CN109433177A - A kind of 2D-TiO2(B)/preparation method of graphene high-efficiency catalysis material and the application of the material - Google Patents
A kind of 2D-TiO2(B)/preparation method of graphene high-efficiency catalysis material and the application of the material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 67
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- 229910010251 TiO2(B) Inorganic materials 0.000 title claims abstract description 28
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 51
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002294 plasma sputter deposition Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000005457 ice water Substances 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 29
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- 238000006303 photolysis reaction Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000000527 sonication Methods 0.000 claims description 5
- 239000003292 glue Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000010189 synthetic method Methods 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 15
- 229910052786 argon Inorganic materials 0.000 description 15
- 230000000149 penetrating effect Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000011160 research Methods 0.000 description 4
- 102000004310 Ion Channels Human genes 0.000 description 3
- 229910003074 TiCl4 Inorganic materials 0.000 description 3
- 229910010455 TiO2 (B) Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of 2D-TiO2(B)/graphene high-efficiency catalysis material preparation method and application, this method key step include: that a certain amount of graphene (GR) is added in ethylene glycol, sonicated rear evenly dispersed mixing.Then under the conditions of ice-water bath, by the TiCl of liquid4It is instilled dropwise into ethylene glycol (EG), ultrasonic treatment 30min-60min hydrolyzes to form gelatinous TiO2(B)-GR presoma；A certain amount of TiO is weighed again2(B)-GR presoma is placed in a beaker, and deionized water is added into solution according to the volume ratio of 1:30-1:60 and stirs evenly to form TiO2(B)-GR precursor water solution；Then by TiO2(B)-GR precursor water solution carries out 130 DEG C of -170 DEG C of hydro-thermal reactions in closed reaction kettle, the hydro-thermal reaction time is not more than 6h, sample absolute alcohol and deionized water to obtain after reaction alternately rinse 3-5 times, and are dried to obtain 2D-TiO in 100 DEG C of drying box2(B)/graphene catalysis material；TGN is subjected to plasma sputtering processing in argon atmosphere, TGN plasma light catalysis material is obtained after 0-60min.Its large specific surface area and ultrathin nanometer structure with certain photocatalytic activity, it is a kind of synthetic method of high-efficiency and economic that implementation cost is low, stable structure, easy to operate, short preparation period.
Description
Technical field
The present invention relates to a kind of novel 2D structure nano material, the production hydrogen catalyst material that is mainly used in photodissociation water system
Material, and in particular to a kind of 2D-TiO2 (B)/preparation method of graphene high-efficiency catalysis material and the application of the material.
Background technique
In recent years, with the development of economy and society, coal, the non-renewable energy resources such as petroleum are largely consumed, in order to
Mitigate the dependence to fossil energy, searching and utilization can replace the new energy such as Hydrogen Energy of non-renewable energy resources become
The hot issue of current era research.Wherein, the conversion efficiency of hydrogen energy source Yin Qigao and cleanliness without any pollution are in new energy field
It is receive more and more attention.In numerous catalysis materials, TiO2Because of its environmentally protective nontoxicity, preferable stability and resistance to
Acid-base property and stable continuous H2-producing capacity have received extensive research and application in photocatalysis field.However, existing
TiO2(B) mutually research temperature gradually decreases, and is on the one hand that light-catalysed compound type is suitble to more to limit to due to it, on the other hand
Be cause in practical applications because of self structure existing for defect there is also many problems, such as traditional rutile with
And the TiO of two kinds of crystal forms of anatase2Material catalytic activity is low, and high performance catalyst preparation process complexity and low output；Coupling
Conjunction Semiconductor Chemistry property is unstable and long-time service is easy to be corroded to generate catalyst poisoning phenomenon；Ion doping technique
It is complicated and limited to catalytic performance raising；Simple physical load noble metal granule with binding force it is weaker, in use process
In be easy to fall off to cause catalytic capability to decline the problems such as all limit the commercial applications of the material.
