CN108355678A - A kind of compound micron bouquet of artificial gold-bismuth tungstate and its preparation method and application - Google Patents
A kind of compound micron bouquet of artificial gold-bismuth tungstate and its preparation method and application Download PDFInfo
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- CN108355678A CN108355678A CN201810193853.XA CN201810193853A CN108355678A CN 108355678 A CN108355678 A CN 108355678A CN 201810193853 A CN201810193853 A CN 201810193853A CN 108355678 A CN108355678 A CN 108355678A
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title description 4
- AJZRPMVVFWWBIW-UHFFFAOYSA-N [Au].[Bi] Chemical compound [Au].[Bi] AJZRPMVVFWWBIW-UHFFFAOYSA-N 0.000 title description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 22
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 238000001338 self-assembly Methods 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 87
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 27
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 12
- 235000014121 butter Nutrition 0.000 claims description 11
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 17
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 34
- 235000019441 ethanol Nutrition 0.000 description 18
- 238000005406 washing Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 238000005119 centrifugation Methods 0.000 description 12
- 238000001035 drying Methods 0.000 description 10
- 238000005286 illumination Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 229910020350 Na2WO4 Inorganic materials 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 239000006069 physical mixture Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000009849 vacuum degassing Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 206010020591 Hypercapnia Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
-
- 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
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of SnS2‑Bi2WO6Compound micron bouquet and preparation method thereof, this kind of catalyst include the spherical SnS of petal2And Bi2WO6Particle；The spherical SnS of the petal2By SnS2Piece self assembly forms, the Bi2WO6Distribution of particles is in the SnS2Piece surface.In the present invention, Bi2WO6Distribution of particles is in the SnS2Surface, form hetero-junctions, promote efficiently separating for electron hole pair so that the photocatalytic activity of composite material significantly improves.The present invention generates organic-fuel, petal chondritic SnS using the compound micron bouquet as catalyst for photocatalysis carbon dioxide2Presence help to improve the specific surface area of composite material, and then improve the absorption to visible light, the contact area of bigger and more active sites provided for light-catalyzed reaction system, to improve the photocatalysis efficiency of composite material.
Description
Technical field
The invention belongs to catalysis material technical field more particularly to a kind of SnS2-Bi2WO6Compound micron bouquet and its system
Preparation Method and application.
Background technology
With industrialized development, great amount of carbon dioxide greenhouse gas has been discharged in a large amount of uses of fossil fuel.2015
The data in March show that the carbon dioxide gas in air has reached 400.83ppm, have been the tops since 600,000 years, result in
Serious greenhouse effects and global warming more bring the problems such as sea level rise, solve what carbon dioxide was brought
Greenhouse effects problem is extremely urgent.Researcher trial now cures carbon dioxide, and being translated into the mankind can profit
The energy.
The method of fixed carbon dioxide relates generally to these two issues：(1) how the required energy is cleanly obtained；
(2) how the carbon dioxide molecule of activation stable.Since Inoue etc. reported in 1979 carbon dioxide photocatalysis generate it is organic
The precedent of object, the catalysis material of photocatalytic reduction of carbon oxide become a focus of researcher research.
Traditional wide band gap semiconducter photochemical catalyst, such as：TiO2, the forbidden bands broadband such as ZnO it is larger, to the utilization rate of solar energy
It is relatively low, in solar energy 4% ultraviolet light can only be absorbed, photocatalysis efficiency is relatively low.In order to more effectively solar energy be utilized to realize
Solidification to carbon dioxide, researcher are dedicated to developing novel visible responsive photocatalyst.Bi2WO6It is one kind to have
The semiconductor multivariant oxide of layer structure has certain response, (Bi being alternately present with it under visible light2O2)2+Layer
With octahedral (WO4)2-Structure feature made of accumulation, have higher photocatalytic activity, carbon dioxide solidification field by
To extensive concern.
But Bi2WO6It is a kind of direct band-gap semicondictor, and energy gap is only 2.75eV or so, when illumination generates
Light induced electron and hole direct combination probability it is higher, it is seen that photoresponse is weaker, and photo-quantum efficiency is relatively low, and Bi2WO6Material
Specific surface area it is small, photogenerated charge migration distance is longer, and then that there are still photocatalysis efficiencies is relatively low, and photocatalysis effect is still undesirable
The problem of.
