CN105727927A - Preparation method of netted efficient photocatalyst BiVO4 - Google Patents
Preparation method of netted efficient photocatalyst BiVO4 Download PDFInfo
- Publication number
- CN105727927A CN105727927A CN201610187038.3A CN201610187038A CN105727927A CN 105727927 A CN105727927 A CN 105727927A CN 201610187038 A CN201610187038 A CN 201610187038A CN 105727927 A CN105727927 A CN 105727927A
- Authority
- CN
- China
- Prior art keywords
- bivo
- netted
- preparation
- catalyst
- edta
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 80
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229960001484 edetic acid Drugs 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000002738 chelating agent Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000003980 solgel method Methods 0.000 claims abstract description 9
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000003483 aging Methods 0.000 claims abstract description 3
- 230000032683 aging Effects 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000007788 liquid Substances 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 20
- 238000005352 clarification Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 229910021529 ammonia Inorganic materials 0.000 claims description 10
- 235000005979 Citrus limon Nutrition 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 244000248349 Citrus limon Species 0.000 claims description 8
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 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 description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 4
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 230000002779 inactivation Effects 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract 1
- 239000007857 degradation product Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 235000015096 spirit Nutrition 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000011260 aqueous acid Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 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
- 230000000903 blocking effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to the field of a functional material and specifically relates to a method for preparing a netted efficient photocatalyst BiVO4 through a double-chelating agent sol-gel method. The preparation method comprises the following steps: mixing citric acid with bismuth nitrate pentahydrate and ammonium metavanadate, thereby forming precursor solutions A and B; mixing the precursor solutions A and B, thereby forming a mixed solution C; adding edetic acid into the mixed solution C at twice; adjusting the pH value of the system, thereby forming clear transparent BiVO4 gel; ageing, drying and calcining, thereby acquiring the netted monoclinic scheelite phase BiVO4 catalyst. The preparation method is simple and easily controllable in technique, is free from pollution and has low requirements on equipment; the prepared netted monoclinic scheelite phase BiVO4 catalyst can be used for effectively degrading methylene blue and has excellent photocatalytic activity; by virtue of the feature of multiple pores of the netted structure, a huge diffusion path can be formed, so that in a use process, the blockage of a duct caused by degradation products can be restrained, the catalyst inactivation can be avoided and the catalyst can be reused.
Description
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of double chelating agent sol-gel process and prepare netted high efficiency photocatalyst
BiVO4Method.
Background technology
From 20 century 70s, BiVO4Because it has the structure of uniqueness, physicochemical characteristics, the scientific research personnel couple of various countries
Which create dense research interest.It is the semi-conducting material of a kind of typical layer structure, has corrosion resistance, ferroelasticity
And ionic conductivity, be also simultaneously the visible-light-responsive photocatalyst of a kind of great application prospect, photocatalytic pollutant degradation,
Decomposition water is prepared the field such as hydrogen and oxygen and is caused and pay close attention to widely.
BiVO4Having narrower energy gap and unique crystal structure, it has three kinds of main crystal formations, respectively monocline scheelite
Phase (s-m), four directions zircon phase (z-t) and four directions scheelite phase (s-t), the wherein BiVO of monocline scheelite phase4Energy gap the narrowest,
It is about 2.4eV, shows the most prominent photocatalysis characteristic under visible light illumination, and overcome tradition photochemical catalyst titanium dioxide
The shortcoming that titanium can only absorb ultraviolet light.
There are some researches show, the difference of the pattern of photochemical catalyst, size and structure can directly influence the photocatalysis efficiency of catalyst.
Therefore, the BiVO using multiple method to prepare various special appearance it is attempted in recent years4, to obtaining higher specific surface
Long-pending, construct more carrier catalysis center, thus improve catalytic performance.Synthesis BiVO4The method of photochemical catalyst common are water
Hot method, the precipitation method, colloidal sol--gel method etc., wherein colloidal sol--gel method is extensively applied due to synthesis condition gentleness.Colloidal sol at present
The single citric acid of the many employings of-gel method is that chelating agent prepares BiVO4Powder and film, as silicate journal (Liu Hongyan, 2011,
12:1974-1980) citric acid complex method is used to prepare visible-light-responsive photocatalyst powder, Chinese patent CN 102949991
A uses sol-gel process to prepare the BiVO with photocatalysis performance4Film.
