiment 3:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 600 DEG C of Muffle furnace and calcines 2h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；
Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·6H2O) and the NaOH of 19.6g is dissolved in 70mL deionized water
In, ultrasonic treatment is then transferred into 100mL polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is put into 120 DEG C of baking ovens
Middle reaction is for 24 hours, then multiple with deionized water and ethanol washing to take out reaction kettle cooled to room temperature after reaction,
It is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.075g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL respectively
In methanol solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to the methanol of CNNS dropwise
In solution, mixed solution is stirred at room temperature for 24 hours, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 5mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 2.30 μm of ol/ (gh), and the yield of methane is 1.12 μm of ol/ (gh).
Embodiment 4:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 550 DEG C of Muffle furnace and calcines 4h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；
Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·6H2O) and the NaOH of 29.4g is dissolved in 70mL deionized water
In, ultrasonic treatment is then transferred into 100mL polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is put into 130 DEG C of baking ovens
Middle reaction is for 24 hours, then multiple with deionized water and ethanol washing to take out reaction kettle cooled to room temperature after reaction,
It is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.1g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL first respectively
In alcoholic solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to dropwise CNNS methanol it is molten
In liquid, mixed solution is stirred at room temperature for 24 hours, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 7mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 2.83 μm of ol/ (gh), and the yield of methane is 1.45 μm of ol/ (gh).
Embodiment 5:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 550 DEG C of Muffle furnace and calcines 3h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；
Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·6H2O) and the NaOH of 19.6g is dissolved in 70mL deionized water
In, ultrasonic treatment is then transferred into 100mL polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is put into 140 DEG C of baking ovens
Middle reaction is for 24 hours, then multiple with deionized water and ethanol washing to take out reaction kettle cooled to room temperature after reaction,
It is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.25g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL first respectively
In alcoholic solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to dropwise CNNS methanol it is molten
In liquid, mixed solution is stirred at room temperature for 24 hours, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 3mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 3.12 μm of ol/ (gh), and the yield of methane is 1.87 μm of ol/ (gh).
Embodiment 6:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 550 DEG C of Muffle furnace and calcines 4h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·
6H2O it) is dissolved in 70mL deionized water with the NaOH of 19.6g, is ultrasonically treated, is then transferred into 100mL polytetrafluoroethyllining lining
In stainless steel cauldron, reaction kettle is put into 120 DEG C of baking ovens and reacts 48h, to take out reaction kettle natural cooling after reaction
It is then multiple with deionized water and ethanol washing to room temperature, it is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.075g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL respectively
In methanol solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to the methanol of CNNS dropwise
In solution, 48h is stirred at room temperature in mixed solution, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 5mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 3.44 μm of ol/ (gh), and the yield of methane is 1.96 μm of ol/ (gh).
Embodiment 7:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 550 DEG C of Muffle furnace and calcines 4h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·
6H2O it) is dissolved in 70mL deionized water with the NaOH of 19.6g, is ultrasonically treated, is then transferred into 100mL polytetrafluoroethyllining lining
In stainless steel cauldron, reaction kettle is put into 120 DEG C of baking ovens and reacts 72h, to take out reaction kettle natural cooling after reaction
It is then multiple with deionized water and ethanol washing to room temperature, it is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.05g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL first respectively
In alcoholic solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to dropwise CNNS methanol it is molten
In liquid, 48h is stirred at room temperature in mixed solution, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 5mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 1.68 μm of ol/ (gh), and the yield of methane is 0.83 μm of ol/ (gh).
Embodiment 8:
(1) preparation of GO:
Implement according to the step (1) in embodiment 1.
(2)g-C3N4Nanometer sheet (CNNS) and rodlike CeO2(R-CeO2) preparation:
The cyanuric acid of 5g is put into crucible with cover, then crucible is put into 500 DEG C of Muffle furnace and calcines 2h, to
After dropping to room temperature, collects light yellow sample and obtain g-C3N4Sheet (CNNS)；Weigh 1.7364g cerium nitrate hexahydrate (Ce (NO3)3·
6H2O it) is dissolved in 70mL deionized water with the NaOH of 9.8g, is ultrasonically treated, is then transferred into 100mL polytetrafluoroethyllining lining
In stainless steel cauldron, reaction kettle is put into 120 DEG C of baking ovens and reacts 48h, to take out reaction kettle natural cooling after reaction
It is then multiple with deionized water and ethanol washing to room temperature, it is dried to obtain rodlike CeO2(R-CeO2)。
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
0.5g CNNS and the 0.05g R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in 40mL first respectively
In alcoholic solution, ultrasonic treatment 40min obtains suspension, then by R-CeO2Methanol solution be added drop-wise to dropwise CNNS methanol it is molten
In liquid, 48h is stirred at room temperature in mixed solution, and drying obtains R-CeO after stirring2/ CNNS binary composite photo-catalyst.
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of 0.5g step (3) preparation2/ CNNS composite photo-catalyst is dispersed in 40mL deionized water, then
The GO solution for taking 3mL step (1) to prepare is added in above-mentioned solution, is stirred at room temperature for 24 hours, is after reaction put into mixed solution
It is dried into baking oven to get two dimension rGO/R-CeO is arrived2/ CNNS hierarchical structure composite photo-catalyst.
(5) sample 0.1g in (3) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield for measuring carbon monoxide is 0.85 μm of ol/ (gh), and the yield of methane is 0.48 μm of ol/ (gh).
