CN106925305A - A kind of Co BiOBr/TiO2The preparation method of/GO Three-element composite photocatalysts - Google Patents
A kind of Co BiOBr/TiO2The preparation method of/GO Three-element composite photocatalysts Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 79
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 38
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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
- 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
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- 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
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- 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
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- 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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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
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Abstract
The invention discloses a kind of Co BiOBr/TiO2The preparation method of/GO Three-element composite photocatalysts, belongs to photocatalysis technology field, comprises the following steps：1) doping Co is prepared2+BiOBr photochemical catalysts；2) Co BiOBr/TiO are prepared2Binary composite photo-catalyst；3) Co BiOBr/TiO are prepared2/ GO Three-element composite photocatalysts；The present invention is by the Co that adulterates2+And and TiO2Hetero-junctions is compounded to form, GO good electric conductivity makes light induced electron quickly move, suppresses charge recombination；Meanwhile, GO larger specific surface area can increase the adsorption capacity of photochemical catalyst, be more beneficial for the degraded of dyestuff；Its modified Co BiOBr/TiO for preparing2/ GO Three-element composite photocatalysts 20min is up to 96.8% to the degradation rate of rhodamine B, and improved solvent-thermal method and the relatively simple convenience of ultrasonic method, reaction condition is more gentle, and compared to some in BiOBr surfaces depositing noble metal, the raw material of the preparation method of this catalyst is easy to get, cost is relatively low, can be used for the treatment of extensive dyeing waste water, possess good practicality.
Description
Technical field
The invention belongs to photocatalysis technology field, and in particular to a kind of Co-BiOBr/TiO2/ GO Three-element composite photocatalysts
Preparation method.
Background technology
With developing rapidly for industry, the problem of current environmental pollution and energy shortage is increasingly highlighted.Photocatalysis technology is
The high-level oxidation technology of a kind of effective utilization solar energy and solution water pollution, causes the concern of more and more people in recent years.It is many
Well known, dyeing waste water is a kind of waste water difficult to deal with, and photocatalysis technology has its uniqueness in terms of dyeing waste water is processed
Advantage.
BiOBr is a kind of novel semiconductor material, and its crystal layer structure can allow atom and atomic orbital to produce polarization, point
From light induced electron and hole such that it is able to improve photocatalysis effect；But the light induced electron that BiOBr indirect band-gap semiconductors are excited
Have to pass through k layers and get to valence band location, thus greatly reduce the recombination probability in light induced electron and hole again.Just because of tool
Standby special open structure and indirect transition form, BiOBr can just cause the migration and separation in electronics and hole, can just gather around
There is the photocatalytic activity of superelevation.At present at the modified aspect of BiOBr, mainly including semiconductors coupling, metal and nonmetallic ion
Doping, surface sensitization and noble metal loading etc..
TiO2It is the earliest photochemical catalyst of mankind's discovery, because its is stable in properties, redox ability is strong, nontoxic, nothing two
The advantages of secondary pollution, be more satisfactory photochemical catalyst generally acknowledged at present.However, TiO2It is right because its energy gap is larger (3.2eV)
The utilization ratio of solar energy is relatively low, and only about 5%, hinder its extensive use.Therefore other semiconductors and TiO are sought2It is compound
Also the emphasis of research is turned into.Semiconductors coupling can make photo-generated carrier in height using the difference of energy level between each semiconductor
Transition between the energy level for differing, such that it is able to lift the separative efficiency of light induced electron and hole, so as to improve photocatalysis performance.
Graphene oxide (graphene oxide, abbreviation GO) is the oxide of Graphene, and oxygen-containing functional group increases after oxidation
Make property more active more, can be modified by the reaction with oxygen-containing functional group.GO good electric conductivity and stronger
Adsorption capacity makes it more and more be applied to photocatalysis field.