Invention content
In view of this, the purpose of the present invention is to provide a kind of SnS2-Bi2WO6Compound micron bouquet and preparation method thereof and
Using SnS provided by the invention2-Bi2WO6Compound micron bouquet has higher photocatalysis efficiency.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
A kind of SnS2-Bi2WO6Compound micron bouquet, including Bi2WO6With the SnS of flower ball-shaped2；The SnS of the flower ball-shaped2By
SnS2Piece self assembly forms, the Bi2WO6It is distributed in the SnS2Piece surface.
Preferably, the SnS2-Bi2WO6The grain size of compound micron bouquet is 5~6 μm；
The SnS2-Bi2WO6SnS in compound micron bouquet2And Bi2WO6Substance amount ratio be (0.025~0.15)：1.
The present invention provides the SnS described in above-mentioned technical proposal2-Bi2WO6The preparation method of compound micron bouquet, including with
Lower step：
(1) butter of tin, thiocarbamide and ethylene glycol are mixed, carries out heating reaction, obtains flower ball-shaped SnS2；
(2) sodium tungstate and bismuth nitrate are added to the flower ball-shaped SnS2Ethylene glycol dispersion liquid in, carry out solvent heat seal
At reaction, SnS is obtained2-Bi2WO6Compound micron bouquet.
Preferably, the amount of the substance of butter of tin in the step (1), thiocarbamide substance amount and ethylene glycol volume ratio
For 1.5~2mmol：8~10mmol：80mL.
Preferably, the temperature of heating reaction is 180~200 DEG C in the step (1), the time for heating reaction is 18~
20h。
Preferably, SnS in the step (2)2Ethylene glycol dispersion liquid in SnS2Substance amount and organic solvent volume
Than for (0.0125~0.075) mmol：80mL.
Preferably, the amount ratio of the substance of the amount and bismuth nitrate of the substance of sodium tungstate is 0.5~0.6 in the step (2):1；
Sodium tungstate and SnS in the step (2)2Substance amount ratio be 1：(0.025~0.15).
Preferably, the temperature that solvent-thermal process reacts in the step (2) is 160~180 DEG C, solvent-thermal process reaction
Time be 20~for 24 hours.
The present invention also provides the SnS described in above-mentioned technical proposal2-Bi2WO6Compound micron bouquet or above-mentioned preparation method
Obtained SnS2-Bi2WO6Application of the compound micron bouquet as photochemical catalyst in carbon dioxide light-catalyzed reaction.
Preferably, the application includes the following steps：By the SnS2-Bi2WO6Compound micron bouquet is mixed with water, is obtained
SnS2-Bi2WO6The aqueous dispersions of compound micron bouquet；Remove the SnS2-Bi2WO6In the aqueous dispersions of compound micron bouquet
After gas, it is passed through CO2Gas is stood under non-illuminated conditions, and catalysis reaction is then carried out under illumination condition.
The present invention provides a kind of SnS2-Bi2WO6Compound micron bouquet, includes the SnS of flower ball-shaped2And Bi2WO6Particle；Institute
State the SnS of flower ball-shaped2By SnS2Piece self assembly forms, the Bi2WO6Distribution of particles is in the SnS2Piece surface.In the present invention,
Bi2WO6Distribution of particles is in the SnS2The surface of piece, forms hetero-junctions, promotes efficiently separating for electron-hole pair, simultaneously
The formation of hetero-junctions can make SnS2Hole in valence band and Bi2WO6Electronics on conduction band combines, and effectively prevents electron hole pair
Combination, and then can effectively prevent the compound of Pair production so that the photocatalytic activity of composite material significantly improves；And
Petal chondritic SnS2Presence help to improve the specific surface area of composite material, increase the absorption area of visible light and anti-
Active site is answered, to improve the photocatalysis efficiency of composite material.In the present invention, the sheet knot of the compound micron bouquet
Structure, is conducive to light and is constantly reflected among, fully allows incident light and composite material to interact, light is avoided only to limit to
In the position directly struck by light, and then improve photocatalysis efficiency.Embodiment the result shows that, by the present invention be prepared it is compound
When material is used for carbon dioxide light-catalyzed reaction, methanol and ethyl alcohol are generated, by 4h light-catalyzed reactions, the yield of methanol reaches
50.20 μm of ol/g-Cat, the yield of ethyl alcohol is up to 19.70 μm of ol/g-Cat.
