CN106082333A - 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G31/00—Compounds of vanadium
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- 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
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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 comprises the steps: to 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 is carried out electrostatic spinning and obtains solid precursor fiber；After through calcination processing BiVO4Full meso-porous nano carrying material.The present invention is by regulation and control raw material composition, Effective Regulation BiVO4The structure of mesoporous nano belt, and the present invention entirely regulates and controls BiVO4The method of full mesoporous nano belt is the most controlled, has good repeatability.
Description
Technical field
The present invention relates to a kind of regulate and control BiVO4 full meso-porous nano carrying material method, belong to nanofiber technology field.
Background technology
Pucherite (BiVO4) monodimension nanometer material has the good and specific geometric shape of steady some property nontoxic, chemical because of it
Important role is taken on constructing nano electron device field.The BiVO of full meso-hole structure4Nanofiber is one-dimensional at inheriting tradition
While nano material advantage, possesses again high-specific surface area and the macropore capacitive matter of uniqueness, in catalysis, the energy, sensing, medical treatment etc.
Field, has and is more widely applied value.But, from the point of view of reality application and commercialization, full meso-hole structure
BiVO4Nano belt need nonetheless remain for further Optimum Regulation, in the hope of obtaining what performance was strengthened by conveniently technology
BiVO4Material.Recent research report shows, the BiVO of one-dimensional full meso-hole structure4Nano material has low-density and bigger ratio
The novel characteristics such as surface area, thus if able to effectively preparing complete mesoporous BiVO4While band, it is achieved to complete mesoporous one-dimensional
Regulation and control prepared by fibrous material, by collaborative raising BiVO4The permeability of material and adsorptivity, as catalyst such as photocatalyst etc.
Field has the most tempting application prospect.
One of the important foundation that the research of nano material can agree with to reality application is that to realize the simplicity of its material controlled
Synthesis.BiVO based on above-mentioned regulatable full meso-hole structure4The potential researching value of nano belt.Still do not have both at home and abroad at present
There is the preparation method of mesoporous nano belt.Therefore, it is achieved the BiVO of full meso-hole structure4The controlled preparation of simplicity of nano belt, still face
Face difficulty and challenge.
Summary of the invention
It is an object of the invention to there are the problems referred to above for existing technology, it is proposed that a kind of equipment and technique simply may be used
Control, and there is the most repeatable regulation and control BiVO4The method of full meso-porous nano carrying material.
The purpose of the present invention can be realized by following technical proposal: a kind of regulation and control BiVO4Full meso-porous nano carrying material
Method, described method comprises the steps:
Configuration 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 continuing stir before
Drive body spinning liquid；
Spinning liquid as precursor is carried out electrostatic spinning and obtains solid precursor fiber；
By above-mentioned prepared solid precursor fiber through calcination processing, BiVO4Full meso-porous nano carrying material.
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, described polyvinylpyrrolidone (PVPK30, MW≈
40000) with polyvinylpyrrolidone (PVPK90, MW≈ 1300000) mass ratio be 2-4:1.
At above-mentioned BiVO4In the preparation method of nanobelt material, described five nitric hydrate 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 pattern and the diameter affecting fiber by affecting solution viscosity.If presoma
The concentration of spinning liquid is too low, and in electrostatic spinning, solution viscosity is extremely low, is difficult to maintain the seriality of spray webbing thread, it is impossible to formed
Stable fluid, and define injection drop, therefore obtain in irregular blocks nano material.If spinning liquid as precursor is dense
Spending height, nano material has slightly to be had carefully, and bonding phenomenon even occurs in skewness, and its reason is, between polymer molecule
Interacting and start to affect the motion of polymer chain, polymer molecular chain mutually tangles, if concentration continues to increase, polymer is mutual
Friendship is worn, and forms frozen glue.The fluid of high concentration is dried rapidly and polymer forms the fluid that causes of frozen glue at syringe needle stream at syringe needle
Dynamic instability, it is difficult to maintain spray webbing thread, cause shower nozzle adhesion simultaneously, make electrostatic spinning cannot be carried out.Therefore, before preparation
Drive in body spinning liquid, need to control well the relationship between quality between each raw material, so that spinning liquid as precursor reaches suitable concentration,
And then form fine fiber morphology, the uniform nanofiber of diameter Distribution.Bi (NO of the present invention3)3·5H2O provides Bi source；VO
(acac)2V source is provided；Add the PVP (PVP of different proportion molecular mass simultaneouslyK30And PVPK90, PVPK30For MW≈40000、
PVPK90For MW≈ 1300000), it is achieved BiVO4Nanofiber to the preparation of nano belt, two kinds of PVP all controllable spinning liquid simultaneously
Viscosity and decomposing during calcination processing volatilize completely；The present invention is also added with appropriate foaming agent, and foaming agent exists
Discharge substantial amounts of gas during calcination processing thus realize the purpose to fibrous matrix pore-creating.
