CN107983373A - Method for rapidly preparing carbon-supported BiOBr visible-light-driven photocatalyst in situ by microwave - Google Patents
Method for rapidly preparing carbon-supported BiOBr visible-light-driven photocatalyst in situ by microwave Download PDFInfo
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 183
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 4
- 150000001621 bismuth Chemical class 0.000 claims abstract description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002270 dispersing agent Substances 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 239000003610 charcoal Substances 0.000 claims description 12
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000007792 addition Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 125000001246 bromo group Chemical group Br* 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 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 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 13
- 229940012189 methyl orange Drugs 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000013019 agitation Methods 0.000 description 6
- 239000003755 preservative agent Substances 0.000 description 6
- 230000002335 preservative effect Effects 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 230000004913 activation Effects 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 238000001179 sorption measurement Methods 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
- FOQHYNYNHYNUIN-UHFFFAOYSA-N [O].[Br] Chemical compound [O].[Br] FOQHYNYNHYNUIN-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 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
- 238000004042 decolorization Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Catalysts (AREA)
Abstract
A method for rapidly preparing a carbon-supported BiOBr visible-light-driven photocatalyst in situ by microwaves belongs to the technical field of preparation of photocatalyst materials. Bismuth nitrate pentahydrate is used as a bismuth source, potassium bromide is used as a bromine source, Activated Carbon (AC) is used as a load, deionized water is used as a dispersing agent, and BiOBr is synthesized in situ by hydrolyzing bismuth salt in pores and on the surface of the activated carbon by a microwave method to obtain the carbon-loaded BiOBr visible light catalyst. Firstly, putting activated carbon particles into a clean container, adding a proper amount of deionized water, and stirring to uniformly disperse the activated carbon particles; then adding bismuth nitrate pentahydrate and potassium bromide into the dispersion liquid, stirring uniformly, and then putting into a microwave oven for reaction; and after the reaction is finished, filtering, washing and drying the product. The BiOBr/AC composite material has good visible light catalytic effect and can be applied to the field of organic dye sewage treatment. The invention has the advantages of less raw materials and equipment required in the preparation process, simple operation process and low production cost.
Description
Technical field
The present invention relates to a kind of method that microwave in-situ quickly prepares charcoal load BiOBr visible light catalysts, belong to light and urge
Agent technical field of material.
Background technology
Compared to TiO2, energy gap of the BiOX photocatalyst with smaller can be to the light in larger wave-length coverage
Response is produced, there is larger photocatalytic activity.Though BiOX is considered as high catalytic activity, has response in visible region
Novel photocatalysis semi-conducting material, but its energy gap cannot still reach ideal scope, therefore, in order to effectively improve halogen
The photocatalytic activity of bismuth oxide BiOX (X=Cl, Br, I), using such as semiconductors coupling, noble metal decorated, ion doping, bears
The means such as load improve its photocatalytic activity.
Fabricated in situ is a kind of novel method for synthesizing, i.e., reactant molecule or ion are in carrier duct or surface is touched
Hit and carry out reaction synthesising target compound, which causes reaction to be limited in duct or carried out on surface without that can make over long distances
Movement.In-situ method essence is that compound raw material is not previously prepared compound again, but during compound each
Generation, has the characteristics that synthesis technique is simple, two-phase is compound uniform.
The present invention is loaded using activated carbon, with the microwave heating loading BiOBr of fabricated in situ carbon, and uses methyl
Orange makees degraded substrate, lives to study the photocatalysis of different loads amount (0,10%, 20%, 30%) In-situ BiOBr/AC materials
Property, and using the means such as scanning electron microscope, X-ray diffractometer and uv-visible absorption spectra to different loads amount (0,
10%th, 20%, the configuration of surface of the loading BiOBr of In-situ carbon 30%), crystal plane structure, optical absorption characteristics etc. carry out table
Sign and analysis.
The content of the invention
The present invention is directed to the shortcoming in the presence of the prior art, there is provided a kind of preparation principle is novel, it is easy to operate, into
The microwave in-situ that this is cheap, performance is controllable, can produce in batches quickly prepares the side of charcoal load BiOBr visible light catalysts
Method.