The novel 2D-TiO that we study2(B)/graphen catalyst shows preferable catalytic activity, which is based on
The ultrathin nanometer multilayered structure of graphene grows TiO2 (B) nanometer flocculent structure on the surface of graphene, effectively raises this
The specific surface area of grapheme material is conducive to the single-crystal surface that exposure has more active sites after plasma sputtering,
And then improve catalytic activity；This 2D ultrathin nanometer material possesses the TiO of very high specific surface area and compact stratiform simultaneously2Knot
Structure, and graphene-based bottom can be improved the efficiency of transmission of electronics, and material surface is dispersed with many opening ion channels, can very
Big degree promotes the transfer and redox reaction in light induced electron and hole.Therefore consider from performance, economy etc., 2D-
TiO2(B) research of/graphene is all necessary and reasonable.
Summary of the invention
For the prior art, the present invention provides one kind at low cost, the simple 2D-TiO of preparation process2(B)/graphene light is urged
Change the preparation method of material, it is a kind of efficiently warp that its of the invention implementation cost is low, stable structure, easy to operate, short preparation period
The synthetic method of Ji.The 2D nano structural material that the present invention is prepared is mainly used for the catalyst in photocatalytic system.
In order to solve the above-mentioned technical problems, the present invention provides a kind of 2D-TiO2 of (B)/graphene high-efficiency catalysis materials
Preparation method, comprising the following steps:
1) graphene is added into ethylene glycol, obtains graphene-ethylene glycol mixed solution, is cooled to room after ultrasonic treatment
Temperature；
2) under conditions of ice-water bath, by the TiCl of liquid4It is instilled dropwise into graphene-ethylene glycol mixed solution, is surpassed
TiO is formed after sonication2(B)-GR glue presoma；
3) step 2) is taken into TiO2(B)-GR precursor solution is placed in a beaker, and deionized water shape is then added into solution
At TiO2(B) it-GR precursor water solution and stirs evenly；
4) by TiO made from step 3)2(B)-GR precursor water solution carries out hydro-thermal reaction in closed reaction kettle, will
After reaction, sample absolute alcohol obtained and deionized water are alternately rinsed, and are subsequently placed in drying box and are dried to obtain
2D-TiO2(B)/graphene composite material (hereinafter be expressed as TGN)；
5) composite material made from step 4) is completed to plasma sputtering processing in argon atmosphere, after a period of time
To TGN plasma light catalysis material (hereinafter be expressed as TGN/Plasma).
Concentration of the graphene GR in ethylene glycol EG is 1-3mg/ml in the step 1).
Sonication treatment time is 30-60min in the step 1).
TiCl in the step 2)4With TiO2(B) volume ratio of-GR glue presoma is 0.1:15-1:15.
Sonication treatment time is 30min-60min in the step 2).
10-20ml TiO is measured in the step 3)2(B)-GR precursor solution is in beaker.
The additive amount and TiO of deionized water in the step 3)2(B) volume ratio of-GR precursor solution is 1:30-1:
60。
TiO in the step 4)2(B)-GR precursor water solution is in closed reaction kettle in 130-170 DEG C of progress hydro-thermal
Reaction, the hydro-thermal reaction time 0.5-6h.
Reaction product in the step 4) after washing is dry at 90-100 DEG C.
2D-TiO in the step 5)2(B)/graphene composite material carries out the plasma sputtering time in argon atmosphere
For 1-60min.
Second technical solution of the invention is to prepare 2D-TiO2 (B)/graphene high-efficiency light according to above-mentioned preparation method to urge
Change the application of material, is used for photodissociation aquatic products hydrogen catalyst material.
