CN107876039A - The preparation method of graphene cerium oxide hybrid material - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 29
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229960002163 hydrogen peroxide Drugs 0.000 claims abstract description 11
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 11
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 11
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 8
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims abstract description 6
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 5
- 230000000593 degrading effect Effects 0.000 abstract description 3
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 3
- 239000003054 catalyst Substances 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Polymers C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003911 water pollution 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention discloses a kind of preparation method of graphene cerium oxide hybrid material, comprises the following steps:(1)Graphite powder, sodium nitrate are mixed, the concentrated sulfuric acid and potassium permanganate is sequentially added, is stirred, is heated, deionized water is added, hydrogenperoxide steam generator is added dropwise, filter while hot, by washing of precipitate, vacuum drying, obtains graphene oxide;(2)By CeCl3·7H2O dissolves in deionized water, obtains solution A;Sodium hydroxide is dissolved in deionized water, obtains solution B;Solution B is added dropwise in solution A, filtered, by washing of precipitate, vacuum drying, obtains cerium oxide CeO2;(3)By graphene oxide dissolving in deionized water, ultrasonic disperse;Then cerium oxide stirring is added, continues to react after microwave heating, filters, by washing of precipitate, vacuum drying, obtains graphene cerium oxide hybrid material.This method is simple to operate, and the graphene cerium oxide hybrid material being prepared is high to the degrading activity of ammonia nitrogen.
Description
Technical field
The invention belongs to photocatalyst technology field, and in particular to a kind of preparation side of graphene-cerium oxide hybrid material
Method.
Background technology
Traditional sewage water denitrification is frequently with nitrification-denitrification method, and it is easily by environment temperature, mud year, pollutant component etc.
The influence of factor, its nitric efficiency are not sufficiently stable, and elapsed time is grown.Therefore need to develop new denitrogenation technology.
1972, it was recently reported that photoelectrocatalysis hydrogen production by water decomposition;Then, it was recently reported that TiO2Degraded polystream phenol, has started half
Application study of the conductor photochemical catalyst in water pollution control.Photocatalytic method can with oxidation of organic compounds, reducing heavy metal ion with
And kill germ.So the technology has broad application prospects.Cerium oxide (CeO2) it is a kind of and TiO2With similarity
Semi-conducting material, and CeO2In Ce there is variable valence state, band structure can be with artificial regulatory.Graphene is big because of it
Specific surface area is considered as good catalyst carrier, and graphene is compound with photochemical catalyst, can strengthen its absorption property, and
Its spectral response range is widened, so as to improve the utilization rate to solar energy.At present, there are cerium oxide and graphene composite material can be with
Photochemical catalytic oxidation organic pollution, still, the catalyst of CeO- graphene hydridization photocatalyst for degrading ammonia nitrogens are less, exist and urge
Change the problem of efficiency is low.
The content of the invention
The defects of for prior art, the present invention provide a kind of preparation method of graphene-cerium oxide hybrid material.
The preparation method of graphene-cerium oxide hybrid material, comprises the following steps:
(1)The preparation of graphene oxide:Graphite powder, sodium nitrate are mixed, then sequentially add the concentrated sulfuric acid and potassium permanganate, is stirred
Mixing, reacts 2h at 20 DEG C, reacts 30min after then heating to 35-40 DEG C, and 5 times of concentrated sulfuric acid volume is added into system
Deionized water, continue to react 20min, then the hydrogenperoxide steam generator that mass concentration is 5% is added dropwise into system, filter while hot, will be heavy
Shallow lake hydrochloric acid solution and the water washing sulfate radical-free ion into filtrate, then precipitation is dried in vacuo, that is, obtains graphene oxide;
(2)The preparation of cerium oxide:Take CeCl3·7H2O is according to solid-liquid ratio 1:5 dissolvings in deionized water, obtain solution A;Will
Sodium hydroxide is according to solid-liquid ratio 2:15 are dissolved in deionized water, obtain solution B;In the state of stirring, solution B is added dropwise to molten
In liquid A, stirring reaction 4h, 8-10h then is reacted at 180-200 DEG C, after naturally cooling to room temperature, filtering, precipitation is spent
Ion water washing 3 times, is then dried in vacuo 4h at 50 DEG C, obtains cerium oxide CeO2;
(3)The preparation of graphene-cerium oxide hybrid material:By graphene oxide according to solid-liquid ratio 1:15 are dissolved in deionized water
In, ultrasonic disperse 10min, obtain graphene oxide suspension;Then by step(2)Obtained cerium oxide adds oxidation stone
In black alkene suspension, the stirring reaction 4h under 3000rpm rotating speed, then microwave heats 20min under 200W power,
8h is reacted at 200-250 DEG C, after naturally cooling to room temperature, filtering, precipitation is washed with deionized 3 times, then at 60 DEG C
4h is dried in vacuo, obtains graphene-cerium oxide hybrid material.