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, described solvent is DMF
(DMF), dehydrated alcohol and the mixed liquor of glacial acetic acid.DMF act as the solvent of acetylacetone,2,4-pentanedione oxygen alkane；Ethanol act as five hydration nitre
The solvent of acid bismuth；While glacial acetic acid is as solvent, also provide acetate ion to improve spinnability for electrostatic spinning solution
Can, during spinning, owing to the effect foaming agent of electrostatic force is distributed evenly in inside presoma, divide after calcination processing
Solve volatilization and produce substantial amounts of gas (NO2、HO2、CO2Etc.) cause the formation of full meso-hole structure；Due to foaming agents content not
With, ultimately form the BiVO of different internal structure4Full meso-porous nano carrying material.
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, described DMF (DMF), nothing
The mass ratio of water-ethanol and glacial acetic acid is 4-6:4-6:4.As preferably, described DMF (DMF), dehydrated alcohol
It is 5:5:4 with the mass ratio of glacial acetic acid.
At above-mentioned regulation and control BiVO4In the method for full mesoporous nano belt, described foaming agent is diisopropyl azodiformate
(DIPA), the addition of foaming agent is the 3-15wt% accounting for spinning liquid as precursor gross mass.Nano belt of the present invention uses foaming auxiliary
Helping method of electrostatic spinning to make full meso-hole structure, wherein DIPA adds the purpose that can realize fibrous matrix pore-creating as foaming agent.
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the method for described electrostatic spinning is: by presoma
Spinning liquid injects in needle tubing, is placed on micro-injection pump, and metal needle is made Electrospun anode, tinfoil paper or wire gauze and made to receive material
The negative electrode of material, under high pressure carries out electrostatic spinning, then obtains solid precursor fiber from tinfoil paper or iron wire online collection.
Electrostatic spinning is one and prepares fibre technology simply, flexibly, and its ultimate principle is: in the effect of high voltage electric field
Under, the spinning liquid as precursor droplet deformation being suspended from capillary outlet is taylor cone.Along with the further raising of electric field intensity, work as drop
Surface due to the electrostatic repulsion forces of electrically charged formation exceed itself surface tension time, form liquid on the top of taylor cone
Thread, the liquid stream with electric charge flows in the electric field, is stretched effect further, solvent evaporation simultaneously (or melt is cold
But), become fiber and deposit on the reception device, forming organic precursor fibre material.During electrostatic spinning, impact fibre
The electrospinning parameter of dimension performance mainly has: the distance between the concentration of spinning liquid as precursor, spinning voltage, anode and negative electrode and solution
Flow velocity etc..
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, in electrostatic spinning, spinning liquid as precursor injects pin
Injection speed in pipe is 0.15-0.25mm/min, and described in electrostatic spinning, the distance between anode and negative electrode is 18cm-
22cm, described high pressure is 10kV-13kV.In the present invention, if the applied voltage of electrostatic spinning is too high, can cause prepared
Nano belt is because electrostatic field force is excessive so that the diameter of nano belt is excessive, and the phenomenon of bonding can occurs at receiving pole.If
Negative electrode is shorter with the distance of anode, and fiber can be caused during forming this of receiving pole owing to solvent can not be waved in time
Sending out, same also results in the phenomenon that can occur bonding at receiving pole.Therefore, comprehensive each factor, cloudy in electrostatic spinning of the present invention
Distance between pole and anode is 18cm-22cm, and the voltage of electrostatic spinning application is 10kV-13kV.