Fig. 1 is two dimension rGO/R-CeO2The XRD spectra of/CNNS hierarchical structure composite photo-catalyst, the exhibition being apparent in figure
Rodlike CeO is shown2Characteristic peak, the characteristic peak of GO and the characteristic peak of CNNS.
Fig. 2 is two dimension rGO/R-CeO2The UV-vis spectrogram of/CNNS hierarchical structure composite photo-catalyst is clearly opened up in figure
Show that the photoresponse ability of Three-element composite photocatalyst has been widened in the introducing of GO.
Fig. 3 is two dimension rGO/R-CeO2The TEM photo of/CNNS hierarchical structure composite photo-catalyst, it can be seen that R-CeO2Point
It is dispersed in the surface CNNS, rGO is successfully covered on R-CeO2The surface of/CNNS.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of two dimension rGO/R-CeO2The preparation method of/CNNS hierarchical structure composite photo-catalyst, which is characterized in that according to
Lower step carries out:
(1) graphene oxide GO is prepared, spare:
(2)g-C3N4Nanometer sheet and rodlike CeO2Preparation:
A certain amount of cyanuric acid is put into crucible with cover, then crucible is put into Muffle furnace and is calcined, room temperature to be dropped to
Afterwards, it collects light yellow sample and obtains g-C3N4Sheet is denoted as CNNS；
Cerium nitrate hexahydrate (Ce (NO is weighed respectively3)3·6H2O it) is dissolved in deionized water with sodium hydroxide (NaOH), at ultrasound
Reason, is then transferred into polytetrafluoroethyllining lining stainless steel cauldron, reaction kettle is put into baking oven and is reacted, to after reaction
Reaction kettle cooled to room temperature is taken out, it is then multiple with deionized water and ethanol washing, it is dried to obtain rodlike CeO2, it is denoted as R-
CeO2；
(3)R-CeO2The preparation of/CNNS binary composite photo-catalyst:
The CNNS and R-CeO of step (2) preparation are weighed respectively2, and they are dispersed in methanol solution respectively, it is ultrasonically treated
To suspension, then by R-CeO2Methanol solution be added drop-wise in the methanol solution of CNNS dropwise, mixed solution is stirred at room temperature, and stirs
Drying obtains R-CeO after mixing2/ CNNS binary composite photo-catalyst；
(4) two dimension rGO/R-CeO2The preparation of/CNNS hierarchical structure composite photo-catalyst:
Weigh the R-CeO of step (3) preparation2/ CNNS composite photo-catalyst disperses in deionized water, step (1) then to be taken to prepare
GO solution be added in above-mentioned solution, be stirred at room temperature, mixed solution be put into baking oven dry to get arriving after reaction
Two-dimentional rGO/R-CeO2/ CNNS hierarchical structure composite photo-catalyst.
2. preparation method according to claim 1, which is characterized in that in step (1), the preparation of graphene oxide GO is walked
Suddenly include: to be put into three-necked flask in ice-water bath, 1g graphite powder and 2.5g sodium nitrate is added, the 30mL concentrated sulfuric acid, magnetic is then added
Power is uniformly mixed；Then 4g potassium permanganate is added in three-necked flask several times, after having added, in the condition of ice-water bath
Lower continuation magnetic agitation 2h；35 DEG C are then heated to, after stirring 30min at such a temperature, 40mL deionized water is slowly added to
Into three-necked flask；98 DEG C are then heated to, after reacting 40min at such a temperature, stirring continues, and closes heating；To water-bath
Temperature when being down to 70 DEG C, be that 30% hydrogen peroxide is added in three-necked flask by 10mL volume fraction, will after dropping to room temperature
Mixed solution in three-necked flask is transferred in beaker, and is washed three times with 5%HCl solution, is removed foreign ion, is finally spent
The pH of ion water washing GO, washing to pH value are 6 or so, and freeze-drying, collection obtain GO powder；Then the GO for preparing 1mg/mL is molten
Liquid.
3. preparation method according to claim 1, which is characterized in that in step (2), the calcining temperature of the cyanuric acid
Degree is 500-600 DEG C；Calcination time 2-4h.
4. preparation method according to claim 1, which is characterized in that in step (2), the Ce (NO3)3·6H2O、
NaOH and the amount ratio of deionized water are 1g:(5.64-16.93) g:70mL.
5. preparation method according to claim 1, which is characterized in that in step (2), the hydrothermal temperature is 100-
140 DEG C, the hydro-thermal time is 24-72h.
6. preparation method according to claim 1, which is characterized in that in step (3), the rodlike cerium oxide, nitridation
The amount ratio of carbon nanosheet and methanol solution is 1g:(2-10) g:40mL.
7. preparation method according to claim 1, which is characterized in that in step (3), the mixing time is 24-
48h。
8. preparation method according to claim 1, which is characterized in that in step (4), the R-CeO2/ CNNS's and GO
Mass ratio is 1:(0.002-0.014), it is for 24 hours that the time, which is stirred at room temperature,.
9. a kind of two dimension rGO/R-CeO2/ CNNS hierarchical structure composite photo-catalyst, which is characterized in that be by claim 1~
Made from any one of 8 preparation methods, pattern is two-dimentional hierarchical structure, and rodlike cerium oxide is randomly distributed over rGO and CNNS
Between.
10. by two dimension rGO/R-CeO as claimed in claim 92/ CNNS hierarchical structure composite photo-catalyst is used under ultraviolet light also
Former CO2Purposes.
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Application publication date: 20190920 |