Photocatalysis technology generally uses BiVO4Suspension or immobilization technology such as film, but both approaches is problematic in that:
BiVO in suspension system4Photochemical catalyst is difficult to sedimentation separation, causes cost recovery to increase；Urge although immobilization technology solves
The problem of agent separation and recovery, but be supported on supported catalyst and easily cause inactivation during Long-Time Service, mainly because of
Being combined loosely for catalyst with carrier, during use, catalyst is easy to fall off, and catalyst surface can be contaminated thing blocking, resistance simultaneously
Hinder the species diffusion to reaction active site that is degraded, thus resulted in catalytic efficiency and be greatly lowered.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming existing BiVO4Deposit when suspension system and immobilization photocatalyst for degrading pollutant
Problem, it is provided that a kind of double chelating agent sol-gel processes prepare netted pure monocline scheelite phase BiVO4Light-catalysed method,
Its technique is simple, and preparation condition is gentle.Netted pure monocline scheelite phase BiVO prepared according to the present invention4Have under visible light
High efficiency photocatalysis activity and being easily recycled, thus solve BiVO4Photochemical catalyst is not easily recycled in suspension system and fixes
The problem that after change, photocatalysis efficiency is low.
A kind of netted high efficiency photocatalyst BiVO4Preparation method, use sol-gel process, first by the first chelating agent i.e. lemon
Lemon acid (CA) respectively with five water bismuth nitrate (Bi (NO3)3·5H2O), ammonium metavanadate (NH4VO3) it is mixed to form precursor liquid A
And B；Then A and B is mixed to form mixed solution C；Again by the second chelating agent i.e. ethylenediamine tetra-acetic acid (EDTA) point
Adding for twice in mixed solution C, regulation system pH value forms clear BiVO4Gel；Eventually pass ageing, be dried and forge
Burn, obtain netted monocline scheelite phase BiVO4Catalyst.
Precursor liquid A is by citric acid (CA) and five water bismuth nitrate (Bi (NO3)3·5H2O) according to Bi and citric acid (CA)
Mol ratio is that 1:1.5～3 is dissolved in aqueous solution of nitric acid, stirs until solution clarification obtains, five water bismuth nitrates
(Bi(NO3)3·5H2And the molar concentration of citric acid (CA) is 0.1～0.5mol/L, 0.15～1.5mol/L O).
Precursor liquid B is by citric acid (CA) and ammonium metavanadate (NH4VO3) it is 1 according to V and citric acid (CA) mol ratio:
In 1.5～3 ammonia spirits being dissolved in 80 DEG C, stir until solution clarification obtains, ammonium metavanadate (NH4VO3) and lemon
The molar concentration of lemon acid (CA) is 0.1～0.5mol/L, 0.15～1.5mol/L.
Being that precursor liquid A is dropped in precursor liquid B by 1:1 according to Bi Yu V mol ratio, constant temperature stirs, and obtains navy blue
Mixed solution C.
It is that 4:0.5～1.5 weighs ethylenediamine tetra-acetic acid according to citric acid (CA) and ethylenediamine tetra-acetic acid (EDTA) mol ratio
(EDTA), during wherein half is dissolved in ammonia spirit, the EDTA aqueous solution D that molar concentration is 0.25～1.0mol/L is obtained,
And second half EDTA solid is designated as E.
Under vigorous stirring, being slowly added in mixed solution C by EDTA aqueous solution D, being adjusted to pH with ammoniacal liquor is 5.0～9.0,
Add E, form the BiVO that clarification is well-illuminated4Colloidal sol.
The BiVO that will obtain4Gel stirs 3～6h in 65～85 DEG C of water-baths, is then aged 12～36h at 10～30 DEG C,
Form the navy blue well-illuminated gel of clarification, then in baking oven 80～160 DEG C be dried 1～6h, in Muffle furnace 350～600 DEG C
Calcining 1～6h, thus shape webbed monocline scheelite phase BiVO4Catalyst.
The netted high efficiency photocatalyst BiVO of the present invention4Preparation method, show relative to the beneficial effect of prior art:
The present invention uses double chelating agent sol-gel process to prepare netted monocline scheelite phase BiVO4Photochemical catalyst, the method work
Skill is simple and easy to control, pollution-free, low for equipment requirements.Netted monocline scheelite phase BiVO that the present invention prepares4Can effectively drop
Solving methylene blue, have preferably photocatalytic activity, the most cancellated many mesh feature is beneficial to form the biggest diffusion admittance,
In use can suppress the thing blocking to duct that is degraded, it is to avoid the inactivation of catalyst, can repeatedly use.