To achieve these goals, the technical solution adopted in the present invention is：A kind of microwave in-situ quickly prepares charcoal load
The method of BiOBr visible light catalysts, is bromine source by bismuth source, potassium bromide of five water bismuth nitrates, is loaded with activated carbon (AC),
Deionized water is dispersant, hydrolyzes fabricated in situ BiOBr by bismuth salt in activated carbon capillary and on surface using microwave method, obtains
Obtain charcoal load BiOBr visible light catalysts.
As the optimal technical scheme of preparation method of the present invention, concretely comprise the following steps：Active carbon particle is placed in cleaning first
Container in, add appropriate amount of deionized water, stirring make active carbon particle dispersed；Then five water bismuth nitrates and potassium bromide are added
Enter in dispersion liquid, be put into micro-wave oven and reacted after stirring evenly；Product is filtered after reaction, wash, drying obtains
Charcoal loads BiOBr visible light catalysts.
As the optimal technical scheme of preparation method of the present invention, active carbon particle passes through following steps pre-treatment：
A certain amount of activated carbon is taken, twice is washed with cold water first and is filtered, is then added in round-bottomed flask,
It is heated to reflux in dilute hydrochloric acid, to remove the impurity in activated carbon, then repeatedly washs with distilled water suction filtration until filtrate is in neutrality, most
Dry in an oven afterwards.
As the optimal technical scheme of preparation method of the present invention, BiOBr load capacity is the BiOBr generated with hydrolysis
Quality with addition activated carbon (AC) mass ratio represent, BiOBr load capacity be 0~30%, preferably 5%, 10%,
15%th, 25%, 30%, most preferably 20%.
As the optimal technical scheme of preparation method of the present invention, the molar ratio between five water bismuth nitrates and potassium bromide is 1:1.
Microwave reaction condition is：Low fire, reaction 10~30 minutes.Product utilizes deionized water and anhydrous after filtering after reaction
Ethanol alternately washs, and then dries.Drying temperature is 40~80 DEG C, when drying time is 5~15 small.
Compared with prior art, the present invention has the following advantages：
1) BiOBr/AC composite materials prepared by the present invention have good visible light catalytic effect, can be applied to organic
Dye wastewater process field.
2) the present invention required raw material and equipment in preparation process is all less, and operating procedure is simple, and production cost is low.
Brief description of the drawings
Fig. 1 is the XRD spectra of activated carbon, BiOBr and different loads amount BiOBr/AC；
Fig. 2 a are the FE-SEM figures of activated carbon raw material used in embodiment 1；
The FE-SEM figures that Fig. 2 b are gained 10%BiOBr/AC in embodiment 1；
The FE-SEM figures that Fig. 2 c are gained 20%BiOBr/AC in embodiment 1；
The FE-SEM figures that Fig. 2 d are gained 30%BiOBr/AC in embodiment 1；
Fig. 3 is different loads amount BiOBr/AC and activated carbon at different moments to the degradation rate curve of methyl orange.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Structure, pattern and the photocatalysis performance of the method for the present invention products therefrom are characterized, and select x-ray powder to spread out respectively
(XRD), field emission scanning electron microscope (FE-SEM) and ultraviolet-visible spectrometer (UV-Vis.) are penetrated, using simulation methyl
Orange aqueous solution carries out the photocatalysis performance analysis of product.
Embodiment 1：The preparation and representation of activated carbon supported catalyst
BiOBr/AC is prepared using the method for In-situ fabricated in situ, BiOBr load capacity is to react generated BiOBr
Quality and AC mass ratio represent.The method for preparing the BiOBr/AC of 10% load capacity is specific as follows：
(1) a certain amount of activated carbon is taken, twice is washed with cold water first and is filtered, be then added to round-bottomed flask
In, be heated to reflux in dilute hydrochloric acid 10 it is small when or so, to remove the ZnCl in activated carbon2Repeatedly washed Deng impurity, then with distilled water
Suction filtration is washed until filtrate is in neutrality, when finally drying 4 is small at 120 DEG C in an oven.
