CN109926085A - A kind of preparation method of amorphous/crystallized catalyst - Google Patents
A kind of preparation method of amorphous/crystallized catalyst Download PDFInfo
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- CN109926085A CN109926085A CN201910273847.XA CN201910273847A CN109926085A CN 109926085 A CN109926085 A CN 109926085A CN 201910273847 A CN201910273847 A CN 201910273847A CN 109926085 A CN109926085 A CN 109926085A
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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
- 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 preparation method of amorphous/crystallized catalyst, step includes: that 1) pentavalent tantalum salt is added in certain volume alcoholic solution, and 20h is then reacted at 100~200 DEG C, arrives amorphous TaO after washing is dryxPresoma (about 4nm).2) flaky crystal type g-C is obtained using melamine thermal polymerization method3N4.3) sample obtained in step 1) and step 2) is added in 50mL ethanol solution by certain mass ratio, it is evaporated at 70 DEG C in water-bath, the lower 525 DEG C of calcining 1h of argon nitrogen atmosphere in tube furnace are subsequently placed in get the amorphous containing nitrogen vacancy/crystal type TaO is arrivedx/ DCN catalyst.This method is simple, easy to operate, reproducible and can be mass produced, and good photocatalytic activity is shown on visible light photolysis water hydrogen, with certain industrial applications prospect.
Description
Technical field
The present invention relates to photocatalyst technology fields, and in particular to a kind of novel amorphous (TaOx)/crystallization (defect state C3N4,
It is denoted as DCN) type photochemical catalyst (TaOx/ DCN) and preparation method.
Background technique
In order to break through the dependence to the non-renewable fuel of tradition, meet the green requirement curbed environmental pollution, develop advanced
, efficient clean energy resource become the focus of world attention.Hydrogen is considered as most promising clean energy resource carrier, with biography
System fossil fuel is compared, and hydrogen has many advantages, such as that green, efficient, calorific value is high, renewable and abundant raw materials.And the sun contain it is huge
Big energy, therefore using sun photodegradation water prepare hydrogen and can alleviate energy shortage and can be reduced pollution remission again.But now
Photolysis water hydrogen efficiency is still very low, is primarily due to weak photochemical catalyst visible absorption, photogenerated charge low separation efficiency, reaction
Active site is few.Therefore, it is extremely urgent to find a kind of efficient, stable, inexpensive photochemical catalyst for development.
g-C3N4The features such as material is because of suitable position of energy band, cheap, raw material sources are abundant, unique two-dimensional structure
Photocatalysis field is very promising, but g-C3N4Itself photo-generated carrier is easy the disadvantages of compound, visible absorption is weak and limits again
Its extensive use.Therefore it itself proposes building amorphous/crystallized catalyst (TaO hereinx/ DCN), introduce nitrogen defect and non-
Brilliant TaOx, not only increase the response range of visible light, improve the separative efficiency of photogenerated charge.And relative to crystallization/knot
Crystal form hetero-junctions, amorphous proposed in this paper/crystal type configuration avoid lattice mismatch situation between interface, reduce composite material circle
Face hinders, and then substantially increases the hydrogen generation efficiency under catalyst visible light.About the research of the composite catalyst, at home and abroad
Without report.
Summary of the invention
The object of the invention is that providing a kind of amorphous/crystallized catalyst (TaO to solve the above-mentioned problemsx/
) and preparation method DCN.The catalyst contains nitrogen vacancy and amorphous composition, the advantage of the two can be combined together.TaOx/DCN
It is to be synthesized by pentavalent tantalum salt and melamine, good dispersion, pattern, ingredient are controllable；The preparation method is that first shifting to an earlier date
Nano amorphous TaO is prepared by solvent-thermal methodxG-C is synthesized with thermal polymerization method3N4, then adjust TaOxWith g-C3N4Mass ratio
Example, obtains amorphous/crystallized catalyst (TaO of different quality ratiox/DCN).This method is simple, easy to operate, reproducible, simultaneously
It can be mass produced, apply it on visible light photolysis water hydrogen and show good photocatalytic activity, there is certain work
Industry application prospect.
The present invention through the following technical solutions to achieve the above objectives:
According to an aspect of the invention, there is provided amorphous (TaOx)/crystal type (DCN) catalyst, these materials are used for
Photodissociation aquatic products hydrogen has good catalytic activity.
The amorphous TaOxPresoma partial size is about 4nm；DCN is thin nano-sheet；TaOx/ DCN is the amorphous of 4nm or so
TaOxIt is uniformly dispersed in DCN nanometer sheet.
