CN106378158A - Preparation method of bismuth sulfide/titanium dioxide/graphene compound with high-catalysis degradation activity under visible light - Google Patents
Preparation method of bismuth sulfide/titanium dioxide/graphene compound with high-catalysis degradation activity under visible light Download PDFInfo
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- CN106378158A CN106378158A CN201610994086.3A CN201610994086A CN106378158A CN 106378158 A CN106378158 A CN 106378158A CN 201610994086 A CN201610994086 A CN 201610994086A CN 106378158 A CN106378158 A CN 106378158A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 215
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 80
- -1 graphene compound Chemical class 0.000 title claims abstract description 67
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 58
- 230000015556 catabolic process Effects 0.000 title claims abstract description 54
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 54
- 230000000694 effects Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006555 catalytic reaction Methods 0.000 title abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 claims abstract description 36
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000000725 suspension Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 230000001699 photocatalysis Effects 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 230000003197 catalytic effect Effects 0.000 claims description 19
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 14
- 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 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 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
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 3
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 1
- 239000011941 photocatalyst Substances 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 abstract 1
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- 238000007146 photocatalysis Methods 0.000 description 12
- 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 11
- 238000002835 absorbance Methods 0.000 description 11
- 239000007864 aqueous solution Substances 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 11
- 238000005119 centrifugation Methods 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 11
- 229960000907 methylthioninium chloride Drugs 0.000 description 11
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 239000006228 supernatant Substances 0.000 description 11
- 238000003786 synthesis reaction Methods 0.000 description 11
- 239000002253 acid Substances 0.000 description 10
- 239000004575 stone Substances 0.000 description 10
- 238000010792 warming Methods 0.000 description 10
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 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
-
- B01J35/39—
Abstract
The invention provides a preparation method of a bismuth sulfide/titanium dioxide/graphene compound with high-catalysis degradation activity under visible light and belongs to the technical field of preparation of photocatalysts. According to the preparation method, tetrabutyl titanate and graphene oxide are used as raw materials, and bismuth nitrate pentahydrate and sodium sulfide nonahydrate are used as bismuth sulfide raw materials; the raw materials are subjected to solvent thermal and calcination treatment; finally, the bismuth sulfide/titanium dioxide/graphene compound is obtained. According to the synthesized bismuth sulfide/titanium dioxide/graphene compound, an adsorption capability on organic pollutants is enhanced, and the compound has a relatively high absorption capability on the visible light; the service life of an electron-hole pair can be prolonged; the catalysis degradation capability on the organic pollutants is enhanced and the degradation rate is 2.93 times as much as that of TiO2 nanoparticles and is 1.42 times as much as that of bismuth sulfide/TiO2, so that the bismuth sulfide/titanium dioxide/graphene compound has a relatively high actual application value.
Description
Technical field
The present invention relates to a kind of bismuth sulfide/titanium dioxide/graphene under visible light with high catalytic degradation activity is multiple
The preparation method of compound, belongs to the technical field of photochemical catalyst preparation.
Background technology
In catalysis and energy related field, TiO2Paid close attention to by a lot of scientists quickly.TiO2Unique electron energy band knot
Structure and excellent surface-active give it and are producing hydrogen, photovoltaic, catalyst, lithium ion battery, fuel cell, gas sensor, solution
The fields such as poison, ultracapacitor are widely used however, TiO2Relatively small charge transport capability and broad-band gap (～3.2eV)
It is two principal elements limiting its application.In order to overcome these problems to take a lot of measures, such as with other semiconductors, metal
Nonmetal doping and material with carbon element are combined (RSC Advances, 2014,4,1120-1127) etc. so as to expand to light absorbs to can
The life-span seen light region and extend photo-generate electron-hole pair.
Graphene (Graphene) be a kind of by carbon atom with sp2Hybridized orbit forms the plane that hexangle type is in honeycomb lattice
Film, the two-dimensional material of only one of which carbon atom thickness, there are excellent electrical, thermal and mechanical properties, conduct in inorganic composite
A kind of backing material and electro transfer medium, are applied to the different field such as electro-catalysis, super capacitor, hydrogen deposit and photovoltaic apparatus.
Recently, numerous studies show, have and can be TiO compared with the Graphene of Large ratio surface2The supporter of nano material.With original TiO2Phase
Ratio TiO2With Graphene compound increased the absorption to pollutant, extend photo-absorption region, improve carrier separation and
Transfer efficiency (Applied Catalysis, B:Environmental, 2014,144,893-899), so substantially increase it
Photocatalysis performance.
