CN106475083A - The preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor - Google Patents
The preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor Download PDFInfo
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- CN106475083A CN106475083A CN201610810336.3A CN201610810336A CN106475083A CN 106475083 A CN106475083 A CN 106475083A CN 201610810336 A CN201610810336 A CN 201610810336A CN 106475083 A CN106475083 A CN 106475083A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 112
- 239000002131 composite material Substances 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 60
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 37
- 239000002243 precursor Substances 0.000 title claims abstract description 37
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 65
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000012467 final product Substances 0.000 claims description 20
- 239000010453 quartz Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003708 ampul Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- 238000006552 photochemical reaction Methods 0.000 claims description 9
- 230000004044 response Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 3
- 230000009977 dual effect Effects 0.000 abstract description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 17
- 230000003647 oxidation Effects 0.000 description 11
- 238000007254 oxidation reaction Methods 0.000 description 11
- 239000011941 photocatalyst Substances 0.000 description 9
- 229960005196 titanium dioxide Drugs 0.000 description 9
- 239000010936 titanium Substances 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000002242 deionisation method Methods 0.000 description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 5
- -1 graphite alkene Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- 229910014033 C-OH Inorganic materials 0.000 description 1
- 229910014570 C—OH Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910003088 Ti−O−Ti Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
-
- B01J35/58—
Abstract
The invention discloses a kind of preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprise the following steps：The preparation of S1, graphene oxide/butyl titanate composite；S2, the preparation of graphene oxide/composite titania material.The preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor that the present invention provides, can prepare the optic catalytic composite material presoma of uniform load titanium dioxide.TiO in presoma2Achieve organic composite with graphene oxide, TiO 2 particles are equably supported in graphene oxide layer, the introducing of graphene oxide serves load TiO2Particle and the dual function improving photocatalytic activity, effectively lift the disposal efficiency.The persursor material of the present invention also has excellent coating functions.The inventive method has that step is simple, and easy to operate, preparation condition is gently easy to control, the features such as efficiency high.
Description
Technical field
The present invention relates to the preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, particularly belong to
Light-catalyzed reaction technical field.
Background technology
With developing rapidly of nowadays industry, environmental pollution is increasingly serious, as poisonous in industrial wastewater, harmful, difficult degradation
Deng, and conventional process mode cannot meet the environment amenable demand of today's society.Photocatalysis technology is as a kind of new ring
Border pollutant abatement technology, has important breakthrough in terms of removing removal organic polluter, and searching can effective catalytic degradation organic pollution
Environment-friendly type catalyst become urgent problem.Ti02For n-type semiconductor catalyst, have that chemical stability is high, corrosion-resistant, urge
Many advantages, such as change active good, harmless to the human body, has been widely used as photocatalyst.Under the irradiation of uviol lamp, TiO2
Electronics and hole pair can be produced, there is very strong reproducibility and oxidisability, the organic contamination in photocatalyst surface can be adsorbed
Thing deep oxidation, ultimately generates C02And H20 grade innocuous substance is so that it obtains extensively should in terms of the process of Recalcitrant chemicals
With.
Currently, nano-TiO2Application in light-catalyzed reaction is more and more extensive, and it is expected and requires with also more and more higher.
Modified nano-TiO2Photocatalyst can effectively be degraded majority of organic pollutants, and degradation efficiency also improves continuous
In.However, how by these nano-TiOs2Effectively application in produce reality is faced with larger difficulty to photocatalyst powder body:Powder
Body nano-TiO2Be applied directly to utilization rate in the process of pollutant effluents low it is also possible to cause secondary pollution.Solve this problem
Best approach is by nano-TiO2Load on the carriers such as fiber, while reusing, increase operation rate.At present, load
Nano-TiO2Main method include collosol and gel, organotitanium precursor body method etc., wherein the efficiency highest of organotitanium precursor body method,
It is easiest to realize industrialized production.But, the preparation of this presoma needs anhydrous and oxygen-free environment, and molecular weight of product is relatively low, and negative
Carry nano-TiO2Activity do not allow easy-regulating.In order to solve the above problems, research one kind can prepare payload nano-TiO2's
The method of optic catalytic composite material precursor process, it appears particularly necessary.