The content of the invention
Goal of the invention：It is an object of the invention to provide a kind of Co-BiOBr/TiO2The system of/GO Three-element composite photocatalysts
Preparation Method, method is simple, with low cost, can be applied to the treatment of fairly large dyeing waste water, and the Co-BiOBr/ for preparing
TiO2/ GO Three-element composite photocatalysts have photocatalysis performance very high under simulated solar irradiation.
Technical scheme：To achieve the above object, the present invention provides following technical scheme：
A kind of Co-BiOBr/TiO2The preparation method of/GO Three-element composite photocatalysts, comprises the following steps：
1) doping Co is prepared2+BiOBr photochemical catalysts
According to Bi:Co mol ratios are 100:(0.5~3) weighs Bi (NO3)3`5H2O and Co (NO3)2·6H2O is dissolved in polarity
In organic solvent, be subsequently adding NaBr, surfactant added after stirring and dissolving, sonic oscillation after stirring, ultrasound after
Solution be transferred in polytetrafluoroethylene (PTFE) autoclave, after first time insulation reaction wash, filtering, dry, obtain Co-
BiOBr photochemical catalysts；
2) Co-BiOBr/TiO is prepared2Binary composite photo-catalyst
According to Bi:Ti mol ratios are (0.25~0.75)：1 weigh Co-BiOBr photochemical catalysts and with solvent-thermal method prepare
TiO2Respective sonic oscillation in deionized water is respectively put into, both is then mixed into sonic oscillation again, washed, filter, dry,
Obtain Co-BiOBr/TiO2Binary composite photo-catalyst presoma, second insulation is forged during presoma then is put into Muffle furnace
Burn, obtain Co-BiOBr/TiO2Binary composite photo-catalyst；
3) Co-BiOBr/TiO is prepared2/ GO Three-element composite photocatalysts
Weigh Co-BiOBr/TiO2Binary composite photo-catalyst and the GO prepared with closed oxidizing process add deionized water
In, then both are mixed sonic oscillation again by respective sonic oscillation, and heating stirring is washed, filters, dried, and obtains Co-
BiOBr/TiO2/ GO Three-element composite photocatalysts.
Step 1) in, described polar organic solvent is ethylene glycol.
Step 1) in, described surfactant is polyvinylpyrrolidone.
Step 1) in, the time of sonic oscillation is 30~40min, and the temperature of first time insulation reaction is 160~170 DEG C,
Reaction time is 6~8h.
Step 2) in, the temperature of second insulation calcining is 280~300 DEG C, and calcination time is 4~5h.
Step 2) and step 3) in, the time of respective sonic oscillation is 30~40min, and the time of sonic oscillation is 2 again
~3h.
Step 3) in, the Co-BiOBr/TiO for weighing2Binary composite photo-catalyst is with the GO's prepared with closed oxidizing process
Mass ratio is 100：(0.5~2).
Step 3) in, the temperature of heating stirring is 60~70 DEG C, and mixing time is 12~15h.
Inventive principle：Co-BiOBr/TiO is prepared by improved solvent-thermal method and ultrasonic method2/ GO tri compound photocatalysis
Agent, by adding Co (NO3)2·6H2O, introduces Co2+, work as Co2+The intracell for moving to BiOBr forms defect, changes and urges
The energy gap of agent, so as to promote the separation of light induced electron and hole, oxidation activity is improved.BiOBr/TiO2It is multiple
The energy gap for closing semiconductor is smaller, and conduction band potential is higher than BiOBr conduction band potentials in itself, thus promotes light induced electron and sky
The movement in cave, the life-span of photohole is also extended, and it has high-crystallinity, meso-hole structure and corresponding specific surface area
Big the characteristics of, absorbability can be improved in visible region, heterojunction structure is formed between coupling particle at two, promote photoproduction
The separation of carrier, GO has fabulous electric conductivity, transparency higher and larger specific surface area, by sonic oscillation
And heating stirring makes GO closely be supported on Co-BiOBr/TiO2On, so as to modified Co-BiOBr/TiO is obtained2/ GO ternarys
Composite photo-catalyst.