Additionally, by with semiconductor combine to form heterojunction structure it is also possible to increase absorption to visible ray, suppress photoproduction
Being combined of electron-hole pair, makes TiO2The photocatalytic activity of/graphene complex is strengthened further.Than if any research
(Journal of Physical Chemistry C, 2013,40,20406-20414) reports CdS composite Ti O2Nanometer
Grain can effectively improve TiO with the compound of Graphene2Photocatalytic activity, be applied to complexity optoelectronic pole, solar cell, hydrogen manufacturing
In field.Based on this background, the present invention has synthesized a kind of bismuth sulfide/titanium dioxide under visible light with high catalytic degradation activity
Titanium/graphene complex photochemical catalyst.
Content of the invention
The purpose of the present invention：Modified and be combined three kinds of method of modifying to original with Graphene in conjunction with semiconductors coupling, pattern
TiO2Carry out deep modification, it both can have been made light absorbs to be expanded to visible region, increased catalytic effect under visible ray；Can make again
TiO2It is in granular form and is dispersed on graphene layer, reduce and reunite, increase catalytic effect；The suction to pollutant also can be increased
Receive, improve carrier separation and transfer efficiency, finally prepare and there is to organic pollution high catalytic degradation under visible light
The photochemical catalyst of activity.
Technical scheme：A kind of bismuth sulfide/titanium dioxide/stone under visible light with high catalytic degradation activity
The preparation method of black alkene compound.Follow the steps below：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature graphene oxide is dissolved in
Continuously stir in 60mL absolute ethyl alcohol, ultrasonic disperse, stirring is lower to add 0.0227g five water bismuth nitrate and the sulfuration of 0.0186g nine water
Sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to butyl titanate to above-mentioned suspension, and
Drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to containing polytetrafluoroethyl-ne after obtaining uniform suspension
Carry out solvent thermal reaction in the high-pressure hydrothermal reaction kettle of alkene liner, reaction naturally cools to room temperature after terminating, the product obtaining according to
Secondary deionized water, absolute ethyl alcohol respectively wash 3 times, and the sample being centrifugally separating to obtain is dried 8h at 80 DEG C, under nitrogen atmosphere
Heated up with 4 DEG C/min heating rate and calcine, finally give bismuth sulfide/titanium dioxide/graphene compound.In order to contrast, use class
As method synthesized TiO2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 85%～198% and 28%～74%.
In above-mentioned steps (1), the amount of graphene oxide is 10～200mg；The graphene oxide ultrasonic disperse time be 0.5～
10h；The addition of butyl titanate is 4～8mL；Solvent thermal reaction temperature is 160～200 DEG C, and the solvent thermal reaction time is 18
～30h；Calcining heat is 450～600 DEG C, and calcination time is 2～6h.
The present invention adopts easy method, has first synthesized through calcination processing through solvent heat again and has had height under visible light and urge
Change the bismuth sulfide/titanium dioxide/graphene compound photochemical catalyst of activity.Result shows, bismuth sulfide/TiO2Can be in granular form all
Even be distributed in graphene layer surface, reduce TiO2Reunion on graphene layer, enhances TiO2Phase interaction between Graphene
With improve photocatalytic activity.
The technological merit of the present invention：Bismuth sulfide/titanium dioxide/graphene compound passes through solvent heat one-step synthesis method, then
Through calcination processing, method is simple；The synergy being combined with Graphene by bismuth sulfide, reduces TiO2Band gap, improve
Its adsorption capacity to organic pollution, enhances the utilization rate to visible ray, reduces photo-generate electron-hole to being combined
Rate, extends the life-span of carrier；Bismuth sulfide/TiO simultaneously2Nano particle uniformly adheres on Graphene, greatly reduces
TiO2Reunite, improve the chemical action and between Graphene, degraded has in visible region thus drastically increasing compound
The ability of organic pollutants.
Specific embodiment
Example below can make those skilled in the art be fully understood by the present invention, but limits this never in any form
Bright.
