CN107308929A - A kind of preparation method of graphene nano titanium dioxide compound photochemical catalyst - Google Patents
A kind of preparation method of graphene nano titanium dioxide compound photochemical catalyst Download PDFInfo
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- CN107308929A CN107308929A CN201710333122.6A CN201710333122A CN107308929A CN 107308929 A CN107308929 A CN 107308929A CN 201710333122 A CN201710333122 A CN 201710333122A CN 107308929 A CN107308929 A CN 107308929A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 58
- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- -1 graphene nano titanium dioxide compound Chemical class 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 66
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 17
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 84
- 239000000243 solution Substances 0.000 claims description 63
- 239000004408 titanium dioxide Substances 0.000 claims description 55
- 239000000843 powder Substances 0.000 claims description 24
- 239000003643 water by type Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 238000010828 elution Methods 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 8
- 239000012467 final product Substances 0.000 claims description 8
- 229960002163 hydrogen peroxide Drugs 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 235000010344 sodium nitrate Nutrition 0.000 claims description 8
- 239000004317 sodium nitrate Substances 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 abstract 1
- 235000010215 titanium dioxide Nutrition 0.000 description 39
- 238000010790 dilution Methods 0.000 description 6
- 239000012895 dilution Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- UXAMZEYKWGPDBI-UHFFFAOYSA-N C(CCCCCCCCCCCCCCC)Br(C)(C)C Chemical class C(CCCCCCCCCCCCCCC)Br(C)(C)C UXAMZEYKWGPDBI-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 102100030310 5,6-dihydroxyindole-2-carboxylic acid oxidase Human genes 0.000 description 1
- 208000019901 Anxiety disease Diseases 0.000 description 1
- 101000773083 Homo sapiens 5,6-dihydroxyindole-2-carboxylic acid oxidase Proteins 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- 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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- 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
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- Toxicology (AREA)
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- Hydrology & Water Resources (AREA)
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Abstract
The present invention is to be related to a kind of preparation method of graphene nano titanium dioxide compound photochemical catalyst, using graphite powder, the concentrated sulfuric acid, titanium trichloride, n-hexane, n-amyl alcohol, cetyl trimethylammonium bromide as raw material, reacted by hydro-thermal method and graphene nano titanium dioxide compound photochemical catalyst is made.Present invention synthesis is simple, and operation is more convenient, and cost is low, pollution-free;Graphene nano titanium dioxide compound prepared by the present invention has excellent photocatalysis performance, and the ability of degradable organic pollutant is strong, and can follow bad utilization, and this catalyst also has the characteristic of absorption in addition.
Description
Technical field
The present invention relates to a kind of preparation method of graphene-titanium dioxide compound photochemical catalyst, photocatalysis is particularly belonged to
Agent technical field.
Background technology
With developing rapidly for science and technology, the living standard of the mankind gradually rises.China is in terms of economic growth
Significant progress is achieved, productivity is greatly improved.But many areas of China be by cost of welding from
And economy is significantly lifted, therefore it may be seen that the small square built everywhere, to river in have discharged substantial amounts of industry dirty
Water, pm2.5 indexes are only increased, and our living environment causes anxiety.Water is Source of life, and water pollution is into the public affairs of the whole mankind
Enemy, how to reduce the influence that water pollution brings is the problem of we will consider.Now in terms of sewage disposal, there is absorption, manually
Salvage etc., sum it up, very single.And absorption method often causes secondary pollution, lose more than gain, in addition at many sewage
Manage technical costs high, be not easy to promote the use of.
Photocatalysis presents its good advantage as a kind of new technology.Compared to common sewage disposal technology, light is urged
Changing has lot of advantages, and first, reaction condition is gentle, and degradable organic pollutant effect is good.;Secondly, it is with low cost, prepare letter
It is single, it is easy to operate;Furthermore, it can be recycled, and photocatalysis Decomposition product is H2O ﹑ CO2﹑ N2Etc. pollution-free material, it will not produce
Secondary pollution.Therefore, it has very high economic value and social benefit.
