CN105148950A - Preparing method for flower-shaped BiOI microspheres - Google Patents
Preparing method for flower-shaped BiOI microspheres Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 10
- 239000004005 microsphere Substances 0.000 title abstract description 10
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 38
- 239000002608 ionic liquid Substances 0.000 claims abstract description 24
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 55
- 238000002360 preparation method Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 14
- HWIUYZBEKKGMCW-UHFFFAOYSA-N CN1CN(C=C1)CCCC.I(=O)(=O)O Chemical compound CN1CN(C=C1)CCCC.I(=O)(=O)O HWIUYZBEKKGMCW-UHFFFAOYSA-N 0.000 claims description 13
- 150000002500 ions Chemical class 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000000593 microemulsion method Methods 0.000 abstract description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 229910052740 iodine Inorganic materials 0.000 abstract 1
- 239000011630 iodine Substances 0.000 abstract 1
- 239000002736 nonionic surfactant Substances 0.000 abstract 1
- ORZGULPODBRYCV-UHFFFAOYSA-M bismuth;oxygen(2-);iodide Chemical compound [O-2].[I-].[Bi+3] ORZGULPODBRYCV-UHFFFAOYSA-M 0.000 description 56
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- 230000007613 environmental effect Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000003911 water pollution Methods 0.000 description 6
- 238000003905 indoor air pollution Methods 0.000 description 5
- 230000005291 magnetic effect Effects 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- UOZDOLIXBYLRAC-UHFFFAOYSA-L [2-hydroxy-3-(trimethylazaniumyl)propyl]-trimethylazanium;diiodide Chemical compound [I-].[I-].C[N+](C)(C)CC(O)C[N+](C)(C)C UOZDOLIXBYLRAC-UHFFFAOYSA-L 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [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 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 101100001677 Emericella variicolor andL gene Proteins 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000004064 cosurfactant Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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Abstract
The invention relates to a preparing method for flower-shaped BiOI microspheres, and belongs to the field of nanometer photocatalytic material preparing. The preparing method includes the following specific preparing steps that bismuth nitrate is added into nitric acid to obtain a solution A; ionic liquid [Bmin]I and nonionic surfactants PVP are added into distilled water, heated and stirred to form micro-emulsion B; then the solution A and the micro-emulsion B are mixed to be poured into a high pressure kettle, the pH is controlled to range from 1 to 4, centrifuging, washing and drying are carried out after a hydrothermal reaction, and the flower-shaped BiOI microspheres are obtained. According to the preparing method, an ionic liquid micro-emulsion method is adopted for the first time, no organic solvent is added, and the environment-friendly requirement is met; ionic liquid is used as an iodine source and solvents, is also used as an oil phase to form micro-emulsion drops and has the important effect on forming of the flower-shaped BiOI microspheres; the prepared flower-shaped BiOI microspheres have the high application value in the fields of pollution treatment, new energy preparing, selectivity catalytic oxidation and the like.
Description
Technical field
The invention belongs to nano-photocatalyst material preparation field, be specifically related to a kind of preparation method of flower-shaped BiOI microballoon.
Background technology
Along with developing rapidly of industry now, the mankind, while the huge civilization of creation and wealth, also bring day by day serious environmental problem.Particularly water pollution problems, more and more causes the concern of people.Photocatalitic Technique of Semiconductor has remarkable result in some Recalcitrant chemicals in process water.At present, TiO
2be research the most extensively, the most deep a kind of photochemical catalyst.But the band gap of titanium dioxide is very wide, only to ultraviolet light response, and can not absorb in sunshine and account for most visible ray, greatly limit TiO
2practical application.Therefore, seeking new and effective visible light catalyst is the inexorable trend further developed.
Bismuthyl iodide (BiOI) is a kind of important V-VI-VII ternary compound, and in tetragonal structure structure, its crystal structure is by Bi
2o
2the layer structure that layer is formed with the double-deck halogen atom intersected at wherein.BiOI is as a kind of novel semi-conducting material, and because it has unique electronic structure, excellent electricity, magnetics, optics, catalysis and luminescent properties, attracted the extensive concern of researcher.Up to now, people have prepared the BiOI micro nano structure of different-shape by diverse ways.Zhang etc. (XZhang, Z.H.Ai, F.L.Jia, andL.ZZhang, J.Phys.Chem.C, 2008,112,747-753) the spent glycol BiOI microballoon that has been aqueous solvent thermal synthesis, and show good photocatalytic activity; (XXiaoandW.D.Zhang, J.Mater.Chem., 2010 such as Xiao, 20,5866-5870) in alcohol-water reaction system, regulate presoma pH by ammoniacal liquor, prepare 3DBiOI microballoon, under visible light degradation of phenol, show good photocatalytic activity.