Another aspect of the present invention provides a kind of amorphous/crystallized catalyst (TaOx/ DCN) and preparation method, specifically
The following steps are included:
(1) amorphous TaO is preparedxPresoma: pentavalent tantalum salt is added to the polytetrafluoroethylene (PTFE) containing certain volume alcoholic solution
In inner liner of reaction kettle, it is packed into reaction kettle after stirring into clear solution, is heated under certain temperature in an oven, and keep 20h.To anti-
After answering kettle cooling, the suspension generated is washed with a large amount of deionized waters, up to amorphous TaO after dryingxPresoma.
(2) g-C is prepared3N4: it takes 10g melamine powder to be put into aluminium oxide porcelain boat, covers and there are a small amount of gaps, so
It is put into Muffle furnace afterwards and is heated to 540 DEG C with the rate of 10 DEG C/min, and keep 2h.G-C is obtained after cooling3N4。
(3) amorphous/crystal type TaO is preparedx/ DCN: sample obtained in step (1) and step (2) is pressed into certain mass ratio
Example is added in 50mL ethanol solution, and is evaporated at 70 DEG C in water-bath, is then calcined under hydrogen atmosphere in tube furnace, i.e.,
Obtain the amorphous containing nitrogen vacancy/crystallized catalyst (TaOx/DCN)。
The amorphous TaOxWith g-C3N4Mixing mass ratio differ；Preferably, regulate and control amorphous/crystallized catalyst TaOx/
The preparation method of DCN, at least includes the following steps:
Preferably, the pentavalent tantalum salt is selected from least one of ethanol tantalum, tantalic chloride, isopropanol tantalum.
Preferably, the alcoholic solution is selected from least one of methanol, ethyl alcohol, propyl alcohol, isopropanol, and the volume of alcoholic solution is
50mL。
Preferably, the TaOxThe reaction temperature of catalyst controls the reaction time 20h between 100~200 DEG C.
Preferably, the TaOxThe calcination temperature of/DCN be 525 DEG C, retention time 1h, heating rate be 2~5 °/
min。
Preferably, the TaOxThe TaO being added in/DCN synthesis processxMass range be 0~0.08g, g-C3N4Plus
Entering amount is 0.4g.
Another aspect of the present invention, provides a kind of Photocatalyzed Hydrogen Production material, and the material includes the non-of different quality ratio
Brilliant TaOx and defect DCN.That is, the amorphous/crystallized catalyst (TaOx/ DCN) application as catalysis material.
Preferably, the amorphous/crystallized catalyst can be used for water-splitting production hydrogen reaction under visible light.React vacuum degree
For -90Kpa, the triethanolamine aqueous solution that solution is 10%, light source is 300W xenon lamp (λ >=420nm), light application time 10h, instead
Answer temperature control at 15 DEG C.
The beneficial effects of the present invention are:
(1) present invention is for the first time by amorphous TaOxNanoparticle (about 4nm) is supported on the g-C of defect state3N4On, it constructs non-
Crystalline substance/crystallized catalyst reduces lattice, electronic mismatch degree between interface.
(2) N defect and amorphous TaO are introduced simultaneouslyxSolves g-C3N4Material visible-light absorption is weak, photogenerated charge is easily multiple
The shortcomings that conjunction, improves the Photocatalyzed Hydrogen Production performance of material.
(3) presence of N defect increases DCN and amorphous TaOxInteraction force.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrogram of product prepared by embodiment 1,2,3,4,5,6.
Fig. 2 schemes for the TEM of sample 5# in sample 1# in embodiment 1 and embodiment 5.
Fig. 3 schemes for the ESR of sample 5# in sample 2# in embodiment 2 and embodiment 5.
Fig. 4 is the transient photocurrents figure of made sample in embodiment 2,3,4,5,6.
Fig. 5 is the Photocatalyzed Hydrogen Production rate diagram of product prepared by embodiment 1,2,3,4,5,6.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings:
The present invention carries out structural analysis using the miniflex600 powder x-ray diffraction of Rigaku company, Japan；Holland
The Tecnai G2S-Twin F20 transmission electron microscope of FEI Co. carries out TEM morphology analysis；The JES-FA200 of Japan Electronics
Electron spin resonance spectrometer (ESR) carries out defect analysis.
Embodiment 1 prepares amorphous TaOxNano material
By 0.36g TaCl5Powder is slowly added into the aqueous isopropanol that 49ml stirreds, and is continuously stirred until being formed
Clear solution.Then 1.0mL concentrated ammonia liquor is added dropwise dropwise into the solution.After stirring 30 minutes, final solution is transferred to 100mL
Ptfe autoclave in, keep 20h in an oven at 180 DEG C.It, will be in reaction kettle after reaction kettle is cooled to room temperature
White precipitate ethyl alcohol and deionized water are alternately washed, until being washed till neutrality.Then it is dried in vacuo 12h at room temperature to get arriving
TaOx(OH)y, then by dried TaOx(OH)yWhite powder is in tube furnace with the rate liter of 2 DEG C/min under hydrogen atmosphere
Temperature is to 525 DEG C and keeps 1h to get to TaOx, is denoted as 1#.