Beneficial effect：Compared to BiOBr monomers, a kind of Co-BiOBr/TiO of the invention2/ GO Three-element composite photocatalysts
Preparation method, by the Co that adulterates2+And and TiO2Hetero-junctions is compounded to form, GO good electric conductivity makes light induced electron quick
It is mobile, suppress charge recombination；Meanwhile, GO larger specific surface area can increase the adsorption capacity of photochemical catalyst, be more beneficial for dye
The degraded of material；Its modified Co-BiOBr/TiO for preparing2Degradation rates of/GO Three-element composite photocatalysts the 20min to rhodamine B
Up to 96.8%, and improved solvent-thermal method and the relatively simple convenience of ultrasonic method, reaction condition is more gentle, and compares
In some in BiOBr surfaces depositing noble metal, the raw material of the preparation method of this catalyst is easy to get, cost is relatively low, can be used for big rule
The treatment of mould dyeing waste water, possesses good practicality.
Brief description of the drawings
Fig. 1 is Co-BiOBr/TiO2The process chart of/GO Three-element composite photocatalyst preparation methods；
Fig. 2 is Co-BiOBr/TiO2/ GO Three-element composite photocatalysts and Co-BiOBr, TiO2Monomer absorption-photocatalysis is dropped
Solution rhodamine B effect contrast figure.
Specific embodiment
The present invention is further described with specific embodiment below in conjunction with the accompanying drawings.
As shown in figure 1, being Co-BiOBr/TiO2The process chart of/GO Three-element composite photocatalyst preparation methods.Its
In, Bi (NO3)3`5H2O+Co(NO3)2·6H2Solution A is obtained after the mixing of O+ ethylene glycol, B solution, PVP are obtained after solution A+NaBr
It is polyvinylpyrrolidone.
A kind of Co-BiOBr/TiO2The preparation method of/GO Three-element composite photocatalysts, comprises the following steps：
1) doping Co is prepared2+BiOBr photochemical catalysts (Co-BiOBr)
According to Bi:Co mol ratios are 100:(0.5~3) weighs Bi (NO3)3`5H2O and Co (NO3)2·6H2O is dissolved in polarity
In organic solvent, the NaBr of respective amount is subsequently adding, surfactant is added after stirring and dissolving, sonic oscillation after stirring,
Solution after ultrasound is transferred in polytetrafluoroethylene (PTFE) autoclave, is washed after first time insulation reaction, filtered, dried, and is obtained
To Co-BiOBr photochemical catalysts；
2) Co-BiOBr/TiO is prepared2Binary composite photo-catalyst
According to Bi:Ti mol ratios are (0.25~0.75)：1 weighs step 1) in prepare optimum doping amount Co-BiOBr
Photochemical catalyst and the TiO prepared with solvent-thermal method2Respective sonic oscillation in deionized water is respectively put into, then mixes again both
Secondary sonic oscillation, washs, filters, dries, and obtains Co-BiOBr/TiO2Binary composite photo-catalyst presoma, then by forerunner
Body is put into second insulation calcining in Muffle furnace, obtains Co-BiOBr/TiO2Binary composite photo-catalyst；
3) Co-BiOBr/TiO is prepared2/ GO Three-element composite photocatalysts
Weigh step 2) prepare Co-BiOBr/TiO2Binary composite photo-catalyst and with closed oxidizing process prepare GO add
Enter in deionized water, then both are mixed sonic oscillation again by respective sonic oscillation, and heating stirring is washed, filters, dried,
Obtain Co-BiOBr/TiO2/ GO Three-element composite photocatalysts.
Step 1) in, polar organic solvent is ethylene glycol.Surfactant is polyvinylpyrrolidone (PVP).Ultrasound is shaken
The time swung is 30~40min, and the temperature of first time insulation reaction is 160~170 DEG C, and the reaction time is 6~8h.
Step 2) in, the temperature of second insulation calcining is 280~300 DEG C, and calcination time is 4~5h.
Step 2) and step 3) in, the time of respective sonic oscillation is 30~40min, and the time of sonic oscillation is 2 again
~3h.