Accompanying drawing explanation
Fig. 1 is the XRD that the present invention implements the pure monocline scheelite phase pucherite of preparation.
Fig. 2 is the SEM figure that the present invention implements the pure monocline scheelite phase pucherite of preparation.
Fig. 3 is the photocatalysis that the present invention implements the pure monocline scheelite phase pucherite degradation of methylene blue solution under visible light of preparation
Degradation rate figure.
Detailed description of the invention
Below in conjunction with the accompanying drawings the preferred embodiment of the present invention is described in further detail.
Embodiment 1
Step 1., take the Bi (NO of 0.01mol3)3·5H2O is dissolved in the aqueous solution of nitric acid of 40ml, with the lemon of 0.02mol
Aqueous acid mixing is made into the precursor liquid A that clarification is well-illuminated.
Step 2., by the NH of 0.01mol4VO3It is dissolved in 80 DEG C of ammonia spirits of 40ml, with the citric acid water of 0.02mol
Solution mixing is made into the precursor liquid B that clarification is well-illuminated.
3., dropped in precursor liquid B by precursor liquid A, constant temperature stirs step, obtains navy blue mixed solution C.
Step 4., weigh the EDTA of 0.005mol, during wherein half is dissolved in 10ml ammonia spirit, obtain EDTA water-soluble
Liquid D (molar concentration is 0.25mol/L), and second half EDTA solid is designated as E.
EDTA aqueous solution D 5., under vigorous stirring, is slowly added in mixed solution C by step, is adjusted to pH with ammoniacal liquor and is
7, add E, form the BiVO that clarification is well-illuminated4Colloidal sol.
Step 6., will obtain BiVO4Gel stirs 4.5h in 75 DEG C of water-baths, is then aged 24h at 20 DEG C, is formed
The gel that navy blue clarification is well-illuminated, then 120 DEG C of dry 3h in baking oven, 500 DEG C of calcining 3h in Muffle furnace, thus formed
Netted monocline scheelite phase BiVO4Catalyst.
From the XRD of accompanying drawing 1 it can be seen that prepared sample is pure monocline scheelite phase BiVO4Catalyst, does not has
Observe the existence of other impurity peaks；In spectrogram, each spectral peak is sharp-pointed, illustrates that sample crystallization degree is good.
Scheme it can be seen that prepared BiVO from the SEM of accompanying drawing 24Catalyst has network structure, the netting twine phase of flat
Interweave mutually, define various sizes of mesh.
From the photocatalytic activity figure of accompanying drawing 3 it can be seen that prepared BiVO4Catalyst with methylene blue for simulating pollution thing,
Through 120 minutes, photocatalytic activity reached 94%, showed that photochemical catalyst has preferably photocatalytic activity.
Therefore, it can be seen that molten by double chelating agents from the analysis result of XRD, SEM figure and photocatalytic activity figure
This method simple and easy to control of glue-gel method, can easily prepare netted monocline scheelite phase BiVO4, and there is preferably light
Catalysis activity.
Embodiment 2
Step 1., take the Bi (NO of 0.01mol3)3·5H2O is dissolved in the aqueous solution of nitric acid of 40ml, with the lemon of 0.03mol
Aqueous acid mixing is made into the precursor liquid A that clarification is well-illuminated.
Step 2., by the NH of 0.01mol4VO3It is dissolved in 80 DEG C of ammonia spirits of 100ml, with the citric acid of 0.15mol
Aqueous solution mixing is made into the precursor liquid B that clarification is well-illuminated.
3., dropped in precursor liquid B by precursor liquid A, constant temperature stirs step, obtains navy blue mixed solution C.
Step 4., weigh the EDTA of 0.0675mol, during wherein half is dissolved in 67.5ml ammonia spirit, obtain EDTA water
Solution D (molar concentration is 0.5mol/L), and second half EDTA solid is designated as E.
EDTA aqueous solution D 5., under vigorous stirring, is slowly added in mixed solution C by step, is adjusted to pH with ammoniacal liquor and is
5.5, add E, form the BiVO that clarification is well-illuminated4Colloidal sol.