Embodiment 2 prepares defect state carbon nitrogen (DCN) material
Load weighted 10g melamine powder is put into aluminium oxide porcelain boat, cover and there are a small amount of gap, be then placed in
In Muffle furnace, under air atmosphere, 540 DEG C are heated to the rate of 10 DEG C/min, and kept for two hours.It is taken after cooling down completely
Out, the yellow powder obtained after grinding is g-C3N4.Then by g-C3N4With 2 DEG C/min's under hydrogen atmosphere in tube furnace
Rate is warming up to 525 DEG C and keeps 1h to get to DCN, is denoted as 2#.
Embodiment 3 prepares Ta1/CN material
Take the above-mentioned g-C prepared of 0.4g3N4With the TaO of 0.01gx(OH)yMixing, is then added to together containing 50mL
In the beaker of ethyl alcohol, and it is put into 70 DEG C of stirring in water bath in water-bath and is evaporated.Sample will be evaporated to grind and move on in aluminium oxide porcelain boat,
It is subsequently placed in tube furnace and is heated under hydrogen atmosphere, be heated to 525 DEG C with the rate of 2 DEG C/min and keep 1h.It is down to temperature
After room temperature, grinding is denoted as 3# to get Ta1/CN is arrived.
Embodiment 4 prepares Ta3/CN material
Take the above-mentioned g-C prepared of 0.4g3N4With the TaO of 0.03gx(OH)yMixing, is then added to together containing 50mL
In the beaker of ethyl alcohol, and it is put into 70 DEG C of stirring in water bath in water-bath and is evaporated.Sample will be evaporated to grind and move on in aluminium oxide porcelain boat,
It is subsequently placed in tube furnace and is heated under hydrogen atmosphere, be heated to 525 DEG C with the rate of 2 DEG C/min and keep 1h.It is down to temperature
After room temperature, grinding is denoted as 4# to get Ta3/CN is arrived.
Embodiment 5 prepares Ta5/CN material
Take the above-mentioned g-C prepared of 0.4g3N4With the TaO of 0.05gx(OH)yMixing, is then added to together containing 50mL
In the beaker of ethyl alcohol, and it is put into 70 DEG C of stirring in water bath in water-bath and is evaporated.Sample will be evaporated to grind and move on in aluminium oxide porcelain boat,
It is subsequently placed in tube furnace and is heated under hydrogen atmosphere, be heated to 525 DEG C with the rate of 2 DEG C/min and keep 1h.It is down to temperature
After room temperature, grinding is denoted as 5# to get Ta5/CN is arrived.
Embodiment 6 prepares Ta7/CN material
Take the above-mentioned g-C prepared of 0.4g3N4With the TaO of 0.07gx(OH)yMixing, is then added to together containing 50mL
In the beaker of ethyl alcohol, and it is put into 70 DEG C of stirring in water bath in water-bath and is evaporated.Sample will be evaporated to grind and move on in aluminium oxide porcelain boat,
It is subsequently placed in tube furnace and is heated under hydrogen atmosphere, be heated to 525 DEG C with the rate of 2 DEG C/min and keep 1h.It is down to temperature
After room temperature, grinding is denoted as 6# to get Ta7/CN is arrived.
The structure of 7 sample of embodiment, morphology characterization
It is as shown in Figure 1 that material phase analysis has been carried out to sample 1#~6# using X-ray powder.The result shows that synthesized sample
1# is amorphous TaOx, 2# DCN, 3#~6# are TaOxWith the compound of DCN different proportion.By transmission electron microscope to sample
Product 1# and 5# carry out selected diffraction and morphology analysis, as shown in Fig. 2, sample 1# is the nano particle of 4nm or so, disperse in illustration
Diffraction ring demonstrate the amorphous characteristic of 1#, sample 5# is amorphous nano particulate load to DCN on piece.
The test of 8 electron spin resonance spectroscopy of embodiment
Sample 1# and 5# are subjected to defect test characterization, as shown in Figure 3.It can be seen that having in sample 1# and 5# apparent
Nitrogen null signals, and after TaOx is dispersed on DCN, nitrogen signal enhancing.
The test of 9 transient photocurrents of embodiment
The preparation of working electrode: the PEG 20000 powder of 30mg catalyst and 10mg are put in agate mortar, ground
Mill was uniformly mixed it at 30 minutes or so, was then dispersed in the ethanol solution of 0.5mL, and ultrasonic treatment is just formed after 30 minutes
Uniform suspension.Spin coating instrument is opened, program is set, i.e., first keeps 20s at 2000rpm, then further accelerates 3000rpm
Lower maintenance 15s.1 × 1cm is first allowed before opening instrument2FTO glass is inhaled on instrument, and then instrument starts dropwise addition when rotation
Sample, and guarantee that each sample is added dropwise in first program.It is finished to program operation, FTO is removed and is done at normal temperature
It is dry, working electrode has thus been made.