Content of the invention
For solving the deficiencies in the prior art, it is an object of the invention to provide a kind of graphene oxide/titanium-dioxide photo is urged
Change the preparation method of composite material precursor, the optic catalytic composite material forerunner of uniform load titanium dioxide can be prepared
Body.
In order to realize above-mentioned target, the present invention adopts the following technical scheme that：
The preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprises the following steps：S1, oxygen
The preparation of graphite alkene/butyl titanate composite；S2, the preparation of graphene oxide/composite titania material.
Further, the preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, including with
Lower step：The preparation of S1, graphene oxide/butyl titanate composite：Graphene oxide is dispersed in metatitanic acid four fourth
In the mixed solution of ester and dehydrated alcohol, ultraviolet lighting obtains final product；
S2, the preparation of graphene oxide/composite titania material：Graphene oxide/metatitanic acid four that S1 is prepared
Butyl ester composite prepares graphene oxide/composite titania material by hydro-thermal method.
In the preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, step S1, oxidation stone
The preparation of black alkene/butyl titanate composite, comprises the following steps：
S1.1, take graphene oxide, butyl titanate and dehydrated alcohol to add in quartz ampoule, stir, be passed through nitrogen
After seal；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting, filter, obtain final product after washing.Its
In, filter using being filtered using vacuum filtration machine and teflon membrane filter (0.45 μm, oil phase), washing can wash away not
Butyl titanate with graphite oxide alkene reaction.
Specifically, in the preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, step
The preparation of S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, take graphene oxide, butyl titanate and dehydrated alcohol to add in quartz ampoule, stir, be passed through nitrogen 2
Seal after～4 minutes；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 1～2h, filter, dehydrated alcohol is washed
Obtain final product after washing.
The preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, in step S1.1, according to
Solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.003～0.005g 30～40mL, 0.5～0.8g.
In the preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, step S2, oxidation stone
The preparation of black alkene/composite titania material, comprises the following steps：Take graphene oxide/butyl titanate that S1 prepares
Composite, deionized water and dehydrated alcohol add in inner liner of reaction kettle, are subsequently placed in vacuum response kettle, 200 DEG C～250
React 4～6h at DEG C, obtain final product after being dried.
Specifically, in the preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, step
S2, the preparation of graphene oxide/composite titania material, comprise the following steps：Take graphene oxide/titanium that S1 prepares
Sour four butyl ester composites, deionized water and dehydrated alcohol add in inner liner of reaction kettle, are subsequently placed in vacuum response kettle,
React 4h at 200 DEG C, obtain final product after being dried.
In the preparation method of aforementioned oxidation Graphene/optically catalytic TiO 2 composite material precursor, according to volume ratio, go
Ionized water dehydrated alcohol=1～5 10～50.
The present invention selects with butyl titanate as titanium source, with graphene oxide as carbon source, is combined and obtains graphene oxide/bis-
Titanium oxide photochemical catalyst composite material precursor.Using the supermolecule lamellar structure of graphene oxide, butyl titanate is bonded to
Surface of graphene oxide and then formation supramolecular structure.Under ultraviolet light, butyl titanate can form 2D lamellar structure, should
The formation of structure has beneficial to butyl titanate sprawling on graphene oxide and loads.Ester bond on this supermolecule can be
The fiber surface processing carries out being bonded, large area cladding.Meanwhile, the introducing of graphene oxide effectively raises photocatalytic
Energy.Additionally, under ultraviolet lighting, graphene oxide partial reduction is redox graphene.