(2) active carbon particles of the 1.0160g after hydrochloric acid activation is weighed in clean small beaker with assay balance, use
100mL graduated cylinders measure the homemade deionized waters of 50mL, through magnetic agitation so that active carbon particle is dispersed in deionized water
In.According still further to molar ratio 1：1 KBr for weighing five water bismuth nitrates of 0.1455g and 0.0357g respectively is added to activated carbon and water at the same time
In suspension, magnetic agitation 8h, makes uniformly to mix between reactant, takes out stirrer with clean tweezers, is sealed with preservative film,
And several apertures are opened on preservative film, and it is put into heating in micro-wave oven and is reacted, microwave reaction condition：Low fire, time are 20 points
Clock.
(3) after reaction, the insoluble solid product of grey black is obtained, suction filtration behaviour is carried out after cooled to room temperature
Make, carry out repeatedly washing with deionized water and absolute ethyl alcohol to remove some foreign ions.Finally by products therefrom 10%
BiOBr/AC is put in small beaker together with filter paper, is put in thermostatic drying chamber at a temperature of 60 DEG C to pack after 10h and is collected.
20%th, the preparation method of 30% load capacity BiOBr/AC is same as above, and is differed only in five water bismuth nitrates and KBr respectively
Usage amount increase by 100%, 200%.
The structure and form of the product obtained respectively to above-mentioned condition using X diffractometers and scanning electron microscope are carried out
Preliminary characterization.Fig. 1 is the XRD spectra (a) of activated carbon, BiOBr and different loads amount BiOBr/AC：AC, (b)：10%BiOBr/
AC, (c)：20%BiOBr/AC, (d)：30%BiOBr/AC, (e)：BiOBr.Fig. 2 a are the FE-SEM of activated carbon raw material used
Figure；Fig. 2 b~d are respectively gained 10% in embodiment 1~3,20%, the FE-SEM figures of 30%BiOBr/AC.
XRD spectra can be seen that prepared BiOBr samples and Tetragonal BiOBr (JCPDS File as shown in Figure 1
No.09-0393 characteristic diffraction peak) is consistent, it can be seen that and its diffraction maximum is more sharp, shows that crystallinity is higher, and almost
There is no the appearance of impurity peaks, show that BiOBr purity prepared by this experimental method is also higher.It was found from the XRD spectra of activated carbon,
23 ° nearby there is characteristic diffraction peak, during In-situ fabricated in situ BiOBr/AC photochemical catalysts, the diffraction of activated carbon
Peak is covered by the diffraction maximum of BiOBr substantially, and also there occurs some changes, its appearance near 33 ° for BiOBr crystal forms
(102) and (110) two crystal plane structures, after it is loaded on activated carbon, only there is a diffraction maximum, this be probably because
Influenced each other each other for BiOBr and the diffraction maximum of activated carbon so that the two crystal plane structures are overlapped together.
It can be seen that activated carbon has abundant pore passage structure and micropore, and surface folding from the SEM figures (Fig. 2 a) of activated carbon
Very much, show that the specific surface area of activated carbon is sufficiently large.By observing Fig. 2 b~d, table of the BiOBr basic loads in activated carbon
In face and duct, the load capacity in micropore is seldom.Scheme (Fig. 2 b) by the SEM that load capacity is 10%BiOBr/AC can be seen that, it is living
Property charcoal load BiOBr amount it is less；After load capacity brings up to 20%, the amount of activated carbon surface absorption is proper and divides
Dissipate more uniform；When load capacity is 30%, in activated carbon surface more serious agglomeration occurs for excessive BiOBr.
Embodiment 2：Different loads amount BiOBr/AC photocatalytic activities are analyzed
10%, the 20% and 30%BiOBr/AC prepared using embodiment 1, and with activated carbon (i.e. BiOBr load capacity be 0)
As control.The simulating pollution thing of photocatalytic activity experiment selects methyl orange, and 0.2g is added into the MO solution of 50mL, 10mg/L
BiOBr/AC, after dark treatment half an hour, carry out light degradation under 300W xenon lamps, every 10 minutes sampling 4mL or so are in centrifuge tube
In, successive reaction 40min, 4min is centrifuged by materialsing under the 10000r/min of setting, then take supernatant with clean
In cuvette, (0~800nm) measures the absorbance at its characteristic wavelength (463nm) place in complete wavelength range.