Description of the drawings
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the spherical SnS of the petal that is prepared of embodiment 12Field emission scanning electron microscope figure；
Fig. 2 is the SnS that embodiment 1 is prepared2-Bi2WO6The field emission scanning electron microscope figure of compound micron bouquet；
Fig. 3 is the SnS that Examples 1 to 4 is prepared2-Bi2WO6Bi in compound micron bouquet and embodiment 12WO6With
SnS2XRD diagram.
Specific implementation mode
The present invention provides a kind of SnS2-Bi2WO6Compound micron bouquet, including Bi2WO6With the SnS of flower ball-shaped2；The flower
Spherical SnS2By SnS2Piece self assembly forms, the Bi2WO6It is distributed in the SnS2Piece surface.
In the present invention, the SnS of the flower ball-shaped2By SnS2Piece self assembly forms；In the present invention, the SnS2Piece
Self-assembling method is preferably SnS2Piece cluster is at radial.In the present invention, the SnS2The thickness of piece preferably stands alone as 50~
60nm, further preferably 52~55nm；In the present invention, the SnS2Bouquet diameter is preferably 5~6 μm.In the present invention,
The SnS2The laminated structure of piece, is conducive to light and is constantly reflected among, fully allows incident light and composite material phase interaction
With avoiding light from being only confined in certain part, and then improve photocatalysis efficiency.
In the present invention, the Bi2WO6For nano-grade structure；The Bi2WO6It is preferably dimensioned to be 25~30nm.
In the present invention, the Bi2WO6It is distributed in the SnS2The surface of piece, the Bi under intermolecular force2WO6With the flower
Petaloid SnS2It is stably connected with, forms hetero-junctions, promote efficiently separating for electron-hole pair so that the light of composite material is urged
Change activity to significantly improve.
In the present invention, the SnS2-Bi2WO6The grain size of compound micron bouquet is preferably 5~6 μm, further preferably
5.2~5.5 μm.In the present invention, Bi2WO6It is distributed in the SnS2The surface of piece forms compound micron bouquet, keeps flower ball-shaped
SnS2Bouquet diameter.
In the present invention, the SnS2-Bi2WO6SnS in compound micron bouquet2And Bi2WO6The amount ratio of substance be preferably
(0.025~0.15)：1, further preferably (0.05~0.10)：1.
In the present invention, the SnS2-Bi2WO6The presence of the petal chondritic of compound micron bouquet helps to improve multiple
The specific surface area of condensation material, and then the absorption to visible light is improved, the contact area of bigger is provided for light-catalyzed reaction system
With more active sites, to improve the photocatalysis efficiency of composite material.
The present invention provides the SnS described in above-mentioned technical proposal2-Bi2WO6The preparation method of compound micron bouquet, including with
Lower step：
(1) butter of tin, thiocarbamide and ethylene glycol are mixed, carries out heating reaction, obtains flower ball-shaped SnS2；
(2) sodium tungstate and bismuth nitrate are added to the flower ball-shaped SnS2Ethylene glycol dispersion liquid in, carry out solvent heat seal
At reaction, SnS is obtained2-Bi2WO6Compound micron bouquet.
The present invention mixes butter of tin, thiocarbamide and ethylene glycol, carries out heating reaction, obtains the SnS of flower ball-shaped2.At this
In invention, the volume ratio of the amount of the substance of butter of tin, the amount of the substance of thiocarbamide and ethylene glycol is preferably 1.5~2mmol：8~
10mmol：80mL, further preferably 1.8mmol：9mmol：80mL.The present invention is to the butter of tin, thiocarbamide and ethylene glycol
Source there is no particular/special requirement, using well-known to those skilled in the art；In an embodiment of the present invention, the tetrachloro
It is specially stannic chloride pentahydrate to change tin.