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, from tinfoil paper or wire gauze described in electrostatic spinning
Upper collection obtains solid precursor fiber and also needs to be dried process.Further preferably, the temperature of described dried is 60-
100℃。
At above-mentioned regulation and control BiVO4In the method for full meso-porous nano carrying material, the temperature of described calcination processing is 480-520
DEG C, temperature retention time is 0.4-2h.And in order to improve BiVO4The degree of crystallinity of material, calcination processing is carried out in air atmosphere.
The present invention is formed nano belt by nanofiber and mainly includes two aspects:
Reason one: in precursor solution, the present invention with the addition of the PVP of different molecular quality, is respectively as follows: PVPK30With
PVPK90, and PVPK30With PVPK90Mass ratio be 2-4:1, through stirring after PVPK30And PVPK90Mix homogeneously.Homogeneous transparent
Precursor solution carries out electrostatic spinning, can be divided into two-layer, and reason is as follows: under equal electrospinning conditions, it is ensured that identical
Field intensity (E), flow velocity (Q), electric current (I), the distance of syringe needle to receiving pole.Explore relevant fine according to Baumgarten with Rurledge
Dimension diameter is as follows with the two of the relation of viscosity equations:
R=c η1/2......................(1)
R=c (I/Q)-2/3γ1/3.........................(2)
In formula, R is jet radius, 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 is common constant.From two equations, it is appreciated 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
The PVP that invention usesK30And PVPK90Viscosity be respectively as follows: 2.1-2.7mpa s and 39.5-45.8mpa s.Therefore, have two
The precursor solution of kind different molecular quality PVP, during spinning, can be distributed in the PVP jet process of less molecular mass
In centre, and the PVP of macromole quality can be distributed in outer layer, so the PVP of mix homogeneously in precursor solutionK30And PVPK90
Spinning fibre is separated thus defines two-layer.Due to PVPK30Viscosity and molecular weight all than PVPK90Little, and PVPK30
The volume ratio of equal in quality is relatively big, so can cause the PVP that internal layer is distributedK30Occupy bigger volume, but molecular mass is less
PVPK30Strand does not has PVPK90Long, cause intensity to be not so good as PVPK90, so ground floor there will be and caves in during calcining
Phenomenon, thus define nano belt, add the PVP of different proportionK30And PVPK90, internal degree of subsiding is different, along with
PVPK30The increase of content, volume shared by internal layer is the biggest, collapses the most serious, and the diameter of nano belt also will be the biggest.BiVO4
The mechanism figure such as Fig. 1 of the reason one that nano belt is formed by nanofiber.
Reason two: during electrostatic spinning, precursor solution falls at receiving pole through jet under the effect of electrostatic field force
Upper formation fiber, along with the volatilization of solvent during this.Do not add PVPK30Time, prepared sample 1 is cylindric
Nanofiber.When adding PVPK30And after increasing its content, due to PVPK30There is the effect of lyosoption, solvent can be caused to volatilize
Slower.As Fig. 2 is not added with PVPK30Sample 1 and with the addition of PVPK30Sample 2, sample 2 before 250 DEG C, weight loss ratio
(sample 1 and sample 2 with the addition of PVP except sample 2 to relatively sample more than 1K30In addition, other holdings are constant), same at about 430 DEG C
Having most of mass loss, this is by PVPK30And PVPK90Thermal decomposition simultaneously causes.Thermogravimetric result illustrates, along with PVPK30Contain
The increase of amount, in presoma, solvent can increase, and after being placed on baking oven or calcining, the volatilization of a large amount of solvents can cause nanometer
Subsiding of fiber, this also results in the formation of nano belt, and this is also consistent with the result that SEM observes.