Preferably, step(1)Middle graphite powder, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, the adding proportion of hydrogenperoxide steam generator
For 2g:1g:50mL:6g:10mL.
Preferably, step(1)The mass concentration of middle hydrochloric acid solution is 5%.
Preferably, step(1)In vacuum drying condition to be dried in vacuo 4h at 40 DEG C.
Preferably, step(2)The volume ratio of middle solution A and solution B is 1:1.
Preferably, step(3)The power of middle ultrasonic disperse is 300-500W.
Preferably, step(3)The mass ratio of middle graphene oxide and cerium oxide is 1:20.
Advantages of the present invention:
Method provided by the invention is simple to operate, and the graphene being prepared-cerium oxide hybrid material is that a kind of catalytic activity is high
Photochemical catalyst, it is high to the degrading activity of ammonia nitrogen.
Embodiment
Embodiment 1
The preparation method of graphene-cerium oxide hybrid material, comprises the following steps:
(1)The preparation of graphene oxide:Graphite powder, sodium nitrate are mixed, then sequentially add the concentrated sulfuric acid and potassium permanganate, is stirred
Mixing, react 2h at 20 DEG C, react 30min after then heating to 40 DEG C, into system add 5 times of concentrated sulfuric acid volume go from
Sub- water, continue to react 20min, then the hydrogenperoxide steam generator that mass concentration is 5% is added dropwise into system, filter while hot, precipitation is used
Mass concentration is 5% hydrochloric acid solution and the water washing sulfate radical-free ion into filtrate, then will be deposited at 40 DEG C and be dried in vacuo
4h, that is, obtain graphene oxide;Wherein, the adding proportion of graphite powder, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, hydrogenperoxide steam generator
For 2g:1g:50mL:6g:10mL;
(2)The preparation of cerium oxide:Take CeCl3·7H2O is according to solid-liquid ratio 1:5 dissolvings in deionized water, obtain solution A;Will
Sodium hydroxide is according to solid-liquid ratio 2:15 are dissolved in deionized water, obtain solution B;In the state of stirring, according to volume ratio 1:1 will
Solution B is added dropwise in solution A, stirring reaction 4h, then reacts 10h at 200 DEG C, and after naturally cooling to room temperature, filtering will be heavy
Shallow lake is washed with deionized 3 times, is then dried in vacuo 4h at 50 DEG C, obtains cerium oxide CeO2;
(3)The preparation of graphene-cerium oxide hybrid material:By graphene oxide according to solid-liquid ratio 1:15 are dissolved in deionized water
In, ultrasonic disperse 10min, obtains graphene oxide suspension under conditions of power 500W;Then by step(2)Obtained oxygen
Change cerium to add in graphene oxide suspension, wherein, the mass ratio of graphene oxide and cerium oxide is 1:20,
Stirring reaction 4h under 3000rpm rotating speed, then microwave heats 20min under 200W power, reacts 8h at 250 DEG C, from
After being so cooled to room temperature, filtering, precipitation is washed with deionized 3 times, then 4h is dried in vacuo at 60 DEG C, obtains graphite
Alkene-cerium oxide hybrid material.
