CN108906085A - A kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material - Google Patents
A kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material Download PDFInfo
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- CN108906085A CN108906085A CN201810784797.7A CN201810784797A CN108906085A CN 108906085 A CN108906085 A CN 108906085A CN 201810784797 A CN201810784797 A CN 201810784797A CN 108906085 A CN108906085 A CN 108906085A
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- composite photocatalyst
- photocatalyst material
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- 239000000463 material Substances 0.000 title claims abstract description 55
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 230000001699 photocatalysis Effects 0.000 claims abstract description 18
- 238000007146 photocatalysis Methods 0.000 claims abstract description 17
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960003431 cetrimonium Drugs 0.000 claims abstract description 7
- RLGQACBPNDBWTB-UHFFFAOYSA-N cetyltrimethylammonium ion Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)C RLGQACBPNDBWTB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 abstract description 6
- 239000000243 solution Substances 0.000 abstract 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 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 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 230000001603 reducing effect Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 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 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010409 thin film Substances 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
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
-
- 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
Abstract
The invention discloses a kind of Bi2S3The preparation method and applications of/BiOBr composite photocatalyst material will be added the ethylene glycol solution of cetrimonium bronmide, synthesize BiOBr material using hydro-thermal reaction in the ethylene glycol solution of polyvinylpyrrolidone and bismuth nitrate；The aqueous solution of thioacetamide is prepared, and is added dropwise in the dispersion liquid of BiOBr material, obtains Bi in room temperature reaction 3h2S3/ BiOBr composite photocatalyst material.Bi in optic catalytic composite material produced by the present invention2S3There is good contact interface with BiOBr, be conducive to the transmission of photo-generated carrier and the raising of separative efficiency, so that photocatalysis performance greatly improves.
Description
Technical field
The invention belongs to the synthesis technical fields of composite photocatalyst material, and in particular to a kind of Bi2S3/ BiOBr complex light is urged
Change the preparation method and applications of material.
Background technique
Nitrogen is the main component of earth atmosphere, and can directly synthesize ammonia as raw material（NH3）.It is traditional by N2
Synthesize NH3Method need high-temperature and high-pressure conditions.Photocatalysis technology utilizes sunlight as the energy, selects suitable photocatalysis
Agent activates N using photon energy2Molecule synthesis NH3It is a kind of environmental-friendly, mild condition synthesis NH3Method.But light
Catalyze and synthesize NH3Efficiency it is also relatively low, therefore seek photocatalyst material be improve photocatalysis nitrogen reduction synthesis ammonia efficiency
Important channel.The band gap width of BiOBr is ~ 2.6eV, has layer structure, provides enough spaces, layer and layer to atom polarization
Between built in field facilitate efficiently separating for carrier, therefore BiOBr is a kind of catalysis of excellent photocatalysis nitrogen reduction
Agent material.However BiOBr is narrow in the absorption region of visible light, can only absorb 450nm visible light below.In order to improve
For BiOBr in the response range of visible region, forming composite photo-catalyst with narrow gap semiconductor is a kind of widely applied method.
Patent if notification number is 104659157B discloses a kind of preparation method of BiOBr/CdS optoelectronic thin film material, and CdS is as light
Sensitive semiconductor can effectively improve service life and transmission and the separative efficiency of photo-generated carrier.
