CN105854860A - Preparation method for titanium dioxide/graphene aerogel with high specific surface area - Google Patents
Preparation method for titanium dioxide/graphene aerogel with high specific surface area Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 163
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 105
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 73
- 239000004964 aerogel Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000017 hydrogel Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 230000008569 process Effects 0.000 claims abstract description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 230000002349 favourable effect Effects 0.000 claims description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 4
- 235000010323 ascorbic acid Nutrition 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- -1 graphite Alkene Chemical class 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims 3
- 239000010439 graphite Substances 0.000 claims 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 238000002242 deionisation method Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 12
- 239000008367 deionised water Substances 0.000 abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000010907 mechanical stirring Methods 0.000 abstract 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000002336 sorption--desorption measurement Methods 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 241000790917 Dioxys <bee> Species 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
-
- B01J35/23—
-
- B01J35/31—
-
- B01J35/39—
-
- B01J35/615—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- 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
Abstract
The invention relates to a preparation method for titanium dioxide/graphene aerogel with a high specific surface area, belonging to the technical field of energy and catalysis. The preparation method comprises the following steps: mixing graphene oxide powder with deionized water and carrying out ultrasonic dispersion and mechanical stirring so as to obtain a stable aqueous graphene oxide solution with good dispersibility; adding titanium dioxide powder into the aqueous graphene oxide solution, adding a reducing agent at the same time and carrying out ultrasonic dispersion and mechanical stirring until a stable titanium dioxide/graphene mixed solution is formed; and putting the prepared mixed solution into a baking oven, preparing three-dimensional titanium dioxide/graphene hydrogel by using a constant-temperature hydrothermal method and subjecting the titanium dioxide/graphene hydrogel to freeze drying to remove a solvent so as to obtain the titanium dioxide/graphene aerogel with a high specific surface area. The method provided by the invention is simple in process, good in operability, low in energy consumption, free of pollution and high in the specific surface area and has great application prospects in the fields of energy and catalysis.
Description
Technical field
The present invention relates to the preparation method of a kind of high specific surface area titanic oxide/graphene aerogel, belong to the energy and
Catalysis technical field.
Background technology
At present, environmental pollution and energy crisis are the significant problems of puzzlement countries in the world.Catalysis material has light
Hydrogen production by water decomposition and the big function of light degradation pollutant two, utilize catalysis material both can be turned by low-density solar energy
Turn to storable highdensity Hydrogen Energy, it is possible to make full use of the pollutant in solar energy degraded and mineralising environment,
Therefore the problem in terms of solving the energy and environment has important application prospect.
Titanium dioxide is studied the most extensive in numerous catalysis materials, and concerned degree is the highest, is considered
It it is one of the most promising catalysis material.Although titanium dioxide meets as a kind of excellent catalysis material
Basic demand, but its extensive application to be still limited by the photocatalysis efficiency of material own the highest and without visible light-responded two
Individual bottleneck.It is multiple with titanium dioxide that many documents report employing new carbon such as CNT, Graphene etc.
Close and form composite, due to both synergism, can be with the reinforcing material degradation property to organic pollution.
Graphene is the preferable two dimensional crystal tightly packed by monolayer carbon atom six side.As a kind of novel
Material with carbon element, it has the excellent properties such as huge specific surface area, excellent absorption property and high chemical heat stability.
Grapheme material is prepared as aeroge so that it is there is loose structure, not only remain the excellent mechanics of Graphene,
Calorifics and electric property, also make Graphene be provided with three-dimensional porous structure, and this characteristic also makes the research of Graphene
Pilot is turned to the block materials of macroscopic view by microcosmic nano material.
Titanium dioxide and graphene aerogel are combined, on the one hand, the specific surface area that composite is huge improves
The material absorbability to organic pollution；On the other hand, the formation of Graphene-titanium dioxide interface suppression knot
Improve being combined between light induced electron and hole；It addition, after graphenic surface absorbs photon, inject electrons into
Titanium dioxide conduction band, forms the hydroxyl radical free radical (OH) of degradable organic pollutant.Therefore, titanium dioxide/
Graphene aerogel has the biggest advantage compared to traditional catalysis material.Meanwhile, the method prepares dioxy
Changing titanium/graphene aerogel technique simple, workable, energy consumption is low pollution-free, and the specific surface area of material is high,
At the energy and catalytic field, there is bigger application prospect.