Step 3) in, the Co-BiOBr/TiO for weighing2Binary composite photo-catalyst is with the GO's prepared with closed oxidizing process
Mass ratio is 100:(0.5~2).The temperature of heating stirring is 60~70 DEG C, and mixing time is 12~15h.
Embodiment 1
A kind of preparation method of Co-BiOBr photochemical catalysts, it is specific as follows：
According to Bi:Co mol ratios are 100:0.5 weighs 2.4254gBi (NO3)3`5H2O and 0.0073gCo (NO3)2·6H2O
It is dissolved in 35mL ethylene glycol, then weighs 0.5145gNaBr and be slowly added into above-mentioned solution, stirring is until completely dissolved
0.20gPVP is added thereto to, then the solution after vibration is transferred to 50mL poly- four by sonic oscillation 30min after stirring
In PVF autoclave, 6h is reacted under the conditions of 160 DEG C, be washed with deionized three times with remove in sediment it is unnecessary from
Son and other impurity, three organic matters to remove remnants of absolute ethanol washing, are positioned in 80 DEG C of air dry ovens after washing
6h is dried, 0.5%atm Co-BiOBr photochemical catalysts are obtained.
Embodiment 2
A kind of preparation method of Co-BiOBr photochemical catalysts, it is specific as follows：
According to Bi:Co mol ratios are 100:1 weighs 2.4254gBi (NO3)3`5H2O and 0.0146gCo (NO3)2·6H2O is molten
In 35mL ethylene glycol, then weigh 0.5145gNaBr and be slowly added into above-mentioned solution, stirring until completely dissolved to
0.20gPVP is wherein added, then the solution after vibration is transferred to 50mL polytetrafluoros by sonic oscillation 35min after stirring
In ethylene high pressure reactor, 7h is reacted under the conditions of 165 DEG C, be washed with deionized three times to remove unnecessary ion in sediment
And other impurity, absolute ethanol washing three times is positioned in 80 DEG C of air dry ovens after washing and done removing remaining organic matter
Dry 6h, obtains 1%atm Co-BiOBr photochemical catalysts.
Embodiment 3
A kind of preparation method of Co-BiOBr photochemical catalysts, it is specific as follows：
According to Bi:Co mol ratios are 100:3 weigh 2.4254gBi (NO3)3`5H2O and 0.0437gCo (NO3)2·6H2O is molten
In 35mL ethylene glycol, then weigh 0.5145gNaBr and be slowly added into above-mentioned solution, stirring until completely dissolved to
0.20gPVP is wherein added, then the solution after vibration is transferred to 50mL polytetrafluoros by sonic oscillation 40min after stirring
In ethylene high pressure reactor, 8h is reacted under the conditions of 170 DEG C, be washed with deionized three times to remove unnecessary ion in sediment
And other impurity, absolute ethanol washing three times is positioned in 80 DEG C of air dry ovens after washing and done removing remaining organic matter
Dry 6h, obtains 3%atm Co-BiOBr photochemical catalysts.
Embodiment 4
A kind of Co-BiOBr/TiO2The preparation method of binary composite photo-catalyst, it is specific as follows：
(1) preparation of Co-BiOBr photochemical catalysts
Specific such as embodiment 2
(2)TiO2Preparation
Pipette during 1mL butyl titanates (TBOT) and 1mL ethylene glycol adds 30mL glacial acetic acids, sonic oscillation 30min, then to
0.25mL hydrofluoric acid (HF) is wherein added, is transferred in 50mL polytetrafluoroethylene (PTFE) autoclaves, be put into baking oven, 180 DEG C, instead
Answer 24h.With respectively washing 3 times of deionized water and absolute ethyl alcohol, 80 DEG C of drying in air dry oven are transferred to, grind standby into bag.