Embodiment 1：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 10mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 0.5h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g
Nine water vulcanized sodium, continue stirring 30min and obtain homodisperse suspension；Then, it is slowly added to 4mL metatitanic acid to above-mentioned suspension
Four butyl esters, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension
In high-pressure hydrothermal reaction kettle containing teflon-lined, 160 DEG C carry out solvent thermal reaction 18h, and reaction naturally cools to after terminating
Room temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dry at 80 DEG C
Dry 8h, under nitrogen atmosphere with 4 DEG C/min heating rate be warming up to 450 DEG C calcining 2h, finally give bismuth sulfide/titanium dioxide/
Graphene complex.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 103% and 49%.
Embodiment 2：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 10mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 4h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 6mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 180 DEG C carry out solvent thermal reaction 20h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 500 DEG C of calcining 4h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 99% and 45%.
Embodiment 3：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 60mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 1h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 4mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 200 DEG C carry out solvent thermal reaction 30h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 600 DEG C of calcining 6h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 98% and 47%.
Embodiment 4：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 60mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 10h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 8mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 160 DEG C carry out solvent thermal reaction 24h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 500 DEG C of calcining 3h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 195% and 69%.
Embodiment 5：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 100mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 6h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 6mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 180 DEG C carry out solvent thermal reaction 30h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 450 DEG C of calcining 3h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 112% and 48%.
Embodiment 6：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 100mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 1h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 8mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 200 DEG C carry out solvent thermal reaction 20h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 600 DEG C of calcining 4h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 142% and 64%.
Embodiment 7：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 150mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 6h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 6mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 160 DEG C carry out solvent thermal reaction 26h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 450 DEG C of calcining 4h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 105% and 50%.
Embodiment 8：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 150mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 0.5h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g
Nine water vulcanized sodium, continue stirring 30min and obtain homodisperse suspension；Then, it is slowly added to 4mL metatitanic acid to above-mentioned suspension
Four butyl esters, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension
In high-pressure hydrothermal reaction kettle containing teflon-lined, 180 DEG C carry out solvent thermal reaction 24h, and reaction naturally cools to after terminating
Room temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dry at 80 DEG C
Dry 8h, under nitrogen atmosphere with 4 DEG C/min heating rate be warming up to 500 DEG C calcining 2h, finally give bismuth sulfide/titanium dioxide/
Graphene complex.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 85% and 28%.
Embodiment 9：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 200mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 4h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 8mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 160 DEG C carry out solvent thermal reaction 26h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 600 DEG C of calcining 3h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 111% and 49%.
Embodiment 10：
(1) synthesis of bismuth sulfide/titanium dioxide/graphene compound：At ambient temperature will be molten for 200mL graphene oxide
Solution continuously stirs in 60mL absolute ethyl alcohol, ultrasonic disperse 10h, and stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine
Water vulcanized sodium, continues stirring 30min and obtains homodisperse suspension；Then, it is slowly added to 6mL metatitanic acid four to above-mentioned suspension
Butyl ester, and drip 10mL water under conditions of continuously stirring, continue stirring 1h；Stirring is transferred to after obtaining uniform suspension and contains
In teflon-lined high-pressure hydrothermal reaction kettle, 200 DEG C carry out solvent thermal reaction 24h, and reaction naturally cools to room after terminating
Temperature, deionized water, absolute ethyl alcohol respectively wash 3 times the product obtaining successively, and the sample being centrifugally separating to obtain is dried at 80 DEG C
8h, is warming up to 450 DEG C of calcining 6h with 4 DEG C/min heating rate under nitrogen atmosphere, finally gives bismuth sulfide/titanium dioxide/stone
Black alkene compound.In order to contrast, synthesize TiO with similar method2Nano particle and bismuth sulfide/TiO2.
(2) bismuth sulfide/titanium dioxide/graphene compound light degradation organic pollution：By above-mentioned made 100mg photocatalysis
Agent is added in the aqueous solution of methylene blue that 500mL concentration is 10mg/L, and stirring 60min is carried out under visible ray in the dark
Photocatalytic degradation is tested, and the light degradation time continues 90min, during every 30min pipette 5mL solution, after centrifugation, supernatant is entered
Row absorbance measuring is to calculate degradation effect.With same method to TiO2Nano particle and bismuth sulfide/TiO2Carry out catalytic degradation
Effect detection.Result shows, compares TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/titanium dioxide/graphene compound
Photocatalytic activity has been respectively increased 114% and 52%.