As seen from Figure 3, when the load capacity of BiOBr is 0, i.e. only suction-operated of the activated carbon to methyl orange, absorption
Carry out after ten minutes, the percent of decolourization of methyl orange solution is almost unchanged, also there was only 8.7% after 30 minutes, it is known that simple activity
Charcoal absorption methyl orange ability is not strong.
When activated carbon surface loads suitable BiOBr, experiment finds that the ability of photo-catalytic degradation of methyl-orange is obvious at this time
It is improved.Under the conditions of the irradiation of 300W xenon lamps, react after forty minutes, drops of the BiOBr/AC that load capacity is 10% to methyl orange
Up to 54.8%, the photocatalytic Degradation collaboration of the suction-operated of activated carbon and the BiOBr of adsorption play a role solution rate,
Degradation capabilities of the BiOBr/AC to methyl orange is substantially increased, still, the palliating degradation degree of the load capacity Methyl Orange does not make us
It is satisfied, it may be possible to which that 10% BiOBr load capacity is smaller.
And the BiOBr/AC that load capacity is 20% has reached the degradation rate of methyl orange 97.5%, methyl orange solution at this time
It is in substantially colourless, effect is satisfactory, shows that 20% BiOBr load capacity is more suitable, schemes with reference to SEM, it can be seen that this is negative
The BiOBr amounts that activated carbon surface adsorbs under carrying capacity are proper and scattered more uniform.
It is 30% to continue to increase BiOBr load capacity, and BiOBr/AC photo-catalytic degradation of methyl-orange ability drops on the contrary at this time
79.6%, it may be possible to since the load capacity of activated carbon surface bismuth oxybromide is larger, cause it in the surface and micropore of activated carbon
Distribution is excessively intensive, or even there occurs agglomeration, on the one hand, excessive bismuth oxybromide can cover the activated carbon table of larger area
Face and micropore (shown in Fig. 2 d), so as to reduce adsorbance of the activated carbon to methyl orange so that activated carbon adsorption effect and bromine oxygen
Changing the cooperative effect of bismuth photocatalytic Degradation cannot fully bring into play；Mutual shading between another aspect BiOBr
Reduce the assimilation effect of light.
Therefore, load capacity optimal BiOBr is 20%, and load capacity and load effect at this time is best.
Embodiment 3
15%BiOBr/AC is prepared using the method for In-situ fabricated in situ：
(1) a certain amount of activated carbon is taken, twice is washed with cold water first and is filtered, be then added to round-bottomed flask
In, be heated to reflux in dilute hydrochloric acid 10 it is small when or so, to remove the ZnCl in activated carbon2Repeatedly washed Deng impurity, then with distilled water
Suction filtration is washed until filtrate is in neutrality, when finally drying 4 is small at 120 DEG C in an oven.
(2) active carbon particles of the 1.0160g after hydrochloric acid activation is weighed in clean small beaker with assay balance, use
100mL graduated cylinders measure the homemade deionized waters of 50mL, through magnetic agitation so that active carbon particle is dispersed in deionized water
In.According still further to molar ratio 1：1 KBr for weighing five water bismuth nitrates of 0.2183g and 0.0536g respectively is added to activated carbon and water at the same time
In suspension, magnetic agitation 8h, makes uniformly to mix between reactant, takes out stirrer with clean tweezers, is sealed with preservative film,
And several apertures are opened on preservative film, and it is put into heating in micro-wave oven and is reacted, microwave reaction condition：Low fire, time are 10 points
Clock.
(3) after reaction, the insoluble solid product of grey black is obtained, suction filtration behaviour is carried out after cooled to room temperature
Make, carry out repeatedly washing with deionized water and absolute ethyl alcohol to remove some foreign ions.Finally by products therefrom 15%
BiOBr/AC is put in small beaker together with filter paper, is put in thermostatic drying chamber at a temperature of 40 DEG C to pack after 15h and is collected.