Titanium dioxide has very excellent chemical property, such as chemical stability, electrical conductivity.Just because of it has a lot
Advantage, so being applied to many fields.Titanium dioxide has three types, rutile-type, Detitanium-ore-type, brookite type.Wherein,
Anatase titanium dioxide stability is good, and oxygen uptake ability is high, therefore is more widely applied.Anatase titanium dioxide has fine
Photo-catalysis capability, therefore photocatalyst for degrading pollutant can be made.Anatase titanium dioxide is full of electronics by one
Low-energy zone is constituted with an empty high energy band, and low-energy zone and high energy band are separated by forbidden band, and it is wide bandgap semiconductor, works as TiO2 Receive
Rice rod is by after the photon irradiation more than or equal to energy gap energy, and electronics is stimulated from valence band jump to conduction band, can be in valence band
Upper generation hole, and hole has strong oxidizing property with light induced electron, can be with degradable organic pollutant.But due to titanium dioxide only
Ultraviolet light can be absorbed, and UV energy accounting in solar energy is extremely low, therefore titanium dioxide can not make full use of sunlight;
Other light induced electron and the recombination rate in hole are much larger than its speed being had an effect with organic matter, because the two shortcomings, make
Optically catalytic TiO 2 performance is obtained to have a greatly reduced quality.
In order to solve the shortcoming of titanium dioxide nano-rod, it is considered to introduce graphene particles.Graphene is one kind by monolayer carbon
Former molecular bi-dimensional cellular shape lattice structure carbonaceous material, with good electric conductivity, and specific surface area is very big.By its with
Titanium dioxide nano-rod is combined, and can substantially improve that titanium dioxide absorptivity is low, light induced electron and hole easily compound shortcoming.
Its reason is as follows, and graphene has certain adsorption capacity, and pollutant can be adsorbed onto to the surface of catalyst, accelerates reaction speed
Rate, in addition the satisfactory electrical conductivity of graphene can delay the compound of electron hole, the bonding of graphene and titanium dioxide reduces energy
Extreme difference, makes catalyst improve the utilization rate of sunshine.
The preparation for graphene-titanium dioxide compound has had certain methods at present, but more or less has
In place of some shortcomings.In the preparation method for example in patent CN105551828A stated, there is wastage of material, it is remarkable to operate
Shortcoming, it is suppressed that its application industrially.
The content of the invention
It is an object of the invention to provide a kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, with
Graphite powder, the concentrated sulfuric acid, CATB, pentane, n-amyl alcohol, titanium oxide etc. is raw material, passes through a series of reaction and graphite is made
Alkene-nanometer titanium dioxide compound photochemical catalyst.This catalyst preparation process is simple, and cost is relatively low, possesses good catalytic
Can, under normal temperature and pressure, sunshine irradiation, you can, catabolite is pollution-free by organic pollution catalytic degradation completely.
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 200-500mg graphite powders, the mixed solution of 1.5-2.5g sodium nitrate, add 15-25ml mass concentrations for 98% it is dense
Sulfuric acid, stirs at a temperature of less than 5 DEG C, allows it to react 1.0-1.5h in beaker;By potassium permanganate grind into powder, then
In 0.5h, 1.5-3.0g powder is added in beaker, 1.5-2.0h is reacted in temperature is less than 5 DEG C;Beaker is placed on constant temperature
35-40 DEG C is warming up in case, then constant temperature 1.0-1.5h, constant temperature terminates to add 40-50mL deionized waters in backward beaker, then will
Temperature rises to 85-100 DEG C, constant temperature 10-20min;Then the solution in beaker is cooled to indoor temperature, adds 60-90ml and go
Ionized water is diluted, and solution is changed into glassy yellow, and the hydrogenperoxide steam generator that 10-15ml mass concentrations are 35% is added afterwards;Then enter
Row filtering, by the filter residue salt acid elution that 250-410ml mass concentrations are 5%, repeated washing is drained with aspiration pump three times, then
It is washed with deionized three times, is finally dialysed two days with bag filter again, vacuum drying chamber is put into afterwards 24h is dried at 60 DEG C,
Finally clay into power and obtain graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 8-10mg is taken, 8-10ml deionized waters are added, using processor for ultrasonic wave in 60W
Ultrasonically treated 20-60min under power, just can obtain the graphene oxide solution that mass concentration is 1mg/ml;By 5.5-6.0g ten
Six alkyl trimethyl ammonium bromides are dissolved in the mixed solution of 5-20ml n-amyl alcohols and 50-65ml n-hexanes, obtain cetyl
Trimethylammonium bromide solution;Cetyl trimethylammonium bromide solution is added to graphene oxide solution simultaneously, at room temperature
Stir 30min;After solution turns into gold matter emulsion, the mass concentration for adding 0.6-6ml is 28% titanium oxide solution,
And stir after 30min, pour into autoclave, be placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put
Enter in rotary evaporator reduced pressure treatment and precipitate, remove organic reagent, obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly,
Remove surfactant and other impurities, obtained final product dries 1-2h under the conditions of being placed on 80 DEG C, that is, obtain graphene-
Titanium dioxide compound photochemical catalyst.