Summary of the invention
In view of the application prospect of titanium dioxide/graphene aeroge, it is an object of the invention to provide a kind of high ratio
The preparation method of surface area titanic oxide/graphene aerogel.
For reaching above-mentioned purpose, the present invention provides following technical scheme:
A kind of preparation method of high specific surface area titanic oxide/graphene aerogel, its step is as follows:
(1) being mixed with deionized water by graphene oxide powder, ultrasonic disperse, mechanical agitation are divided successively
Dissipate the graphene oxide water solution that property is good, stable.
(2) adding titania powder in the graphene oxide water solution in step (1), mechanical agitation obtains
To titanium dioxide/graphene oxide mixed solution.
(3) adding reducing agent in the mixed solution that will obtain in step (2), after stirring, hydro-thermal reaction obtains
To three-dimensional titanium dioxide/graphene hydrogel.
(4) the titanium dioxide/graphene hydrogel that step (3) obtains is dried process to remove solvent,
Titanium dioxide/graphene aeroge is i.e. can get after removing.
In described step (1), as preferably, the preferred concentration of graphene oxide water solution is 1.0～2.5mg/mL.
In described step (2), as preferably, in titanium dioxide/graphene mixed solution, titanium dioxide and stone
The mass ratio of ink alkene is 1:3～3:1.
In described step (3), preferably, the reducing agent of use is hydrazine hydrate, sodium borohydride, Vitamin C
The mass ratio of the one in acid, reducing agent and graphene oxide is 1:1～4:1.
In described step (3), as preferably, hydrothermal temperature is 80～95 DEG C, and the response time is 2～10
Hour.
In described step (4), as preferably, the drying mode of titanium dioxide/graphene hydrogel is freezing dry
Dry, lyophilization temperature is-60～-50 DEG C, and vacuum is 10～30Pa, and drying time is 12～24 hours.
In the preparation process of carbon dioxide/Graphene hydrogel, graphene oxide is as presoma, when its concentration
When reaching preferred concentration 1.0～2.5mg/mL, by the reduction of reducing agent, nanometer in graphene oxide water solution
Electrostatic repulsion between lamella reduces, and Interaction enhanced can induce it to be assembled into Graphene hydrogel.?
Formed during hydrogel, carbon dioxide particle along with the reunion shrinkage of Graphene enter hydrogel skeleton and
In hole, formed carbon dioxide/Graphene hydrogel, afterwards by i.e. can get after solvent removal titanium dioxide/
Graphene aerogel.
In sum, present invention generally provides the preparation method of a kind of titanium dioxide/graphene aeroge, mainly
It is applied to the energy and catalysis technical field, compared with traditional catalysis material, the invention have the advantages that
1. use graphene aerogel as the carrier of catalysis material.As emerging graphene-based composite,
The advantage of Graphene and aeroge is combined by graphene aerogel, has density low by (60～165mg/cm3),
Specific surface area high (108～225m2/ g), electrical conductivity advantages of higher.
2. titanium dioxide/graphene aeroge has the biggest specific surface area, can improve material to organic contamination
The absorbability of thing.
3. after Graphene absorbs photon, inject electrons into titanium dioxide conduction band, form degradable organic pollutant
Hydroxyl radical free radical (OH).
4. the photocatalysis performance of titanium dioxide/graphene aerogel material is excellent, and 30 minutes to organic pollution
Degradation rate can reach 95.5%
5. the method prepares titanium dioxide/graphene aeroge technique simply, workable, and energy consumption is low without dirty
Dye, has bigger application prospect at the energy and catalytic field.
Accompanying drawing explanation
Fig. 1 is the flow chart of titanium dioxide/graphene aeroge preparation method.
Fig. 2 is the SEM figure of the titanium dioxide/graphene aeroge of embodiment 1.
Fig. 3 is the nitrogen adsorption desorption curve of the titanium dioxide/graphene aeroge of embodiment 1
Fig. 4 is the SEM figure of the titanium dioxide/graphene aeroge of embodiment 2.
Fig. 5 is the nitrogen adsorption desorption curve of the titanium dioxide/graphene aeroge of embodiment 2
Fig. 6 is the SEM figure of the titanium dioxide/graphene aeroge of embodiment 3.