In recent years, microemulsion method has been widely applied to by people on the material of synthesis special construction.This microemulsion is transparent dispersion, be by two kinds and two or more immiscible liquid at a certain amount of surfactant or have cosurfactant to mix once in a while, spontaneous formation optically isotropic, transparent in thermodynamically stable system.But, be that template is synthesized BiOI microballoon under hydrothermal conditions there is not been reported with ion liquid microemulsion.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of flower-shaped BiOI microballoon.
For solving the problem, technical scheme provided by the invention is:
The first step, bismuth nitrate is dissolved in acid solution, obtains solution A;
Second step, be dissolved in distilled water by ionic liquid iodate 1-butyl-3-methylimidazole and non-ionic surface active agent PVP, normal temperature magnetic agitation 1h forms microemulsion B; In course of reaction, ionic liquid [Bmin] I is not only used as propiodal and solvent, also forms microemulsion B, to the formation important role of flower-shaped BiOI microballoon as oil phase simultaneously.
3rd step, solution A mixed with microemulsion B, wherein the volume ratio of solution A and microemulsion B is 1:5, and control pH is 1-4, stirs;
4th step, pour in autoclave, hydro-thermal reaction;
5th step, washing, centrifugal, dry, obtain flower-shaped BiOI microballoon.
Flower-shaped BiOI microballoon prepared by the present invention not only can be used in treating indoor air pollution as visible light catalyst, and also has higher using value in water pollution control, new forms of energy and selective catalytic oxidation etc.
Preferably, acid solution described in the first step is salpeter solution, wherein, described nitric acid and the mol ratio of bismuth nitrate are 2:1, because hydrochloric acid, sulfuric acid all react to be formed with bismuth nitrate and precipitates, be unfavorable for the preparation of flower-shaped BiOI microballoon, so adopt nitric acid, and concentration of nitric acid is higher than the concentration of bismuth nitrate, make bismuth nitrate easily molten.
Preferably, 2molL is used during control pH in the 3rd step
-1naOH solution regulate.Also the NaOH solution of other concentration can be adopted.
Preferably, the mol ratio of described bismuth nitrate and ionic liquid iodate 1-butyl-3-methylimidazole is 1:1 ~ 2.
Preferably, in second step, the described quality of ionic liquid iodate 1-butyl-3-methylimidazole and the ratio of the volume of distilled water are 0.533 ~ 1.065:25g/mL, and the mass ratio of ionic liquid iodate 1-butyl-3-methylimidazole and PVP is 1:0.2 ~ 1.5.
Preferably, in the 3rd step, described solution A and microemulsion B mixing condition are: under stirring, solution A is dropwise joined microemulsion B, form brick-red suspension, and stir and make it fully react in 1-2 hour, then load in autoclave.
Preferably, in the 4th step, described hydro-thermal reaction is by the mixed solution in autoclave, is placed in baking oven and reacts, and the temperature of hydro-thermal reaction is 100-160 DEG C in an oven, 12 hours reaction time.Adopt ion liquid microemulsion drop to be soft template first, do not add any organic solvent, synthesized flower-shaped BiOI microballoon catalysis material under hydrothermal conditions, met the requirement of environmental protection.
Preferably, the product after hydro-thermal reaction by deionized water and absolute ethanol washing, removes foreign ion and surfactant PVP, then carries out centrifugal, dries afterwards, namely obtain flower-shaped BiOI microballoon at 60 DEG C.Adopt the flower-shaped BiOI microballoon prepared by said method, its crystal formation and standard powder diffraction card (JCPDSCardNO.10-0445) fit like a glove.
The present invention is with bismuth nitrate and ionic liquid for raw material, and in hydro-thermal, next step has synthesized flower-shaped BiOI microballoon.Compare with the preparation method of traditional BiOX, the present invention adopts ion liquid microemulsion drop to be soft template, does not add any organic solvent, mild condition, course of reaction is simple, and meet the requirement of environmental protection, single step reaction just can obtain the catalyst of higher degree.
