CN108906086A - The preparation method of floating bead load bismuth oxybromide photocatalyst - Google Patents
The preparation method of floating bead load bismuth oxybromide photocatalyst Download PDFInfo
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- CN108906086A CN108906086A CN201810817062.XA CN201810817062A CN108906086A CN 108906086 A CN108906086 A CN 108906086A CN 201810817062 A CN201810817062 A CN 201810817062A CN 108906086 A CN108906086 A CN 108906086A
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- floating bead
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- 239000011324 bead Substances 0.000 title claims abstract description 113
- 238000007667 floating Methods 0.000 title claims abstract description 110
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000758 substrate Substances 0.000 claims abstract description 33
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 22
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000010881 fly ash Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 11
- 238000011049 filling Methods 0.000 claims abstract description 11
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 239000000428 dust Substances 0.000 claims abstract description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 38
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 27
- 239000012153 distilled water Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 15
- 238000007146 photocatalysis Methods 0.000 description 15
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 11
- 229940043267 rhodamine b Drugs 0.000 description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 239000011521 glass Substances 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 230000005611 electricity Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052797 bismuth Inorganic materials 0.000 description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 150000004703 alkoxides Chemical class 0.000 description 3
- 229910001451 bismuth ion Inorganic materials 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- FOQHYNYNHYNUIN-UHFFFAOYSA-N [O].[Br] Chemical compound [O].[Br] FOQHYNYNHYNUIN-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 239000002879 Lewis base Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/36—Organic compounds containing halogen
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
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Abstract
The present invention provides a kind of preparation method of floating bead load bismuth oxybromide photocatalyst.Preparation method is：Flyash is poured into the beaker for filling water, is stood after stirring, the floating bead particle floated on the water surface is sub-elected；The floating bead particle sub-elected is immersed in dust technology after 10-14h and filters, be dried to obtain floating bead；The addition of five nitric hydrate bismuths, potassium bromide and polyvinylpyrrolidone is filled in glycol reaction container and obtains substrate liquid, the substrate liquid is stirred；Under conditions of being stirred continuously, adds the floating bead and PH to adjust liquid into the molten substrate and obtain attachment liquid；It filters the attachment liquid and obtains attachment floating bead；Heat preservation obtains concentration floating bead after attachment floating bead is dried；Rinsing filtering is carried out to the concentration floating bead and is dried to obtain finished product.The preparation method of floating bead provided by the present invention load bismuth oxybromide photocatalyst solves in the prior art that bismuth oxybromide particle is tiny, the more complicated technical problem of separation process.
Description
Technical field
The present invention relates to visible light photocatalysis fields, and in particular to a kind of system of floating bead load bismuth oxybromide photocatalyst
Preparation Method.
Background technique
Photocatalysis is just found 1967, and people were very interested in this new technology at that time, but until 1992 years
Photocatalysis technology is used to pollute by the proposition of Japanology mechanism in photocatalyst of titanium dioxide (i.e. photocatalysis) international symposium
The processing of object, correlative study of the photocatalytic applications in the fields such as antibacterial, antifouling, air cleaning sharply increase.Wherein sent out earliest
Existing photochemical catalyst TiO2It is always the heat of photocatalysis research field due to its very high photostability, lower-price characteristic
Point.Although TiO2, have no toxic side effect, at low cost the advantages that stable with its chemical property, which becomes, studies most commonly used photocatalysis
Agent, but due to TiO2Band-gap energy be 3.2eV, only wavelength less than 387nm ultraviolet light could excite its generate electronics-
Hole is to showing oxidation, and the ultraviolet light (400nm or less) in sunlight has only been accounted for less than 5%.As it can be seen that
If only merely with TiO2For photochemical catalyst, using sunlight as the energy, actual efficiency is not high, and the efficiency of light energy utilization is low.
Therefore, people start to put among the research to visible-light photocatalyst.
Wherein, BiOX BiOX (X=Cl, Br, I) is with its unique layer structure, suitable forbidden bandwidth and Qi Gao
The photocatalysis performance of effect is always the hot spot of visible light catalyst research.