Compared with prior art, the beneficial effects of the present invention are:
2D-TiO2(B)/graphene is possessing its unique advantage as catalysis material, nontoxic, harmless, cheap, object
Physicochemical property is stablized, while the material has very high specific surface area, is effectively increased light contact area, improves activity
The catalytic efficiency in site and active total amount, TiO before largely improving2Material reactivity site utilization rate is low to ask
Topic；In addition, 2D-TiO2(B)/grapheme material is based on graphene institutional framework, material while possessing ultra-thin atomic-level thickness
Material surface is dispersed with many opening ion channels, transference and light conducive to light induced electron, hole between layers
It is catalyzed the progress of reaction, and compact layer structure enhances the radially connected stability of matrix valence link itself, so as to protect
Demonstrate,prove the service life of material in photocatalytic process.Therefore before the preparation field of photodissociation aquatic products hydrogen catalyst has preferable application
Scape is expected to photocatalytic water catalyst as economy of new generation and stable.2D-TiO prepared by the present invention2(B)/graphene light
Catalysis material chemical property is stablized, and the full optical tests of 8h are passed through in the test of photodissociation aquatic products hydrogen, generates hydrogen total amount and reaches
To 1688 μm of ol.
Detailed description of the invention
Fig. 1 is 2D-TiO prepared by the embodiment of the present invention 12(B)/graphene catalysis material surface topography TEM figure:
(a): the TEM image of TGN/Plasma；
(b): the high-resolution TEM image of TGN/Plasma；
(c): the selective electron diffraction image of TGN/Plasma；
Fig. 2 is 2D-TiO2(B)/graphene catalysis material specific surface area test chart；
Fig. 3 is 2D-TiO under the conditions of full light2(B)/graphene catalysis material hydrogen output；
Fig. 4 is 2D-TiO2(B)/graphene catalysis material XRD spectrum.
Specific embodiment
The method of the present invention is described further combined with specific embodiments below.There is provided embodiment is the side for understanding
Just, it is in no way intended to limit the present invention.
Embodiment 1
Prepare 2D-TiO2(B)/graphene high-efficiency catalysis material method, preparation step are as follows:
It is added Step 1: weighing 30mg graphene (GR) into 15ml ethylene glycol (EG), is cooled to room after being ultrasonically treated 1h
Temperature；
Step 2: under conditions of ice-water bath, by the TiCl of 0.5ml liquid4It is instilled dropwise to graphene-ethylene glycol mixing
In solution (GR-EG), gelatinous TiO is all hydrolyzed to form to TiCl4 after ultrasound 30min under ultrasonic treatment2(B)-GR forerunner
Body；
Step 3: by TiO made from step 22(B)-GR precursor solution weighs 15ml and is placed in a beaker, then basis
Deionized water is added into solution and forms TiO for the volume ratio of 1:302(B) it-GR precursor water solution and stirs evenly；
Step 4: by TiO made from step 32(B)-GR precursor water solution carries out 152 DEG C in closed reaction kettle
Hydro-thermal reaction, the hydro-thermal reaction time 4h sample absolute alcohol obtained and deionized water will be rushed alternately after reaction
It washes 3-5 times, and obtains 2D-TiO after drying in 100 DEG C of drying box2(B)/graphene composite material.
Step 5: being 2D- after composite material made from step 4 is carried out argon ion plasma sputtering processing 15min
TiO2(B)/graphene catalysis material.
2D-TiO is prepared in embodiment 12(B)/graphene catalysis material, Fig. 1 show the 2D-TiO2(B)/graphite
The TEM of alkene nanostructure schemes.The catalysis material has high specific surface area, ultra-thin layer thickness and high stability and energy
Enough promote mass transfer, therefore has preferable application prospect in the preparation field of photodissociation aquatic products hydrogen catalyst.Compared to other
The TiO of crystal form2(B) catalysis material, 2D-TiO2(B) material table while/graphene composite material possesses ultra-thin atomic-level thickness
EDS maps many opening ion channels, conducive to the transference and photocatalysis of light induced electron, hole between layers
The progress of reaction, and compact layer structure enhances the radially connected stability of matrix valence link itself, thereby may be ensured that light
The service life of material in catalytic process.Therefore there is preferable application prospect in the preparation field of photodissociation aquatic products hydrogen catalyst,
It is expected to photocatalytic water catalyst as economy of new generation and stable.2D-TiO prepared by the present invention2(B)/graphene light is urged
Change materials chemistry property to stablize, the full optical tests of 8h are passed through in the test of photodissociation aquatic products hydrogen, generates hydrogen total amount and reach
1688μmol.Fig. 2 shows the 2D-TiO that embodiment 1 is prepared2(B)/graphene catalysis material specific surface area test chart
And hydrogen output map.
