CN106929948A - A kind of titanium oxide meso-porous nano fiber producing processes and its application based on coaxial electrostatic spinning - Google Patents
A kind of titanium oxide meso-porous nano fiber producing processes and its application based on coaxial electrostatic spinning Download PDFInfo
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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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
- C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
- C04B35/62259—Fibres based on titanium oxide
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
A kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning, comprise the following steps：S1：The preparation of spinning precursor solution；S2：By coaxial electrostatic spinning technique, spinning precursor solution prepared by step S1 is poured into electrospinning in coaxial injectors and obtains nanofiber；S3：By step S2 prepare nanofiber be put into annealing furnace, after being made annealing treatment can acquisition titanium oxide meso-porous nano fiber or titanium oxide composite reactive carbon nanofibers.Its advantage is：Precursor solution is prepared by by raw material of polyvinylpyrrolidone, paraffin oil, butyl titanate, glacial acetic acid and absolute ethyl alcohol, and is equipped with coaxial electrostatic spinning technology so that the nanofiber of preparation is hollow structure；Meanwhile, beneficial to the stability maintained before titanium source annealing, it is hollow out tube wall that the addition of paraffin oil is conducive to the hollow structure for preparing, and increases specific surface area and porosity for the addition of glacial acetic acid in precursor solution.
Description
Technical field
The present invention relates to the preparing technical field of material, specifically a kind of titanium oxide based on coaxial electrostatic spinning
Meso-porous nano fiber producing processes and its application.
Background technology
Ultracapacitor (supercapacitor) is called electrochemical capacitor, be one kind between traditional capacitor and electric power storage
New type of energy storage device between pond.Ultracapacitor have high power than, cycle life is high, charge-discharge velocity is fast, environment-friendly
The features such as, therefore ultracapacitor is a kind of preferable secondary power supply, in low-power consumption such as：Mobile communication, information technology etc. and height
Power consumption is such as：The aspects such as electric automobile, Aero-Space and science and techniques of defence suffer from application prospect of crucial importance and wide.
Ultracapacitor includes electrode material, electrolyte and barrier film, and wherein electrode material is the core of ultracapacitor.Reason
Electrode material requirement good conductivity, high-specific surface area, the high porosity thought.Present electrode material has porous carbon material, your gold
Category oxide, conductive polymer polymer and advanced composite material (ACM) etc..Metal oxide containing precious metals are limited due to the high development of cost
System, it is therefore necessary to which research environment is friendly, metal oxide electrode material with low cost.
The content of the invention
In view of this, it is an object of the invention to proposing a kind of preparation method of titanium oxide meso-porous nano fiber and its answering
With, and will prepare titanium oxide meso-porous nano fiber and its with activated carbon be combined mesoporous nano fiber be used for ultracapacitor
Research.
One aspect of the present invention provides a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning, bag
Include following steps：
S1：The preparation of spinning precursor solution：With polyvinylpyrrolidone, paraffin oil, butyl titanate, glacial acetic acid and nothing
Water-ethanol prepares precursor solution for raw material；
S2：By coaxial electrostatic spinning technique, spinning precursor solution prepared by step S1 is poured into outer shaft syringe
In, perfusion paraffin oil prepares butyl titanate nanofiber in interior axle syringe, or spinning presoma prepared by step S1
Infusion obtains butyl titanate composite activated carbon in interior axle syringe, outer shaft perfusion paraffin oil and the mixed solution of activated carbon
Nanofiber；
S3：By step S2 prepare nanofiber be put into annealing furnace, after being made annealing treatment can acquisition titanium oxide
Meso-porous nano fiber or titanium oxide composite reactive carbon nanofibers.
Second aspect present invention provides a kind of ultracapacitor, the titanium that electrode material is prepared using the above method in capacitor
Oxide mesoporous nanofiber or titanium oxide composite reactive carbon nanofibers.
A kind of preparation method and applications of titanium oxide meso-porous nano fiber, its advantage is：
Forerunner is prepared by by raw material of polyvinylpyrrolidone, paraffin oil, butyl titanate, glacial acetic acid and absolute ethyl alcohol
Liquid solution, and it is equipped with coaxial electrostatic spinning technology so that the nanofiber of preparation is hollow structure；Meanwhile, in precursor solution
Beneficial to the stability maintained before titanium source annealing, it is hollow out that the addition of paraffin oil is conducive to the hollow structure for preparing for the addition of glacial acetic acid
Tube wall, increases specific surface area and porosity；
Furthermore, the titanium oxide meso-porous nano fiber or titanium oxide composite reactive carbon nanofibers of preparation can be used as super
The electrode material of level capacitor is used, and titanium oxide meso-porous nano fiber is improved on the basis of fake capacitance effect is not influenceed
Porosity strengthens its electric double layer capacitance effect；Titanium oxide composite reactive carbon nanofibers, further increase ultracapacitor
Specific capacitance, power density and energy density；Have that with low cost, environment-friendly, the good characteristic such as have extended cycle life simultaneously.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram of the titanium oxide meso-porous nano fiber that 1 500 DEG C of embodiment is obtained；
Fig. 2, Fig. 3 are respectively 500 DEG C in embodiment 2,600 DEG C when the annealing titanium oxide meso-porous nano fiber that obtains sweep
Retouch electron microscope picture；
Fig. 4 is the scanning electron microscope diagram of the titanium oxide composite reactive carbon nanofibers that 3 600 DEG C of embodiment is obtained；
Fig. 5 is titanium oxide meso-porous nano fiber, the titanium oxide composite activated carbon nanofiber electrode electrical property for preparing
Can test chart.