(3)Co-BiOBr/TiO2The preparation of binary composite photo-catalyst
According to Bi:Ti mol ratios are 0.25:1 weighs 0.3050gCo-BiOBr and 0.3195gTiO2It is respectively put into and is equipped with
In the small beaker of 30mL deionized waters, then both are mixed sonic oscillation 2h again, washing, mistake by respective sonic oscillation 30min
Filter, dry, obtain Co-BiOBr/TiO2, then be put into presoma 300 DEG C in Muffle furnace by binary composite photo-catalyst presoma
Under the conditions of calcine 4h, obtain Co-BiOBr/TiO2Binary composite photo-catalyst.
Embodiment 5
A kind of Co-BiOBr/TiO2The preparation method of binary composite photo-catalyst, it is specific as follows：
(1) preparation of Co-BiOBr photochemical catalysts
Specific such as embodiment 2；
(2)TiO2Preparation
The specific such as step of embodiment 4 (2)；
(3)Co-BiOBr/TiO2The preparation of binary composite photo-catalyst
According to Bi:Ti mol ratios are 0.5:1 weighs 0.3050gCo-BiOBr and 0.1598gTiO2It is respectively put into and is equipped with
In the small beaker of 30mL deionized waters, then both are mixed sonic oscillation 3h again by respective sonic oscillation 40min, spend from
Sub- water and absolute ethyl alcohol respectively washing 3 times, filtering dry 6h, obtain Co-BiOBr/TiO in 80 DEG C of air dry ovens2Binary is combined
, then be put into presoma in Muffle furnace and calcine 5h under the conditions of 280 DEG C by photochemical catalyst presoma, obtains Co-BiOBr/TiO2Two
First composite photo-catalyst.
Embodiment 6
A kind of Co-BiOBr/TiO2The preparation method of binary composite photo-catalyst, it is specific as follows：
(1) preparation of Co-BiOBr photochemical catalysts；
Specific such as embodiment 2；
(2)TiO2Preparation
The specific such as step of embodiment 4 (2)；
(3)Co-BiOBr/TiO2The preparation of binary composite photo-catalyst
According to Bi:Ti mol ratios are 0.75:1 weighs 0.3050gCo-BiOBr and 0.1065gTiO2It is respectively put into and is equipped with
In the small beaker of 30mL deionized waters, then both are mixed sonic oscillation 2.5h again by respective sonic oscillation 35min, are spent
Ionized water and absolute ethyl alcohol respectively washing 3 times, filtering dry 6h, obtain Co-BiOBr/TiO in 80 DEG C of air dry ovens2Binary is answered
, then be put into presoma in Muffle furnace and calcine 4.5h under the conditions of 290 DEG C by closing light catalyst precursor, obtains Co-BiOBr/
TiO2Binary composite photo-catalyst.
Embodiment 7
A kind of Co-BiOBr/TiO2/ GO Three-element composite photocatalyst preparation methods, it is specific as follows：
(1)Co-BiOBr/TiO2It is prepared by binary composite photo-catalyst
Specific such as embodiment 5；
(2) preparation of GO (graphene oxide)
The graphite for first weighing 1g is placed in 100mL reactor bottoms, then weighs the potassium permanganate of 5g and be covered on graphite, then
Reactor and the concentrated sulfuric acid are put in cold compartment of refrigerator (4 DEG C) and cool down 2h；Reactor is opened after 2h, the concentrated sulfuric acid of 50mL is added,
Low-temp reaction (- 2~2 DEG C) 2h；Kettle courage is taken out after 2h is placed in still shell, after reacting 2h under the conditions of 80 DEG C in baking oven, taken out,
Cooling.Kettle is driven, product is poured into water agitation and dilution, add hydrogen peroxide to become golden yellow or khaki up to solution, stood, it is heavy to take
Starch is washed.By sediment centrifuge washing, three times are first washed with watery hydrochloric acid to remove sulfate ion, deionized water is washed three times
Sediment is washed till neutrality, the defecation of the yellow colloidal on sediment upper strata is finally taken out into drying, GO samples are obtained；
(3)Co-BiOBr/TiO2It is prepared by/GO Three-element composite photocatalysts
By Co-BiOBr/TiO2It is 100 with the mass ratio of GO:0.5 weighs 0.20gCo-BiOBr/TiO2And 0.0010gGO,
It is added separately in two small beakers equipped with 30min deionized waters, respectively sonic oscillation 30min, after then both are mixed
Ultrasound 2h, 12h is stirred under the conditions of 60 DEG C again, with respectively washing 3 times of deionized water and absolute ethyl alcohol, filtering, 80 DEG C of forced air dryings
6h is dried in case, Co-BiOBr/TiO is obtained2/ GO Three-element composite photocatalysts.