The present invention mixes butter of tin and thiocarbamide with ethylene glycol, makes full use of the viscosity advantage of ethylene glycol, hinders particle
Mass transport process, and then reduce crystal growth rate, avoid agglomeration traits caused by too fast growth, and ethylene glycol can rise
To the effect of surfactant；The present invention is using ethylene glycol as directed agents, to SnS2Crystal growth when nucleation process controlled
System plays the role of structure directing during Crystallization, and then forms laminated structure, and effectively finishing is in self assembly
Pattern finally obtains the spherical SnS of petal2。
The present invention does not have particular/special requirement to the hybrid mode of the butter of tin, thiocarbamide and ethylene glycol, using this field skill
Material hybrid mode known to art personnel.
After the mixing, the mixture of the butter of tin, thiocarbamide and ethylene glycol is carried out heating reaction by the present invention, is obtained
The SnS of flower ball-shaped2.In the present invention, the temperature of the heating reaction is preferably 180~200 DEG C, further preferably 185~
190℃.In the present invention, the time of the heating reaction is preferably 18~20h, further preferably 19~19.5h.The present invention
There is no particular/special requirement to the specific implementation mode of the heating, using the embodiment of heating well-known to those skilled in the art
.In the present invention, the heating reaction preferably carries out in a kettle.
After the heating reaction, the present invention preferably post-processes the heating reaction product, obtains flower ball-shaped SnS2。
In the present invention, the post-processing preferably includes：The heating reaction product is cooling successively, washing, centrifugation and drying.At this
In invention, the temperature after cooling is preferably room temperature, further preferably 25~30 DEG C.The present invention is to the crystallisation by cooling
Mode does not have particular/special requirement, uses crystallisation by cooling mode well-known to those skilled in the art can realize the abundant analysis of solute
Go out.
In the present invention, the washing preferably use successively ethyl alcohol and distilled water to the heating reaction product of the precipitation into
Row washing.The present invention does not have particular/special requirement to the mode of the washing, using mode of washing well-known to those skilled in the art
.In an embodiment of the present invention, the washing is specially to be washed 3 times using ethyl alcohol, adopt and be washed with distilled water 3 times.
After completing the washing, the present invention preferably centrifuges the washed product, obtains SnS2Bouquet.The present invention couple
The specific implementation mode of the centrifugation does not have particular/special requirement, uses centrifugation well-known to those skilled in the art can realize
The separation of feed liquid.In the present invention, the centrifugation carries out preferably in centrifuge, and the present invention does not have the model of the centrifuge
Particular/special requirement.
After completing the centrifugation, the present invention is preferably dried solid product after the centrifugation, and it is spherical to obtain petal
SnS2.In the present invention, the temperature of the drying is preferably 60~80 DEG C, further preferably 65~70 DEG C；In the present invention,
The time of the drying is preferably 10~12h, further preferably 11~11.5h.The present invention does not have the mode of the drying
Particular/special requirement, using drying mode well-known to those skilled in the art；In an embodiment of the present invention, the dry tool
Body carries out in an oven.
In the present invention, the SnS2For flower ball-shaped structure, by SnS2Piece self assembly forms；The SnS2The thickness of piece is excellent
It is selected as 50~60nm.In the present invention, the SnS2The diameter of bouquet is preferably 5~6 μm.
Obtain the SnS of bouquet structure2Afterwards, sodium tungstate and bismuth nitrate are added to the SnS by the present invention2Ethylene glycol dispersion
In liquid, solvent-thermal process reaction is carried out, SnS is obtained2-Bi2WO6Compound micron bouquet.
In the present invention, the SnS2Ethylene glycol dispersion liquid in SnS2Substance amount and ethylene glycol volume ratio it is preferred
For (0.0125~0.075) mmol：80mL, further preferably (0.025~0.055) mmol：80mL.In the present invention, institute
The use of ethylene glycol is stated, can not only be realized to SnS2Dispersion, moreover it is possible to contribute to the dispersion of sodium tungstate and bismuth nitrate, Jin Erbian
In sodium tungstate and bismuth nitrate and SnS2Come into full contact with, it is ensured that Bi2WO6Synthesis.The present invention is to the SnS2Ethylene glycol point
The manner of formulation of dispersion liquid does not have particular/special requirement, using the manner of formulation of organic solution well-known to those skilled in the art；
In an embodiment of the present invention, the SnS2Ethylene glycol dispersion liquid specifically using by SnS2It is scattered in ethylene glycol.