In a word, BiVO of the present invention4Nano belt be formed as the coefficient effect of two above reason.
Compared with prior art, present invention have the advantage that
1, the present invention is by regulation and control raw material composition, by regulation and control different molecular quality PVP content, effectively realizes BiVO4Receive
BiVO prepared by rice fiber4The regulation and control of nanobelt material, by controlling the content of foaming agent, Effective Regulation BiVO4Full mesoporous nano belt
Structure.
2, the present invention regulates and controls BiVO4The method of full mesoporous nano belt is the most controlled, has good repeatability.
Accompanying drawing explanation
Fig. 1 is BiVO of the present invention4Full mesoporous nano belt is formed the mechanism figure of nano belt reason one by nanofiber；
Fig. 2 is BiVO of the present invention4Full mesoporous nano belt is formed in nano belt reason two by nanofiber and is not added with PVPK30's
Sample 1 and with the addition of PVPK30The thermal multigraph of presoma of sample 2；
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 figure of full mesoporous nano belt；
Fig. 6 is the BiVO obtained by the embodiment of the present invention 14The Raman figure 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 is obtained without mesoporous BiVO in comparative example of the present invention4Low power scanning electron microscope (SEM) figure of nano belt；
Figure 14 is obtained without mesoporous BiVO in comparative example of the present invention4High power scanning electron microscope (SEM) figure of nano belt.
Detailed description of the invention
The following is the specific embodiment of the present invention and combine accompanying drawing, technical scheme is further described,
But the present invention is not limited to these embodiments.
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 dehydrated alcohol, N-N diformazan
In the mixed liquor of base Methanamide (DMF) 2.5g and 2g glacial acetic acid, under room temperature, stirring mixing added 0.55g azo diformazan after 6 hours
Acid diisopropyl ester (foaming agent, DIPA) also continues to stir the clear solution obtaining shallow breen.By after the microemulsion spun stands
Measuring in 6ml injected plastic needle tubing, be placed on micro-injection pump, arranging and injecting speed is 0.2mm/min.Metal needle makees electricity
Spinning anode, wire gauze work receives the negative electrode of material, and the distance between anode and negative electrode is 20cm, carries out quiet under 12kV high pressure
Electrospun, prepares organic precursor fibrous material.Then organic precursor fibrous material is placed in 80 DEG C of constant temp. drying boxes, obtains
Obtain the organic precursor fiber of core solid-state.Finally SOLID ORGANIC presoma is placed in quartz boat, in air atmosphere in 500 DEG C
It is incubated and carries out calcination processing, then furnace cooling in 1 hour, prepare BiVO4Nano material.
The BiVO prepared4The low power scanning electron microscope (SEM) of nano material and high power scanning electron microscope (SEM) such as Fig. 3 and Fig. 4 institute
Show, show that prepared material is mesoporous nano belt.Fig. 5 and Fig. 6 is XRD figure and the Raman figure 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 of material and high-resolution-ration transmission electric-lens (HRTEM) figure, prove BiVO further4Nano belt is complete mesoporous knot
Structure and BiVO4Full mesoporous nano belt is monocline scheelite phase BiVO4。
Embodiment 2
The present embodiment differs only in embodiment 1, the diisopropyl azodiformate (foaming added in the present embodiment
Agent, DIPA) it is 1.16g, other are same as in Example 1, are not repeated herein.
The BiVO prepared4The low power scanning electron microscope (SEM) of nano material and high power scanning electron microscope (SEM) are such as Fig. 9 and Figure 10
Shown in, show that prepared material is mesoporous nano belt.
Embodiment 3
The present embodiment differs only in embodiment 1, the diisopropyl azodiformate (foaming added in the present embodiment
Agent, DIPA) it is 1.85g, other are same as in Example 1, are not repeated herein.
The BiVO prepared4The low power scanning electron microscope (SEM) of nano material and high power scanning electron microscope (SEM) are such as Figure 11 and Figure 12
Shown in, show that prepared material is mesoporous nano belt.