Gained flower-like microsphere of the present invention is compared with other patterns, and have larger specific area, improve absorption property, therefore photocatalytic activity significantly improves.Flower-shaped BiOI microballoon not only can be used in treating indoor air pollution as visible light catalyst, and also has higher using value in water pollution control, new forms of energy and selective catalytic oxidation etc.;
Flower-shaped BiOI microballoon prepared by the present invention, its crystal formation and standard powder diffraction card (JCPDSCardNO.10-0445) fit like a glove.
3. beneficial effect
Adopt technical scheme provided by the invention, compared with prior art, there is following beneficial effect:
(1) ionic liquid iodate 1-butyl-3-methylimidazole and non-ionic surface active agent PVP are dissolved in distilled water by the present invention, and normal temperature magnetic agitation 1h forms microemulsion B; In course of reaction, ionic liquid [Bmin] I is not only used as propiodal and solvent, also forms microemulsion B, to the formation important role of flower-shaped BiOI microballoon as oil phase simultaneously;
(2) the flower-shaped BiOI microballoon that prepared by the present invention not only can be used in treating indoor air pollution as visible light catalyst, and also has higher using value in water pollution control, new forms of energy and selective catalytic oxidation etc.;
(3) acid solution described in the first step of the present invention is salpeter solution, wherein, described nitric acid and the mol ratio of bismuth nitrate are 2:1, because hydrochloric acid, sulfuric acid all react to be formed with bismuth nitrate and precipitate, be unfavorable for the preparation of flower-shaped BiOI microballoon, so adopt nitric acid, and concentration of nitric acid is higher than the concentration of bismuth nitrate, make bismuth nitrate easily molten, be more conducive to the preparation of flower-shaped BiOI microballoon;
(4) hydro-thermal reaction of the present invention is by the mixed solution in autoclave, be placed in baking oven to react, the temperature of hydro-thermal reaction is 100-160 DEG C in an oven, 12 hours reaction time, ion liquid microemulsion drop is adopted to be soft template first, do not add any organic solvent, synthesized flower-shaped BiOI microballoon catalysis material under hydrothermal conditions, met the requirement of environmental protection;
(5) the present invention is with bismuth nitrate and ionic liquid for raw material, and in hydro-thermal, next step has synthesized flower-shaped BiOI microballoon.Compare with the preparation method of traditional BiOX, the present invention adopts ion liquid microemulsion drop to be soft template, does not add any organic solvent, mild condition, course of reaction is simple, and meet the requirement of environmental protection, single step reaction just can obtain the catalyst of higher degree;
(6) gained flower-like microsphere of the present invention is compared with other patterns, and have larger specific area, improve absorption property, therefore photocatalytic activity significantly improves.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction spectrogram of flower-shaped BiOI microballoon prepared by the present invention;
Fig. 2 is ESEM (SEM) figure of flower-shaped BiOI microballoon prepared by the embodiment of the present invention 1;
Fig. 3 is ESEM (SEM) enlarged drawing of flower-shaped BiOI microballoon prepared by the embodiment of the present invention 1;
Fig. 4 is the specific surface figure of flower-shaped BiOI microballoon prepared by the embodiment of the present invention 1;
Fig. 5 is the graph of pore diameter distribution of flower-shaped BiOI microballoon prepared by inventive embodiments 1.
Detailed description of the invention
For understanding content of the present invention further, by reference to the accompanying drawings and embodiment the present invention is described in detail.
Embodiment 1
A preparation method for flower-shaped BiOI microballoon, the steps include:
The first step, bismuth nitrate is dissolved in acid solution, obtains solution A; Acid solution is salpeter solution, and wherein, described nitric acid and the mol ratio of bismuth nitrate are 2:1, because hydrochloric acid, sulfuric acid all react to be formed with bismuth nitrate and precipitates, be unfavorable for the preparation of flower-shaped BiOI microballoon, so adopt nitric acid, and concentration of nitric acid is higher than the concentration of bismuth nitrate, make bismuth nitrate easily molten.
Second step, be dissolved in distilled water by ionic liquid iodate 1-butyl-3-methylimidazole and non-ionic surface active agent PVP, normal temperature magnetic agitation 1h forms microemulsion B; The ratio of the quality of ionic liquid iodate 1-butyl-3-methylimidazole and the volume of distilled water is 0.533 ~ 1.065:25g/mL, and the mass ratio of ionic liquid iodate 1-butyl-3-methylimidazole and PVP is 1:0.2 ~ 1.5; In course of reaction, ionic liquid [Bmin] I is not only used as propiodal and solvent, also forms microemulsion B, to the formation important role of flower-shaped BiOI microballoon as oil phase simultaneously.