Obtain SnS2Ethylene glycol dispersion liquid after, sodium tungstate and bismuth nitrate are added to the SnS by the present invention2Ethylene glycol
In dispersion liquid, solvent-thermal process reaction is carried out, SnS is obtained2-Bi2WO6Compound micron bouquet.In the present invention, the sodium tungstate
Amount ratio with the substance of bismuth nitrate is preferably 0.5~0.6:1, further preferably 0.55:1；The sodium tungstate and SnS2Object
The amount of matter is than preferably 1：(0.025~0.15), further preferably 1：(0.05~0.10).In the present invention, the wolframic acid
Sodium and bismuth nitrate are added to the SnS2The process of ethylene glycol dispersion liquid preferably carry out under agitation, help to disperse
It is even；The present invention does not have particular/special requirement to the specific implementation mode of the stirring, using stirring well-known to those skilled in the art
Mode.
Sodium tungstate and bismuth nitrate are added to and are dispersed with SnS by the present invention2Ethylene glycol dispersion liquid in, contribute to solvent heat seal
Bi is obtained at reaction process2WO6When, it is dispersed in SnS in granular form2Petal surface.
The present invention carries out solvent-thermal process reaction to obtained mixed solution, obtains SnS2-Bi2WO6Compound micron bouquet.
In the present invention, the temperature of the solvent-thermal process reaction is preferably 160~180 DEG C, further preferably 165~170 DEG C；Institute
The time for stating solvent-thermal process reaction is preferably 20~for 24 hours, further preferably 22~23h.In the present invention, the solvent heat
Synthetic reaction preferably carries out in a kettle；The present invention does not have particular/special requirement to the model of reaction kettle, using people in the art
Known to member.
The present invention realizes that the synthetic reaction of bismuth nitrate and sodium tungstate obtains wolframic acid in the solvent-thermal process reaction process
Bismuth, and synthesized bismuth tungstate can it is fully dispersed in a solvent, synthesized bismuth tungstate and SnS2Between because intermolecular
Graininess Bi is realized in the effect of interaction force2WO6In SnS2The attachment of petal surface.
After the solvent-thermal process reaction, the present invention preferably post-processes the solvent-thermal process reaction product, obtains
To SnS2-Bi2WO6Compound micron bouquet.In the present invention, the post-processing preferably includes：The solvent-thermal process is reacted and is produced
Object cooling, washing, centrifugation and drying successively.In the present invention, the temperature after cooling is preferably room temperature, further preferably
25~30 DEG C.The present invention does not have particular/special requirement to the mode of the crystallisation by cooling, using well-known to those skilled in the art cold
But crystallization mode is can realize the abundant precipitation of solute.
In the present invention, the washing preferably use successively ethyl alcohol and distilled water to the heating reaction product of the precipitation into
Row washing.The present invention does not have particular/special requirement to the mode of the washing, using mode of washing well-known to those skilled in the art
.In an embodiment of the present invention, the washing is specially to be washed 3 times using ethyl alcohol, adopt and be washed with distilled water 3 times.
After completing the washing, the present invention preferably centrifuges the washed product, obtains SnS2-Bi2WO6It is compound micro-
Popped rice ball.The present invention does not have particular/special requirement, use well-known to those skilled in the art the specific implementation mode of the centrifugation
Centrifugation is can realize the separation of feed liquid.In the present invention, the centrifugation carries out preferably in centrifuge, and the present invention is to described
The model of centrifuge does not have particular/special requirement.
After completing the centrifugation, the present invention is preferably dried solid product after the centrifugation, obtains SnS2-Bi2WO6
Compound micron bouquet.In the present invention, the temperature of the drying is preferably 60~80 DEG C, further preferably 65~70 DEG C；
In the present invention, the time of the drying is preferably 10~12h, further preferably 10.5~11h.The present invention is to the drying
Mode does not have particular/special requirement, using drying mode well-known to those skilled in the art.
