CN110237838A - A kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material - Google Patents
A kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material Download PDFInfo
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- CN110237838A CN110237838A CN201910370065.8A CN201910370065A CN110237838A CN 110237838 A CN110237838 A CN 110237838A CN 201910370065 A CN201910370065 A CN 201910370065A CN 110237838 A CN110237838 A CN 110237838A
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- oxygen defect
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- tungsten oxide
- light absorption
- absorption type
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000001301 oxygen Substances 0.000 title claims abstract description 37
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 37
- 230000007547 defect Effects 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 24
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims description 17
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims description 16
- 238000002360 preparation method Methods 0.000 title claims description 15
- 230000002708 enhancing effect Effects 0.000 title claims description 11
- 230000031700 light absorption Effects 0.000 title claims description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000003760 magnetic stirring Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- QUBBAXISAHIDNM-UHFFFAOYSA-N ethyldimethylbenzene Natural products CCC1=CC=CC(C)=C1C QUBBAXISAHIDNM-UHFFFAOYSA-N 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 230000001360 synchronised effect Effects 0.000 abstract description 2
- 230000002787 reinforcement Effects 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 238000003756 stirring Methods 0.000 description 10
- 239000011259 mixed solution Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- -1 WO3 Chemical class 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 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 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- WXGOYJBSGSFYJG-UHFFFAOYSA-N [W]O[W] Chemical class [W]O[W] WXGOYJBSGSFYJG-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- VVRQVWSVLMGPRN-UHFFFAOYSA-N oxotungsten Chemical compound [W]=O VVRQVWSVLMGPRN-UHFFFAOYSA-N 0.000 description 1
- 238000001126 phototherapy Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009423 ventilation Methods 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
It is an object of the invention to introduce a kind of WO rich in oxygen defect by one-step method3Nanometer sheet material when being used for photocatalytic degradation catalyst, shows good light degradation property.A kind of WO rich in oxygen defect proposed by the present invention3Nanometer sheet material, it is by introducing agent-nitric acid synchronous reaction with oxygen defect while generating nanometer chip architecture, namely during generating nanometer sheet, oxygen defect is constantly introduced on its surface, the introducing of these oxygen defects, be conducive to its absorbing properties of the nanometer sheet Material reinforcement, to be conducive to the promotion of its light degradation property.
Description
Technical field
The present invention relates to the preparation technical fields of catalysis material, are specifically related to a kind of oxygen defect enhancing light absorption type oxygen
Change the preparation method of tungsten material.
Background technique
Tungsten oxide is a kind of important n-type semiconductor, which are mainly applied to gas sensor, electrochromism, photocatalysis and
The fields such as electro-catalysis.
Perfect tungsten oxide is a kind of octoploids structure, and wherein W is in octahedral center, and O is then in octahedral 8
On a vertex.But it in practice, octahedral structure perfect in this way and is not present, can have certain bending or torsion and become
Shape, this also has led to, and there are a series of tungsten tungsten oxide, such as WO3、W18O49、W3O8And W19O55Etc..For these tungsten oxygen
Change tungsten, there is a large amount of research, if WO3 is a kind of highly stable oxide, can stablize in air, acidity or alkalinity
In the presence of, and also there is extensive basis to the research of its pattern, this is so as to be applied in many catalysis reactions, most often
The catalysis reaction seen has HER(document 1:Tungsten Oxides for Photocatalysis, Electrochemistry,
And Phototherapy, Adv. Mater. 2015；Document 2:Noble-Metal-free Hybrid Membranes for
Highly Efficient Hydrogen Evolution, Adv. Mater. 2017).
Recently it was discovered by researchers that its reactivity worth can be obviously improved rich in the nano material of oxygen defect, as it can be with
The light abstraction width for improving fertile material, improve the electric conductivity of fertile material and increase its catalytic activity and other effects.This makes
Research for how to increase oxygen defect has significant meaning.When introducing a large amount of oxygen defect into tungsten oxide, also table
Infusive effect is revealed.Such as the novel hydrogenation catalyst that University Of Tianjin Song Jiajia et al. is studied, it uses different
Tungsten oxide, and by introducing oxygen defect, these catalyst are studied to chain olefin, cyclic olefin and aromatic nitro compound
Hydrogenation introduces the catalyst of oxygen defect from the point of view of final conclusion, is more conducive to the activation of molecular hydrogen.And Chinese section
The Zeng Jie professor seminar for learning technology university proposes a kind of WO in patent CN106824190A3-xThe preparation of nanocatalyst,
It is prepared for tungsten oxide nanometer material by ultrasound removing, and is used in electrolysis aquatic products hydrogen reaction, shows close to quotient
The performance of industry Pt/C catalyst.
Although having had many research now for oxygen defect is introduced in tungsten oxide, these methods are all more or less
There are step complexity, oxygen defect introduces not high enough the problems such as waiting of content, for this purpose, it is an object of the invention to be drawn by one-step method
Enter a kind of WO rich in oxygen defect3Nanometer sheet material when being used for photocatalytic degradation catalyst, shows good light
Degradation property.