Fig. 7 is the nitrogen adsorption desorption curve of the titanium dioxide/graphene aeroge of embodiment 3
Detailed description of the invention
Below in conjunction with being embodied as example, the present invention will be further described.Only it should be understood that these embodiments
For the present invention is described, rather than limit the scope of the present invention.
Embodiment 1
Take graphene oxide powder 32mg, add deionized water 16mL, ultrasonic disperse after 2 hours machinery stir
Mix until forming favorable dispersibility, stable graphene oxide water solution；Water-soluble to the graphene oxide configured
Liquid adds the titanium dioxide powder of 10.67mg, mechanical agitation 1 hour, forms the dioxy of favorable dispersibility
Change titanium/graphene oxide mixed solution；In above-mentioned mixed solution, add 50mg ascorbic acid, stir
After proceed in hydrothermal reaction kettle, 90 DEG C of isothermal reactions 6 hours, prepare the titanium dioxide/graphene water of three-dimensional
Gel；Lyophilization 24 hours under the conditions of-60～-50 DEG C, obtain the titanium dioxide/graphene of high-specific surface area
Aeroge.
Embodiment 2
Take graphene oxide powder 32mg, add deionized water 16mL, ultrasonic disperse after 2 hours machinery stir
Mix until forming favorable dispersibility, stable graphene oxide water solution；Water-soluble to the graphene oxide configured
Liquid adds the titanium dioxide powder of 32mg, mechanical agitation 1 hour, forms the titanium dioxide of favorable dispersibility
/ graphene oxide mixed solution；In above-mentioned mixed solution, add 50mg ascorbic acid, turn after stirring
Enter in hydrothermal reaction kettle, 90 DEG C of isothermal reactions 6 hours, prepare the titanium dioxide/graphene hydrogel of three-dimensional；
Lyophilization 24 hours under the conditions of-60～-50 DEG C, obtain the titanium dioxide/graphene aeroge of high-specific surface area.
Embodiment 3
Take graphene oxide powder 32mg, add deionized water 16mL, ultrasonic disperse after 2 hours machinery stir
Mix until forming favorable dispersibility, stable graphene oxide water solution；Water-soluble to the graphene oxide configured
Liquid adds the titanium dioxide powder of 96mg, mechanical agitation 1 hour, forms the titanium dioxide of favorable dispersibility
/ graphene oxide mixed solution；In above-mentioned mixed solution, add 50mg ascorbic acid, turn after stirring
Enter in hydrothermal reaction kettle, 90 DEG C of isothermal reactions 6 hours, prepare the titanium dioxide/graphene hydrogel of three-dimensional；
Lyophilization 24 hours under the conditions of-60～-50 DEG C, obtain the titanium dioxide/graphene aeroge of high-specific surface area.
The titanium dioxide/graphene aeroge obtained in above example has been carried out scanning electron microscope (SEM)
Observation, Fig. 2, Fig. 4 and Fig. 6 are respectively mass ratio 1:3,1:1 of titanium dioxide and graphene oxide raw material
With the SEM collection of illustrative plates of the titanium dioxide/graphene aeroge of 3:1, this it appears that the porous of material from figure
Characteristic, Graphene shrinkage forms the skeleton of porous material, and aperture is 1～3 μm, and titania powder is distributed in
In Graphene skeleton and aperture, along with the increase of titanium dioxide amount, the dioxy in graphene sheet layer skeleton and hole
Changing titanium load capacity the most, Fig. 6 is it can be seen that the titanium dioxide of the excess pore space structure to graphene aerogel
There is certain destruction.
The titanium dioxide/graphene aeroge obtained in above example carries out nitrogen adsorption desorption test, Fig. 3,
Fig. 5 and Fig. 7 is the titanium dioxide of mass ratio 1:3,1:1 and 3:1 of titanium dioxide and graphene oxide raw material respectively
The nitrogen adsorption desorption curve of titanium/graphene aerogel.Use the specific surface area of BET method test material, obtain
The specific surface area of three kinds of aeroges is respectively 225m2/ g, 174m2/ g and 108m2/ g, this illustrates titanium dioxide
Addition be filled with in the hole of graphene aerogel, cause the reduction of specific surface area, this shows with SEM
Result match.