The principle of the present invention is that titanium dioxide can be produced the transition phenomenon of electronics by light irradiation, so as to produce light induced electron
And hole, light induced electron and hole all have strong oxidizing property, can by the organic pollutant degradation in solution into small molecule thing
Matter.But titanium dioxide is too low to the utilization rate of sunshine, also light induced electron and hole easily compound shortcoming, it is considered to introduce
Graphene improves its property, that is, strengthens the absorption to sunshine, suppresses the compound of light induced electron and hole.In addition, titanium dioxide
Increase with the compound specific surface area that can allow catalyst of graphene, accelerate reaction rate, improve the performance of catalyst.
Advantages of the present invention is:
1. 1-3 of the embodiment of the present invention is by controlling the solvent of n-amyl alcohol and n-hexane than preparing three kinds of graphene-nanometer titanium dioxides
Titanium compound, i.e., 5:65,10:60,20:50, and best one of photocatalysis performance has therefrom been selected by photocatalysis experiment
Catalyst is planted, experiment shows that solvent ratio is 10:Catalytic performance is best when 60.
2. the product graphene of the present invention-nano titanic oxide catalyst purity is high, almost without any impurity, constituent
That is titanium dioxide and redox graphene, and preparation method is easy, it is with low cost, can volume production.
3. the present invention will not produce secondary pollution to biological nontoxic.
4. application method is very simple, use condition is gentle, with regard to energy successful decomposition organic pollution under sunshine irradiation,
10mg catalyst can degrade 50ml 10mg/ml methyl orange solution completely in 30min.
5. graphene-nanometer titanium dioxide compound has good activity, bad utilization can be followed.
Brief description of the drawings
Fig. 1:Photocatalysis performance figure of the different solvents than obtained graphene-nanometer titanium dioxide compound photochemical catalyst.
Fig. 2:The structure chart of graphene made from the embodiment of the present invention 1-nanometer titanium dioxide compound photochemical catalyst.
Fig. 3:The structure chart of graphene made from the embodiment of the present invention 3-nanometer titanium dioxide compound photochemical catalyst.