Embodiment 8
A kind of Co-BiOBr/TiO2/ GO Three-element composite photocatalyst preparation methods, it is specific as follows：
(1)Co-BiOBr/TiO2It is prepared by binary composite photo-catalyst
Specific such as embodiment 5；
(2) preparation of GO
The specific such as step of embodiment 7 (2)；
(3)Co-BiOBr/TiO2It is prepared by/GO Three-element composite photocatalysts
By Co-BiOBr/TiO2It is 100 with the mass ratio of GO:1 weighs 0.20gCo-BiOBr/TiO2And 0.0020gGO, point
It is not added in two small beakers equipped with 30min deionized waters, respectively sonic oscillation 30min, after then both are mixed again
Secondary ultrasonic 2h, 14h is stirred under the conditions of 65 DEG C, with respectively washing 3 times of deionized water and absolute ethyl alcohol, filtering, 80 DEG C of air dry ovens
In dry 6h, obtain Co-BiOBr/TiO2/ GO Three-element composite photocatalysts.
Embodiment 9
A kind of Co-BiOBr/TiO2/ GO Three-element composite photocatalyst preparation methods, it is specific as follows：
(1)Co-BiOBr/TiO2It is prepared by binary composite photo-catalyst
Specific such as embodiment 5；
(2) preparation of GO
The specific such as step of embodiment 7 (2)；
(3)Co-BiOBr/TiO2It is prepared by/GO Three-element composite photocatalysts
By Co-BiOBr/TiO2It is 100 with the mass ratio of GO:2 weigh 0.20gCo-BiOBr/TiO2And 0.0040gGO, point
It is not added in two small beakers equipped with 30min deionized waters, respectively sonic oscillation 30min, after then both are mixed again
Secondary ultrasonic 2h, 15h is stirred under the conditions of 70 DEG C, with respectively washing 3 times of deionized water and absolute ethyl alcohol, filtering, 80 DEG C of air dry ovens
In dry 6h, obtain Co-BiOBr/TiO2/ GO Three-element composite photocatalysts.
Comparative example
Co-BiOBr/TiO prepared by embodiment 1~9 is determined respectively2/ GO Three-element composite photocatalysts are to Luo Dan in solution
Absorption-the photocatalytic degradation capability of bright B：
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr photochemical catalysts for adding 10mg embodiments 1 to prepare,
Now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, it is flat that first lucifuge stirring 1h reaches photochemical catalyst absorption-desorption
Weighing apparatus, carries out photocatalytic degradation under subsequent Xenon light shining, institute's sample is centrifuged after terminating per sub-sampling for sampling interval 10min,
Measure absorbance and calculate corresponding concentration, according to formulaClearance is obtained, in formula：C0It is solution crowd Luo Dan
The initial concentration of bright B, CtIt is the concentration of rhodamine B in solution after t absorption-photocatalytic degradation, R is clearance (%).
