CN104772134B - Method for massively preparing mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst - Google Patents
Method for massively preparing mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst Download PDFInfo
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Abstract
The invention relates to a method for massively preparing a mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst. The method for massively preparing the mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst takes metal inorganic salt-bismuth nitrate pentahydrate (Bi (NO3) 3.5H2O) as a reaction precursor, polyvinylpyrrolidone (PVP) as a surface active agent as well as sodium oxalate (Na2C2O4) and sodium metavanadate (NaVO3) as reactants; the method comprises the steps of feeding the surface active agent into the reaction precursor, carrying out a solvothermal reaction, centrifuging, washing, drying, and carrying out solid-phase reaction calcination on the obtained product at the temperature of 300-400 DEG C to obtain the BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst. The prepared mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst has the length of about 3.5-4.5mu m, the diameter of about 0.7-0.9mu m and the mesoporous average diameter of 30.0nm. The prepared mesoporous BiVO4/Bi2O3 composite micro-rod p-n heterojunction photocatalyst has the characteristics of being low in cost, easy to control, good in repeatability, and the like.
Description
Technical field
The invention belongs to mesoporous bivo4/bi2o3Compound micro- rod preparing technical field, more particularly to a kind of mesoporous bivo4/
bi2o3It is combined the chemical synthesis process of the solid phase reaction of micro- film/nanorod p-n junction photochemical catalyst.
Background technology
Pucherite (bivo4) as a kind of important semi-conducting material, because it is safe from harm to human body and environment, become mesh
Front popular inorganic material.bivo4Chemical reaction can be promoted when contacting the light of the sun and fluorescent lamp, it can be killed
Multiple mushrooms and virus etc., in accelerating chemical reaction process, do not cause the wasting of resources to be formed with additional pollution, this is symbol
Close the growth requirement of low-carbon economy, therefore bivo4Have a wide range of applications in the field such as pigment and photocatalytic degradation.At present,
Document report prepares bivo4The method of nano material has: hydro-thermal method, microwave method, chemical deposition and high temperature solid state reaction etc. are many
The method of kind.Reported solvent structure in " physical chemistry magazine c " (2009, volume 113 page 20228) of American Chemical Society
Spindle build bivo4.Patent cn201310138022.x discloses solvent structure different-shape bivo4Method.But it is a lot
Method prepares single bivo4Size mostly heterogeneity, cost of manufacture is of a relatively high, performance has certain defect etc., therefore closes
The nano material of one-tenth hybrid structure is already known to the focus of scientists study.
P-n junction photochemical catalyst is the photochemical catalyst being compounded to form by p-type semiconductor and n-type semiconductor, and it is good to be that one kind has
The specific function material of good chemical functional, can efficiently separate light induced electron and hole.P-n junction photocatalyst material can not only be opened up
The wave-length coverage of broadening gap semiconductor, and the compound of carrier can be suppressed by internal electric field, drastically increase material
Photocatalysis performance, receive significant attention." JACS " (2013, volume 135 page 10286) as American Chemical Society
Report the method that hydro-thermal method synthesizes mos2/n-rgo p-n junction photochemical catalyst hydrogen manufacturing.Meanwhile, patent cn201410360916.8
Also report electrodeposition process preparation bi2o3/bipo4The method of p-n junction photocatalysis film material.But a lot of methods be related to high temperature,
Low pressure etc. operates, and not only consumes energy but also time-consuming.Synthesising mesoporous bivo at present4/bi2o3Compound micro- rod is realized inexpensive, easily-controllable simultaneously
System, reproducible method it is not yet reported that.The method of this patent introduction can not only easily control mesoporous bivo4/bi2o3Multiple
Close the growth of micro- rod, and can effectively reduce the production cost of material, building-up process is simple, easy to control, product yield is big, repetition
Property is good, and has excellent photo catalytic reduction performance.
Content of the invention
The present invention is directed to mesoporous bivo4/bi2o3It is combined the problem that micro- rod is difficult to synthesize, there is provided a kind of inexpensive, easily-controllable
System, reproducible prepare mesoporous bivo4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst.