Embodiment 4
25%BiOBr/AC is prepared using the method for In-situ fabricated in situ：
(1) active carbon particles of the 1.0160g after hydrochloric acid activation is weighed in clean small beaker with assay balance, use
100mL graduated cylinders measure the homemade deionized waters of 50mL, through magnetic agitation so that active carbon particle is dispersed in deionized water
In.According still further to molar ratio 1：1 KBr for weighing five water bismuth nitrates of 0.3637g and 0.0893g respectively is added to activated carbon and water at the same time
In suspension, magnetic agitation 8h, makes uniformly to mix between reactant, takes out stirrer with clean tweezers, is sealed with preservative film,
And several apertures are opened on preservative film, and it is put into heating in micro-wave oven and is reacted, microwave reaction condition：Low fire, time are 30 points
Clock.
(2) after reaction, the insoluble solid product of grey black is obtained, suction filtration behaviour is carried out after cooled to room temperature
Make, carry out repeatedly washing with deionized water and absolute ethyl alcohol to remove some foreign ions.Finally by products therefrom 25%
BiOBr/AC is put in small beaker together with filter paper, is put in thermostatic drying chamber at a temperature of 80 DEG C to pack after 5h and is collected.
Above content is only to design example and explanation of the invention, affiliated those skilled in the art
Various modifications or additions are done to described specific embodiment or are substituted in a similar way, without departing from invention
Design or surmount scope defined in the claims, be within the scope of protection of the invention.
Claims (10)
1. a kind of method that microwave in-situ quickly prepares charcoal load BiOBr visible light catalysts, it is characterised in that with five water nitric acid
Bismuth is bismuth source, potassium bromide is bromine source, is loaded with activated carbon (AC), deionized water is dispersant, using microwave method in activated carbon
Fabricated in situ BiOBr is hydrolyzed in micropore and by bismuth salt on surface, obtains charcoal load BiOBr visible light catalysts.
2. preparation method as claimed in claim 1, it is characterised in that active carbon particle is placed in the container of cleaning first,
Appropriate amount of deionized water is added, stirring makes active carbon particle dispersed；Then five water bismuth nitrates and potassium bromide are added into dispersion liquid
In, it is put into micro-wave oven and is reacted after stirring evenly；Product is filtered after reaction, wash, drying obtains charcoal load
BiOBr visible light catalysts.
3. preparation method as claimed in claim 2, it is characterised in that active carbon particle passes through following steps pre-treatment：
A certain amount of activated carbon is taken, twice is washed with cold water first and is filtered, is then added in round-bottomed flask, in dilute salt
It is heated to reflux in acid, to remove the impurity in activated carbon, then repeatedly washs with distilled water suction filtration until filtrate is in neutrality, finally exist
Dried in baking oven.
4. preparation method as claimed in claim 2, it is characterised in that BiOBr load capacity is generated with hydrolysis
What the quality of BiOBr and the mass ratio of the activated carbon (AC) of addition represented, BiOBr load capacity is 0~30%.
5. preparation method as claimed in claim 4, it is characterised in that BiOBr load capacity is 20%.
6. preparation method as claimed in claim 2, it is characterised in that the molar ratio between five water bismuth nitrates and potassium bromide is 1:
1。
7. preparation method as claimed in claim 2, it is characterised in that microwave reaction condition is：Low fire, 10~30 points of reaction
Clock.
8. preparation method as claimed in claim 2, it is characterised in that product utilizes deionized water after filtering after reaction
And absolute ethyl alcohol alternately washs, and then dries.
9. preparation method as claimed in claim 8, it is characterised in that drying temperature is 40~80 DEG C, and drying time is 5~15
Hour.
10. a kind of charcoal prepared such as claim 1~9 the method loads BiOBr visible light catalysts at photocatalytic degradation
Manage the application in organic pollution.
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| CN115845801A (en) * | 2022-12-08 | 2023-03-28 | 云南民族大学 | Preparation method and application of high-stability BiOI/activated carbon |
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| CN115845801A (en) * | 2022-12-08 | 2023-03-28 | 云南民族大学 | Preparation method and application of high-stability BiOI/activated carbon |
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