Fig. 1 is the infrared spectrum of graphene oxide/butyl titanate composite.In figure curve 1 and 2 refers to respectively by metatitanic acid
Four butyl esters, graphene oxide and ethanol are proportionally added into gained mixed liquor in quartz ampoule, under nitrogen protection after ultraviolet light
And do not carry out the infrared spectrum of products therefrom after illumination.As can be seen from Figure, in curve 1, after ultraviolet lighting, C=O
Key, C-OH key and C-O key present the situation being obviously reduced or even disappearing, and graphene oxide is reacted with butyl titanate.
And in 600cm-1Nearby occur in that Ti-O-Ti key stretching vibration peak, show under conditions of ultraviolet lighting, titanium source produces photoelectricity
Son, graphene oxide partial reduction in graphene oxide/butyl titanate composite is redox graphene, titanium simultaneously
There is the effect of Ti-C key between sour four butyl esters and graphene oxide.Illustrate after ultraviolet light, butyl titanate and oxygen
Graphite alkene composite effect is notable.
Table 1 is the elementary analysiss table of graphene oxide/optically catalytic TiO 2 composite material precursor.As can be seen that
Graphenic surface has loaded TiO 2 particles, shows that butyl titanate has successfully been carried on graphene oxide layer
On.
Table 1
| Element | Wt% | Atomic percent |
| C | 47.58 | 68.69 |
| O | 17.10 | 18.53 |
| Ti | 35.32 | 12.78 |
| Total amount: | 100.00 | 100.00 |
By EDS/SEM, the graphene oxide/optically catalytic TiO 2 composite material precursor of the present invention is tested,
Result is as shown in Figure 2.It is dispersed in graphene oxide by can be seen that titanium dioxide in Fig. 2.
The present invention also has good coating, compared with the photocatalyst of powder, finely dispersed graphene oxide/bis-
Titanium oxide photochemical catalyst composite material precursor can be applied directly to quartz fiber surface, efficiently solves dusty material rear
The low problem of continuous degraded application aspect utilization rate, improves the utilization rate of titanium dioxide optical catalyst, applied range.
The invention has benefit that：Before graphene oxide/optically catalytic TiO 2 composite that the present invention provides
Drive the preparation method of body, the optic catalytic composite material presoma of uniform load titanium dioxide can be prepared.In presoma
TiO2Achieve organic composite with graphene oxide, TiO 2 particles are equably supported in graphene oxide layer, oxidation
The introducing of Graphene serves load TiO2Particle and the dual function improving photocatalytic activity, effectively lift TiO2
The disposal efficiency of photocatalyst, under action of ultraviolet light, organic pollutant degradation can be inorganic matters by titanium dioxide.With work as
Front technology is compared, and the persursor material of the inventive method preparation can not only overcome TiO2Disperse uneven problem, also effectively
The contact area that increased photocatalyst, improve catalytic efficiency, improve the degradation property of photocatalyst.Additionally, the present invention
Persursor material also has excellent coating functions, compared with the photocatalyst of powder, finely dispersed Graphene/TiO2Light is urged
Change composite material precursor and can be applied directly to quartz fiber surface, increase operation rate.The presoma of the inventive method preparation
Material may be directly applied to the fields such as Pollutant Treatment and household cleaning.The preparation method step of the present invention is simple, easy to operate, system
Standby mild condition is easy to control, efficiency high.
Brief description
Fig. 1 is the infrared figure of the graphene oxide/optically catalytic TiO 2 composite material precursor of the present invention；
Fig. 2 is the SEM figure of graphene oxide/optically catalytic TiO 2 composite material precursor；
In figure reference implication：Fig. 1：1- ultraviolet light, the non-illumination of 2-；Fig. 2：(1)-graphene oxide/titanium dioxide
Titanium composite material, (2)-graphene oxide scattergram, (3)-titanium elements scattergram；(4)-oxygen element scattergram.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is further introduced.
In the present invention, agents useful for same is commercially available prod, and analysis is pure.