Embodiment 2
The preparation method of graphene-cerium oxide hybrid material, comprises the following steps:
(1)The preparation of graphene oxide:Graphite powder, sodium nitrate are mixed, then sequentially add the concentrated sulfuric acid and potassium permanganate, is stirred
Mixing, react 2h at 20 DEG C, react 30min after then heating to 35 DEG C, into system add 5 times of concentrated sulfuric acid volume go from
Sub- water, continue to react 20min, then the hydrogenperoxide steam generator that mass concentration is 5% is added dropwise into system, filter while hot, precipitation is used
Mass concentration is 5% hydrochloric acid solution and the water washing sulfate radical-free ion into filtrate, then will be deposited at 40 DEG C and be dried in vacuo
4h, that is, obtain graphene oxide;Wherein, the adding proportion of graphite powder, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, hydrogenperoxide steam generator
For 2g:1g:50mL:6g:10mL;
(2)The preparation of cerium oxide:Take CeCl3·7H2O is according to solid-liquid ratio 1:5 dissolvings in deionized water, obtain solution A;Will
Sodium hydroxide is according to solid-liquid ratio 2:15 are dissolved in deionized water, obtain solution B;In the state of stirring, according to volume ratio 1:1 will
Solution B is added dropwise in solution A, stirring reaction 4h, then reacts 8h at 180 DEG C, and after naturally cooling to room temperature, filtering will be heavy
Shallow lake is washed with deionized 3 times, is then dried in vacuo 4h at 50 DEG C, obtains cerium oxide CeO2;
(3)The preparation of graphene-cerium oxide hybrid material:By graphene oxide according to solid-liquid ratio 1:15 are dissolved in deionized water
In, ultrasonic disperse 10min, obtains graphene oxide suspension under conditions of power 300W;Then by step(2)Obtained oxygen
Change cerium to add in graphene oxide suspension, wherein, the mass ratio of graphene oxide and cerium oxide is 1:20,
Stirring reaction 4h under 3000rpm rotating speed, then microwave heats 20min under 200W power, reacts 8h at 200 DEG C, from
After being so cooled to room temperature, filtering, precipitation is washed with deionized 3 times, then 4h is dried in vacuo at 60 DEG C, obtains graphite
Alkene-cerium oxide hybrid material.
Embodiment 3
The preparation method of graphene-cerium oxide hybrid material, comprises the following steps:
(1)The preparation of graphene oxide:Graphite powder, sodium nitrate are mixed, then sequentially add the concentrated sulfuric acid and potassium permanganate, is stirred
Mixing, react 2h at 20 DEG C, react 30min after then heating to 38 DEG C, into system add 5 times of concentrated sulfuric acid volume go from
Sub- water, continue to react 20min, then the hydrogenperoxide steam generator that mass concentration is 5% is added dropwise into system, filter while hot, precipitation is used
Mass concentration is 5% hydrochloric acid solution and the water washing sulfate radical-free ion into filtrate, then will be deposited at 40 DEG C and be dried in vacuo
4h, that is, obtain graphene oxide;Wherein, the adding proportion of graphite powder, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, hydrogenperoxide steam generator
For 2g:1g:50mL:6g:10mL;
(2)The preparation of cerium oxide:Take CeCl3·7H2O is according to solid-liquid ratio 1:5 dissolvings in deionized water, obtain solution A;Will
Sodium hydroxide is according to solid-liquid ratio 2:15 are dissolved in deionized water, obtain solution B;In the state of stirring, according to volume ratio 1:1 will
Solution B is added dropwise in solution A, stirring reaction 4h, then reacts 9h at 190 DEG C, and after naturally cooling to room temperature, filtering will be heavy
Shallow lake is washed with deionized 3 times, is then dried in vacuo 4h at 50 DEG C, obtains cerium oxide CeO2;
(3)The preparation of graphene-cerium oxide hybrid material:By graphene oxide according to solid-liquid ratio 1:15 are dissolved in deionized water
In, ultrasonic disperse 10min, obtains graphene oxide suspension under conditions of power 400W;Then by step(2)Obtained oxygen
Change cerium to add in graphene oxide suspension, wherein, the mass ratio of graphene oxide and cerium oxide is 1:20,
Stirring reaction 4h under 3000rpm rotating speed, then microwave heats 20min under 200W power, reacts 8h at 220 DEG C, from
After being so cooled to room temperature, filtering, precipitation is washed with deionized 3 times, then 4h is dried in vacuo at 60 DEG C, obtains graphite
Alkene-cerium oxide hybrid material.