Bismuth sulfide（Bi2S3）Band gap be ~ 1.3eV, can absorbing wavelength be 800nm within visible light, and bismuth sulfide have
There are good stability and photocatalytic activity, be widely used as catalysis material or mentioned with other materials formation composite photo-catalyst
The photocatalysis performance of high composite material.Notification number is that the patent of 103611551B discloses and a kind of prepares Bi2S3/Bi2MoO6 is heterogeneous
The method for tying composite material, Bi2S3Introducing can widen photochemical catalyst to the response range of sunlight, improve to incident light
Capture ability.Bi2S3Compared with CdS, service life and transmission and the separation of the photo-generated carrier of composite photo-catalyst not only can be improved
Efficiency, and Bi2S3With better photostability and environment friendly.Therefore Bi2S3Forming composite material with BiOBr will
It can show excellent photocatalysis nitrogen reducing property.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of simple processes, Bi low in cost and environmental-friendly2S3/
The preparation method of BiOBr composite photocatalyst material, this method synthesize different Bi by the additional amount of control thioacetamide2S3It is negative
The composite photocatalyst material of carrying capacity can preferably be applied to photocatalysis fixed nitrogen and react.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of Bi2S3/ BiOBr composite photocatalyst material
Preparation method, it is characterised in that the specific steps are：
Step S1：By 0.200g polyvinylpyrrolidone（PVP）With 1.455g Bi (NO3)3·5H2O is added to 10mL ethylene glycol
In solution and it is sufficiently mixed and uniformly obtains dispersion liquid A；
Step S2：By 3.280g cetrimonium bronmide（CTAB）It is dissolved in 10mL ethylene glycol and obtains solution B；
Step S3：The dispersion liquid A that step S1 is obtained is mixed with the obtained solution B of step S2 and is placed in autoclave, in
160 DEG C of reaction 30min, cooled to room temperature, is centrifugated after product is taken out, is dried to obtain BiOBr material after reaction
Material；
Step S4：By 10 ~ 40mg thioacetamide（TAA）It is added in 20mL deionized water and dissolution is sufficiently stirred and obtain solution
C；
Step S5：The BiOBr material that step S3 is obtained is dispersed in 20mL deionized water and obtains dispersion liquid D, by step
The solution C that S4 is obtained is added dropwise in dispersion liquid D, in room temperature reaction 3h, is dried to obtain Bi after centrifuge separation2S3/ BiOBr is multiple
Light combination catalysis material.
Bi produced by the present invention2S3/ BiOBr composite photocatalyst material is used for photocatalysis as photocatalysis nitrogen reducing catalyst
Fixed nitrogen reaction.
The present invention has the advantages that compared with prior art：
1, Bi produced by the present invention2S3The preparation process of/BiOBr composite photocatalyst material is simple, energy consumption is lower, it is low in cost and
It is environmental-friendly；
2, Bi produced by the present invention2S3/ BiOBr composite photocatalyst material can be urged as photocatalysis nitrogen reducing catalyst for light
Change fixed nitrogen reaction, compared with BiOBr, the photocatalysis performance of composite photocatalyst material is significantly improved；
3, the present invention synthesizes Bi using ion-exchange2S3/ BiOBr composite photocatalyst material, is conducive to Bi2S3Between BiOBr
Form good contact interface, be conducive to the transmission of photo-generated carrier, effectively improve photo-generated carrier service life and transmission and point
From efficiency, and then improve photocatalysis performance.
Detailed description of the invention
Fig. 1 is BiOBr made from embodiment 1-4 and Bi2S3The scanning electron microscope (SEM) photograph of/BiOBr composite photocatalyst material, from figure
In it can be seen that BiOBr and Bi2S3/ BiOBr composite photocatalyst material is the aggregation of laminated structure, and Bi2S3Modify it
Afterwards, there is no significant changes for the pattern of composite photocatalyst material；
Fig. 2 is Bi made from embodiment 32S3The transmission electron microscope picture of/BiOBr composite photocatalyst material, spacing of lattice in figure
0.279nm and 0.22nm respectively correspond BiOBr（110）And Bi2S3（141）Crystal face；
Fig. 3 is BiOBr made from embodiment 1-4 and Bi2S3The X-ray diffracting spectrum of/BiOBr composite photocatalyst material, by scheming
Know the increase with thioacetamide dosage, Bi in diffracting spectrum2S3Diffraction maximum gradually increase；
Fig. 4 is BiOBr made from embodiment 1-4 and Bi2S3The optical absorption spectra of/BiOBr composite photocatalyst material, as seen from the figure
Bi2S3/ BiOBr composite photocatalyst material is remarkably reinforced compared with BiOBr in the absorption of visible region；
Fig. 5 is BiOBr made from embodiment 1-4 and Bi2S3The photocatalysis nitrogen reducing property of/BiOBr composite photocatalyst material is bent
Line, as seen from the figure Bi2S3/ BiOBr composite photocatalyst material is compared with BiOBr, NH3Yield dramatically increase, illustrate Bi2S3/
BiOBr composite photocatalyst material has better photocatalysis nitrogen reduction activation.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Step S1：By 0.200g polyvinylpyrrolidone and 1.455g Bi (NO3)3·5H2O is added in 10mL ethylene glycol solution
And it is sufficiently mixed and uniformly obtains dispersion liquid A；
Step S2：3.280g cetrimonium bronmide is dissolved in 10mL ethylene glycol and obtains solution B；
Step S3：The dispersion liquid A that step S1 is obtained is mixed with the obtained solution B of step S2 and is placed in autoclave, in
160 DEG C of reaction 30min, cooled to room temperature, is centrifugated after product is taken out, is dried to obtain BiOBr material after reaction
Material.