The present invention also provides the SnS described in above-mentioned technical proposal2-Bi2WO6Compound micron bouquet exists as photochemical catalyst
Application in carbon dioxide light-catalyzed reaction.In the present invention, the application is preferred is specially：By the SnS2-Bi2WO6It is compound
Micron bouquet is used for carbon dioxide light-catalyzed reaction as catalyst, obtains methanol and ethyl alcohol.The present invention is by the SnS2-
Bi2WO6Compound micron bouquet is used for photo catalytic reduction CO as catalyst2Organic-fuel is generated, hypercapnia can be solved
Caused environmental hazard, moreover it is possible to provide effective way to generate more cleaning organic-fuels.
In the present invention, described apply further preferably includes：By the SnS2-Bi2WO6Compound micron bouquet is mixed with water
It closes, obtains SnS2-Bi2WO6The aqueous dispersions of compound micron bouquet；Remove the SnS2-Bi2WO6The moisture of compound micron bouquet
After gas in dispersion liquid, it is passed through CO2Gas is stood under non-illuminated conditions, and catalysis reaction is then carried out under illumination condition.
In the present invention, the SnS2-Bi2WO6SnS in the aqueous solution of compound micron bouquet2-Bi2WO6The quality and water of compound micron bouquet
Volume ratio be preferably 20~50mg：50~100mL；The removing method of the gas is preferably vacuum degassing, and the present invention is to institute
Stating vacuum degassed mode does not have particular/special requirement, using vacuum degassing mode well-known to those skilled in the art.At this
In invention, the CO2Gas is from the SnS2-Bi2WO6It is risen after gas removal in the aqueous dispersions of compound micron bouquet to carrying
For being continually fed into before illumination condition.In the present invention, the CO2The rate that is passed through of gas is preferably 50~100mL/min.
In the present invention, the time of the standing under the non-illuminated conditions is preferably 0.5~1h；Under the non-illuminated conditions
Standing make CO2It is fully adsorbed on catalyst surface, reaches adsorption equilibrium, while CO2Solubility in water also reaches full
With.In the present invention, the illumination condition is preferably the illumination condition within the scope of wavelength >=420nm；The wave of the illumination condition
Long is more preferably 450~720nm；The catalysis reaction time under the illumination condition is preferably 4~6h.
In an embodiment of the present invention, the temperature of the light-catalyzed reaction is preferably 4 DEG C；The light-catalyzed reaction preferably exists
It is carried out in closed quartz reactor.The light-catalyzed reaction is specially：(1) by 50mL ultra-pure waters and 50mg SnS2-Bi2WO6
Compound micron bouquet mixing；(2) after removing the gas in water removal by the way of vacuumizing under the conditions of magnetic agitation, with 50mL/
The rate of min is passed through high-purity CO2After light reaction 4h being carried out after gas half an hour under the 300W Xenon light shinings of wavelength >=420nm,
Qualitative and quantitative analysis is carried out to the product in solution, determines the content of methanol and ethyl alcohol in product.
With reference to embodiment to a kind of SnS provided by the invention2-Bi2WO6Compound micron bouquet and preparation method thereof and
Using being described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) flower-shaped SnS2Synthesis：Weigh the SnCl of 0.525g4·5H2O is dissolved in 80mL ethylene glycol, will after dissolving
The thiocarbamide of 0.61g is added thereto, and stirring is to dissolving, and ultrasonic disperse moves in the reaction kettle of 100mL, hydro-thermal under the conditions of 180 DEG C
18h, after reaction cooled to room temperature.Product is washed repeatedly with ethyl alcohol and deionized water respectively, is centrifuged, at 60 DEG C
Oven drying 12h to get petal-shaped SnS2。
(2)SnS2/Bi2WO6Synthesis:Bi (the NO of 0.485g are weighed respectively3)3·5H2The Na of O and 0.16g2WO4·2H2O
It is separately added into and is dispersed with 0.0125mmol SnS280mL ethylene glycol solutions in, stir and ultrasonic disperse it is uniform, it is molten to obtain yellow
Liquid is transferred in 100mL reaction kettles, is heated at 160 DEG C for 24 hours, after reaction cooled to room temperature.
Product is washed repeatedly with ethyl alcohol and deionized water respectively, is realized and is separated by solid-liquid separation, and reaction solid product is obtained, at 60 DEG C
Oven drying 12h, obtain SnS2-Bi2WO6Compound micron bouquet.