Embodiment
Embodiment 1
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 500mg graphite powders, the mixed solution of 2.0g sodium nitrate, add the concentrated sulfuric acid that 18ml mass concentrations are 98%, less than
Stirred at a temperature of 5 DEG C, allow it to react 1.0h in beaker;By potassium permanganate grind into powder, then in 0.5h, in beaker
Middle addition 3.0g powder, 1.5h is reacted in temperature is less than 5 DEG C;Beaker is placed in insulating box and is warming up to 35 DEG C, then constant temperature
1.0h, constant temperature terminates to add 40mL deionized waters in backward beaker, then temperature is risen into 100 DEG C, constant temperature 15min;Then burning
Solution in cup is cooled to indoor temperature, adds the dilution of 70ml deionized waters, and solution is changed into glassy yellow, 10ml matter is added afterwards
Measure the hydrogenperoxide steam generator that concentration is 35%;Then filtered, the filter residue salt acid elution that 400ml mass concentrations are 5% is used
Aspiration pump drains repeated washing three times, is then washed with deionized again three times, is finally dialysed two days, be put into afterwards with bag filter
Vacuum drying chamber dries 24h at 60 DEG C, finally clays into power and obtains graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 10mg is taken, 10ml deionized waters are added, using processor for ultrasonic wave in 60W power
Under ultrasonically treated 20-60min, just can obtain mass concentration be 1mg/ml graphene oxide solution;By 5.8g cetyls three
Methyl bromide ammonium is dissolved in the mixed solution of 5ml n-amyl alcohols and 65ml n-hexanes, obtains cetyl trimethylammonium bromide molten
Liquid;Cetyl trimethylammonium bromide solution is added to graphene oxide solution simultaneously, 30min is stirred at room temperature;Molten
Liquid turns into after gold matter emulsion, and the mass concentration for adding 1.524ml is 28% titanium oxide solution, and stirs 30min
Afterwards, pour into autoclave, be placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put into rotary evaporator
Reduced pressure treatment is simultaneously precipitated, and removes organic reagent, and obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly, removes surfactant
And other impurities, obtained final product dry 2h under the conditions of being placed on 80 DEG C, that is, obtain graphene-titanium dioxide compound light
Catalyst.
Embodiment 2
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
In the step of preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
In the mixed solution that 5.8g cetyl trimethylammonium bromides are dissolved in 10ml n-amyl alcohols and 60ml n-hexanes, remaining is same
Embodiment 1.
Embodiment 3
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
In the step of preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
In the mixed solution that 5.8g cetyl trimethylammonium bromides are dissolved in 20ml n-amyl alcohols and 50ml n-hexanes, remaining is same
Embodiment 1.
Embodiment 4
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 200mg graphite powders, the mixed solution of 1.5g sodium nitrate, add the concentrated sulfuric acid that 15ml mass concentrations are 98%, less than
Stirred at a temperature of 5 DEG C, allow it to react 1.0h in beaker;By potassium permanganate grind into powder, then in 0.5h, in beaker
Middle addition 1.5g powder, 1.5h is reacted in temperature is less than 5 DEG C;Beaker is placed in insulating box and is warming up to 35 DEG C, then constant temperature
1.0h, constant temperature terminates to add 40mL deionized waters in backward beaker, then temperature is risen into 85 DEG C, constant temperature 10min;Then beaker
In solution be cooled to indoor temperature, add the dilution of 60ml deionized waters, solution is changed into glassy yellow, 10ml mass is added afterwards
Concentration is 35% hydrogenperoxide steam generator;Then filtered, by the filter residue salt acid elution that 250ml mass concentrations are 5%, with taking out
Air pump drains repeated washing three times, is then washed with deionized three times, is finally dialysed two days with bag filter again, is put into afterwards true
Empty drying box dries 24h at 60 DEG C, finally clays into power and obtains graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 8mg is taken, 8ml deionized waters are added, using processor for ultrasonic wave under 60W power
Ultrasonically treated 20min, just can obtain the graphene oxide solution that mass concentration is 1mg/ml;By 5.5g cetyl trimethyl bromines
Change ammonium to be dissolved in the mixed solution of 5ml n-amyl alcohols and 50ml n-hexanes, obtain cetyl trimethylammonium bromide solution;By ten
Six alkyl trimethyl ammonium bromide solution are added to graphene oxide solution simultaneously, and 30min is stirred at room temperature;Turn into Huang in solution
After golden emulsion, the mass concentration for adding 0.6ml is 28% titanium oxide solution, and stirs after 30min, pours into high pressure
In reactor, it is placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put into rotary evaporator reduced pressure treatment simultaneously
Precipitation, removes organic reagent, and obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly, removes surfactant and other impurities,
Obtained final product dries 1h under the conditions of being placed on 80 DEG C, that is, obtains graphene-titanium dioxide compound photochemical catalyst.