Although bismuth oxybromide can show good photocatalytic activity, in practical applications, still there is certain limitation
Property.Since bismuth oxybromide particle is tiny, separation process is more complicated, and particle suspension liquid will be by filtering, centrifugation, copolymerization, sedimentation
The methods of separated, process is many and diverse to affect its practical working efficiency.So people have had been put into support type bromine oxygen
Change the research of bismuth, the carrier of common photochemical catalyst has following several：
Ceramic-like materials, ceramics are a kind of porous masses, sturdy and durable with its, percent opening is high, regenerability is good, chemistry
Property is stable, acid and alkali-resistance and it is cheap the advantages that be often used as the carrier of photochemical catalyst.
Glass-like materials, glass are a kind of transparent solid matters, and there is good translucency to be adapted as photocatalysis
The carrier of agent.Category of glass carrier includes glass fibre, sheet glass, glass ball, glass infuser, organic glass etc..However ceramics and
That there are the fastnesses that load capacity is few and catalyst loads is low etc. insufficient for category of glass carrier.Reduce the photocatalysis effect of photochemical catalyst
Rate；
Carbon material, such as active carbon, carbon black, graphite, carbon nanotube.By on photocatalyst to this kind of carriers,
Although the problem of can solve catalyst separation aspect, costly, while intensity is again for this kind of materials such as active carbon price
It is relatively weak, although being easy recycling, limit the number of its recycling.If by being used as the catalyst of carrier
The processing of sewage often will increase the cost of water process.
Metal group material, the metallic carrier being commonly used at present are mainly nickel foam, titanium sheet, aluminium flake etc..Metal is as load
Have heat-resisting and corrosion resistance when body, and there is very strong interaction between metallic carrier and photochemical catalyst.Such as：Shanghai
University of communications Yuan etc. is prepared for foamed nickel supported TiO by using sol-gel method2, Al2O2-SiO2 as TiO2 with
Tie coat between nickel foam improves TiO2Photocatalytic activity.However that there are translucency is poor, flexibility is poor for metallic carrier
The defects such as low with voidage limit its development.
So find superior performance, raw material it is cheap and easy to get to carrier become technical problem urgently to be resolved.
Summary of the invention
It is not easily recycled technical problem to solve the bismuth oxybromide of the prior art, the present invention provides a kind of floating bead load bromine oxygen
Change the preparation method of bismuth photochemical catalyst.
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling water, is stood after stirring, the floating bead floated on the water surface is sub-elected
Grain；
Step 2：The floating bead particle sub-elected is immersed in dust technology and is filtered after 10-14h and is dried to obtain floating bead；
Step 3：Five nitric hydrate bismuths, potassium bromide and polyvinylpyrrolidone are added to the reaction vessel for filling ethylene glycol
In obtain substrate liquid, substrate liquid is stirred；
Step 4：Under conditions of being stirred continuously, adds floating bead and PH to adjust liquid into molten substrate and obtain attachment liquid；
Step 5：Filtering attachment liquid obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead after attachment floating bead is dried；
Step 7：Concentration floating bead is subjected to rinsing filtering and is dried to obtain finished product.
Optionally, used water is distilled water.
Optionally, in step 2, the floating bead particle after immersion further includes before filtration：It is repeatedly floated with distilled water
It washes, until the pH value of rinsing liquid is neutrality.
Optionally, the drying temperature range in step 2 is 90-120 DEG C.
Optionally, in step 3, reaction vessel is placed on universal mixer and is stirred, stirring is placed on ultrasound
Ultrasonic wave dispersion is carried out in wave cleaning machine until the solid in solution is completely dissolved and the color of solution is in yellow.
Optionally, in step 4, it is potassium hydroxide that PH, which adjusts liquid,.
Optionally, in step 4, the pH value magnitude range for adhering to liquid is 8-10.
Optionally, in step 6, drying temperature range is 150-180 DEG C, and soaking time range is 12-18h.
Optionally, in step 7, drying temperature range is 90-120 DEG C.
Optionally, in step 3, the molar ratio of five nitric hydrate bismuths and potassium bromide is 2: 1.
Compared to the prior art, vitrified agent provided by the invention and preparation method thereof and application method have beneficial below
Effect：Since raw material flyash is the sa hollow glass bead by sorting out in the flyash of coal-burning power plant's discharge,
Its appearance is many in honeycomb hole, and inside has hole more abundant and large specific surface area, and light transmittance is good, surface
Easily film forming, relative low price and quality is lighter, swim in the water surface, are easy to separate with water, as long as from the water surface after reaction
It salvages, can be re-used by being simply heat-treated.So using manufactured by preparation method provided by the present invention
Floating bead load bismuth oxybromide photocatalyst, at low cost, high catalytic efficiency, after recycling performance stablize, in addition, of the invention
The preparation condition proposed can effectively improve floating bead load bismuth oxybromide photocatalyst end properties.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described reality
Applying example is only a part of the embodiments of the present invention, instead of all the embodiments.