Step 6., will obtain BiVO4Gel stirs 6h in 70 DEG C of water-baths, is then aged 20h at 15 DEG C, is formed deep
The gel that blue clarification is well-illuminated, then 90 DEG C of dry 6h in baking oven, 550 DEG C of calcining 2h in Muffle furnace, thus formed netted
Monocline scheelite phase BiVO4Catalyst.
Embodiment 3
Step 1., take the Bi (NO of 0.01mol3)3·5H2O is dissolved in the aqueous solution of nitric acid of 100ml, with the lemon of 0.15mol
Aqueous acid mixing is made into the precursor liquid A that clarification is well-illuminated.
Step 2., by the NH of 0.01mol4VO3It is dissolved in 80 DEG C of ammonia spirits of 40ml, with the citric acid water of 0.03mol
Solution mixing is made into the precursor liquid B that clarification is well-illuminated.
3., dropped in precursor liquid B by precursor liquid A, constant temperature stirs step, obtains navy blue mixed solution C.
Step 4., weigh the EDTA of 0.045mol, during wherein half is dissolved in 22.5ml ammonia spirit, obtain EDTA water-soluble
Liquid D (molar concentration is 1mol/L), and second half EDTA solid is designated as E.
EDTA aqueous solution D 5., under vigorous stirring, is slowly added in mixed solution C by step, is adjusted to pH with ammoniacal liquor and is
8.5, add E, form the BiVO that clarification is well-illuminated4Colloidal sol.
Step 6., will obtain BiVO4Gel stirs 3.5h in 85 DEG C of water-baths, is then aged 30h at 25 DEG C, is formed
The gel that navy blue clarification is well-illuminated, then 140 DEG C of dry 2h in baking oven, 400 DEG C of calcining 4h in Muffle furnace, thus formed
Netted monocline scheelite phase BiVO4Catalyst.
The various embodiments described above are simply to illustrate that the technology design of the present invention and feature, and its objective is to be to allow in this area is common
Technical staff will appreciate that present disclosure and implements according to this, can not limit the scope of the invention with this.Every basis
The change of the equivalence done by the essence of present invention or modification, all should contain within the scope of the present invention.
Claims (7)
1. a netted high efficiency photocatalyst BiVO4Preparation method, use sol-gel process, it is characterised in that first
By the first chelating agent i.e. citric acid (CA) respectively with five water bismuth nitrate (Bi (NO3)3·5H2O), ammonium metavanadate (NH4VO3)
It is mixed to form precursor liquid A and B；Then A and B is mixed to form mixed solution C；Again by the second chelating agent i.e. second two
Amine tetraacethyl (EDTA) adds in mixed solution C at twice, and regulation system pH value forms clear BiVO4Gel；
Eventually pass ageing, drying and calcining, obtain netted monocline scheelite phase BiVO4Catalyst.
Netted high efficiency photocatalyst BiVO the most as claimed in claim 14Preparation method, it is characterised in that precursor liquid A
It is by citric acid (CA) and five water bismuth nitrate (Bi (NO3)3·5H2O) it is 1 according to Bi and citric acid (CA) mol ratio:
1.5～3 are dissolved in aqueous solution of nitric acid, stir until solution clarification obtains, five water bismuth nitrate (Bi (NO3)3·5H2O)
It is 0.1～0.5mol/L, 0.15～1.5mol/L with the molar concentration of citric acid (CA).
Netted high efficiency photocatalyst BiVO the most as claimed in claim 14Preparation method, it is characterised in that precursor liquid B
It is by citric acid (CA) and ammonium metavanadate (NH4VO3) it is 1:1.5～3 according to V and citric acid (CA) mol ratio
It is dissolved in the ammonia spirit of 80 DEG C, stirs until solution clarification obtains, ammonium metavanadate (NH4VO3) and lemon
The molar concentration of acid (CA) is 0.1～0.5mol/L, 0.15～1.5mol/L.
4. the netted high efficiency photocatalyst BiVO as described in claim 1 or 2 or 34Preparation method, it is characterised in that
Being that precursor liquid A is dropped in precursor liquid B by 1:1 according to Bi Yu V mol ratio, constant temperature stirs, and obtains navy blue
Mixed solution C.
Netted high efficiency photocatalyst BiVO the most as claimed in claim 14Preparation method, it is characterised in that according to lemon
Acid (CA) and ethylenediamine tetra-acetic acid (EDTA) mol ratio are that 4:0.5～1.5 weighs ethylenediamine tetra-acetic acid (EDTA),
During wherein half is dissolved in ammonia spirit, obtain the EDTA aqueous solution D that molar concentration is 0.25～1.0mol/L, and another
Half EDTA solid is designated as E.