Embodiment 5
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 350mg graphite powders, the mixed solution of 2.0g sodium nitrate, add the concentrated sulfuric acid that 20ml mass concentrations are 98%, less than
Stirred at a temperature of 5 DEG C, allow it to react 1.2h in beaker;By potassium permanganate grind into powder, then in 0.5h, in beaker
Middle addition 2.0g powder, 1.8h is reacted in temperature is less than 5 DEG C;Beaker is placed in insulating box and is warming up to 38 DEG C, then constant temperature
1.2h, constant temperature terminates to add 45mL deionized waters in backward beaker, then temperature is risen into 90 DEG C, constant temperature 15min;Then beaker
In solution be cooled to indoor temperature, add the dilution of 75ml deionized waters, solution is changed into glassy yellow, 12ml mass is added afterwards
Concentration is 35% hydrogenperoxide steam generator;Then filtered, by the filter residue salt acid elution that 350ml mass concentrations are 5%, with taking out
Air pump drains repeated washing three times, is then washed with deionized three times, is finally dialysed two days with bag filter again, is put into afterwards true
Empty drying box dries 24h at 60 DEG C, finally clays into power and obtains graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 9mg is taken, 9ml deionized waters are added, using processor for ultrasonic wave under 60W power
Ultrasonically treated 40min, just can obtain the graphene oxide solution that mass concentration is 1mg/ml;By 5.8g cetyl trimethyl bromines
Change ammonium to be dissolved in the mixed solution of 10ml n-amyl alcohols and 55ml n-hexanes, obtain cetyl trimethylammonium bromide solution;Will
Cetyl trimethylammonium bromide solution is added to graphene oxide solution simultaneously, and 30min is stirred at room temperature;Turn into solution
After gold matter emulsion, the mass concentration for adding 3ml is 28% titanium oxide solution, and stirs after 30min, pours into high pressure
In reactor, it is placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put into rotary evaporator reduced pressure treatment simultaneously
Precipitation, removes organic reagent, and obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly, removes surfactant and other impurities,
Obtained final product dries 1.5h under the conditions of being placed on 80 DEG C, that is, obtains graphene-titanium dioxide compound photochemical catalyst.
Embodiment 6
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 500mg graphite powders, the mixed solution of 2.5g sodium nitrate, add the concentrated sulfuric acid that 25ml mass concentrations are 98%, less than
Stirred at a temperature of 5 DEG C, allow it to react 1.5h in beaker;By potassium permanganate grind into powder, then in 0.5h, in beaker
Middle addition 3.0g powder, 2.0h is reacted in temperature is less than 5 DEG C;Beaker is placed in insulating box and is warming up to 40 DEG C, then constant temperature
1.5h, constant temperature terminates to add 50mL deionized waters in backward beaker, then temperature is risen into 100 DEG C, constant temperature 20min;Then burning
Solution in cup is cooled to indoor temperature, adds the dilution of 90ml deionized waters, and solution is changed into glassy yellow, 15ml matter is added afterwards
Measure the hydrogenperoxide steam generator that concentration is 35%;Then filtered, the filter residue salt acid elution that 410ml mass concentrations are 5% is used
Aspiration pump drains repeated washing three times, is then washed with deionized again three times, is finally dialysed two days, be put into afterwards with bag filter
Vacuum drying chamber dries 24h at 60 DEG C, finally clays into power and obtains graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 10mg is taken, 10ml deionized waters are added, using processor for ultrasonic wave in 60W power
Under ultrasonically treated 60min, just can obtain mass concentration be 1mg/ml graphene oxide solution;By 6.0g cetyl trimethyls
Ammonium bromide is dissolved in the mixed solution of 20ml n-amyl alcohols and 65ml n-hexanes, obtains cetyl trimethylammonium bromide solution;
Cetyl trimethylammonium bromide solution is added to graphene oxide solution simultaneously, 30min is stirred at room temperature;Solution into
After gold matter emulsion, the mass concentration for adding 6ml is 28% titanium oxide solution, and stirs after 30min, pours into height
Press in reactor, be placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put into reduced pressure treatment in rotary evaporator
And precipitate, organic reagent is removed, obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly, remove surfactant and other are miscellaneous
Matter, obtained final product dries 2h under the conditions of being placed on 80 DEG C, that is, obtains graphene-titanium dioxide compound photochemical catalyst.