3rd step, solution A mixed with microemulsion B, wherein the volume ratio of solution A and microemulsion B is 1:5, and control pH is 1-4, stirs; 2molL is used during control pH
-1naOH solution regulate, also can adopt the NaOH solution of other concentration; The mol ratio of bismuth nitrate and ionic liquid iodate 1-butyl-3-methylimidazole is 1:1 ~ 2; Solution A and microemulsion B mixing condition are: under stirring, solution A is dropwise joined microemulsion B, form brick-red suspension, and stir and make it fully react in 1-2 hour.
4th step, pour in autoclave, hydro-thermal reaction; Hydro-thermal reaction is by the mixed solution in autoclave, is placed in baking oven and reacts, and the temperature of hydro-thermal reaction is 100-160 DEG C in an oven, 12 hours reaction time.Adopt ion liquid microemulsion drop to be soft template first, do not add any organic solvent, synthesized flower-shaped BiOI microballoon catalysis material under hydrothermal conditions, met the requirement of environmental protection.
5th step, washing, centrifugal, dry, obtain flower-shaped BiOI microballoon.The product after hydro-thermal reaction by deionized water and absolute ethanol washing, removes foreign ion and surfactant PVP, then carries out centrifugal, dries afterwards, namely obtain flower-shaped BiOI microballoon at 60 DEG C.Adopt the flower-shaped BiOI microballoon prepared by said method, its crystal formation and standard powder diffraction card (JCPDSCardNO.10-0445) fit like a glove.
Flower-shaped BiOI microballoon prepared by the present invention not only can be used in treating indoor air pollution as visible light catalyst, and also has higher using value in water pollution control, new forms of energy and selective catalytic oxidation etc.
The present invention is with bismuth nitrate and ionic liquid for raw material, and in hydro-thermal, next step has synthesized flower-shaped BiOI microballoon.Compare with the preparation method of traditional BiOX, the present invention adopts ion liquid microemulsion drop to be soft template, does not add any organic solvent, mild condition, course of reaction is simple, and meet the requirement of environmental protection, single step reaction just can obtain the catalyst of higher degree.
Gained flower-like microsphere of the present invention, compared with other patterns, has larger specific area, and specific area is 29.7m
2/ g, improves absorption property, is therefore conducive to improving photocatalytic activity.Flower-shaped BiOI microballoon not only can be used in treating indoor air pollution as visible light catalyst, and also has higher using value in water pollution control, new forms of energy and selective catalytic oxidation etc.
In the present embodiment, by 2mmolBi (NO
3)
3, Bi (NO
3)
3molecular weight is 485, and namely quality is 0.97gBi (NO
3)
3be dissolved in 5mL nitric acid (0.8molL
-1) in solution, obtain solution A; The molecular weight of 0.692g ionic liquid [Bmin] I, [Bmin] Cl is 174.67, and namely molal weight is 4mmol, is dissolved in 25mL distilled water, normal temperature magnetic agitation 1h, obtains microemulsion B by 0.692g ionic liquid [Bmin] I and 0.5gPVP; Use the method for the 3rd step to mix with microemulsion B solution A again, use 2molL
-1naOH solution regulate pH to be 3, stir after 1h, obtain equally distributed solution.Above-mentioned solution is poured in 50mL autoclave, hydro-thermal 12h at the temperature of 120 DEG C.Reaction terminates rear deionized water and absolute ethanol washing product, filters, and dries, namely obtains flower-shaped BiOI microballoon.
Fig. 1 is the XRD spectra of flower-shaped BiOI microballoon prepared by the embodiment of the present invention 1, and as we know from the figure, the flower-shaped BiOI microballoon obtained is BiOI tetragonal phase (JCPDSCardNO.10-0445), and free from admixture generates.
Fig. 2 is the SEM figure of flower-shaped BiOI microballoon prepared by the embodiment of the present invention 1, and Fig. 3 is the enlarged drawing of Fig. 2, and as can be seen from Fig. 2 and Fig. 3, BiOI prepared by the present embodiment is the flower-like microsphere of nanometer sheet enrichment.
Fig. 4 is the specific surface figure of flower-shaped BiOI microballoon prepared by the embodiment of the present invention 1, and Fig. 5 is graph of pore diameter distribution, and as can be seen from Fig. 4 and Fig. 5, prepared BiOI has larger specific area and pore volume.Fig. 4 and Fig. 5 is the nitrogen adsorption desorption performance of the flower-shaped BiOI microballoon of gained of the present invention, shows that the BiOI of flower-like microsphere structure is greatly improved relative to common laminated structure BiOI (sheet BiOI specific area is generally at below 10m2/g) specific area.