Embodiment 2
Step S1：By 0.200g polyvinylpyrrolidone and 1.455g Bi (NO3)3·5H2O is added in 10mL ethylene glycol solution
And it is sufficiently mixed and uniformly obtains dispersion liquid A；
Step S2：3.280g cetrimonium bronmide is dissolved in 10mL ethylene glycol and obtains solution B；
Step S3：The dispersion liquid A that step S1 is obtained is mixed with the obtained solution B of step S2 and is placed in autoclave, in
160 DEG C of reaction 30min, cooled to room temperature, is centrifugated after product is taken out, is dried to obtain BiOBr material after reaction
Material；
Step S4：10mg thioacetamide is added in 20mL deionized water and dissolution is sufficiently stirred and obtains solution C；
Step S5：The BiOBr material that step S3 is obtained is dispersed in 20mL deionized water and obtains dispersion liquid D, by step
The solution C that S4 is obtained is added dropwise in dispersion liquid D, in room temperature reaction 3h, is dried to obtain Bi after centrifuge separation2S3/ BiOBr is multiple
Light combination catalysis material.
Embodiment 3
Step S1：By 0.200g polyvinylpyrrolidone and 1.455g Bi (NO3)3·5H2O is added in 10mL ethylene glycol solution
And it is sufficiently mixed and uniformly obtains dispersion liquid A；
Step S2：3.280g cetrimonium bronmide is dissolved in 10mL ethylene glycol and obtains solution B；
Step S3：The dispersion liquid A that step S1 is obtained is mixed with the obtained solution B of step S2 and is placed in autoclave, in
160 DEG C of reaction 30min, cooled to room temperature, is centrifugated after product is taken out, is dried to obtain BiOBr material after reaction
Material；
Step S4：20mg thioacetamide is added in 20mL deionized water and dissolution is sufficiently stirred and obtains solution C；
Step S5：The BiOBr material that step S3 is obtained is dispersed in 20mL deionized water and obtains dispersion liquid D, by step
The solution C that S4 is obtained is added dropwise in dispersion liquid D, in room temperature reaction 3h, is dried to obtain Bi after centrifuge separation2S3/ BiOBr is multiple
Light combination catalysis material.
Embodiment 4
Step S1：By 0.200g polyvinylpyrrolidone and 1.455g Bi (NO3)3·5H2O is added in 10mL ethylene glycol solution
And it is sufficiently mixed and uniformly obtains dispersion liquid A；
Step S2：3.280g cetrimonium bronmide is dissolved in 10mL ethylene glycol and obtains solution B；
Step S3：The dispersion liquid A that step S1 is obtained is mixed with the obtained solution B of step S2 and is placed in autoclave, in
160 DEG C of reaction 30min, cooled to room temperature, is centrifugated after product is taken out, is dried to obtain BiOBr material after reaction
Material；
Step S4：40mg thioacetamide is added in 20mL deionized water and dissolution is sufficiently stirred and obtains solution C；
Step S5：The BiOBr material that step S3 is obtained is dispersed in 20mL deionized water and obtains dispersion liquid D, by step
The solution C that S4 is obtained is added dropwise in dispersion liquid D, in room temperature reaction 3h, is dried to obtain Bi after centrifuge separation2S3/ BiOBr is multiple
Light combination catalysis material.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. a kind of Bi2S3The preparation method of/BiOBr composite photocatalyst material, it is characterised in that the specific steps are：
Step S1：By 0.200g polyvinylpyrrolidone and 1.455g Bi (NO3)3·5H2O is added in 10mL ethylene glycol solution
And it is sufficiently mixed and uniformly obtains dispersion liquid A；
Step S2：3.280g cetrimonium bronmide is dissolved in 10mL ethylene glycol and obtains solution B；
Step S3：The dispersion liquid A that step S1 is obtained is mixed with the obtained solution B of step S2 and is placed in autoclave, in
160 DEG C of reaction 30min, cooled to room temperature, is centrifugated after product is taken out, is dried to obtain BiOBr material after reaction
Material；
Step S4：10 ~ 40mg thioacetamide is added in 20mL deionized water and dissolution is sufficiently stirred and obtains solution C；
Step S5：The BiOBr material that step S3 is obtained is dispersed in 20mL deionized water and obtains dispersion liquid D, by step
The solution C that S4 is obtained is added dropwise in dispersion liquid D, in room temperature reaction 3h, is dried to obtain Bi after centrifuge separation2S3/ BiOBr is multiple
Light combination catalysis material.