Comparative example
This comparative example differs only in embodiment 1, and this comparative example is also not added with diisopropyl azodiformate (foaming
Agent, DIPA), other are same as in Example 1, are not repeated herein.
The BiVO prepared4The low power scanning electron microscope (SEM) of nano material and high power scanning electron microscope (SEM) are such as Figure 13 and Figure 14
Shown in, show that prepared material is not the most mesoporous nano belt.
Embodiment 1 is compared with comparative example, shows when the amount of foaming agent is less in initial feed, by calcining institute
The material of preparation is meso-hole structure, illustrates that adding a small amount of foaming agent can obtain mesoporous nano belt.
Embodiment 2 is compared with embodiment 1, comparative example, along with the increase of the addition of foaming agent, increases to 10%
During wt, it is possible to obtain the preferably full mesoporous nano belt of pattern and structure.
Embodiment 3 is compared with embodiment 1, embodiment 2, comparative example, along with the increase of the addition of foaming agent, increases
When being added to 15%wt, still can obtain the most mesoporous nano belt, and hole content and size all increased.
The data parameters of the present invention is not limited in above-described embodiment, such as polyvinylpyrrolidone (PVPK30) and poly-second
Alkene pyrrolidone (PVPK90) mass ratio can be arbitrarily ratio 2.0:1,2.1:1,2.2:1,2.3:1, the 2.5:1 in 2-4:1,
2.8:1,3.2:1,2.5:1,3.6:1,3.8:1 etc.；Five nitric hydrate bismuth (Bi (NO3)3·5H2O) with vanadyl acetylacetonate (VO
(acac)2) mass ratio can be arbitrarily ratio 1.5:1,1.8:1,2.1:1,2.2:1,2.4:1, the 2.5:1 in 1.5-2.5:1
Deng；The addition of foaming agent can be the arbitrary value in the 3-15wt% accounting for spinning liquid as precursor gross mass: 3wt%, 4wt%,
5wt%, 8wt%, 10wt%, 12wt%, 15wt%；N,N-dimethylformamide (DMF), dehydrated alcohol and glacial acetic acid in solvent
Mass ratio can also be arbitrarily ratio 4:4:4,4:5:4,5:4:4,5:5:4,6:4:4,6:5:4, the 5:6 in 4-6:4-6:4:
4,4:6:4 etc.；Injection speed in spinning liquid as precursor injects needle tubing in electrostatic spinning can be in 0.15-0.25mm/min
Arbitrary value: 0.15mm/min, 0.16mm/min, 0.18mm/min, 0.21mm/min, 0.22mm/min, 0.25mm/min, electrostatic
Distance between spinning Anodic and negative electrode can be the arbitrary value in 18cm-22cm: 18cm, 19cm, 21cm, 22cm etc., should
Can be the arbitrary value in 10kV-13kV with high pressure: 10kV, 10.5kV, 11kV, 11.5kV, 12.5kV, 13kV etc.；It is dried place
Reason temperature can be 60-100 DEG C in arbitrary value: 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 85 DEG C, 90 DEG C, 95 DEG C, 100；Calcining
The temperature processed can be 480-520 DEG C in arbitrary value: 480 DEG C, 490 DEG C, 510 DEG C, 520 etc., temperature retention time is 0.4-2h
In arbitrary value: 0.4h, 0.5h, 0.6h, 0.8h, 1.2h, 1.5h, 1.8h, 2h etc..
Specific embodiment described herein is only to present invention spirit explanation for example.Technology neck belonging to the present invention
Described specific embodiment can be made various amendment or supplements or use similar mode to replace by the technical staff in territory
Generation, but without departing from the spirit of the present invention or surmount scope defined in appended claims.