Summary of the invention
As above, it is an object of the invention to introduce a kind of WO rich in oxygen defect by one-step method3Nanometer sheet material, by it
When for photocatalytic degradation catalyst, good light degradation property is shown.It is proposed by the present invention a kind of rich in oxygen defect
WO3Nanometer sheet material, be by while generating nanometer chip architecture with oxygen defect introduce agent-nitric acid synchronous reaction,
It is exactly constantly to introduce oxygen defect on surface during generating nanometer sheet, the introducing of these oxygen defects is conducive to this and receives
Rice sheet material enhances its absorbing properties, to be conducive to the promotion of its light degradation property.
In order to make those skilled in the art know that technical solution of the present invention, now carries out technical solution of the present invention
As described in detail below.
A kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material, mainly includes the following steps:
The first step weighs suitable tungsten hexachloride, is dissolved in the in the mixed solvent of ethyl alcohol and dimethylbenzene, is sufficiently stirred, directly
Extremely it is uniformly mixed；
Second step adds suitable PVP and nitric acid into uniformly mixed mixed liquor, continues to be stirred until homogeneous；
The mixed liquor stirred evenly in step 2 is transferred in hydrothermal reaction kettle, then seals, at 180-220 DEG C by third step
Lower reaction 15-20h；
4th step is removed reaction kettle cooled to room temperature, is then washed using deionized water and alcohol mixeding liquid after reaction
Product 3 times to suspend in a kettle are washed, later, drying grinding just can be used.
Preferably, it in the first step of the present invention, due to needing that dimethylbenzene is added, needs for magnetic stirring equipment to be placed on ventilation
The preparation of reaction raw materials is carried out in cupboard, after tungsten hexachloride is added, with the extension of mixing time, solution colour after yellow from becoming
Navy blue.
Preferably, in the first step of the present invention, the mass volume ratio of hexachloride and ethyl alcohol is 0.1-0.2:30-50；And its
The volume ratio of middle ethyl alcohol and dimethylbenzene is 1:0.05-0.1.
Preferably, in second step of the present invention, the dosage of PVP is 5-10 times of tungsten hexachloride, and the additional amount of nitric acid is total molten
The 1-5% of agent volume.
Preferably, in second step of the present invention, the PVP of K30 is used.
Preferably, in third step of the present invention, preferred reaction temperature is 185-200 DEG C, reaction time 16-18h.
Preferably, in the 4th step of the invention, the in the mixed solvent of ethyl alcohol and deionized water, volume ratio is any volume
Than preferred volume ratio is 1:1.
Preferably, prepared by the present invention to be rich in oxygen defect WO3The length of nanometer sheet is in the micron-scale.
In addition, it is further proposed that by being prepared rich in oxygen defect WO3Nanometer sheet is led applied to photocatalytic degradation
Domain.Preferably, it is used for degradation of methylene blue.
The advantageous effects that the present invention obtains mainly have following several respects, by regulating and controlling reaction condition, pass through a step water
Thermal method has prepared the WO rich in oxygen defect3Nanometer sheet, this has great importance in this field, and the nanometer sheet material,
Due to the introducing of oxygen defect, so that its absorbing properties is greatly improved.
Detailed description of the invention
Fig. 1 WO prepared by the present invention rich in oxygen defect3Nanometer sheet；
Fig. 2 WO prepared by the present invention rich in oxygen defect3Nanometer sheet is used for methylene blue Degrading experiment test chart.
Specific embodiment
Technology contents of the invention are described in detail below by specific embodiment, but it should be recognized that this
More only show that column illustrate, can not be construed as limiting the invention, any tiny change for not departing from present inventive concept,
Belong to the claimed content of the present invention.
Embodiment 1
The tungsten hexachloride for weighing 0.15g is dissolved in configured 40mL ethyl alcohol and two with magnetic stirring apparatus by it in draught cupboard
In toluene mixed solution (volume ratio 1:0.05), after stirring after a period of time, after liquid color to be mixed becomes navy blue, then
Be slowly added to the nitric acid of the PVP and 1mL of 1.0g thereto, continue to stir, then by mixed liquor be transferred in hydrothermal reaction kettle into
Row hydro-thermal reaction, reaction temperature are 200 DEG C, reaction time 16h, after reaction, cooled to room temperature, then using going
Ionized water and alcohol mixeding liquid washing may be used for subsequent use using conventional wash drying.
Embodiment 2
The tungsten hexachloride for weighing 0.15g is dissolved in configured 40mL ethyl alcohol and two with magnetic stirring apparatus by it in draught cupboard
In toluene mixed solution (volume ratio 1:0.05), after stirring after a period of time, after liquid color to be mixed becomes navy blue, then
Be slowly added to the nitric acid of the PVP and 1mL of 1.0g thereto, continue to stir, then by mixed liquor be transferred in hydrothermal reaction kettle into
Row hydro-thermal reaction, reaction temperature are 190 DEG C, reaction time 17h, after reaction, cooled to room temperature, then using going
Ionized water and alcohol mixeding liquid washing may be used for subsequent use using conventional wash drying.