Embodiment 1
A kind of preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprises the following steps：
The preparation of S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, according to solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.003g 30mL 0.5g, take oxygen
Graphite alkene, butyl titanate and dehydrated alcohol add in quartz ampoule, stir, are passed through nitrogen and seal after 2 minutes；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 2h, filter, absolute ethanol washing
After obtain final product.
S2, the preparation of graphene oxide/composite titania material, comprise the following steps：According to volume ratio, deionization
Anhydrous water ethanol=1 50, take graphene oxide/butyl titanate composite that S1 prepares, deionized water and anhydrous
Ethanol adds in inner liner of reaction kettle, is subsequently placed in vacuum response kettle, reacts 6h at 200 DEG C, obtains final product after being dried.
Embodiment 2
A kind of preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprises the following steps：
The preparation of S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, according to solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.005g 40mL 0.8g, take oxygen
Graphite alkene, butyl titanate and dehydrated alcohol add in quartz ampoule, stir, are passed through nitrogen and seal after 4 minutes；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 1h, filter, absolute ethanol washing
After obtain final product.
S2, the preparation of graphene oxide/composite titania material, comprise the following steps：According to volume ratio, deionization
Anhydrous water ethanol=5 10, take graphene oxide/butyl titanate composite that S1 prepares, deionized water and anhydrous
Ethanol adds in inner liner of reaction kettle, is subsequently placed in vacuum response kettle, reacts 4h at 250 DEG C, obtains final product after being dried.
Embodiment 3
A kind of preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprises the following steps：
The preparation of S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, according to solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.004g 35mL 0.6g, take oxygen
Graphite alkene, butyl titanate and dehydrated alcohol add in quartz ampoule, stir, are passed through nitrogen and seal after 3 minutes；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 1.5h, filter, dehydrated alcohol is washed
Obtain final product after washing.
S2, the preparation of graphene oxide/composite titania material, comprise the following steps：According to volume ratio, deionization
Anhydrous water ethanol=1 10, take graphene oxide/butyl titanate composite that S1 prepares, deionized water and anhydrous
Ethanol adds in inner liner of reaction kettle, is subsequently placed in vacuum response kettle, reacts 5h at 220 DEG C, obtains final product after being dried.
Embodiment 4
A kind of preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprises the following steps：
The preparation of S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, according to solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.0035g 32mL 0.7g, take
Graphene oxide, butyl titanate and dehydrated alcohol add in quartz ampoule, stir, are passed through nitrogen and seal after 4 minutes；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 1.3h, filter, dehydrated alcohol is washed
Obtain final product after washing.
S2, the preparation of graphene oxide/composite titania material, comprise the following steps：According to volume ratio, deionization
Anhydrous water ethanol=3 40, take graphene oxide/butyl titanate composite that S1 prepares, deionized water and anhydrous
Ethanol adds in inner liner of reaction kettle, is subsequently placed in vacuum response kettle, reacts 5.5h at 210 DEG C, obtains final product after being dried.
Embodiment 5
A kind of preparation method of graphene oxide/optically catalytic TiO 2 composite material precursor, comprises the following steps：
The preparation of S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, according to solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.0045g 38mL 0.65g, take
Graphene oxide, butyl titanate and dehydrated alcohol add in quartz ampoule, stir, are passed through nitrogen and seal after 3 minutes；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 1.9h, filter, dehydrated alcohol is washed
Obtain final product after washing.
S2, the preparation of graphene oxide/composite titania material, comprise the following steps：According to volume ratio, deionization
Anhydrous water ethanol=2 35, take graphene oxide/butyl titanate composite that S1 prepares, deionized water and anhydrous
Ethanol adds in inner liner of reaction kettle, is subsequently placed in vacuum response kettle, reacts 4.5h at 240 DEG C, obtains final product after being dried.