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr photochemical catalysts for adding 10mg embodiments 2 to prepare,
Now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, it is flat that first lucifuge stirring 1h reaches photochemical catalyst absorption-desorption
Weighing apparatus, carries out photocatalytic degradation under subsequent Xenon light shining, institute's sample is centrifuged after terminating per sub-sampling for sampling interval 10min,
Measure absorbance and calculate corresponding concentration, and calculate the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr photochemical catalysts for adding 10mg embodiments 3 to prepare,
Now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, it is flat that first lucifuge stirring 1h reaches photochemical catalyst absorption-desorption
Weighing apparatus, carries out photocatalytic degradation under subsequent Xenon light shining, institute's sample is centrifuged after terminating per sub-sampling for sampling interval 10min,
Measure absorbance and calculate corresponding concentration, and calculate the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr/TiO for adding 10mg embodiments 4 to prepare2Binary
Composite photo-catalyst, now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, first lucifuge stirring 1h reaches photochemical catalyst
Absorption-desorption balance, carries out photocatalytic degradation, sampling interval 10min, by institute after terminating per sub-sampling under subsequent Xenon light shining
Sample is centrifuged, and is measured absorbance and is calculated corresponding concentration, and calculates the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr/TiO for adding 10mg embodiments 5 to prepare2Binary
Composite photo-catalyst, now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, first lucifuge stirring 1h reaches photochemical catalyst
Absorption-desorption balance, carries out photocatalytic degradation, sampling interval 10min, by institute after terminating per sub-sampling under subsequent Xenon light shining
Sample is centrifuged, and is measured absorbance and is calculated corresponding concentration, and calculates the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr/TiO for adding 10mg embodiments 6 to prepare2Binary
Composite photo-catalyst, now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, first lucifuge stirring 1h reaches photochemical catalyst
Absorption-desorption balance, carries out photocatalytic degradation, sampling interval 10min, by institute after terminating per sub-sampling under subsequent Xenon light shining
Sample is centrifuged, and is measured absorbance and is calculated corresponding concentration, and calculates the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr/TiO for adding 10mg embodiments 7 to prepare2/ GO tri-
First composite photo-catalyst, now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, first lucifuge stirring 1h reaches photocatalysis
Agent absorption-desorption balance, carries out photocatalytic degradation under subsequent Xenon light shining, sampling interval 10min will after terminating per sub-sampling
Institute's sample is centrifuged, and is measured absorbance and is calculated corresponding concentration, and calculates the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr/TiO for adding 10mg embodiments 8 to prepare2/ GO tri-
First composite photo-catalyst, now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, first lucifuge stirring 1h reaches photocatalysis
Agent absorption-desorption balance, carries out photocatalytic degradation under subsequent Xenon light shining, sampling interval 10min will after terminating per sub-sampling
Institute's sample is centrifuged, and is measured absorbance and is calculated corresponding concentration, and calculates the clearance in each stage.
50mL concentration is taken for 20mg/L rhodamine B solution, the Co-BiOBr/TiO for adding 10mg embodiments 9 to prepare2/ GO tri-
First composite photo-catalyst, now photochemical catalyst consumption is 0.2g/L.In photochemical reaction instrument, first lucifuge stirring 1h reaches photocatalysis
Agent absorption-desorption balance, subsequent Xenon light shining 40min, sampling interval 10min, per sub-sampling terminate after by institute's sample carry out from
The heart, measures absorbance and calculates corresponding concentration, and calculate the clearance in each stage.
Co-BiOBr/TiO prepared by embodiment 1~92To in solution during/GO Three-element composite photocatalyst light degradation 40min
The removal ability of rhodamine B is as shown in table 1.
Removal ability of the table 1 to rhodamine B in solution
| Rhodamine B residual concentration (mg/L) in solution | Clearance (%) | |
| The catalyst of embodiment 1 | 5.072 | 74.64 |
| The catalyst of embodiment 2 | 3.886 | 80.57 |
| The catalyst of embodiment 3 | 5.408 | 72.96 |
| The catalyst of embodiment 4 | 4.230 | 78.85 |
| The catalyst of embodiment 5 | 2.088 | 89.56 |
| The catalyst of embodiment 6 | 3.438 | 82.81 |
| The catalyst of embodiment 7 | 1.654 | 91.73 |
| The catalyst of embodiment 8 | 0.288 | 97.56 |
| The catalyst of embodiment 9 | 2.262 | 88.69 |
From table 1, it is apparent that comparative example 1~3, catalytic effect is best in finding Co-BiOBr photochemical catalysts
It is 1%atmCo-BiOBr, 40min has reached 80.57% to the clearance of rhodamine B.Comparative example 4~6, find Co-
BiOBr/TiO2Effect in binary composite photo-catalyst in effect by the preparation of embodiment 5 is best, now Bi:Ti mol ratios are
0.5:1.Comparative example 7~9, find Co-BiOBr/TiO2By preparation in embodiment 8 in/GO Three-element composite photocatalysts
Ternary complex catalyst effect is best, this moment Co-BiOBr/TiO2Load the GO of 1%wt, clearances of the 40min to rhodamine B
Reach 97.56%.