Comparative example 1
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 150mg graphite powders, the mixed solution of 1.0g sodium nitrate, add the concentrated sulfuric acid that 10ml mass concentrations are 98%, less than
Stirred at a temperature of 5 DEG C, allow it to react 0.5h in beaker;By potassium permanganate grind into powder, then in 0.5h, in beaker
Middle addition 1.0g powder, 1.0h is reacted in temperature is less than 5 DEG C;Beaker is placed in insulating box and is warming up to 30 DEG C, then constant temperature
1.0-1.5h, constant temperature terminates to add 35mL deionized waters in backward beaker, then temperature is risen into 80 DEG C, constant temperature 5min;Then
Solution in beaker is cooled to indoor temperature, adds the dilution of 50ml deionized waters, and solution is changed into glassy yellow, 5ml is added afterwards
Mass concentration is 35% hydrogenperoxide steam generator;Then filtered, by the filter residue salt acid elution that 200ml mass concentrations are 5%,
Repeated washing is drained with aspiration pump three times, be then washed with deionized three times, finally dialysed two days with bag filter again, Zhi Houfang
Enter vacuum drying chamber and 24h is dried at 60 DEG C, finally clay into power and obtain graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 6mg is taken, 6ml deionized waters are added, using processor for ultrasonic wave under 60W power
Ultrasonically treated 15min, just can obtain the graphene oxide solution that mass concentration is 1mg/ml;By 5.0g cetyl trimethyl bromines
Change ammonium to be dissolved in the mixed solution of 3ml n-amyl alcohols and 45ml n-hexanes, obtain cetyl trimethylammonium bromide solution;By ten
Six alkyl trimethyl ammonium bromide solution are added to graphene oxide solution simultaneously, and 30min is stirred at room temperature;Turn into Huang in solution
After golden emulsion, the mass concentration for adding 0.5ml is 28% titanium oxide solution, and stirs after 30min, pours into high pressure
In reactor, it is placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put into rotary evaporator reduced pressure treatment simultaneously
Precipitation, removes organic reagent, and obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly, removes surfactant and other impurities,
Obtained final product dries 0.5h under the conditions of being placed on 80 DEG C, that is, obtains graphene-titanium dioxide compound photochemical catalyst.
Comparative example 2
A kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, is comprised the following steps that:
Synthesize graphene oxide:
In 550mg graphite powders, the mixed solution of 3g sodium nitrate, the concentrated sulfuric acid that 30ml mass concentrations are 98% is added, less than 5
Stirred at a temperature of DEG C, allow it to react 2h in beaker;By potassium permanganate grind into powder, then in 0.5h, in beaker
3.5g powder is added, 2.5h is reacted in temperature is less than 5 DEG C;Beaker is placed in insulating box and is warming up to 45 DEG C, then constant temperature
2.0h, constant temperature terminates to add 55mL deionized waters in backward beaker, then temperature is risen into 105 DEG C, constant temperature 30min;Then burning
Solution in cup is cooled to indoor temperature, adds the dilution of 100ml deionized waters, and solution is changed into glassy yellow, 20ml is added afterwards
Mass concentration is 35% hydrogenperoxide steam generator;Then filtered, by the filter residue salt acid elution that 450ml mass concentrations are 5%,
Repeated washing is drained with aspiration pump three times, be then washed with deionized three times, finally dialysed two days with bag filter again, Zhi Houfang
Enter vacuum drying chamber and 24h is dried at 60 DEG C, finally clay into power and obtain graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 12mg is taken, 12ml deionized waters are added, using processor for ultrasonic wave in 60W power
Under ultrasonically treated 70min, just can obtain mass concentration be 1mg/ml graphene oxide solution;By 6.5g cetyl trimethyls
Ammonium bromide is dissolved in the mixed solution of 25ml n-amyl alcohols and 70ml n-hexanes, obtains cetyl trimethylammonium bromide solution;
Cetyl trimethylammonium bromide solution is added to graphene oxide solution simultaneously, 30min is stirred at room temperature;Solution into
After gold matter emulsion, the mass concentration for adding 7ml is 28% titanium oxide solution, and stirs after 30min, pours into height
Press in reactor, be placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put into reduced pressure treatment in rotary evaporator
And precipitate, organic reagent is removed, obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly, remove surfactant and other are miscellaneous
Matter, obtained final product dries 2.5h under the conditions of being placed on 80 DEG C, that is, obtains graphene-titanium dioxide compound photocatalysis
Agent.