The technical scheme is that and realize in the following way: one kind prepares mesoporous bivo in a large number4/bi2o3Compound micro-
The method of film/nanorod p-n junction photochemical catalyst, with metal inorganic salt five water bismuth nitrate (bi (no3)3·5h2O) it is pre-reaction material, add
Surfactant polyvinylpyrrolidone (pvp), with sodium oxalate (na2c2o4) and sodium metavanadate (navo3) it is reactant, solvent
After thermal response, through centrifugation, washing, dry, the product obtaining is obtained by 300～400 DEG C of solid phase reactions calcinings mesoporous
bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
Prepare mesoporous bivo in described one kind in a large number4/bi2o3It is combined in the method for micro- film/nanorod p-n junction photochemical catalyst, preparation
Mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst to comprise the steps of
(1) take a certain amount of inorganic salts bismuth nitrate (bi (no3)3·5h2O) with ethylene glycol (eg), it is made into bi3+Molar concentration is
The solution of 0.01～0.035m, adds appropriate polyvinylpyrrolidone (pvp) to be dissolved in wherein, obtains colourless transparent solution a, will be molten
Liquid a puts in container and carries out magnetic agitation at room temperature；
(2) take a certain amount of sodium oxalate (na2c2o4) and water, it is made into the solution that oxalate molar concentration is 0.016～0.04m
B, solution b is added dropwise in solution a, and solution gradually becomes muddy, treats the whole completion of dropwise addition of solution b, continues stirring 15～20 minutes,
Obtain mixed solution c；
(3) take a certain amount of sodium metavanadate (navo3) and water, being configured to metavanadic acid root molar concentration is 0.002～0.007m
Solution d, then by solution d be added dropwise over step (2) in the mixed solution c that obtains, reacted gradually turn yellow, treat that solution d drips
Terminate, continue stirring 15～20 minutes, obtain the mixed liquor e of yellow gum shape；
(4) mixed liquor e is transferred in reactor, at 160～180 DEG C, after 8～12 hours of reaction, centrifuge washing, baking
Dry, obtain mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is put in tube furnace, in 300～400
Calcine 3～5 hours in DEG C air atmosphere, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
Using the mesoporous bivo prepared by the present invention4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst, its length is about 3.5-
4.5 μm, diameter is about 0.7-0.9 μm, and mesoporous average diameter is 30.0nm.The mesoporous bivo of present invention preparation4/bi2o3Compound micro-
Film/nanorod p-n junction photochemical catalyst have product cost low, easy to control, reproducible the features such as.
Brief description
Fig. 1 is the mesoporous of preparation in the embodiment 1 that Dutch PHILIPS Co. pw3040/60 type X-ray diffraction instrument is surveyed
bivo4/bi2o3It is combined the X-ray diffraction figure of micro- film/nanorod p-n junction photochemical catalyst, wherein: abscissa x is angle of diffraction (2 θ), indulge and sit
Mark y is relative diffracted intensity.
Make in Tu2Shi HIT s-4800 type field emission scanning electron microscope (fe-sem) observation embodiment 2
Standby mesoporous bivo4/bi2o3It is combined the shape appearance figure of micro- film/nanorod p-n junction photochemical catalyst.
In the embodiment 3 that Tu3Shi Jeol Ltd. jem-2100f type transmission electron microscope (tem) observes
The mesoporous bivo of preparation4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst internal structure picture.
The reality that Tu4Shi Jeol Ltd. jem-2100f type high resolution transmission electron microscopy (hrtem) observes
Apply the mesoporous bivo of example 3 preparation4/bi2o3It is combined bivo in micro- film/nanorod p-n junction photochemical catalyst4And bi2o3The heterojunction structure institute being formed
Corresponding lattice fringe picture.
The embodiment 4 intermediary hole bivo that Tu5Shi Micromeritics Instrument Corp. U.S.A asap 2020 type physical adsorption appearance is provided4/
bi2o3It is combined the adsorption isotherm of micro- film/nanorod p-n junction photochemical catalyst, illustration is its graph of pore diameter distribution.