Fig. 2 describes TiO2, 1%atm Co-BiOBr, modified Co-BiOBr/TiO2/ GO photochemical catalyst absorption-light is urged
Change rhodamine B degradation effect contrast figure.As can be seen from the figure under simulated solar irradiation during 40min embodiment 8 prepare it is modified
Co-BiOBr/TiO afterwards2/ GO tri compounds photocatalytic activity has obtained huge lifting compared to monolithic catalyst.
Claims (8)
1. a kind of Co-BiOBr/TiO2The preparation method of/GO Three-element composite photocatalysts, it is characterised in that：Comprise the following steps：
1) doping Co is prepared2+BiOBr photochemical catalysts
According to Bi:Co mol ratios are 100:(0.5~3) weighs Bi (NO3)3`5H2O and Co (NO3)2·6H2It is organic that O is dissolved in polarity
In solvent, be subsequently adding NaBr, surfactant added after stirring and dissolving, sonic oscillation after stirring, ultrasound after it is molten
Liquid is transferred in polytetrafluoroethylene (PTFE) autoclave, is washed after first time insulation reaction, filtered, dried, and obtains Co-BiOBr light
Catalyst；
2) Co-BiOBr/TiO is prepared2Binary composite photo-catalyst
According to Bi:Ti mol ratios are (0.25~0.75)：1 weighs Co-BiOBr photochemical catalysts and the TiO prepared with solvent-thermal method2
Respective sonic oscillation in deionized water is respectively put into, both are then mixed into sonic oscillation again, washed, filter, dry, obtained
Co-BiOBr/TiO2Binary composite photo-catalyst presoma, second insulation is calcined during presoma then is put into Muffle furnace, is obtained
To Co-BiOBr/TiO2Binary composite photo-catalyst；
3) Co-BiOBr/TiO is prepared2/ GO Three-element composite photocatalysts
Weigh Co-BiOBr/TiO2Binary composite photo-catalyst and the GO prepared with closed oxidizing process are added in deionized water, each
Then both are mixed sonic oscillation again by sonic oscillation, and heating stirring is washed, filters, dried, and obtains Co-BiOBr/
TiO2/ GO Three-element composite photocatalysts.
2. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 1) in, described polar organic solvent is ethylene glycol.
3. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 1) in, described surfactant is polyvinylpyrrolidone.
4. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 1) in, the time of sonic oscillation is 30~40min, and the temperature of first time insulation reaction is 160~170 DEG C, reaction
Time is 6~8h.
5. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 2) in, the temperature of second insulation calcining is 280~300 DEG C, and calcination time is 4~5h.
6. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 2) and step 3) in, time of respective sonic oscillation is 30~40min, again the time of sonic oscillation be 2~
3h。
7. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 3) in, the Co-BiOBr/TiO for weighing2The quality of binary composite photo-catalyst and the GO prepared with closed oxidizing process
Than being 100：(0.5~2).
8. a kind of Co-BiOBr/TiO according to claim 12The preparation method of/GO Three-element composite photocatalysts, its feature
It is：Step 3) in, the temperature of heating stirring is 60~70 DEG C, and mixing time is 12~15h.
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| CN114950499A (en) * | 2022-03-11 | 2022-08-30 | 深圳信息职业技术学院 | Preparation method and application of bimetallic Co and Ce composite bismuth-based photocatalytic material |
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