Claims (8)
1. graphene oxide/optically catalytic TiO 2 composite material precursor preparation method it is characterised in that：Walk including following
Suddenly：
The preparation of S1, graphene oxide/butyl titanate composite；S2, the system of graphene oxide/composite titania material
Standby.
2. the preparation method of Graphene according to claim 1/optically catalytic TiO 2 composite material precursor, its feature
It is：Comprise the following steps：
The preparation of S1, graphene oxide/butyl titanate composite：By graphene oxide be dispersed in butyl titanate and
In the mixed solution of dehydrated alcohol, ultraviolet lighting obtains final product；
S2, the preparation of graphene oxide/composite titania material：Graphene oxide/butyl titanate that S1 is prepared
Composite prepares graphene oxide/composite titania material by hydro-thermal method.
3. the preparation side of graphene oxide according to claim 1 and 2/optically catalytic TiO 2 composite material precursor
Method it is characterised in that：The preparation of described step S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, take graphene oxide, butyl titanate and dehydrated alcohol to add in quartz ampoule, stir, be passed through close after nitrogen
Envelope；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting, filter, obtain final product after washing.
4. the preparation method of graphene oxide according to claim 3/optically catalytic TiO 2 composite material precursor, its
It is characterised by：The preparation of described step S1, graphene oxide/butyl titanate composite, comprises the following steps：
S1.1, take graphene oxide, butyl titanate and dehydrated alcohol to add in quartz ampoule, stir, be passed through nitrogen 2～4
Seal after minute；
S1.2, put in photochemical reaction instrument under agitation, after ultraviolet lighting 1～2h, filter, after absolute ethanol washing
Obtain final product.
5. the preparation method of graphene oxide according to claim 3/optically catalytic TiO 2 composite material precursor, its
It is characterised by：In described step S1.1, according to solid-liquid ratio, graphene oxide butyl titanate dehydrated alcohol=0.003～
0.005g 30～40mL, 0.5～0.8g.
6. the preparation side of graphene oxide according to claim 1 and 2/optically catalytic TiO 2 composite material precursor
Method it is characterised in that：Described step S2, the preparation of graphene oxide/composite titania material, comprise the following steps：Take S1
The graphene oxide preparing/butyl titanate composite, deionized water and dehydrated alcohol add in inner liner of reaction kettle, with
After put in vacuum response kettle, at 200 DEG C～250 DEG C react 4～6h, be dried after obtain final product.
7. the preparation method of graphene oxide according to claim 6/optically catalytic TiO 2 composite material precursor, its
It is characterised by：Described step S2, the preparation of graphene oxide/composite titania material, comprise the following steps：S1 is taken to be prepared into
To graphene oxide/butyl titanate composite, deionized water and dehydrated alcohol add in inner liner of reaction kettle, be subsequently placed into
In vacuum response kettle, at 200 DEG C, react 4h, obtain final product after being dried.
8. the preparation of described graphene oxide/optically catalytic TiO 2 composite material precursor according to claim 6
Method it is characterised in that：According to volume ratio, deionized water dehydrated alcohol=1～5 10～50.
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| CN108704635A (en) * | 2018-05-25 | 2018-10-26 | 东北大学 | Graphene titanium dioxide composite nano material and preparation method thereof |
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| CN107029734A (en) * | 2017-05-10 | 2017-08-11 | 浙江工业大学 | A kind of method for improving bismuth ferrite graphene oxide composite material photocatalytic activity |
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| CN108310966A (en) * | 2018-01-30 | 2018-07-24 | 中南林业科技大学 | Film and gas purification integrated apparatus, film and method for gas purification |
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| CN108704635A (en) * | 2018-05-25 | 2018-10-26 | 东北大学 | Graphene titanium dioxide composite nano material and preparation method thereof |
| CN109251363A (en) * | 2018-07-18 | 2019-01-22 | 桐城市明丽碳化硼制品有限公司 | A kind of uvioresistant graphene new material and preparation method thereof |
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Application publication date: 20170308 |