Netted high efficiency photocatalyst BiVO the most as claimed in claim 54Preparation method, it is characterised in that strongly stirring
Mixing down, be slowly added in mixed solution C by EDTA aqueous solution D, being adjusted to pH with ammoniacal liquor is 5.0～9.0, adds E,
Form the BiVO that clarification is well-illuminated4Colloidal sol.
The preparation method of netted high efficiency photocatalyst BiVO4 the most as claimed in claim 1, it is characterised in that will obtain
BiVO4Gel stirs 3～6h in 65～85 DEG C of water-baths, is then aged 12～36h at 10～30 DEG C, is formed
The gel that navy blue clarification is well-illuminated, then 80～160 DEG C dry 1～6h in baking oven, forges for 350～600 DEG C in Muffle furnace
Burning 1～6h, thus shape webbed monocline scheelite phase BiVO4Catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610187038.3A CN105727927B (en) | 2016-03-27 | 2016-03-27 | A kind of netted high efficiency photocatalyst BiVO4Preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610187038.3A CN105727927B (en) | 2016-03-27 | 2016-03-27 | A kind of netted high efficiency photocatalyst BiVO4Preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105727927A true CN105727927A (en) | 2016-07-06 |
| CN105727927B CN105727927B (en) | 2017-11-21 |
Family
ID=56252243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610187038.3A Active CN105727927B (en) | 2016-03-27 | 2016-03-27 | A kind of netted high efficiency photocatalyst BiVO4Preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105727927B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622231A (en) * | 2016-12-30 | 2017-05-10 | 温州大学 | Synthesis and application of Pt/BiVO4 composite photocatalyst adopting laminar structure |
| CN108842158A (en) * | 2018-06-05 | 2018-11-20 | 南京航空航天大学 | A kind of BiVO being precipitated for photoelectrocatalysis oxygen4-Al2O3-Ni4O4Laminated film and preparation method thereof |
| CN109772294A (en) * | 2019-03-18 | 2019-05-21 | 济南大学 | The preparation method and products obtained therefrom of a kind of tetragonal phase BiVO4 film with p-type conductivity and application |
| CN114042459A (en) * | 2021-11-22 | 2022-02-15 | 合肥学院 | Quasi-dendritic soft magnetic Sr2FeMoO6Preparation method of efficient visible light catalyst |
| CN115155561A (en) * | 2022-08-11 | 2022-10-11 | 合肥学院 | Gd and Ce ion co-doped efficient visible-light-driven photocatalyst BiVO 4 Preparation method of (2) |
| CN116060019A (en) * | 2023-03-15 | 2023-05-05 | 天津大学 | Supported multi-metal oxide series catalyst and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683074A (en) * | 2005-03-11 | 2005-10-19 | 南京大学 | Process for preparing visible light responding photo catalytic film layer |
| CN102949991A (en) * | 2012-11-09 | 2013-03-06 | 陕西科技大学 | Method for preparing BiVO4 film with photocatalysis performance by using sol-gel method |
-
2016
- 2016-03-27 CN CN201610187038.3A patent/CN105727927B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683074A (en) * | 2005-03-11 | 2005-10-19 | 南京大学 | Process for preparing visible light responding photo catalytic film layer |
| CN102949991A (en) * | 2012-11-09 | 2013-03-06 | 陕西科技大学 | Method for preparing BiVO4 film with photocatalysis performance by using sol-gel method |
Non-Patent Citations (1)
| Title |
|---|
| SAYURI OKUNAKA ET AL.,: "Preparation of fine particles of sheelite-monoclinic phase BiVO4 via an aqueous chelating method for efficient photocatalytic oxygen evolution under visible-light irradiation", 《J. MATER. CHEM. A》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622231A (en) * | 2016-12-30 | 2017-05-10 | 温州大学 | Synthesis and application of Pt/BiVO4 composite photocatalyst adopting laminar structure |
| CN106622231B (en) * | 2016-12-30 | 2019-06-07 | 温州大学 | Pt/BiVO4The synthesis and its application of laminated structure composite photo-catalyst |
| CN108842158A (en) * | 2018-06-05 | 2018-11-20 | 南京航空航天大学 | A kind of BiVO being precipitated for photoelectrocatalysis oxygen4-Al2O3-Ni4O4Laminated film and preparation method thereof |