Fig. 6 is embodiment 5 intermediary hole bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst photocatalytically degradating organic dye first
Base orange (mo) test chart.
Fig. 7 is mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst Mechanism of Semiconductor Photocatalytic Degradation figure.
Specific embodiment
Below by embodiment to preparing mesoporous bivo in the present invention4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst
Make and further illustrating.
Embodiment 1
One kind prepares mesoporous bivo4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst, this prepares mesoporous bivo4/
bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst comprises the following steps:
(1) weigh 0.1698g (0.35mmol) bi (no3)3·5h2O, 0.5g (4.5mmol) pvp, is dissolved in 15ml second two
Form bi through ultrasonic disperse in alcohol3+Molar concentration is homogeneous solution a of 0.023m, and solution a is poured into round-bottomed flask and in room temperature
Under carry out magnetic agitation；
(2) weigh 0.0375g (0.28mmol) na2c2o4It is dissolved in 10ml distilled water and obtain oxalate (c2o4 2-) mole
Concentration be 0.028m solution b, solution b is added dropwise in solution a, solution gradually becomes muddy, after completion of dropwise addition, stirring 15～
20 minutes, obtain mixed solution c；
(3) weigh 0.0085g (0.07mmol) navo3It is dissolved in 15ml distilled water and obtain metavanadic acid root (vo3 -) mole dense
Spend the solution d for 0.0047m, by solution d be added dropwise over step (2) in the mixed solution that obtains, reacted gradually turn yellow, treat
Solution d completion of dropwise addition, stirs 15～20 minutes, obtains the mixed liquor e of yellow gum shape；
(4) mixed liquor e is put in 50ml reactor, after 180 DEG C of reactions 10 hours, divided with distilled water and absolute ethyl alcohol
Not Xi Di 3 times, at 60 DEG C dry, obtain mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is placed on air atmosphere in tube furnace
Under in 350 DEG C calcine 4 hours, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
Mesoporous bivo for preparation in the present embodiment4/bi2o3Compound micro- film/nanorod p-n junction photochemical catalyst does X-ray diffraction and divides
Analysis, as shown in figure 1, its abscissa x is angle of diffraction (2 θ), ordinate y is relative diffracted intensity to result, in figure bivo4All
Diffraction maximum can be according to monoclinic system (monoclinic) index chemical conversion (011) (121) (040) (200) etc., with international standard
Jcpds in powder xrd diffraction card, 14-0688 are consistent, in figure bi2o3All diffraction maximums can be according to tetragonal crystal system
(tetragonal) index chemical conversion (201) (220) (222) etc., with the jcpds, 27- in international standard powder xrd diffraction card
0050 is consistent.
Embodiment 2
One kind prepares mesoporous bivo4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst, this prepares mesoporous bivo4/
bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst comprises the following steps:
(1) weigh 0.097g (0.2mmol) bi (no3)3·5h2O, 0.5g (4.5mmol) pvp, is dissolved in 15ml ethylene glycol
Middle through ultrasonic disperse formed bi3+Molar concentration is homogeneous solution a of 0.013m, and solution a is poured into round-bottomed flask at room temperature
Carry out magnetic agitation；
(2) weigh 0.0214g (0.16mmol) na2c2o4It is dissolved in 10ml distilled water and obtain oxalate (c2o4 2-) mole
Concentration be 0.016m solution b, solution b is added dropwise in solution a, solution gradually becomes muddy, after completion of dropwise addition, stirring 15～
20 minutes, obtain mixed solution c；
(3) weigh 0.0049g (0.04mmol) navo3It is dissolved in 15ml distilled water and obtain metavanadic acid root (vo3 -) mole dense
Spend the solution d for 0.0027m, by solution d be added dropwise over step (2) in the mixed solution that obtains, reacted gradually turn yellow, treat
Solution d completion of dropwise addition, stirs 15～20 minutes, obtains the mixed liquor e of yellow gum shape；
(4) mixed liquor e is put in 50ml reactor, after 170 DEG C of reactions 10 hours, divided with distilled water and absolute ethyl alcohol
Not Xi Di 3 times, at 60 DEG C dry, obtain mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is placed on air atmosphere in tube furnace
Under in 350 DEG C calcine 5 hours, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
Mesoporous bivo for preparation in the present embodiment4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst and do Flied emission scanning electricity
Mirror is analyzed, the electromicroscopic photograph obtaining as shown in Figure 2 it can be seen that product is that porous is bar-shaped, length at 3.5-4.5 μm about,
Diameter is at 0.7-0.9 μm about.
Embodiment 3
One kind prepares mesoporous bivo4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst, this prepares mesoporous bivo4/
bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst comprises the following steps:
(1) weigh 0.194g (0.4mmol) bi (no3)3·5h2O, 0.5g (4.5mmol) pvp, is dissolved in 15ml ethylene glycol
Middle through ultrasonic disperse formed bi3+Molar concentration is homogeneous solution a of 0.027m, and solution a is poured into round-bottomed flask at room temperature
Carry out magnetic agitation；
(2) weigh 0.0429g (0.32mmol) na2c2o4It is dissolved in 10ml distilled water and obtain oxalate (c2o4 2-) mole
Concentration be 0.032m solution b, solution b is added dropwise in solution a, solution gradually becomes muddy, after completion of dropwise addition, stirring 15～
20 minutes, obtain mixed solution c；
(3) weigh 0.0098g (0.08mmol) navo3It is dissolved in 15ml distilled water and obtain metavanadic acid root (vo3 -) mole dense
Spend the solution d for 0.0053m, by solution d be added dropwise over step (2) in the mixed solution that obtains, reacted gradually turn yellow, treat
Solution d completion of dropwise addition, stirs 15～20 minutes, obtains the mixed liquor e of yellow gum shape；
(4) mixed liquor e is put in 50ml reactor, after 180 DEG C of reactions 8 hours, with distilled water and absolute ethyl alcohol difference
Washing 3 times, dries at 60 DEG C, obtains mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is placed on air atmosphere in tube furnace
Under in 300 DEG C calcine 4 hours, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
For the present embodiment intermediary hole bivo4/bi2o3It is combined micro- rod and do tem study.Can from Fig. 3
Go out, bivo manufactured in the present embodiment4/bi2o3Compound micro- rod surface has pore space structure.
For the present embodiment intermediary hole bivo4/bi2o3It is combined micro- rod and do high resolution transmission electron microscopy analysis.From Fig. 4
As can be seen that bivo4/bi2o3The lattice fringe corresponding to heterojunction structure being formed in compound micro- rod is respectively bivo4And bi2o3
Lattice fringe picture.
Embodiment 4
One kind prepares mesoporous bivo4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst, this prepares mesoporous bivo4/
bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst comprises the following steps:
(1) weigh 0.22g (0.5mmol) bi (no3)3·5h2O, 0.5g (4.5mmol) pvp, is dissolved in 15ml ethylene glycol
Form bi through ultrasonic disperse3+Molar concentration is homogeneous solution a of 0.033m, solution a is poured into round-bottomed flask and enters at room temperature
Row magnetic agitation；
(2) weigh 0.0536g (0.4mmol) na2c2o4It is dissolved in 10ml distilled water and obtain oxalate (c2o4 2-) mole dense
Spend the solution b for 0.04m, solution b is added dropwise in solution a, solution gradually becomes muddy, after completion of dropwise addition, stir 15～20
Minute, obtain mixed solution c；
(3) weigh 0.0122g (0.1mmol) navo3It is dissolved in 15ml distilled water and obtain metavanadic acid root (vo3 -) mole dense
Spend the solution d for 0.0067m, by solution d be added dropwise over step (2) in the mixed solution that obtains, reacted gradually turn yellow, treat
Solution d completion of dropwise addition, stirs 15～20 minutes, obtains the mixed liquor e of yellow gum shape；
(4) mixed liquor e is put in 50ml reactor, after 180 DEG C of reactions 12 hours, divided with distilled water and absolute ethyl alcohol
Not Xi Di 3 times, at 60 DEG C dry, obtain mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is placed on air atmosphere in tube furnace
Under in 350 DEG C calcine 3 hours, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
Mesoporous bivo for preparation in the present embodiment4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst and be n2Adsorption desorption is surveyed
Examination, as shown in figure 5, the absorption isotherm of sample belongs to iv type and has h3 hysteresis loop, these can be further for the information obtaining
Prove that this sample is mesoporous material.Graph of pore diameter distribution in illustration more intuitively reality go out sample pore-size distribution, bore dia
It is about 30.0nm.
Embodiment 5
One kind prepares mesoporous bivo4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst, this prepares mesoporous bivo4/
bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst comprises the following steps:
(1) weigh 0.1698g (0.35mmol) bi (no3)3·5h2O, 0.5g (4.5mmol) pvp, is dissolved in 15ml second two
Form bi through ultrasonic disperse in alcohol3+Molar concentration is homogeneous solution a of 0.023m, and solution a is poured into round-bottomed flask and in room temperature
Under carry out magnetic agitation；
(2) weigh 0.0375g (0.28mmol) na2c2o4It is dissolved in 10ml distilled water and obtain oxalate (c2o4 2-) mole
Concentration be 0.028m solution b, solution b is added dropwise in solution a, solution gradually becomes muddy, after completion of dropwise addition, stirring 15～
20 minutes, obtain mixed solution c；
(3) weigh 0.0085g (0.07mmol) navo3It is dissolved in 15ml distilled water and obtain metavanadic acid root (vo3 -) mole dense
Spend the solution d for 0.0047m, by solution d be added dropwise over step (2) in the mixed solution that obtains, reacted gradually turn yellow, treat
Solution d completion of dropwise addition, stirs 15～20 minutes, obtains the mixed liquor e of yellow gum shape；
(4) mixed liquor e is put in 50ml reactor, after 160 DEG C of reactions 10 hours, divided with distilled water and absolute ethyl alcohol
Not Xi Di 3 times, at 60 DEG C dry, obtain mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is placed on air atmosphere in tube furnace
Under in 400 DEG C calcine 4 hours, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
Mesoporous bivo to preparation in the present embodiment4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst and business bivo4Do light
Catalytic degradation organic dyestuff methyl orange (mo) performance comparison is tested, the test result obtaining as shown in Figure 6 it can be seen that
During 30min, business bivo4Degradation rate be 12.4%, and mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photocatalyst for degrading
Speed is 70.9%, and this shows mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst can more effectively drop at short notice
Solution mo.Prepared bivo4/bi2o3Composite not only has meso pore characteristics effectively to improve photocatalysis efficiency, and it is formed
P-n heterojunction structure as shown in fig. 7, bivo4For n-type semiconductor, bi2o3For p-type semiconductor, both of which can under visible light by
Excite, when both fermi levels reach balance, p-n junction will be formed, and due to electrons spread, formed in its contact interface
One internal electric field, this electric field inhibits the compound, thus improve photocatalysis performance of light induced electron and hole.
Xrd, fe-sem, tem, the result of hrtem, pore structure and absorption property measurement and photocatalytically degradating organic dye
Performance test shows:
Using the preparation-obtained mesoporous bivo of the inventive method4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst, be to use mesh
The catalysis material that front better simply one-step method successfully synthesizes, it have low cost, yield is high, appearance and size uniformity is good,
The features such as reappearance is high, it has been filled up solvent-thermal method and has prepared mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst composite wood
Blank in synthesis field for the material, for synthesising mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photocatalyst material to open further
Send out, application can play certain impetus.
Claims (1)
1. one kind prepares mesoporous bivo in a large number4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst is it is characterised in that with metal
Inorganic salts five water bismuth nitrate (bi (no3)3·5h2O) it is pre-reaction material, add surfactant polyvinylpyrrolidone
(pvp), with sodium oxalate (na2c2o4) and sodium metavanadate (navo3) it is reactant, after solvent thermal reaction, through centrifugation, washing, dry
Dry, the product obtaining is passed through 300～400 DEG C of solid phase reaction calcinings and obtains mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction light to urge
Agent, described one kind prepares mesoporous bivo in a large number4/bi2o3The method being combined micro- film/nanorod p-n junction photochemical catalyst comprises the following steps:
(1) take a certain amount of inorganic salts five water bismuth nitrate (bi (no3)3·5h2O) with ethylene glycol (eg), it is made into bi3+Molar concentration is
The solution of 0.01～0.035m, adds appropriate polyvinylpyrrolidone (pvp) to be dissolved in wherein, obtains colourless transparent solution a, will be molten
Liquid a puts in container and carries out magnetic agitation at room temperature；
(2) take a certain amount of sodium oxalate (na2c2o4) and water, it is made into the solution b that oxalate molar concentration is 0.016～0.04m, will
Solution b is added dropwise in solution a, and solution gradually becomes muddy, treats the whole completion of dropwise addition of solution b, continues stirring 15～20 minutes, obtains
Mixed solution c；
(3) take a certain amount of sodium metavanadate (navo3) and water, being configured to metavanadic acid root molar concentration is the molten of 0.002～0.007m
Liquid d, then by solution d be added dropwise over step (2) in the mixed solution c that obtains, reacted gradually turn yellow, treat solution d dropping knot
Bundle, continues stirring 15～20 minutes, obtains the mixed liquor e of yellow gum shape；
(4) mixed liquor e is transferred in reactor, at 160～180 DEG C, after 8～12 hours of reaction, centrifuge washing, drying, obtain
To mesoporous bivo4/bi2o3Compound micro- rod presoma；
By step (4) in the mesoporous bivo that obtains4/bi2o3Compound micro- rod presoma is put in tube furnace, in 300～400 DEG C of skies
Calcine 3～5 hours in gas atmosphere, obtain mesoporous bivo4/bi2o3It is combined micro- film/nanorod p-n junction photochemical catalyst.
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| CN106345496B (en) * | 2015-07-17 | 2019-04-23 | 广东工业大学 | A kind of compound semiconductor photocatalytic material and preparation method thereof |
| CN106732605B (en) * | 2016-12-27 | 2019-03-15 | 上海应用技术大学 | A kind of non-noble metal oxide catalyst and preparation method with water resistant protective layer |
| CN107029719B (en) * | 2017-05-04 | 2019-11-29 | 辽宁大学 | A kind of Bi2O3/Ag2WO4/Bi2WO6Composite photo-catalyst and the preparation method and application thereof |
| CN107433196B (en) * | 2017-07-24 | 2020-07-03 | 安徽师范大学 | Bismuth oxide-bismuth vanadate heterojunction and preparation method and application thereof |
| CN107626297B (en) * | 2017-09-29 | 2019-09-17 | 中南大学 | A kind of tiny balloon shape bismuth/composite bismuth vanadium photocatalyst and its preparation method 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 |
| CN112516992B (en) * | 2020-12-14 | 2022-04-22 | 三峡大学 | Preparation method and application of bismuth vanadate-based composite material |
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| CN101244385A (en) * | 2008-03-20 | 2008-08-20 | 同济大学 | Process for producing high-efficiency photocatalysis material |
| CN103754837A (en) * | 2013-12-17 | 2014-04-30 | 武汉工程大学 | Method for preparation of bismuth-containing nano-hollow ball by using porous bismuth oxide as template |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244385A (en) * | 2008-03-20 | 2008-08-20 | 同济大学 | Process for producing high-efficiency photocatalysis material |
| CN103754837A (en) * | 2013-12-17 | 2014-04-30 | 武汉工程大学 | Method for preparation of bismuth-containing nano-hollow ball by using porous bismuth oxide as template |
Non-Patent Citations (1)
| Title |
|---|
| Hydrothermal fabrication and visible-light-driven photocatalytic properties of bismuth vanadate with multiple morphologies and/or porous structures for Methyl Orange degradation;Haiyan Jiang, et al.;《Journal of Environmental Science》;20121231;第24卷(第3期);第449-457页 * |
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