To the flower ball-shaped SnS being prepared2And SnS2-Bi2WO6Compound micron bouquet carries out field emission scanning electron microscope point
Analysis, it is as a result as depicted in figs. 1 and 2 respectively.By Fig. 1 and Fig. 2 it is found that the SnS being prepared2With petal chondritic, and
Composites are bouquet structure；It is also known by Fig. 2, Bi2WO6Particle is scattered in sheet SnS2Surface.
Obtained SnS2-Bi2WO6SnS in compound micron bouquet2And Bi2WO6Substance amount ratio be 0.025:1, it uses
SnS2- BW-2.5 is indicated.The SnS that the present invention will obtain2-Bi2WO6Compound micron bouquet and pure Bi2WO6And SnS2It carries out
XRD analysis, from the figure 3, it may be seen that single Bi2WO6XRD diffracting spectrums, all characteristic peaks can be proved that material belongs to orthorhombic system
Bi2WO6, and match with standard card PDF#39-0256, (131), (200), (260), (133) corresponding angle of diffraction difference
For 2 θ=28.3 °, 32.8 °, 47.0 °, 55.9 °；Single SnS2With (001) of standard card PDF#23-0677, (100),
(101), (102), (110), (111), (103), (202), (113) crystal face are consistent, illustrate to successfully synthesize the flower-shaped knot of pure phase
Structure SnS2, the position " ■ " corresponds to SnS in composite material in the diagram of composite material in figure2The position of characteristic peak, it is seen that composite material
In existing Bi2WO6Characteristic peak have SnS again2Characteristic peak, illustrate the composite material being prepared be SnS2-Bi2WO6。
Embodiment 2
Compound micron bouquet is prepared in the way of embodiment 1, difference lies in the present embodiment is according to SnS2And Bi2WO6's
The amount ratio of substance is 0.05：1, control Bi (NO3)3·5H2O and Na2WO4·2H2O and SnS2Dosage, obtained SnS2-
Bi2WO6SnS in compound micron bouquet2And Bi2WO6Substance amount ratio be 0.05:1, use SnS2- BW-5 is indicated.
Embodiment 3
Compound micron bouquet is prepared in the way of embodiment 1, difference lies in the present embodiment is according to SnS2And Bi2WO6's
The amount ratio of substance is 0.1：1, control Bi (NO3)35H2O and Na2WO4·2H2O and SnS2Dosage, obtained SnS2-Bi2WO6
SnS in compound micron bouquet2And Bi2WO6Substance amount ratio be 0.1:1, use SnS2- BW-10 is indicated.
Embodiment 4
Compound micron bouquet is prepared in the way of embodiment 1, difference lies in the present embodiment is according to SnS2And Bi2WO6's
The amount ratio of substance is 0.15：1, control Bi (NO3)3·5H2O and Na2WO4·2H2O and SnS2Dosage, obtained SnS2-
Bi2WO6SnS in compound micron bouquet2And Bi2WO6Substance amount ratio be 0.15:1, use SnS2- BW-15 is indicated.
SnS is prepared to Examples 1 to 42-Bi2WO6The petal that compound micron bouquet and embodiment are prepared is spherical
SnS2And the SnS of petal ball surface2XRD analysis is carried out, the results are shown in Figure 3.From the figure 3, it may be seen that being made under the conditions of different mol ratio
Standby obtained composite material is SnS2-Bi2WO6, the ingredient for forming the laminated structure part of microballoon main body is SnS2。
The flower ball-shaped SnS that embodiment 2~4 is prepared respectively2And SnS2-Bi2WO6Compound micron bouquet carries out field
Emit scanning electron microscope analysis, the SnS that can be clearly prepared2With petal chondritic, and composites are flower
Spherical structure；Bi2WO6Particle is scattered in sheet SnS2Surface.
Embodiment 5：
The SnS that Examples 1 to 4 is prepared2-Bi2WO6Compound micron bouquet, pure Bi2WO6, pure SnS2And SnS2With
Bi2WO6Substance amount ratio be 0.1：1 physical mixture is used for carbon dioxide light-catalyzed reaction respectively as photochemical catalyst.