Embodiment 1
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling distilled water, is stood after stirring, the drift floated on the water surface is sub-elected
Pearl particle；
Step 2：The floating bead particle sub-elected is immersed in 10h in 10% dust technology, is attached in floating bead with removal
Impurity is repeatedly rinsed with distilled water, until rinsing liquid is neutrality, is then filtered with filter paper, then use electric drying oven with forced convection
Dry, drying temperature is 90 DEG C, obtains floating bead；
Step 3：Five nitric hydrate bismuths, potassium bromide by molar ratio for 2: 1 fill second with polyvinylpyrrolidone addition
Substrate liquid is obtained in glycol reaction vessel, reaction vessel is placed on universal mixer, the substrate liquid is stirred,
Stirring is placed on progress ultrasonic wave in supersonic wave cleaning machine and disperses to turn yellow up to the substrate liquid, and the solid in solution
It is completely dissolved；
Step 4：Under conditions of being stirred continuously, the floating bead and potassium hydroxide is added to be adhered into the molten substrate
Liquid, the PH for adhering to liquid is 8；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead, drying temperature after attachment floating bead is dried with electric drying oven with forced convection
It is 150 DEG C, soaking time 12h；
Step 7：Rinsing filtering is carried out to the concentration floating bead and is obtained into after being dried with electric drying oven with forced convection
Product, drying temperature are 90 DEG C.
Embodiment 2
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling distilled water, is stood after stirring, the drift floated on the water surface is sub-elected
Pearl particle；
Step 2：The floating bead particle sub-elected is immersed in 14h in 12% dust technology, floating bead is attached to removal
On impurity, repeatedly rinsed with distilled water, until rinsing liquid be neutrality, then filtered with filter paper, then electricity consumption hot drum air-dry
Dry case is dry, and drying temperature is 120 DEG C, obtains floating bead；
Step 3：It is 2 by molar ratio:1 five nitric hydrate bismuths, potassium bromide fill second with polyvinylpyrrolidone addition
Substrate liquid is obtained in glycol reaction vessel, the reaction vessel is placed on universal mixer, the substrate liquid is carried out
Stirring, stirring are placed on progress ultrasonic wave in supersonic wave cleaning machine and disperse to turn yellow up to the substrate liquid, and in solution
Solid is completely dissolved；
Step 4：Under conditions of being stirred continuously, the floating bead and potassium hydroxide is added to be adhered into the molten substrate
Liquid, the PH for adhering to liquid is 10；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead, drying temperature after attachment floating bead is dried with electric drying oven with forced convection
It is 180 DEG C, soaking time 18h；
Step 7：Rinsing filtering is carried out to the concentration floating bead and is obtained into after being dried with electric drying oven with forced convection
Product, drying temperature are 120 DEG C.
Embodiment 3
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling distilled water, is stood after stirring, the drift floated on the water surface is sub-elected
Pearl particle；
Step 2：The floating bead particle sub-elected is immersed in 12h in 11% dust technology, floating bead is attached to removal
On impurity, repeatedly rinsed with distilled water, until rinsing liquid be neutrality, then filtered with filter paper, then electricity consumption hot drum air-dry
Dry case is dry, and drying temperature is 95 DEG C, obtains floating bead；
Step 3：It is 2 by molar ratio:1 five nitric hydrate bismuths, potassium bromide fill second with polyvinylpyrrolidone addition
Substrate liquid is obtained in glycol reaction vessel, the reaction vessel is placed on universal mixer, the substrate liquid is carried out
Stirring, stirring are placed on progress ultrasonic wave in supersonic wave cleaning machine and disperse to turn yellow up to the substrate liquid, and in solution
Solid is completely dissolved；
Step 4：Under conditions of being stirred continuously, the floating bead and potassium hydroxide is added to be adhered into the molten substrate
Liquid, the PH for adhering to liquid is 8.5；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead, drying temperature after attachment floating bead is dried with electric drying oven with forced convection
It is 160 DEG C, soaking time 13h；
Step 7：Rinsing filtering is carried out to the concentration floating bead and is obtained into after being dried with electric drying oven with forced convection
Product, drying temperature are 100 DEG C.