Embodiment 2:
The method of flower-shaped BiOI microballoon is prepared with embodiment 1, wherein, by 0.97gBi (NO in the present embodiment
3)
3be dissolved in 5mL nitric acid (0.8molL
-1) in solution, obtain solution A; 0.533g [Bmin] I and 0.107gPVP is dissolved in 25mL water, obtains microemulsion B; Again solution A is mixed with microemulsion B, use 2molL
-1naOH solution regulate pH to be 1, stir after 2h, obtain equally distributed solution.Above-mentioned solution is poured in 50mL autoclave, hydro-thermal 12h at the temperature of 100 DEG C.Reaction terminates rear secondary deionized water and absolute ethanol washing product, filters, and dries, namely obtains flower-shaped BiOI microballoon.
Embodiment 3:
By 0.97gBi (NO
3)
3be dissolved in 5mL nitric acid (0.8molL
-1) in solution, obtain solution A; 0.8g [Bmin] I and 0.8gPVP is dissolved in 25mL water, obtains microemulsion B; Again solution A is mixed with microemulsion B, use 2molL
-1naOH solution regulate pH to be 2, stir after 1.5, obtain equally distributed solution.Above-mentioned solution is poured in 50mL autoclave, hydro-thermal 12h at the temperature of 140 DEG C.Reaction terminates rear secondary deionized water and absolute ethanol washing product, filters, and dries, namely obtains flower-shaped BiOI microballoon.
Embodiment 4:
By 1.55gBi (NO
3)
3be dissolved in 7.5mL nitric acid (0.8molL
-1) in solution, obtain solution A; 1.07g [Bmin] I and 1.60gPVP is dissolved in 25mL water, obtains microemulsion B; Again solution A is mixed with microemulsion B, use 2molL
-1naOH solution regulate pH to be 4, stir after 1.7h, obtain equally distributed solution.Above-mentioned solution is poured in 50mL autoclave, hydro-thermal 12h at the temperature of 160 DEG C.Reaction terminates rear secondary deionized water and absolute ethanol washing product, filters, and dries, namely obtains flower-shaped BiOI microballoon.
Schematically above be described the present invention and embodiment thereof, this description does not have restricted, and also just one of the embodiments of the present invention shown in accompanying drawing, actual structure is not limited thereto.So, if those of ordinary skill in the art enlightens by it, when not departing from the invention aim, designing the frame mode similar to this technical scheme and embodiment without creationary, all should protection scope of the present invention be belonged to.
Claims (8)
1. a preparation method for flower-shaped BiOI microballoon, the steps include:
The first step, bismuth nitrate is dissolved in acid solution, obtains solution A;
Second step, ionic liquid iodate 1-butyl-3-methylimidazole and non-ionic surface active agent PVP are dissolved in distilled water, stir and form microemulsion B;
3rd step, solution A mixed with microemulsion B, wherein the volume ratio of solution A and microemulsion B is 1:5, and control pH is 1-4, stirs;
4th step, pour in autoclave, hydro-thermal reaction;
5th step, washing, centrifugal, dry, obtain flower-shaped BiOI microballoon.
2. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 1, it is characterized in that: the acid solution described in the first step is salpeter solution, described nitric acid and the mol ratio of bismuth nitrate are 2:1.
3. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 1, is characterized in that: use 2molL during control pH in the 3rd step
-1naOH solution regulate.
4. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 1, is characterized in that: the mol ratio of described bismuth nitrate and ionic liquid iodate 1-butyl-3-methylimidazole is 1:1 ~ 2.
5. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 2, it is characterized in that: in second step, the described quality of ionic liquid iodate 1-butyl-3-methylimidazole and the ratio of the volume of distilled water are 0.533 ~ 1.065:25g/mL, and the mass ratio of ionic liquid iodate 1-butyl-3-methylimidazole and PVP is 1:0.2 ~ 1.5.
6. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 1, it is characterized in that: in the 3rd step, described solution A and microemulsion B mixing condition are: under stirring, solution A is dropwise joined microemulsion B, form brick-red suspension, and stir and make it fully react in 1-2 hour, then load in autoclave.
7. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 1, it is characterized in that: in the 4th step, described hydro-thermal reaction is by the mixed solution in autoclave, is placed in baking oven and reacts, the temperature of hydro-thermal reaction is 100-160 DEG C in an oven, 12 hours reaction time.
8. the preparation method of a kind of flower-shaped BiOI microballoon according to claim 1-7 any one, it is characterized in that: with deionized water and the product of absolute ethanol washing after hydro-thermal reaction, remove foreign ion and surfactant PVP, then carry out centrifugal, dry at 60 DEG C afterwards, namely obtain flower-shaped BiOI microballoon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510638584.XA CN105148950A (en) | 2015-09-30 | 2015-09-30 | Preparing method for flower-shaped BiOI microspheres |
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| CN105536824A (en) * | 2015-12-30 | 2016-05-04 | 陕西师范大学 | Nano mesoporous microspherical Bi5O7I photocatalyst and hydrothermal-thermal decomposition preparation method thereof |
| CN105664979A (en) * | 2015-12-30 | 2016-06-15 | 陕西师范大学 | Nano-mesoporous micro-spherical Ln-Bi5O7I photocatalyst and preparation method thereof |
| CN105688948A (en) * | 2015-12-29 | 2016-06-22 | 中国科学院海洋研究所 | Photocatalyst and preparing method and application thereof |
| CN107321369A (en) * | 2017-07-06 | 2017-11-07 | 盐城师范学院 | A kind of preparation method and applications of bismuthyl bromide photochemical catalyst |
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| CN108355685A (en) * | 2018-03-13 | 2018-08-03 | 江苏建筑职业技术学院 | A kind of preparation method of composite photo-catalyst |
| CN109395749A (en) * | 2017-08-18 | 2019-03-01 | 中国科学技术大学 | Oxyhalogen bismuth nano material, preparation method and application |
| CN110433830A (en) * | 2019-08-19 | 2019-11-12 | 上海电力大学 | Preparation method of modified flower-shaped bismuth oxyiodide photocatalyst |
| CN111617783A (en) * | 2020-06-05 | 2020-09-04 | 吉林大学 | Dark red BiOI submicron sphere catalyst containing oxygen vacancies, preparation method and application thereof in hydrogen production by photocatalytic water decomposition |
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| CN105688948A (en) * | 2015-12-29 | 2016-06-22 | 中国科学院海洋研究所 | Photocatalyst and preparing method and application thereof |
| CN105664979B (en) * | 2015-12-30 | 2018-07-10 | 陕西师范大学 | A kind of mesoporous nano microspheroidal Ln-Bi5O7I photochemical catalysts and preparation method thereof |
| CN105664979A (en) * | 2015-12-30 | 2016-06-15 | 陕西师范大学 | Nano-mesoporous micro-spherical Ln-Bi5O7I photocatalyst and preparation method thereof |
| CN105536824A (en) * | 2015-12-30 | 2016-05-04 | 陕西师范大学 | Nano mesoporous microspherical Bi5O7I photocatalyst and hydrothermal-thermal decomposition preparation method thereof |
| CN107321369A (en) * | 2017-07-06 | 2017-11-07 | 盐城师范学院 | A kind of preparation method and applications of bismuthyl bromide photochemical catalyst |
| CN109395749A (en) * | 2017-08-18 | 2019-03-01 | 中国科学技术大学 | Oxyhalogen bismuth nano material, preparation method and application |
| CN109395749B (en) * | 2017-08-18 | 2020-08-28 | 中国科学技术大学 | Bismuth oxyhalide nano material, preparation method and application thereof |
| CN107583655A (en) * | 2017-11-02 | 2018-01-16 | 西南石油大学 | Modified BiOX matrix composite photochemical catalyst and its preparation method and application |
| CN107583655B (en) * | 2017-11-02 | 2018-07-31 | 西南石油大学 | Modified BiOX matrix composite photochemical catalyst and its preparation method and application |
| CN108355685A (en) * | 2018-03-13 | 2018-08-03 | 江苏建筑职业技术学院 | A kind of preparation method of composite photo-catalyst |
| CN110433830A (en) * | 2019-08-19 | 2019-11-12 | 上海电力大学 | Preparation method of modified flower-shaped bismuth oxyiodide photocatalyst |
| CN111617783A (en) * | 2020-06-05 | 2020-09-04 | 吉林大学 | Dark red BiOI submicron sphere catalyst containing oxygen vacancies, preparation method and application thereof in hydrogen production by photocatalytic water decomposition |
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