Wherein, Fig. 2 is 2D-TiO2(B)/graphene catalysis material specific surface area test chart；Under the conditions of Fig. 3 is full light
2D-TiO2(B)/graphene catalysis material hydrogen output；Fig. 4 is 2D-TiO2(B)/graphene catalysis material XRD spectrum.
Embodiment 2
Preparation process is substantially the same manner as Example 1, the difference is that only: in step 5, argon ion plasma splashes
A length of 0min when penetrating, i.e., do not carry out argon ion plasma sputtering.
Embodiment 3
Preparation process is substantially the same manner as Example 1, the difference is that only: in step 5, argon ion plasma splashes
A length of 30min when penetrating.
Embodiment 4
Preparation process is substantially the same manner as Example 1, the difference is that only: in step 5, argon ion plasma splashes
A length of 60min when penetrating.
Embodiment 5
Prepare 2D-TiO2(B)/graphene high-efficiency catalysis material method, preparation step are as follows:
It is added Step 1: weighing 45mg graphene (GR) into 15ml ethylene glycol (EG), is cooled to room after being ultrasonically treated 1h
Temperature；
Step 2: under conditions of ice-water bath, by the TiCl of 1ml liquid4It instills dropwise molten to graphene-ethylene glycol mixing
In liquid (GR-EG), gelatinous TiO is all hydrolyzed to form to TiCl4 after ultrasound 30min under ultrasonic treatment2(B)-GR presoma；
Step 3: by TiO made from step 22(B)-GR precursor solution weighs 15ml and is placed in a beaker, then basis
Deionized water is added into solution and forms TiO for the volume ratio of 1:602(B) it-GR precursor water solution and stirs evenly；
Step 4: by TiO made from step 32(B)-GR precursor water solution carries out 170 DEG C in closed reaction kettle
Hydro-thermal reaction, the hydro-thermal reaction time 6h sample absolute alcohol obtained and deionized water will be rushed alternately after reaction
It washes 3-5 times, and obtains 2D-TiO after drying in 100 DEG C of drying box2(B)/graphene composite material.
Step 5: being 2D- after composite material made from step 4 is carried out argon ion plasma sputtering processing 15min
TiO2(B)/graphene catalysis material.
Embodiment 6
Preparation process is substantially the same manner as Example 5, the difference is that only: in step 5, argon ion plasma splashes
A length of 0min when penetrating, i.e., do not carry out argon ion plasma sputtering.
Embodiment 7
Preparation process is substantially the same manner as Example 5, the difference is that only: in step 5, argon ion plasma splashes
A length of 30min when penetrating.
Embodiment 8
Preparation process is substantially the same manner as Example 5, the difference is that only: in step 5, argon ion plasma splashes
A length of 60min when penetrating.
Embodiment 9
Prepare 2D-TiO2(B)/graphene high-efficiency catalysis material method, preparation step are as follows:
It is added Step 1: weighing 15mg graphene (GR) into 15ml ethylene glycol (EG), is cooled to room after being ultrasonically treated 30h
Temperature；
Step 2: under conditions of ice-water bath, by the TiCl of 0.1ml liquid4It is instilled dropwise to graphene-ethylene glycol mixing
In solution (GR-EG), gelatinous TiO is all hydrolyzed to form to TiCl4 after ultrasound 30min under ultrasonic treatment2(B)-GR forerunner
Body；
Step 3: by TiO made from step 22(B)-GR precursor solution weighs 15ml and is placed in a beaker, then basis
Deionized water is added into solution and forms TiO for the volume ratio of 1:302(B) it-GR precursor water solution and stirs evenly；
Step 4: by TiO made from step 32(B)-GR precursor water solution carries out 130 DEG C in closed reaction kettle
Hydro-thermal reaction, the hydro-thermal reaction time 6h sample absolute alcohol obtained and deionized water will be rushed alternately after reaction
It washes 3-5 times, and obtains 2D-TiO after drying in 100 DEG C of drying box2(B)/graphene composite material.