The performance of graphene made from each embodiment and comparative example-titanium dioxide compound photochemical catalyst is by following table institute
Show:
It is can be seen that from upper table data in graphene produced by the present invention-titanium dioxide compound photochemical catalyst(Embodiment 1-6)
Purity can to reach that more than 99.5%, 10mg catalyst degrades 50ml 10mg/ml methyl orange solution completely required
Time is less than 30min, especially with the best results of embodiment 2, hence it is evident that better than not outside present invention process parameter area
The purity and degradation time of graphene-titanium dioxide compound photochemical catalyst made from comparative example 1 and 2, so the present invention is used
Specific technological parameter, not only purity is high for obtained graphene-titanium dioxide compound photochemical catalyst, and degradation time
It is short.
Claims (2)
1. a kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, it is characterized in that:Step is as follows:
Synthesize graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst.
2. a kind of preparation method of graphene-nanometer titanium dioxide compound photochemical catalyst, it is characterized in that:Comprise the following steps that:
Synthesize graphene oxide:
In 200-500mg graphite powders, the mixed solution of 1.5-2.5g sodium nitrate, add 15-25ml mass concentrations for 98% it is dense
Sulfuric acid, stirs at a temperature of less than 5 DEG C, allows it to react 1.0-1.5h in beaker;By potassium permanganate grind into powder, then
In 0.5h, 1.5-3.0g powder is added in beaker, 1.5-2.0h is reacted in temperature is less than 5 DEG C;Beaker is placed on constant temperature
35-40 DEG C is warming up in case, then constant temperature 1.0-1.5h, constant temperature terminates to add 40-50mL deionized waters in backward beaker, then will
Temperature rises to 85-100 DEG C, constant temperature 10-20min;Then the solution in beaker is cooled to indoor temperature, adds 60-90ml and go
Ionized water is diluted, and solution is changed into glassy yellow, and the hydrogenperoxide steam generator that 10-15ml mass concentrations are 35% is added afterwards;Then enter
Row filtering, by the filter residue salt acid elution that 250-410ml mass concentrations are 5%, repeated washing is drained with aspiration pump three times, then
It is washed with deionized three times, is finally dialysed two days with bag filter again, vacuum drying chamber is put into afterwards 24h is dried at 60 DEG C,
Finally clay into power and obtain graphene oxide;
The preparation of graphene-nanometer titanium dioxide compound photochemical catalyst:
Above-mentioned obtained graphene oxide 8-10mg is taken, 8-10ml deionized waters are added, using processor for ultrasonic wave in 60W
Ultrasonically treated 20-60min under power, just can obtain the graphene oxide solution that mass concentration is 1mg/ml;By 5.5-6.0g ten
Six alkyl trimethyl ammonium bromides are dissolved in the mixed solution of 5-20ml n-amyl alcohols and 50-65ml n-hexanes, obtain cetyl
Trimethylammonium bromide solution;Cetyl trimethylammonium bromide solution is added to graphene oxide solution simultaneously, at room temperature
Stir 30min;After solution turns into gold matter emulsion, the mass concentration for adding 0.6-6ml is 28% titanium oxide solution,
And stir after 30min, pour into autoclave, be placed in baking box, in 200 DEG C of constant temperature 6h;Product after constant temperature is put
Enter in rotary evaporator reduced pressure treatment and precipitate, remove organic reagent, obtained precipitation is washed 2 ~ 3 times with water and ethanol repeatedly,
Remove surfactant and other impurities, obtained final product dries 1-2h under the conditions of being placed on 80 DEG C, that is, obtain graphene-
Titanium dioxide compound photochemical catalyst.
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