2. Bi made from the method according to claim 112S3/ BiOBr composite photocatalyst material is urged as the reduction of photocatalysis nitrogen
Agent is reacted for photocatalysis fixed nitrogen.
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| CN110252350A (en) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | Bi2O2SiO3/Si2Bi24O40The preparation of/BiOBr double heterojunction composite photo-catalyst |
| CN112098492A (en) * | 2020-09-11 | 2020-12-18 | 江西师范大学 | Method for photoelectrochemical detection of organophosphorus pesticide by bismuth oxybromide/bismuth sulfide semiconductor heterojunction based on biological induction generation |
| CN112391651A (en) * | 2020-09-18 | 2021-02-23 | 厦门大学 | BiOBr/TiO containing oxygen vacancies2Nanotube array composite electrode, preparation method thereof and application of nanotube array composite electrode in photoelectrocatalysis nitrogen fixation |
| CN115739120A (en) * | 2022-11-08 | 2023-03-07 | 昆明理工大学 | Heterojunction photocatalyst integrating full-spectrum response and photothermal effect and preparation and application thereof |
| CN116586083A (en) * | 2023-07-03 | 2023-08-15 | 辽宁大学 | Mo-doped BiOBr photocatalyst rich in oxygen vacancies and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110252350A (en) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | Bi2O2SiO3/Si2Bi24O40The preparation of/BiOBr double heterojunction composite photo-catalyst |
| CN110252350B (en) * | 2019-06-18 | 2021-09-14 | 陕西科技大学 | Bi2O2SiO3/Si2Bi24O40Preparation of BiOBr double-heterojunction composite photocatalyst |
| CN112098492A (en) * | 2020-09-11 | 2020-12-18 | 江西师范大学 | Method for photoelectrochemical detection of organophosphorus pesticide by bismuth oxybromide/bismuth sulfide semiconductor heterojunction based on biological induction generation |
| CN112098492B (en) * | 2020-09-11 | 2022-09-16 | 江西师范大学 | Method for photoelectrochemical detection of organophosphorus pesticide by bismuth oxybromide/bismuth sulfide semiconductor heterojunction based on biological induction generation |
| CN112391651A (en) * | 2020-09-18 | 2021-02-23 | 厦门大学 | BiOBr/TiO containing oxygen vacancies2Nanotube array composite electrode, preparation method thereof and application of nanotube array composite electrode in photoelectrocatalysis nitrogen fixation |
| CN112391651B (en) * | 2020-09-18 | 2021-10-26 | 厦门大学 | BiOBr/TiO containing oxygen vacancies2Nanotube array composite electrode, preparation method thereof and application of nanotube array composite electrode in photoelectrocatalysis nitrogen fixation |
| CN115739120A (en) * | 2022-11-08 | 2023-03-07 | 昆明理工大学 | Heterojunction photocatalyst integrating full-spectrum response and photothermal effect and preparation and application thereof |
| CN116586083A (en) * | 2023-07-03 | 2023-08-15 | 辽宁大学 | Mo-doped BiOBr photocatalyst rich in oxygen vacancies and preparation method and application thereof |
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Application publication date: 20181130 |