Step 5: being 2D- after composite material made from step 4 is carried out argon ion plasma sputtering processing 15min
TiO2(B)/graphene catalysis material.
Embodiment 10
Preparation process is substantially the same manner as Example 9, the difference is that only: in step 5, argon ion plasma splashes
A length of 0min when penetrating, i.e., do not carry out argon ion plasma sputtering.
Embodiment 11
Preparation process is substantially the same manner as Example 9, the difference is that only: in step 5, argon ion plasma splashes
A length of 30min when penetrating.
Embodiment 12
Preparation process is substantially the same manner as Example 9, the difference is that only: in step 5, argon ion plasma splashes
A length of 60min when penetrating.
It can be concluded by above-described embodiment, be prepared when according to technique shown in claims, available 2D-
TiO2(B)/graphene catalysis material.Also, obtained 2D-TiO2(B)/graphene catalysis material utilizes gas chromatograph
Test generates a large amount of hydrogen, illustrates that the material of preparation is good in photodissociation aquatic products hydrogen field application prospect.
Although above in conjunction with attached drawing, invention has been described, and the invention is not limited to above-mentioned specific implementations
Mode, the above mentioned embodiment is only schematical, rather than restrictive, and those skilled in the art are at this
Under the enlightenment of invention, without deviating from the spirit of the invention, many variations can also be made, these belong to of the invention
Within protection.
Claims (11)
1. a kind of 2D-TiO2(B)/graphene high-efficiency catalysis material preparation method, which comprises the following steps:
1) graphene is added into ethylene glycol, obtains graphene-ethylene glycol mixed solution, is cooled to room temperature after ultrasonic treatment；
2) under conditions of ice-water bath, by the TiCl of liquid4It is instilled dropwise into graphene-ethylene glycol mixed solution, is ultrasonically treated
After form TiO2(B)-GR glue presoma；
3) step 2) is taken into TiO2(B)-GR precursor solution is placed in a beaker, and deionized water is then added into solution and is formed
TiO2(B) it-GR precursor water solution and stirs evenly；
4) by TiO made from step 3)2(B)-GR precursor water solution carries out hydro-thermal reaction in closed reaction kettle, will react
After, sample absolute alcohol obtained and deionized water are alternately rinsed, and are subsequently placed in drying box and are dried to obtain 2D-
TiO2(B)/graphene composite material；
5) by 2D-TiO made from step 4)2(B)/graphene composite material completes plasma sputtering processing in argon atmosphere,
TGN plasma light catalysis material is obtained after a period of time.
2. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, concentration of the graphene in ethylene glycol is 1-3mg/ml in the step 1).
3. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, sonication treatment time is 30-60min in the step 1).
4. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, TiCl in the step 2)4It is 0.1:15-1:15 with graphene-ethylene glycol mixed solution volume ratio.
5. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, sonication treatment time is 30min-60min in the step 2).
6. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, 10-20ml TiO is measured in the step 3)2(B)-GR precursor solution is in beaker.
7. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, the additive amount and TiO of deionized water in the step 3)2(B) volume ratio of-GR precursor solution is 1:30-1:60.
8. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, TiO in the step 4)2(B)-GR precursor water solution is anti-in 130-170 DEG C of progress hydro-thermal in closed reaction kettle
It answers, the hydro-thermal reaction time 0.5-6h.
9. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, the reaction product in the step 4) after washing is dry at 90-100 DEG C.
10. a kind of 2D-TiO according to claim 12(B)/graphene high-efficiency catalysis material preparation method, feature
It is, 2D-TiO in the step 5)2(B)/graphene composite material carries out the plasma sputtering time in argon atmosphere and is
1-60min。
11. one kind prepares a kind of 2D-TiO to the preparation method in any one of 10 according to claim 12(B)/graphene high-efficiency
The preparation method of catalysis material, which is characterized in that in photodissociation aquatic products hydrogen catalyst material.
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