Embodiment 4
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling distilled water, is stood after stirring, the drift floated on the water surface is sub-elected
Pearl particle；
Step 2：The floating bead particle sub-elected is immersed in 12h in 11% dust technology, floating bead is attached to removal
On impurity, repeatedly rinsed with distilled water, until rinsing liquid be neutrality, then filtered with filter paper, then electricity consumption hot drum air-dry
Dry case is dry, and drying temperature is 100 DEG C, obtains floating bead；
Step 3：It is 2 by molar ratio:1 five nitric hydrate bismuths, potassium bromide fill second with polyvinylpyrrolidone addition
Substrate liquid is obtained in glycol reaction vessel, the reaction vessel is placed on universal mixer, the substrate liquid is carried out
Stirring, stirring are placed on progress ultrasonic wave in supersonic wave cleaning machine and disperse to turn yellow up to the substrate liquid, and in solution
Solid is completely dissolved；
Step 4：Under conditions of being stirred continuously, the floating bead and potassium hydroxide is added to be adhered into the molten substrate
Liquid, the PH for adhering to liquid is 9；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead, drying temperature after attachment floating bead is dried with electric drying oven with forced convection
It is 165 DEG C, soaking time 14h；
Step 7：Rinsing filtering is carried out to the concentration floating bead and is obtained into after being dried with electric drying oven with forced convection
Product, drying temperature are 105 DEG C.
Embodiment 5
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling distilled water, is stood after stirring, the drift floated on the water surface is sub-elected
Pearl particle；
Step 2：The floating bead particle sub-elected is immersed in 14h in 12% dust technology, floating bead is attached to removal
On impurity, repeatedly rinsed with distilled water, until rinsing liquid be neutrality, then filtered with filter paper, then electricity consumption hot drum air-dry
Dry case is dry, and drying temperature is 105 DEG C, obtains floating bead；
Step 3：It is 2 by molar ratio:1 five nitric hydrate bismuths, potassium bromide fill second with polyvinylpyrrolidone addition
Substrate liquid is obtained in glycol reaction vessel, the reaction vessel is placed on universal mixer, the substrate liquid is carried out
Stirring, stirring are placed on progress ultrasonic wave in supersonic wave cleaning machine and disperse to turn yellow up to the substrate liquid, and in solution
Solid is completely dissolved；
Step 4：Under conditions of being stirred continuously, the floating bead and potassium hydroxide is added to be adhered into the molten substrate
Liquid, the PH for adhering to liquid is 9.5；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead, drying temperature after attachment floating bead is dried with electric drying oven with forced convection
It is 170 DEG C, soaking time 15h；
Step 7：Rinsing filtering is carried out to the concentration floating bead and is obtained into after being dried with electric drying oven with forced convection
Product, drying temperature are 110 DEG C.
Embodiment 6
A kind of preparation method of floating bead load bismuth oxybromide photocatalyst, specifically includes following steps：
Step 1：Flyash is poured into the beaker for filling distilled water, is stood after stirring, the drift floated on the water surface is sub-elected
Pearl particle；
Step 2：The floating bead particle sub-elected is immersed in 14h in 12% dust technology, floating bead is attached to removal
On impurity, repeatedly rinsed with distilled water, until rinsing liquid be neutrality, then filtered with filter paper, then electricity consumption hot drum air-dry
Dry case is dry, and drying temperature is 115 DEG C, obtains floating bead；
Step 3：It is 2 by molar ratio:1 five nitric hydrate bismuths, potassium bromide fill second with polyvinylpyrrolidone addition
Substrate liquid is obtained in glycol reaction vessel, the reaction vessel is placed on universal mixer, the substrate liquid is carried out
Stirring, stirring are placed on progress ultrasonic wave in supersonic wave cleaning machine and disperse to turn yellow up to the substrate liquid, and in solution
Solid is completely dissolved；
Step 4：Under conditions of being stirred continuously, the floating bead and potassium hydroxide is added to be adhered into the molten substrate
Liquid, the PH for adhering to liquid is 8；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead, drying temperature after attachment floating bead is dried with electric drying oven with forced convection
It is 175 DEG C, soaking time 17h；
Step 7：Rinsing filtering is carried out to the concentration floating bead and is obtained into after being dried with electric drying oven with forced convection
Product, drying temperature are 115 DEG C.