Embodiment 3
The tungsten hexachloride for weighing 0.5g is dissolved in configured 80mL ethyl alcohol and two with magnetic stirring apparatus by it in draught cupboard
In toluene mixed solution (volume ratio 1:0.1), after stirring after a period of time, after liquid color to be mixed becomes navy blue, then
Be slowly added to the nitric acid of the PVP and 2mL of 3.0g thereto, continue to stir, then by mixed liquor be transferred in hydrothermal reaction kettle into
Row hydro-thermal reaction, reaction temperature are 200 DEG C, reaction time 16h, after reaction, cooled to room temperature, then using going
Ionized water and alcohol mixeding liquid washing may be used for subsequent use using conventional wash drying.
Embodiment 4
The tungsten hexachloride for weighing 0.15g is dissolved in configured 40mL ethyl alcohol and two with magnetic stirring apparatus by it in draught cupboard
In toluene mixed solution (volume ratio 1:0.1), after stirring after a period of time, after liquid color to be mixed becomes navy blue, then
Be slowly added to the nitric acid of the PVP and 1mL of 1.0g thereto, continue to stir, then by mixed liquor be transferred in hydrothermal reaction kettle into
Row hydro-thermal reaction, reaction temperature are 200 DEG C, reaction time 16h, after reaction, cooled to room temperature, then using going
Ionized water and alcohol mixeding liquid washing may be used for subsequent use using conventional wash drying.
Embodiment 5
The tungsten hexachloride for weighing 0.3g is dissolved in configured 40mL ethyl alcohol and two with magnetic stirring apparatus by it in draught cupboard
In toluene mixed solution (volume ratio 1:0.05), after stirring after a period of time, after liquid color to be mixed becomes navy blue, then
It is slowly added to the nitric acid of the PVP and 1.5mL of 1.5g thereto, continues to stir, then mixed liquor is transferred in hydrothermal reaction kettle
Hydro-thermal reaction is carried out, reaction temperature is 185 DEG C, and reaction time 18h, after reaction, then cooled to room temperature uses
Deionized water and alcohol mixeding liquid washing may be used for subsequent use using conventional wash drying.
Light source is done using high pressure xenon lamp in the present invention and carries out light degradation test, wherein is obtained entirely using visible reflectance piece
Spectral light is shone, and obtains ultraviolet light using ultraviolet filter, and become using the concentration that ultraviolet specrophotometer constantly detects organic matter
Change.
Claims (8)
1. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material, it is characterised in that: it mainly include the following steps,
The first step weighs suitable tungsten hexachloride, is dissolved in the in the mixed solvent of ethyl alcohol and dimethylbenzene, is sufficiently stirred, directly
Extremely it is uniformly mixed；
Second step adds suitable PVP and nitric acid into uniformly mixed mixed liquor, continues to be stirred until homogeneous；
The mixed liquor stirred evenly in step 2 is transferred in hydrothermal reaction kettle, then seals, at 180-220 DEG C by third step
Lower reaction 15-20h；
4th step is removed reaction kettle cooled to room temperature, is then washed using deionized water and alcohol mixeding liquid after reaction
Product 3 times to suspend in a kettle are washed, later, drying grinding just can be used.
2. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material according to claim 1, feature exist
In: in the first step, due to needing that dimethylbenzene is added, need for magnetic stirring equipment to be placed in draught cupboard that carry out reaction former
The preparation of material, after tungsten hexachloride is added, with the extension of mixing time, solution colour is from becoming navy blue after yellow.
3. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material according to claim 1, feature exist
In: in the first step, the mass volume ratio of hexachloride and ethyl alcohol is 0.1-0.2:30-50；And wherein ethyl alcohol and dimethylbenzene
Volume ratio be 1:0.05-0.1.
4. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material according to claim 1, feature exist
In: in the second step, the dosage of PVP is 5-10 times of tungsten hexachloride, and the additional amount of nitric acid is the 1-5% of total solvent volume.
5. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material according to claim 1, feature exist
In: in the second step, use the PVP of K30.
6. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material according to claim 1, feature exist
In: in the third step, preferred reaction temperature is 185-200 DEG C, reaction time 16-18h.
7. a kind of preparation method of oxygen defect enhancing light absorption type tungsten oxide material according to claim 1, feature exist
In: in the 4th step, the in the mixed solvent of ethyl alcohol and deionized water, volume ratio is any volume ratio, preferred volume ratio
For 1:1.
8. any one of -7 is resulting rich in oxygen defect WO according to claim 13Nanometer sheet, length is in the micron-scale.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743535A (en) * | 2019-11-28 | 2020-02-04 | 湖南大学 | Tungsten oxide homojunction composite photocatalyst and preparation method and application thereof |
| CN111495355A (en) * | 2020-04-26 | 2020-08-07 | 中国科学院合肥物质科学研究院 | WO with visible light region L SPR absorption3-xPhotocatalyst, preparation method and application |
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| CN111495355A (en) * | 2020-04-26 | 2020-08-07 | 中国科学院合肥物质科学研究院 | WO with visible light region L SPR absorption3-xPhotocatalyst, preparation method and application |
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