Claims (9)
1. a kind of preparation method of the bismuth sulfide/titanium dioxide/graphene compound under visible light with high catalytic degradation activity, its
It is characterised by following the steps below：At ambient temperature graphene oxide is dissolved in 60mL absolute ethyl alcohol and continuously stirs
Mix, ultrasonic disperse, stirring is lower to add 0.0227g five water bismuth nitrate and 0.0186g nine water vulcanized sodium, continues stirring 30min and obtains
Homodisperse suspension；Then, it is slowly added to butyl titanate to above-mentioned suspension, and drip under conditions of continuously stirring
10mL water, continues stirring 1h；Stirring is transferred to the hydro-thermal reaction of high pressure containing teflon-lined after obtaining uniform suspension
Carry out solvent thermal reaction, reaction naturally cools to room temperature after terminating, the product obtaining deionized water, absolute ethyl alcohol successively in kettle
Respectively washing 3 times, the sample being centrifugally separating to obtain is dried 8h at 80 DEG C, is heated up with 4 DEG C/min heating rate under nitrogen atmosphere
Calcining, finally gives bismuth sulfide/titanium dioxide/graphene compound.
2. method according to claim 1, the consumption of graphene oxide is 10～200mg.
3. method according to claim 1, the graphene oxide ultrasonic disperse time is 0.5～10h.
4. method according to claim 1, the addition of butyl titanate is 4～8mL.
5. method according to claim 1, solvent thermal reaction temperature is 160～200 DEG C, the solvent thermal reaction time is 18～
30h.
6. method according to claim 1, calcining heat is 450～600 DEG C, and calcination time is 2～6h.
7. according to claim 1 method it is characterised in that the preparation method of compound employs a step solvent-thermal method, process
Simply.
8. according to claim 1 method it is characterised in that in described bismuth sulfide/titanium dioxide/graphene compound
Bismuth sulfide composite Ti O2It is in granular form, and can be evenly distributed on graphene layer.
9. according to claim 1 method it is characterised in that comparing TiO2Nano particle and bismuth sulfide/TiO2, bismuth sulfide/bis-
The photocatalytic activity of titanium oxide/graphene complex has been respectively increased 85%～198% and 28%～74%.
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| CN107930617A (en) * | 2017-11-29 | 2018-04-20 | 江南大学 | A kind of witch culture TiO with high catalytic degradation activity2The preparation method of/graphene complex |
| CN107930616A (en) * | 2017-11-29 | 2018-04-20 | 江南大学 | A kind of preparation method of the molybdenum trioxide with high catalytic degradation activity/titanium dioxide/graphene compound |
| CN108144599A (en) * | 2017-12-25 | 2018-06-12 | 李雪琴 | A kind for the treatment of process of bismuthino composite photocatalyst for degrading dyeing waste water |
| CN109608055A (en) * | 2018-12-29 | 2019-04-12 | 河南科技大学 | A kind of titanium dioxide nano-rod film and preparation method thereof of bismuth sulfide sensitization |
| CN111420685A (en) * | 2019-01-10 | 2020-07-17 | 欧阳峰 | FSBi-doped TiO for efficiently degrading acrylonitrile wastewater by sunlight catalysis2/SiO2Preparation and use of the catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107930617A (en) * | 2017-11-29 | 2018-04-20 | 江南大学 | A kind of witch culture TiO with high catalytic degradation activity2The preparation method of/graphene complex |
| CN107930616A (en) * | 2017-11-29 | 2018-04-20 | 江南大学 | A kind of preparation method of the molybdenum trioxide with high catalytic degradation activity/titanium dioxide/graphene compound |
| CN108144599A (en) * | 2017-12-25 | 2018-06-12 | 李雪琴 | A kind for the treatment of process of bismuthino composite photocatalyst for degrading dyeing waste water |
| CN109608055A (en) * | 2018-12-29 | 2019-04-12 | 河南科技大学 | A kind of titanium dioxide nano-rod film and preparation method thereof of bismuth sulfide sensitization |
| CN109608055B (en) * | 2018-12-29 | 2021-08-20 | 河南科技大学 | Bismuth sulfide sensitized titanium dioxide nanorod film and preparation method thereof |
| CN111420685A (en) * | 2019-01-10 | 2020-07-17 | 欧阳峰 | FSBi-doped TiO for efficiently degrading acrylonitrile wastewater by sunlight catalysis2/SiO2Preparation and use of the catalyst |
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