It should be noted that the floating bead in the present invention, is the sial by sorting out in the flyash of coal-burning power plant's discharge
Matter hollow glass bead, appearance is many in honeycomb hole, and inside has hole more abundant and large specific surface area, and
And light transmittance is good, surface easily forms a film, relative low price and quality is lighter, swims in the water surface, is easy to separate with water, instead
As long as then should be salvaged from the water surface, can be re-used by being simply heat-treated.
The neutralizing hydrolysis preparating mechanism of floating bead load bismuth oxybromide：
Firstly, since ethylene glycol has good crosslinking complexing power, trivalent bismuth ion there are three major key unoccupied orbitals,
Outermost layer has a pair of of lone pair electrons, is easy and lewis base is combined into four-coordination or six coordinate complex matter, so five water nitric acid
Bismuth can dissolve in ethylene glycol, form the metal alkoxide of stable oligomeric complex compound.In course of dissolution, bismuth ion and second two
Pure and mild a small amount of water molecule coordination, while going out a H+ with volume ionization, so the metal alkoxide solution of bismuth becomes acid from neutrality
Property, pH value is remarkably decreased.Such as reaction equation (1), in this stage since the Bi-O unit degree of polymerization is limited, so being produced without solid
Raw, what is obtained is bright solution.But if it is de- that bismuth ion is catalyzed ethylene glycol polymerization under the hydrothermal condition for increasing temperature
The hydrone of water, generation further pushes hydrolysis of alkoxide, thus can further polycondensation and generate Bi-O-Bi, then in system
Existing halogen atom, which combines, forms BiOX micromeritics, then ultimately forms classification and structure by continuous slowly growth
Microballoon, this is the balling-up mechanism of water-heat process.But under conditions of not heating, by adding alkali to introduce hydroxide ion, together
Sample can be nucleated with driving a reaction.Such as reaction equation (2), with the addition of ammonium hydroxide, hydroxide ion can gradually replace ethylene glycol and give birth to
At Bi-O-Bi structure and Bi based compound further is combined into halogen atom.This is also raising of the system with pH value,
Solution is gradually become muddy, is eventually become the reason of sol form from bright.The colloidal sol of this white is easy to be adsorbed to fine coal
The surface of ash, is further dehydrated and is finally fixedly supported on the surface of floating bead in the heat preservation heat treatment process of drying box
This is that the floating bead load bismuth oxybromide being prepared under alkaline condition has the basic reason of better photocatalytic activity.
The load capacity of BiOX is caused to increase under alkaline condition consistent with SEM and XRD characterization result.
xBi3++zH2O+yEG→Bix(EG)y(OH)z+zH+ (1)
Bix(EG)y(OH)z+zOH-+x Br-→xBiOBr-+yEG+zH2O (2)
Influence of the pH value to properties of catalyst in preparation process：
The photocatalysis experimental result for the sample for only having potassium hydroxide additional amount different in sample preparation procedure is listed below
Table:
The absorbance change of the different catalyst degradation rhodamine B of pH value when the preparation of table 3.1
By the relation equation (2.1) of rhodamine B concentration and absorbance that the standard curve of rhodamine B solution obtains：y
=0.2268x-0.0071 can calculate the rhodamine B concentration at each moment in table 3.1, as a result as shown in table 3.2：
The concentration variation of the different catalyst degradation rhodamine B of pH value when the preparation of table 3.2
From experimental result as can be seen that the concentration of rhodamine B, which integrally presents first, reduces the becoming of reducing again of maintaining an equal level afterwards
Gesture.In 0-20min, it is suction-operated due to floating bead that rhodamine B concentration, which reduces, this stage different sample, rhodamine B
Concentration variation it is almost consistent, thus it could be speculated that in preparation process pH value change, to the suction-operated of floating bead almost without
It influences.In 20-60min, the concentration of rhodamine B does not change nearly all, it can be determined that floating bead is to rhodamine B in during this period
Suction-operated had reached adsorption equilibrium.After 60min, since illumination is added, the concentration of rhodamine B reduces again, by
This can prove to truly have photocatalysis under visible light by testing the floating bead being made load bismuth oxybromide composite photo-catalyst
Property.Preparing during catalyst that pH value is different, the photocatalysis performance of sample is also different, when pH is 8, the drift that is made
Pearl loads the photocatalysis performance highest of bismuth oxybromide sample, and pH reduces, and the photocatalysis performance for the sample being made decreases,
When pH reaches 9 higher than 8, the sample photocatalysis performance being made also has decline slightly.Therefore judge, floating bead loads bromine oxidation
The best preparation pH of bismuth is 8.