Claims (10)
1. a regulation and control BiVO4The method of full meso-porous nano carrying material, it is characterised in that described method comprises the steps:
Configuration spinning liquid as precursor: by polyvinylpyrrolidone (PVPK30), polyvinylpyrrolidone (PVPK90), five nitric hydrates
Bismuth (Bi (NO3)3·5H2O), vanadyl acetylacetonate (VO (acac)2) be dissolved in solvent, it is stirring evenly and then adding into foaming agent also
Continue to stir to obtain spinning liquid as precursor；
Spinning liquid as precursor is carried out electrostatic spinning and obtains solid precursor fiber；
By above-mentioned prepared solid precursor fiber through calcination processing, BiVO4Full meso-porous nano carrying material.
Regulation and control BiVO the most according to claim 14The method of full meso-porous nano carrying material, it is characterised in that described polyethylene
Ketopyrrolidine (PVPK30) and polyvinylpyrrolidone (PVPK90) mass ratio be 2-4:1.
Regulation and control BiVO the most according to claim 14The method of full meso-porous nano carrying material, described five nitric hydrate bismuth (Bi
(NO3)3·5H2O) with vanadyl acetylacetonate (VO (acac)2) mass ratio be 1.5-2.5:1.
Regulation and control BiVO the most according to claim 14The method of full meso-porous nano carrying material, it is characterised in that described solvent
For N,N-dimethylformamide (DMF), dehydrated alcohol and the mixed liquor of glacial acetic acid.
Regulation and control BiVO the most according to claim 44The method of full meso-porous nano carrying material, it is characterised in that described N, N-bis-
The mass ratio of methylformamide (DMF), dehydrated alcohol and glacial acetic acid is 4-6:4-6:4.
Regulation and control BiVO the most according to claim 14The method of full meso-porous nano carrying material, it is characterised in that described foaming
Agent is diisopropyl azodiformate (DIPA), and the addition of foaming agent accounts for the 3-15wt% of spinning liquid as precursor gross mass.
Regulation and control BiVO the most according to claim 14The method of full meso-porous nano carrying material, it is characterised in that described Static Spinning
The method of silk is: being injected by spinning liquid as precursor in needle tubing, be placed on micro-injection pump, metal needle makees Electrospun anode,
Tinfoil paper or wire gauze make to receive the negative electrode of material, under high pressure carry out electrostatic spinning, then obtain from tinfoil paper or iron wire online collection
To solid precursor fiber.
Regulation and control BiVO the most according to claim 74The method of full meso-porous nano carrying material, it is characterised 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 negative electrode it
Between distance be 18cm-22cm, described high pressure is 10kV-13kV.
Regulation and control BiVO the most according to claim 74The method of full meso-porous nano carrying material, it is characterised in that in electrostatic spinning
Described obtain solid precursor fiber from tinfoil paper or iron wire online collection and also need to be dried process.
Regulation and control BiVO the most according to claim 14The method of full meso-porous nano carrying material, it is characterised in that described calcining
The temperature processed is 480-520 DEG C, and temperature retention time is 0.4-2h.
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| CN113417032A (en) * | 2021-05-17 | 2021-09-21 | 宁波工程学院 | Preparation method of nitrogen-doped mesoporous carbon fiber-based non-noble metal electrocatalyst |
| CN116023801A (en) * | 2022-12-27 | 2023-04-28 | 成都先进金属材料产业技术研究院股份有限公司 | Coating method of bismuth vanadate pigment powder |
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| CN105420854A (en) * | 2015-12-17 | 2016-03-23 | 宁波工程学院 | BiVO4 full mesoporous fiber material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113417032A (en) * | 2021-05-17 | 2021-09-21 | 宁波工程学院 | Preparation method of nitrogen-doped mesoporous carbon fiber-based non-noble metal electrocatalyst |
| CN116023801A (en) * | 2022-12-27 | 2023-04-28 | 成都先进金属材料产业技术研究院股份有限公司 | Coating method of bismuth vanadate pigment powder |
| CN116023801B (en) * | 2022-12-27 | 2024-05-28 | 成都先进金属材料产业技术研究院股份有限公司 | Coating method of bismuth vanadate pigment powder |
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