Claims (7)
1. the preparation method of graphene-cerium oxide hybrid material, it is characterised in that:Comprise the following steps:
(1)The preparation of graphene oxide:Graphite powder, sodium nitrate are mixed, then sequentially add the concentrated sulfuric acid and potassium permanganate, is stirred
Mixing, reacts 2h at 20 DEG C, reacts 30min after then heating to 35-40 DEG C, and 5 times of concentrated sulfuric acid volume is added into system
Deionized water, continue to react 20min, then the hydrogenperoxide steam generator that mass concentration is 5% is added dropwise into system, filter while hot, will be heavy
Shallow lake hydrochloric acid solution and the water washing sulfate radical-free ion into filtrate, then precipitation is dried in vacuo, that is, obtains graphene oxide;
(2)The preparation of cerium oxide:Take CeCl3·7H2O is according to solid-liquid ratio 1:5 dissolvings in deionized water, obtain solution A;By hydrogen
Sodium oxide molybdena is according to solid-liquid ratio 2:15 are dissolved in deionized water, obtain solution B;In the state of stirring, solution B is added dropwise to solution
In A, stirring reaction 4h, then react 8-10h at 180-200 DEG C, after naturally cooling to room temperature, filtering, by precipitation spend from
Sub- water washing 3 times, is then dried in vacuo 4h at 50 DEG C, obtains cerium oxide CeO2;
(3)The preparation of graphene-cerium oxide hybrid material:By graphene oxide according to solid-liquid ratio 1:15 are dissolved in deionized water
In, ultrasonic disperse 10min, obtain graphene oxide suspension;Then by step(2)Obtained cerium oxide adds oxidation stone
In black alkene suspension, the stirring reaction 4h under 3000rpm rotating speed, then microwave heats 20min under 200W power,
8h is reacted at 200-250 DEG C, after naturally cooling to room temperature, filtering, precipitation is washed with deionized 3 times, then at 60 DEG C
4h is dried in vacuo, obtains graphene-cerium oxide hybrid material.
2. the preparation method of graphene according to claim 1-cerium oxide hybrid material, it is characterised in that:Step(1)In
Graphite powder, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, the adding proportion of hydrogenperoxide steam generator are 2g:1g:50mL:6g:10mL.
3. the preparation method of graphene according to claim 1-cerium oxide hybrid material, it is characterised in that:Step(1)In
The mass concentration of hydrochloric acid solution is 5%.
4. the preparation method of graphene according to claim 1-cerium oxide hybrid material, it is characterised in that:Step(1)In
Vacuum drying condition is to be dried in vacuo 4h at 40 DEG C.
5. the preparation method of graphene according to claim 1-cerium oxide hybrid material, it is characterised in that:Step(2)In
The volume ratio of solution A and solution B is 1:1.
6. the preparation method of graphene according to claim 1-cerium oxide hybrid material, it is characterised in that:Step(3)In
The power of ultrasonic disperse is 300-500W.
7. the preparation method of graphene according to claim 1-cerium oxide hybrid material, it is characterised in that:Step(3)In
The mass ratio of graphene oxide and cerium oxide is 1:20.
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Cited By (5)
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CN110514642A (en) * | 2019-09-24 | 2019-11-29 | 吉林师范大学 | A kind of SERS substrate and preparation method thereof detecting incretion interferent BPA |
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CN112961653A (en) * | 2021-02-07 | 2021-06-15 | 广西立之亿新材料有限公司 | Preparation method of nano cerium oxide-graphene composite particles |
CN113372822A (en) * | 2021-06-29 | 2021-09-10 | 广西立之亿新材料有限公司 | Preparation method of nano cerium oxide-graphene particles |
CN113908807A (en) * | 2021-11-29 | 2022-01-11 | 北京师范大学 | Nitrogen-doped modified graphene electrode material for adsorbing electroreduction radionuclide |
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2017
- 2017-12-04 CN CN201711259005.6A patent/CN107876039A/en not_active Withdrawn
Cited By (6)
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CN110514642A (en) * | 2019-09-24 | 2019-11-29 | 吉林师范大学 | A kind of SERS substrate and preparation method thereof detecting incretion interferent BPA |
CN112209421A (en) * | 2020-07-29 | 2021-01-12 | 复旦大学 | Accordion-like cerium oxide/reduced graphene oxide composite material and preparation and application thereof |
CN112209421B (en) * | 2020-07-29 | 2022-12-16 | 复旦大学 | Accordion-like cerium oxide/reduced graphene oxide composite material and preparation and application thereof |
CN112961653A (en) * | 2021-02-07 | 2021-06-15 | 广西立之亿新材料有限公司 | Preparation method of nano cerium oxide-graphene composite particles |
CN113372822A (en) * | 2021-06-29 | 2021-09-10 | 广西立之亿新材料有限公司 | Preparation method of nano cerium oxide-graphene particles |
CN113908807A (en) * | 2021-11-29 | 2022-01-11 | 北京师范大学 | Nitrogen-doped modified graphene electrode material for adsorbing electroreduction radionuclide |
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