Compared to the prior art, vitrified agent provided by the invention and preparation method thereof and application method have beneficial below
Effect：Since raw material flyash is the sa hollow glass bead by sorting out in the flyash of coal-burning power plant's discharge,
Its appearance is many in honeycomb hole, and inside has hole more abundant and large specific surface area, and light transmittance is good, surface
Easily film forming, relative low price and quality is lighter, swim in the water surface, are easy to separate with water, as long as from the water surface after reaction
It salvages, can be re-used by being simply heat-treated.So using manufactured by preparation method provided by the present invention
Floating bead load bismuth oxybromide photocatalyst, at low cost, high catalytic efficiency, after recycling performance stablize, in addition, of the invention
The preparation condition proposed can effectively improve floating bead load bismuth oxybromide photocatalyst end properties.
Claims (10)
1. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst, which is characterized in that specifically include following steps：
Step 1：Flyash is poured into the beaker for filling water, is stood after stirring, the floating bead particle floated on the water surface is sub-elected；
Step 2：The floating bead particle sub-elected is immersed in dust technology and is filtered after 10-14h and is dried to obtain floating bead；
Step 3：Five nitric hydrate bismuths, potassium bromide and polyvinylpyrrolidone are added in the reaction vessel for filling ethylene glycol and obtained
Substrate liquid is stirred the substrate liquid；
Step 4：Under conditions of being stirred continuously, adds the floating bead and PH to adjust liquid into the molten substrate and obtain attachment liquid；
Step 5：It filters the attachment liquid and obtains attachment floating bead；
Step 6：Heat preservation obtains concentration floating bead after the attachment floating bead is dried；
Step 7：The concentration floating bead is subjected to rinsing filtering and is dried to obtain finished product.
2. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst as described in claim 1, which is characterized in that used
The water arrived is distilled water.
3. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst as described in claim 1, which is characterized in that in institute
It states in step 2, the floating bead particle after immersion further includes before filtration：It is repeatedly rinsed with distilled water, until rinsing liquid
PH value be neutrality.
4. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst a method according to any one of claims 1-3, feature exist
In the drying temperature range in the step 2 is 90-120 DEG C.
5. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst a method according to any one of claims 1-3, feature exist
In in the step 3, the reaction vessel being placed on universal mixer and is stirred, to be placed on ultrasonic wave clear for stirring
Ultrasonic wave dispersion is carried out in washing machine until the solid in solution is completely dissolved and the color of solution is in yellow.
6. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst a method according to any one of claims 1-3, feature exist
In in the step 4, it is potassium hydroxide that the PH, which adjusts liquid,.
7. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst as described in claim 5 is any, which is characterized in that
In the step 4, the pH value magnitude range of the attachment liquid is 8-10.
8. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst a method according to any one of claims 1-3, feature exist
In in the step 6, drying temperature range is 150-180 DEG C, and soaking time range is 12-18h.
9. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst a method according to any one of claims 1-3, feature exist
In in the step 7, drying temperature range is 90-120 DEG C.
10. a kind of preparation method of floating bead load bismuth oxybromide photocatalyst a method according to any one of claims 1-3, feature exist
In in the step 3, the molar ratio of five nitric hydrate bismuths and potassium bromide is 2:1.
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Citations (1)
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| CN106607063A (en) * | 2015-10-27 | 2017-05-03 | 湖南城市学院 | Floating visible-light-induced photocatalyst, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106607063A (en) * | 2015-10-27 | 2017-05-03 | 湖南城市学院 | Floating visible-light-induced photocatalyst, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 林立: ""新型卤氧化铋基光催化剂制备及其污染物去除性能的研究"", 《中国博士学位论文全文数据库》 * |
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