Light-catalyzed reaction carries out in closed quartz reactor, and temperature control is at 4 DEG C with maintaining reaction temperature.It is reacting
50mL ultra-pure waters and 50mg photochemical catalysts are added in device, it is continuous logical after the gas removed in water is vacuumized under the conditions of magnetic agitation
Enter high-purity CO2Gas (flow 50mL/min) continues after dark reaction half an hour under the 300W Xenon light shinings of wavelength >=420nm
After carrying out light reaction 4h, the content of methanol and ethyl alcohol in product, methanol and alcohol yied such as 1 institute of table of different catalysts are measured
Show：
Under the conditions of the different photochemical catalysts of table 1, the methanol of carbon dioxide light-catalyzed reaction and the yield of ethyl alcohol
As shown in Table 1, the SnS that the present invention is prepared2-Bi2WO6Compound micron bouquet is anti-for carbon dioxide photocatalysis
It answers, methanol yield is above 20 μm of ol/g-Cat, and alcohol yied is above 10 μm of ol/g-Cat；Far above pure SnS2, pure Bi2WO6
And Bi2WO6And SnS2Physical mixture as in carbon dioxide light-catalyzed reaction when catalyst methanol and ethyl alcohol yield.
Wherein, the mensuration mode of the yield of methanol and ethyl alcohol is：The content for measuring methanol and ethyl alcohol in water after light reaction first, further according to
The dosage of catalyst calculates the content of methanol and ethyl alcohol that the catalysis of every gram of catalyst theory generates.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of SnS2-Bi2WO6Compound micron bouquet, including Bi2WO6With the SnS of flower ball-shaped2；The SnS of the flower ball-shaped2By
SnS2Piece self assembly forms, the Bi2WO6It is distributed in the SnS2Piece surface.
2. SnS according to claim 12-Bi2WO6Compound micron bouquet, which is characterized in that the SnS2-Bi2WO6It is compound
The grain size of micron bouquet is 5~6 μm；
The SnS2-Bi2WO6SnS in compound micron bouquet2And Bi2WO6Substance amount ratio be (0.025~0.15)：1.
3. SnS as claimed in claim 1 or 22-Bi2WO6The preparation method of compound micron bouquet, includes the following steps：
(1) butter of tin, thiocarbamide and ethylene glycol are mixed, carries out heating reaction, obtains flower ball-shaped SnS2；
(2) sodium tungstate and bismuth nitrate are added to the flower ball-shaped SnS2Ethylene glycol dispersion liquid in, carry out solvent-thermal process it is anti-
It answers, obtains SnS2-Bi2WO6Compound micron bouquet.
4. preparation method according to claim 3, which is characterized in that the amount of the substance of butter of tin in the step (1),
The amount of the substance of thiocarbamide and the volume ratio of ethylene glycol are 1.5~2mmol：8~10mmol：80mL.
5. preparation method according to claim 3 or 4, which is characterized in that the temperature of heating reaction is in the step (1)
180~200 DEG C, the time for heating reaction is 18~20h.
6. preparation method according to claim 3, which is characterized in that SnS in the step (2)2Ethylene glycol dispersion liquid in
SnS2Substance amount and ethylene glycol volume ratio be (0.0125~0.075) mmol：80mL.
7. preparation method according to claim 6, which is characterized in that the amount and nitre of the substance of sodium tungstate in the step (2)
The amount ratio of the substance of sour bismuth is 0.5~0.6:1；
Sodium tungstate and SnS in the step (2)2Substance amount ratio be 1：(0.025~0.15).
8. the preparation method according to claim 3 or 7, which is characterized in that solvent-thermal process reacts in the step (2)
Temperature be 160~180 DEG C, solvent-thermal process reaction time be 20~for 24 hours.
9. SnS as claimed in claim 1 or 22-Bi2WO6It is prepared described in compound micron bouquet or claim 3~8 any one
SnS made from method2-Bi2WO6Application of the compound micron bouquet as photochemical catalyst in carbon dioxide light-catalyzed reaction.
10. application according to claim 9, which is characterized in that the application includes the following steps：By the SnS2-
Bi2WO6Compound micron bouquet is mixed with water, obtains SnS2-Bi2WO6The aqueous dispersions of compound micron bouquet；Remove the SnS2-
Bi2WO6After gas in the aqueous dispersions of compound micron bouquet, it is passed through CO2Gas is stood under non-illuminated conditions, then in light
Catalysis reaction is carried out according under the conditions of.
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