| CN108842158B (en) * | 2018-06-05 | 2020-03-10 | 南京航空航天大学 | BiVO for photoelectrocatalytic oxygen evolution4-Al2O3-Ni4O4Composite film and preparation method thereof |
| CN109772294A (en) * | 2019-03-18 | 2019-05-21 | 济南大学 | The preparation method and products obtained therefrom of a kind of tetragonal phase BiVO4 film with p-type conductivity and application |
| CN109772294B (en) * | 2019-03-18 | 2021-12-07 | 济南大学 | Preparation method of tetragonal phase BiVO4 film with p-type conductivity, obtained product and application |
| CN114042459A (en) * | 2021-11-22 | 2022-02-15 | 合肥学院 | Quasi-dendritic soft magnetic Sr2FeMoO6Preparation method of efficient visible light catalyst |
| CN114042459B (en) * | 2021-11-22 | 2024-01-05 | 合肥学院 | Tree-like soft magnetic Sr 2 FeMoO 6 Preparation method of efficient visible light catalyst |
| CN115155561A (en) * | 2022-08-11 | 2022-10-11 | 合肥学院 | Gd and Ce ion co-doped efficient visible-light-driven photocatalyst BiVO 4 Preparation method of (2) |
| CN116060019A (en) * | 2023-03-15 | 2023-05-05 | 天津大学 | Supported multi-metal oxide series catalyst and preparation method and application thereof |
| CN116060019B (en) * | 2023-03-15 | 2024-05-21 | 天津大学 | Supported multi-metal oxide series catalyst and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105727927B (en) | 2017-11-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105727927A (en) | Preparation method of netted efficient photocatalyst BiVO4 | |
| CN108940338B (en) | Potassium-doped porous carbon nitride photocatalyst and preparation method and application thereof | |
| CN103539210B (en) | A kind of preparation method of cobalt molybdate crystallite | |
| CN101927177B (en) | Preparation method of nitrogen-doped attapulgite load nano TiO2 visible light photocatalyst | |
| CN103480353A (en) | Method for synthesis of carbon quantum dot solution by hydrothermal process to prepare composite nano-photocatalyst | |
| CN104307564B (en) | A kind of Cu-SAPO-34 catalyst of auxiliary agent doping and its preparation method and application | |
| CN102949991A (en) | Method for preparing BiVO4 film with photocatalysis performance by using sol-gel method | |
| CN101791548A (en) | Visible light catalyst BiVO4 and preparation method thereof | |
| CN102698785A (en) | Preparation method of diatomite-loaded nitrogen-doped nanometer TiO2 photocatalysis material | |
| CN104307501B (en) | A kind of preparation method of the nano zine oxide as photochemical catalyst | |
| CN102728342A (en) | Preparation method of bismuth vanadate visible light photocatalysis material | |
| CN104148054A (en) | Preparation method of bismuth vanadate nanorod bundle | |
| CN106076318A (en) | A kind of preparation method of integral catalyzer | |
| CN102553604A (en) | Method for implementing Cu<2+> doping modification on BiVO4 photocatalyst by using microwave hydrothermal method | |
| CN103240073A (en) | Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof | |
| CN102698784A (en) | Visible light response catalyst and preparation method thereof | |
| CN103736480B (en) | A kind of corner star pucherite as catalysis material and preparation method thereof | |
| CN103240105A (en) | Preparation method of hollow silver phosphotungstate visible-light-induced photocatalyst | |
| CN105502468B (en) | A kind of ceric oxide nanorod and its preparation method and application | |
| CN106975509B (en) | Preparation method and application of nitrogen and iron co-doped bismuth vanadate visible-light-driven photocatalyst | |
| CN107215896A (en) | The regulation and control method of monoclinic phase pucherite appearance structure transformation | |
| CN102765758A (en) | Sol-gel-hydrothermal method for preparing bismuth tungstate and indium-doped bismuth tungstate | |
| CN107552042B (en) | Sheet manganese titanate coats attapulgite loaded CeO2Low temperature Photo-SCR denitrating catalyst and preparation method | |
| CN105214644A (en) | Modified titanium and its preparation method and application | |
| CN102527421A (en) | C and N dual-doped nano TiO2 photochemical catalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |