CN106082333B - A kind of regulation and control BiVO4The method of full meso-porous nano carrying material - Google Patents
A kind of regulation and control BiVO4The method of full meso-porous nano carrying material Download PDFInfo
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- CN106082333B CN106082333B CN201610452015.0A CN201610452015A CN106082333B CN 106082333 B CN106082333 B CN 106082333B CN 201610452015 A CN201610452015 A CN 201610452015A CN 106082333 B CN106082333 B CN 106082333B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer
Abstract
The present invention relates to a kind of regulation and control BiVO4The method of full meso-porous nano carrying material, belongs to nanofiber technology field.Described method includes following steps：Configure spinning liquid as precursor：By polyvinylpyrrolidone (PVPK30), polyvinylpyrrolidone (PVPK90), five nitric hydrate bismuth (Bi (NO3)3·5H2O), vanadyl acetylacetonate (VO (acac)2) be dissolved in solvent, it is stirring evenly and then adding into foaming agent and continues to stir to obtain spinning liquid as precursor；Spinning liquid as precursor progress electrostatic spinning is obtained into solid precursor fiber；Most BiVO can be obtained through calcination processing afterwards4Full meso-porous nano carrying material.The present invention is by regulating and controlling raw material composition, Effective Regulation BiVO4The structure of full mesoporous nano belt, and the present invention regulates and controls BiVO4The method of full mesoporous nano belt is simply controllable, has repeatability well.
Description
Technical field
The present invention relates to a kind of methods of the regulation and control full meso-porous nano carrying materials of BiVO4, belong to nanofiber technology field.
Background technology
Pucherite (BiVO4) monodimension nanometer material is because it is with nontoxic, chemical steady property be good and its specific geometric shape
Take on important role constructing nano electron device field.The BiVO of full meso-hole structure4Nanofiber is one-dimensional in inheriting tradition
While nano material advantage, but also with unique high-specific surface area and macropore capacitive matter, in catalysis, the energy, sensing, medical treatment etc.
Field has and is more widely applied value.However, from the point of view of practical application and commercialization, full meso-hole structure
BiVO4Nanobelt is there is still a need for regulation and control are advanced optimized, in the hope of obtaining what performance was strengthened by conveniently technology
BiVO4Material.Recent research reports the BiVO for showing one-dimensional full meso-hole structure4Nano material has low-density and larger ratio
The novel characteristics such as surface area, thus if can complete mesoporous BiVO effectively prepared4While band, realize to complete mesoporous one-dimensional
Collaboration is improved BiVO by regulation and control prepared by fibrous material4The permeability and adsorptivity of material, as catalyst such as photochemical catalyst etc.
Field has very tempting application prospect.
It is to realize that the simplicity of its material is controllable that the research of nano material, which can agree with one of the important foundation to practical application,
Synthesis.BiVO based on above-mentioned regulatable full meso-hole structure4The potential researching value of nanobelt.Still do not have both at home and abroad at present
There is the preparation method of mesoporous nano belt.Therefore, the BiVO of full meso-hole structure is realized4The easy controllable preparation of nanobelt, still face
Face difficult and challenge.
Invention content
The purpose of the present invention is there is the above problem in view of the prior art, it is proposed that a kind of equipment and it is simple for process can
Control, and with the regulation and control BiVO of repeatability well4The method of full meso-porous nano carrying material.
Object of the invention can be realized by the following technical scheme：A kind of regulation and control BiVO4Full meso-porous nano carrying material
Method, described method includes following steps：
Configure spinning liquid as precursor：By polyvinylpyrrolidone (PVPK30, MW≈ 40000), polyvinylpyrrolidone
(PVPK90, MW≈ 1300000), five nitric hydrate bismuth (Bi (NO3)3·5H2O), vanadyl acetylacetonate (VO (acac)2) be dissolved in
In solvent, be stirring evenly and then adding into the diisopropyl azodiformate (foaming agent, DIPA) of different content and continuing stir before
Drive body spinning solution；
Spinning liquid as precursor progress electrostatic spinning is obtained into solid precursor fiber；
By solid precursor fiber obtained above through calcination processing, you can obtain BiVO4Full meso-porous nano carrying material.
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the polyvinylpyrrolidone (PVPK30, MW≈
40000) with polyvinylpyrrolidone (PVPK90, MW≈ 1300000) mass ratio be 2-4:1.
In above-mentioned BiVO4In the preparation method of nanobelt material, the five nitric hydrates bismuth (Bi (NO3)3·5H2O), second
Acyl acetone vanadyl (VO (acac)2) mass ratio be 1.5-2.5:1.
The concentration of spinning liquid as precursor is mainly to influence the pattern and diameter of fiber by influencing solution viscosity.If presoma
The concentration of spinning solution is too low, and in electrostatic spinning, solution viscosity is extremely low, it is difficult to maintain the continuity of spinneret thread, cannot be formed
Stable fluid, and injection drop is formd, therefore obtain being in irregular blocks nano material.If spinning liquid as precursor is dense
Height is spent, nano material is coarse and fine, and is unevenly distributed, or even bonding phenomenon occurs, which is because, between polymer molecule
Interaction starts to influence the movement of polymer chain, and polymer molecular chain mutually tangles, if concentration continues growing, polymer is mutual
Friendship is worn, and frozen glue is formed.The fluid of high concentration fluid caused by syringe needle rapidly dry and polymer formation frozen glue is in syringe needle stream
Dynamic is unstable, it is difficult to maintain spinneret thread, while cause nozzle adhesion, make electrostatic spinning that can not carry out.Therefore, before preparation
It drives in body spinning solution, needs to control the relationship between quality between each raw material, to make spinning liquid as precursor reach suitable concentration,
And then form fine fiber morphology, the nanofiber that diameter is evenly distributed.Bi (NO of the present invention3)3·5H2O provides the sources Bi；VO
(acac)2The sources V are provided；PVP (the PVP of different proportion molecular mass are added simultaneouslyK30And PVPK90, PVPK30For MW≈40000、
PVPK90For MW≈ 1300000), realize BiVO4Nanofiber is to the preparation of nanobelt, while all controllable spinning solutions of two kinds of PVP
Viscosity and will be decomposed during calcination processing completely volatilization；The present invention is also added with suitable foaming agent, and foaming agent exists
A large amount of gas is released during calcination processing to realize the purpose to fibrous matrix pore-creating.
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the solvent is n,N-Dimethylformamide
(DMF), the mixed liquor of absolute ethyl alcohol and glacial acetic acid.DMF act as the solvent of acetylacetone,2,4-pentanedione oxygen alkane；Ethyl alcohol act as five hydrations
The solvent of bismuth nitrate；While glacial acetic acid is as solvent, also providing acetate ion for electrostatic spinning solution can be spun with improving
Performance, during spinning, since the effect foaming agent of electrostatic force is distributed evenly in inside presoma, after calcination processing
It decomposes volatilization and generates a large amount of gas (NO2、HO2、CO2Etc.) lead to the formation of full meso-hole structure；Not due to foaming agents content
Together, the BiVO of different internal structure is ultimately formed4Full meso-porous nano carrying material.
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the N, N- dimethylformamides (DMF), nothing
The mass ratio of water-ethanol and glacial acetic acid is 4-6:4-6:4.Preferably, the n,N-Dimethylformamide (DMF), absolute ethyl alcohol
Mass ratio with glacial acetic acid is 5:5:4.
In above-mentioned regulation and control BiVO4In the method for full mesoporous nano belt, the foaming agent is diisopropyl azodiformate
(DIPA), the additive amount of foaming agent is the 3-15wt% for accounting for spinning liquid as precursor gross mass.Nanobelt of the present invention is auxiliary using foaming
Help method of electrostatic spinning that full meso-hole structure is made, the purpose that fibrous matrix pore-creating can be achieved is added as foaming agent by wherein DIPA.
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the method for the electrostatic spinning is：By presoma
Spinning solution injects in needle tubing, is placed on micro-injection pump, metal needle makees electrospinning wire anode, and tinfoil paper or wire netting make reception material
The cathode of material carries out electrostatic spinning under high pressure, then obtains solid precursor fiber from tinfoil paper or iron wire online collection.
Electrostatic spinning be one it is simple, flexibly prepare fibre technology, basic principle is：In the effect of high voltage electric field
Under, the spinning liquid as precursor droplet deformation for being suspended from capillary outlet is taylor cone.With further increasing for electric field strength, work as drop
Surface by the electrostatic repulsion forces of electrically charged formation be more than itself surface tension when, form liquid on the top of taylor cone
Thread, the liquid stream with charge flow in the electric field, are further stretched effect, while evaporation of the solvent (or melt is cold
But), become fiber and deposit on the reception device, form organic precursor fibre material.During electrostatic spinning, fibre is influenced
The electrospinning parameters of dimension performance mainly have：Concentration, spinning voltage, the distance between anode and cathode and the solution of spinning liquid as precursor
Flow velocity etc..
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, spinning liquid as precursor injection needle in electrostatic spinning
Injection speed in pipe is 0.15-0.25mm/min, and the distance between anode and cathode described in electrostatic spinning is 18cm-
22cm, the high pressure are 10kV-13kV.In the present invention, if the applied voltage of electrostatic spinning is excessively high, can cause prepared
Nanobelt because electrostatic field force it is excessive so that the diameter of nanobelt is excessive, and can receiving pole occur bonding phenomenon.Such as
Fruit cathode is shorter at a distance from anode, can cause fiber during this of formation to receiving pole since solvent cannot be waved in time
Hair, the phenomenon of bonding can be occurred in receiving pole by similarly also resulting in.Therefore, comprehensive each factor, it is cloudy in electrostatic spinning of the present invention
The distance between pole and anode are 18cm-22cm, and the voltage of electrostatic spinning application is 10kV-13kV.
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, from tinfoil paper or wire netting described in electrostatic spinning
Upper collection obtains solid precursor fiber and also needs to that processing is dried.Further preferably, the temperature of the drying process is 60-
100℃。
In above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the temperature of the calcination processing is 480-520
DEG C, soaking time 0.4-2h.And in order to improve BiVO4The crystallinity of material, calcination processing carry out in air atmosphere.
It includes two aspects that the present invention forms nanobelt mainly by nanofiber：
Reason one：In precursor solution, the present invention is added to the PVP of different molecular quality, respectively：PVPK30With
PVPK90, and PVPK30With PVPK90Mass ratio be 2-4:1, the PVP after stirringK30And PVPK90It is uniformly mixed.Homogeneous transparent
Precursor solution carries out electrostatic spinning, can be divided into two layers, the reason is as follows that：Under same electrospinning conditions, ensure identical
The distance of field strength (E), flow velocity (Q), electric current (I), syringe needle to receiving pole.It is explored according to Baumgarten and Rurledge You Guan fine
Two equations for tieing up the relationship of diameter and viscosity are as follows：
R=c η1/2......................(1)
R=c (I/Q)-2/3γ1/3.........................(2)
R is jet radius in formula, and η is the viscosity of precursor solution, and γ is the surface tension of solution, and Q is flow velocity, and I is electricity
Stream, c are common constant.From two equations, it can learn that jet radius R is directly proportional to the square root of the viscosities il of presoma,
It is directly proportional to the cubic root of surface tension γ.For the PVP of different molecular quality, viscosity and surface tension are different from, this
Invent the PVP usedK30And PVPK90Viscosity be respectively：2.1-2.7mpas and 39.5-45.8mpas.Therefore, have
The precursor solution of two kinds of different molecular quality PVP is during spinning, compared with meeting in the PVP jet process of small molecule quality
It is distributed in centre, and the PVP of macromolecular quality can be distributed in outer layer, the PVP being uniformly mixed in this way in precursor solutionK30With
PVPK90It is separated so as to form two layers in spinning fibre.Due to PVPK30Viscosity and molecular weight all compare PVPK90It is small, and
PVPK30The volume of phase homogenous quantities is bigger, the PVP that internal layer can be caused to be distributed in this wayK30Occupy the volume of bigger, but molecule matter
The smaller PVP of amountK30Strand does not have PVPK90It is long, cause intensity to be not so good as PVPK90, so first layer can go out during calcining
Phenomenon of now caving in adds the PVP of different proportion so as to form nanobeltK30And PVPK90, the internal degree that collapses is different,
With PVPK30The increase of content, volume shared by internal layer is also bigger, collapses more serious, the diameter of nanobelt also will be bigger.
BiVO4Mechanism figure such as Fig. 1 of the reason of nanobelt is formed by nanofiber one.
Reason two：During electrostatic spinning, precursor solution is fallen by jet stream in receiving pole under the action of electrostatic field force
Upper formation fiber, along with the volatilization of solvent during this.Do not add PVPK30When, prepared sample 1 be it is cylindric
Nanofiber.As addition PVPK30And after increasing its content, due to PVPK30There is lyosoption, solvent can be caused to volatilize
It is relatively slow.As Fig. 2 is not added with PVPK30Sample 1 and be added to PVPK30Sample 2, sample 2 is before 250 DEG C, weight loss ratio
Compared with sample more than 1, (sample 1 and sample 2 are added to PVP in addition to sample 2K30In addition, other are remained unchanged), it is same at 430 DEG C or so
There is most of mass loss, this is by PVPK30And PVPK90Caused by thermally decomposing simultaneously.Thermogravimetric result illustrates, with PVPK30Contain
The increase of amount, solvent content can increase in presoma, and after being placed on baking oven or calcining, the volatilization of a large amount of solvents can lead to nanometer
Fiber collapses, this also results in the formation of nanobelt, this is also consistent with the result of SEM observations.
In short, BiVO of the present invention4Nanobelt is formed as the coefficient effect of two above reason.
Compared with prior art, the invention has the advantages that：
1, the present invention, by regulating and controlling different molecular quality PVP contents, effectively realizes BiVO by regulating and controlling raw material composition4It receives
Rice fiber prepares BiVO4The regulation and control of nanobelt material, by controlling the content of foaming agent, Effective Regulation BiVO4Full mesoporous nano belt
Structure.
2, present invention regulation and control BiVO4The method of full mesoporous nano belt is simply controllable, has repeatability well.
Description of the drawings
Fig. 1 is BiVO of the present invention4Full mesoporous nano belt is formed the mechanism figure of nanobelt reason one by nanofiber；
Fig. 2 is BiVO of the present invention4Full mesoporous nano belt, which is formed by nanofiber in nanobelt reason two, is not added with PVPK30's
Sample 1 and it is added to PVPK30Sample 2 presoma thermal multigraph；
Fig. 3 is the BiVO obtained by the embodiment of the present invention 14Low power scanning electron microscope (SEM) figure of full mesoporous nano belt；
Fig. 4 is the BiVO obtained by the embodiment of the present invention 14High power scanning electron microscope (SEM) figure of full mesoporous nano belt；
Fig. 5 is the BiVO obtained by the embodiment of the present invention 14The XRD figures of full mesoporous nano belt；
Fig. 6 is the BiVO obtained by the embodiment of the present invention 14The Raman figures of full mesoporous nano belt；
Fig. 7 is the BiVO obtained by the embodiment of the present invention 14Transmission electron microscope (TEM) figure of complete mesoporous band；
Fig. 8 is the BiVO obtained by the embodiment of the present invention 14High-resolution-ration transmission electric-lens (HRTEM) figure of complete mesoporous band；
Fig. 9 is the BiVO obtained by the embodiment of the present invention 24Low power scanning electron microscope (SEM) figure of full mesoporous nano belt；
Figure 10 is the BiVO obtained by the embodiment of the present invention 24High power scanning electron microscope (SEM) figure of full mesoporous nano belt；
Figure 11 is the BiVO obtained by the embodiment of the present invention 34Low power scanning electron microscope (SEM) figure of complete mesoporous carrying material；
Figure 12 is the BiVO obtained by the embodiment of the present invention 34Low power scanning electron microscope (SEM) figure of complete mesoporous band；
Figure 13 be comparative example of the present invention in obtained by without mesoporous BiVO4Low power scanning electron microscope (SEM) figure of nanobelt；
Figure 14 be comparative example of the present invention in obtained by without mesoporous BiVO4High power scanning electron microscope (SEM) figure of nanobelt.
Specific implementation mode
Following is a specific embodiment of the present invention in conjunction with the accompanying drawings, technical scheme of the present invention will be further described,
However, the present invention is not limited to these examples.
Embodiment 1
Weigh polyvinylpyrrolidone (PVPK90) 0.4g, polyvinylpyrrolidone (PVPK30) 1.2g, five nitric hydrate bismuths
(Bi(NO3)3·5H2O) 1.21g and acetylacetone,2,4-pentanedione oxygen alkane (VO (acac)2) 0.662g is dissolved in 2.5g absolute ethyl alcohols, N-N bis-
In the mixed liquor of methylformamide (DMF) 2.5g and 2g glacial acetic acid, 0.55 g azos are added after being stirred at room temperature 6 hours
Dioctyl phthalate diisopropyl ester (foaming agent, DIPA) and the clear solution for continuing to stir to get shallow breen.Microemulsion to be spun is quiet
It postpones and measures in 6ml injected plastic needle tubings, be placed on micro-injection pump, it is 0.2mm/min that speed is injected in setting.Metal needle
Make electrospinning wire anode, wire netting makees to receive the cathode of material, the distance between anode and cathode 20cm, under 12kV high pressures into
Row electrostatic spinning prepares organic precursor fibrous material.Then organic precursor fibrous material is placed in 80 DEG C of constant temperature drying boxes
It is interior, obtain the solid organic precursor fiber of core.Finally SOLID ORGANIC presoma is placed in quartz boat, in air atmosphere in
500 DEG C of heat preservations carry out calcination processing for 1 hour, and BiVO is made in then furnace cooling4Nano material.
BiVO obtained4The low power scanning electron microscope (SEM) and high power scanning electron microscope (SEM) such as Fig. 3 and Fig. 4 institutes of nano material
Show, shows that prepared material is mesoporous nano belt.Fig. 5 and Fig. 6 is the XRD diagram and Raman figures of obtained mesoporous nano belt,
Demonstrate prepared BiVO4Full mesoporous nano belt is monocline scheelite phase BiVO4.Fig. 7 and Fig. 8 is respectively meso-porous nano band
Transmission electron microscope (TEM) figure and high-resolution-ration transmission electric-lens (HRTEM) figure of material, further prove BiVO4Nanobelt is complete mesoporous knot
Structure and BiVO4Full mesoporous nano belt is monocline scheelite phase BiVO4。
Embodiment 2
The present embodiment is differed only in embodiment 1, the diisopropyl azodiformate (foaming being added in the present embodiment
Agent, DIPA) it is 1.16g, other are same as Example 1, are not repeated herein.
BiVO obtained4The low power scanning electron microscope (SEM) and high power scanning electron microscope (SEM) such as Fig. 9 and Figure 10 of nano material
It is shown, show that prepared material is mesoporous nano belt.
Embodiment 3
The present embodiment is differed only in embodiment 1, the diisopropyl azodiformate (foaming being added in the present embodiment
Agent, DIPA) it is 1.85g, other are same as Example 1, are not repeated herein.
BiVO obtained4The low power scanning electron microscope (SEM) and high power scanning electron microscope (SEM) such as Figure 11 and Figure 12 of nano material
It is shown, show that prepared material is mesoporous nano belt.
Comparative example
This comparative example is differed only in embodiment 1, this comparative example is simultaneously not added with diisopropyl azodiformate (foaming
Agent, DIPA), other are same as Example 1, are not repeated herein.
BiVO obtained4The low power scanning electron microscope (SEM) and high power scanning electron microscope (SEM) such as Figure 13 and Figure 14 of nano material
It is shown, show that prepared material is not complete mesoporous nanobelt.
Embodiment 1 is compared with comparative example, when showing that the amount of foaming agent is less in initial feed, by calcining institute
The material of preparation is meso-hole structure, illustrates that mesoporous nanobelt can be obtained by adding a small amount of foaming agent.
Embodiment 2 is compared with embodiment 1, comparative example, with the increase of the additive amount of foaming agent, increases to 10%
When wt, the preferably full mesoporous nano belt of pattern and structure can be obtained.
Embodiment 3 is compared with embodiment 1, embodiment 2, comparative example, with the increase of the additive amount of foaming agent, is increased
When being added to 15%wt, complete mesoporous nanobelt still can be obtained, and hole content and size all increased.
The data parameters of the present invention are not limited in above-described embodiment, such as polyvinylpyrrolidone (PVPK30) and poly- second
Alkene pyrrolidone (PVPK90) mass ratio can be 2-4:Arbitrary ratio in 1：2.0:1,2.1:1,2.2:1,2.3:1,2.5:
1,2.8:1,3.2:1,2.5:1,3.6:1,3.8:1 etc.；Five nitric hydrate bismuth (Bi (NO3)3·5H2) and vanadyl acetylacetonate O
(VO(acac)2) mass ratio can be 1.5-2.5:Arbitrary ratio in 1：1.5:1,1.8:1,2.1:1,2.2:1,2.4:1,
2.5:1 etc.；The additive amount of foaming agent can be the arbitrary value in the 3-15wt% for account for spinning liquid as precursor gross mass：3wt%,
4wt%, 5wt%, 8wt%, 10wt%, 12wt%, 15wt%；N,N-dimethylformamide (DMF), absolute ethyl alcohol in solvent
Mass ratio with glacial acetic acid may be 4-6:4-6:Arbitrary ratio in 4：4:4:4,4:5:4,5:4:4,5:5:4,6:4:4,6:
5:4,5:6:4,4:6:4 etc.；Injection speed in electrostatic spinning in spinning liquid as precursor injection needle tubing can be 0.15-
Arbitrary value in 0.25mm/min：0.15mm/min,0.16mm/min,0.18mm/min,0.21mm/min, 0.22mm/min,
0.25mm/min, the distance between electrostatic spinning Anodic and cathode can be the arbitrary value in 18cm-22cm：18cm,19cm,
21cm, 22cm etc. can be the arbitrary value in 10kV-13kV using high pressure：10kV,10.5kV,11kV, 11.5kV,
12.5kV, 13kV etc.；The temperature of drying process can be the arbitrary value in 60-100 DEG C：60℃,65℃,70℃,75℃,85
℃,90℃,95℃,100；The temperature of calcination processing can be the arbitrary value in 480-520 DEG C：480℃,490℃,510℃,
520 etc., soaking time is the arbitrary value in 0.4-2h：0.4h, 0.5h, 0.6h, 0.8h, 1.2h, 1.5h, 1.8h, 2h etc..
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (4)
1. a kind of regulation and control BiVO4The method of full meso-porous nano carrying material, which is characterized in that described method includes following steps：
Configure spinning liquid as precursor：
By 1.2g PVPK30、0.4g PVPK90, five nitric hydrate bismuths of 1.21g, 0.662g vanadyl acetylacetonates be dissolved in 2.5g without
Water-ethanol,N-NIn the mixed liquor of dimethylformamide 2.5g and 2g glacial acetic acid, it is stirring evenly and then adding into 0.55 g azo diformazans
Sour diisopropyl ester simultaneously continues to stir to obtain spinning liquid as precursor；
Spinning liquid as precursor progress electrostatic spinning is obtained into solid precursor fiber；
By solid precursor fiber obtained above through calcination processing, you can obtain BiVO4Full meso-porous nano carrying material；The calcining
The temperature of processing is 500 DEG C, soaking time 0.4-2h.
2. regulation and control BiVO according to claim 14The method of full meso-porous nano carrying material, which is characterized in that the Static Spinning
Silk method be：Spinning liquid as precursor is injected in needle tubing, is placed on micro-injection pump, metal needle makees electrospinning wire anode,
Tinfoil paper or wire netting are made to receive the cathode of material, carry out electrostatic spinning under high pressure, are then obtained from tinfoil paper or iron wire online collection
To solid precursor fiber.
3. regulation and control BiVO according to claim 24The method of full meso-porous nano carrying material, which is characterized in that in electrostatic spinning
The injection speed that spinning liquid as precursor injects in needle tubing is 0.15-0.25mm/min, anode described in electrostatic spinning and cathode it
Between distance be 18cm-22cm, the high pressure be 10kV-13kV.
4. regulation and control BiVO according to claim 24The method of full meso-porous nano carrying material, which is characterized in that in electrostatic spinning
It is described to obtain solid precursor fiber from tinfoil paper or iron wire online collection and also need to that processing is dried.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610452015.0A CN106082333B (en) | 2016-06-20 | 2016-06-20 | A kind of regulation and control BiVO4The method of full meso-porous nano carrying material |
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| CN201610452015.0A CN106082333B (en) | 2016-06-20 | 2016-06-20 | A kind of regulation and control BiVO4The method of full meso-porous nano carrying material |
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| Publication Number | Publication Date |
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| CN106082333A CN106082333A (en) | 2016-11-09 |
| CN106082333B true CN106082333B (en) | 2018-11-06 |
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