The above-mentioned working electrode prepared is packed into test macro, then timing opening-closing xenon lamp, carries out transient state photoelectricity
Response test is flowed, as a result as shown in figure 4, TaOxThe photogenerated charge separative efficiency of/DCN compound is significantly stronger than DCN.
The test of 10 photodissociation aquatic products hydrogen of embodiment
Photocatalyzed Hydrogen Production test is surveyed under closed condition of negative pressure.By three second of 50mg photochemical catalyst and 50mL10%
Aqueous alkanolamine is separately added into light-catalyzed reaction pond, and is persistently stirred at 400rpm, is then sealed upper cushion rubber, is made vacuum degree
It is maintained at -90Kpa or so.Continuous irradiation 10h under visible light, while with gas-chromatography real-time monitoring hydrogen output, each sample
Three times, the average value of result is Photocatalyzed Hydrogen Production rate three times for test.
Sample 1#~6# is obtained into corresponding Photocatalyzed Hydrogen Production rate diagram according to above-mentioned photocatalysis testing procedure, such as Fig. 5 institute
Show.The hydrogen-producing speed of sample 5# is most fast, is 5348 μm of ol h-1g-1(λ≥420nm)。
Basic principles and main features and advantages of the present invention of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
1. a kind of preparation method of amorphous/crystallized catalyst, it is characterised in that: the following steps are included:
Step A, pentavalent tantalum salt is added in alcoholic solution, then reacts 20h at 100~200 DEG C, after washing is dry to get
To amorphous TaOxPersursor material；
Step B, by melamine, 540 DEG C of calcining 2h obtain crystal type g-C under air atmosphere in Muffle furnace3N4；
Step C, sample obtained in step A and step B is taken to be added separately in 50mL ethanol solution, and 70 DEG C in water-bath
It is evaporated, is subsequently placed in the lower 525 DEG C of calcining 1h of argon nitrogen atmosphere in tube furnace to get the amorphous containing nitrogen vacancy/crystal type TaO is arrivedx/
DCN catalyst.
2. the preparation method of amorphous/crystallized catalyst according to claim 1, which is characterized in that the pentavalent tantalum salt
For one of ethanol tantalum, tantalic chloride, isopropanol tantalum or multiple combinations；The alcoholic solution is methanol, ethyl alcohol, propyl alcohol, isopropyl
One of alcohol or multiple combinations；The volume of alcoholic solution is 50mL.
3. the preparation method of amorphous/crystallized catalyst according to claim 1, which is characterized in that the TaOx forerunner
The synthesis temperature of body material controls the reaction time 20h between 100~200 DEG C.
4. the preparation method of amorphous/crystallized catalyst according to claim 1, which is characterized in that calcination temperature 525
DEG C, retention time 1h, for heating rate between 2~5 DEG C/min, argon hydrogen volume ratio is 90%:10%.
5. the preparation method of amorphous/crystallized catalyst according to claim 1, which is characterized in that TaOx forerunner is added
For the quality of body between 0~0.08g, the additional amount of g-C3N4 is 0.4g.
6. the preparation method of amorphous/crystallized catalyst according to claim 1, which is characterized in that gained TaOx/DCN
Catalyst morphology is that the TaOx nanoparticle of 4nm or so is uniformly anchored on sheet DCN.
7. the preparation method of amorphous/crystallized catalyst according to claim 1, which is characterized in that urged as light
Agent is applied to decompose the reaction of aquatic products hydrogen under visible light.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111477461A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Micro-nano heterojunction and application thereof in field of electrolytic catalyst and/or electric energy storage |
| CN115449834A (en) * | 2022-10-28 | 2022-12-09 | 国家电投集团氢能科技发展有限公司 | Catalyst with amorphous shell layer and preparation method and application thereof |
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| CN101474558A (en) * | 2008-01-04 | 2009-07-08 | 中国科学院金属研究所 | Preparation method of alkali metal tantalate composite visible-light photocatalyst for hydrogen production from photodissociation of water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111477461A (en) * | 2019-11-21 | 2020-07-31 | 中山大学 | Micro-nano heterojunction and application thereof in field of electrolytic catalyst and/or electric energy storage |
| CN115449834A (en) * | 2022-10-28 | 2022-12-09 | 国家电投集团氢能科技发展有限公司 | Catalyst with amorphous shell layer and preparation method and application thereof |
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Application publication date: 20190625 |