Absorption property and light with methylene blue simulation organic pollution test titanium dioxide/graphene aeroge are urged
Change performance, take a certain amount of titanium dioxide/graphene aeroge dark conditions mechanical agitation one hour so that it is point
Dissipate in methylene blue solution, reach adsorption equilibrium, take after supernatant is centrifuged and test its absorbance.Test result table
Bright, the titanium dioxide/graphene gas of mass ratio 1:3,1:1 and 3:1 of titanium dioxide and graphene oxide raw material
Gel degree of absorption to methylene blue in 1 hour has reached 44.8%, 63.1% and 74.8%.Make afterwards
Irradiating it with 500W xenon lamp, every 5min takes a sample, takes its supernatant and test its absorbance after being centrifuged,
After 30 minutes, the aeroge of three kinds of proportionings is respectively 87.9%, 95.5% and 85.4% to the degradation rate of methylene blue.
In conjunction with specific surface area data it can be seen that the absorption property of titanium dioxide/graphene aerogel material and catalytic
There is certain contradiction between energy, its absorption property, content of titanium dioxide can be reduced when content of titanium dioxide is too high
Its catalytic performance can be reduced time too low.From the point of view of comprehensively, the mass ratio 1:1 of titanium dioxide and graphene oxide raw material
Time material the strongest to the degradation capability of pollutant.
Claims (8)
1. a preparation method for high specific surface area titanic oxide/graphene aerogel, described titanium dioxide/graphite
Alkene aeroge 30 minutes to methylene blue degradation rate can reach 95.5%, it is characterised in that concrete steps
As follows:
(1) adding titania powder in graphene oxide water solution, mechanical agitation obtains titanium dioxide/oxygen
Functionalized graphene mixed solution；
(2) adding reducing agent in the mixed solution that will obtain in step (1), after stirring, hydro-thermal reaction obtains
To three-dimensional titanium dioxide/graphene hydrogel；
(3) the titanium dioxide/graphene hydrogel that step (2) obtains is dried process to remove solvent,
Titanium dioxide/graphene aeroge is i.e. can get after removing.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 1,
It is characterized in that: in described step (1), in titanium dioxide/graphene mixed solution, titanium dioxide and graphite
The mass ratio of alkene is 1:3～3:1.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 2,
It is characterized in that: in described step (1), in titanium dioxide/graphene mixed solution, titanium dioxide and graphite
The mass ratio of alkene is 1:1.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 1,
It is characterized in that: in described step (2), the reducing agent of use is hydrazine hydrate, sodium borohydride, ascorbic acid
In one, the mass ratio of reducing agent and graphene oxide is 1:1～4:1.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 1,
It is characterized in that: in described step (2), hydrothermal temperature is 80～95 DEG C, and the response time is 2～10 little
Time.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 1,
It is characterized in that: in described step (3), the drying mode of titanium dioxide/graphene hydrogel is freezing dry
Dry, lyophilization temperature is-60～-50 DEG C, and vacuum is 10～30Pa, and drying time is 12～24 hours.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 1,
It is characterized in that the preparation method of described graphene oxide water solution is as follows: by graphene oxide powder and deionization
Water mixes, and ultrasonic disperse, mechanical agitation obtain favorable dispersibility, stable graphene oxide water solution successively.
The preparation method of a kind of high specific surface area titanic oxide/graphene aerogel the most as claimed in claim 7,
It is characterized in that: the concentration of graphene oxide water solution is 1.0～2.5mg/mL.
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| CN106512975A (en) * | 2016-10-19 | 2017-03-22 | 常州大学 | Preparation method and application of sulfur-doped titanium dioxide-graphene aerogel composite material |
| CN106582518A (en) * | 2016-11-17 | 2017-04-26 | 南京大学 | Graphene-TiO2 nanotube hydrogel, preparation method, and application thereof |
| CN106807328A (en) * | 2017-02-10 | 2017-06-09 | 南京工程学院 | The preparation method and applications of modified sharp titanium titanium dioxide nanotube graphene hydrogel |
| CN106848246A (en) * | 2017-03-01 | 2017-06-13 | 辽宁大学 | A kind of three-dimensional structure TiO2/ graphene aerogel compound and its preparation method and application |
| CN107381560A (en) * | 2017-01-23 | 2017-11-24 | 南通纺织丝绸产业技术研究院 | A kind of fast preparation method of graphene/nanometer granular aerogel |
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