Specific embodiment
One aspect of the present invention provides a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning, bag
Include following steps：
S1：The preparation of spinning precursor solution：With polyvinylpyrrolidone, paraffin oil, butyl titanate, glacial acetic acid and nothing
Water-ethanol prepares precursor solution for raw material；
Preferably, step S1 is comprised the following steps：
S11,0.5g~0.8g polyvinylpyrrolidones are mixed with 3ml~4ml absolute ethyl alcohols, at ambient temperature magnetic force
Stirring is dissolved completely in absolute ethyl alcohol up to polyvinylpyrrolidone, standby；
S12,1.5ml~2.5ml butyl titanates are dropped to 2ml~3ml glacial acetic acid and 1.5ml~2.5ml absolute ethyl alcohols
Mixed liquor in, stir 1~2h, it is standby；
S13, the solution for preparing step S11, S12 are mixed after mixing with 1.0ml~2.0ml paraffin oils, and stirring 2~
3h, just obtains spinning precursor solution；
S2：By coaxial electrostatic spinning technique, spinning precursor solution prepared by step S1 is poured into outer shaft syringe
In, perfusion paraffin oil prepares butyl titanate nanofiber in interior axle syringe, or spinning presoma prepared by step S1
Infusion obtains butyl titanate composite activated carbon in interior axle syringe, outer shaft perfusion paraffin oil and the mixed solution of activated carbon
Nanofiber；
Preferably, in step S2, prepare during butyl titanate nanofiber, 2~4ml paraffin is irrigated in interior axle syringe
Oil；
Preferably, in step S2, the spinning process condition for preparing butyl titanate nanofiber is：The direct current of 10~15KV
Pressure, and nozzle diameter is that distance is set to 12~15cm between 0.2~0.5mm, nozzle and receiver, outer shaft fltting speed is 80~
120um/min, interior axle fltting speed is 10~12um/min, and temperature is 18~25 DEG C, and relative humidity is 24%~50%, spinning
10~15min of time；
Preferably, in step S2, prepare during butyl titanate composite reactive carbon nanofibers, outer shaft irrigates 5ml~7ml
The mixed solution of paraffin oil and 0.1g~0.3g activated carbons；
Preferably, in step S2, the spinning process condition for preparing butyl titanate composite reactive carbon nanofibers is：10~
The DC voltage of 15KV, and nozzle diameter is that distance is set to 12~15cm between 0.2~0.5mm, nozzle and receiver, outer shaft is pushed away
Enter speed for 10~12um/min, interior axle fltting speed is 80~120um/min, temperature is 18~25 DEG C, and relative humidity is
24%~50%, 10~15min of spinning time；
S3：By step S2 prepare nanofiber be put into annealing furnace, after being made annealing treatment can acquisition titanium oxide
Meso-porous nano fiber or titanium oxide composite reactive carbon nanofibers.
Preferably, in step S3, first butyl titanate nanofiber or butyl titanate composite reactive carbon nanofibers are cut out
After be positioned in the middle of two pieces of iron plates so that the nanofiber cut out is wrapped between two panels iron plate, then will be placed with Nanowire
The iron plate of dimension is put into high temperature furnace and is heated to 500~700 DEG C, and heating rate is 3~5 DEG C/min, and soaking time is 3~
5h。
Second aspect present invention provides a kind of ultracapacitor, the titanium that electrode material is prepared using the above method in capacitor
Oxide mesoporous nanofiber or titanium oxide composite reactive carbon nanofibers.
Understand the present invention in order to clearer, the present invention is discussed in detail below in conjunction with drawings and Examples：
Embodiment one：The preparation of titanium oxide meso-porous nano fiber
S1：The preparation of spinning precursor solution：
S11, take 0.5g polyvinylpyrrolidones (PVP；Mx=1,300,000) add 3ml absolute ethyl alcohol in mix, then
At room temperature magnetic agitation 5h until polyvinylpyrrolidone be dissolved completely in absolute ethyl alcohol, obtain PVP solution for standby；
S12,1.5ml butyl titanates are slowly dropped into the mixed solution of 2ml absolute ethyl alcohols and 3ml glacial acetic acid, stir 1h
It is well mixed, it is standby；
S13, the solution for preparing step S11, S12 add the paraffin oil of 1.0ml, magnetic agitation under room temperature condition after mixing
2h, obtains spinning precursor solution；
In S2, the spinning precursor solution injection outer shaft syringe for preparing step S1, injection 2ml stones in interior axle syringe
Wax oil, adjusting electrospinning conditions is：Apply the DC voltage of 12KV, and nozzle diameter is 0.2mm, nozzle and receiver spacing
From being set to 12cm, outer shaft fltting speed 90um/min, interior axle fltting speed is 10um/min, 18 DEG C of temperature, and relative humidity is
24%, spinning time 12min, obtain the uniform butyl titanate nanofiber of spinning；
S3：In step S3, it is positioned in the middle of two pieces of iron plates after first butyl titanate nanofiber prepared by step S2 is cut out,
So that the butyl titanate nanofiber cut out is wrapped between two panels iron plate；The iron of butyl titanate nanofiber will be placed with again
Piece is heated to 500 DEG C in being put into high temperature furnace, and heating rate is 3 DEG C/min, and soaking time is 5h, is annealed naturally, to obtain
Obtain titanium oxide meso-porous nano fiber.
Titanium oxide meso-porous nano fiber such as Fig. 1 (scannings when for annealing temperature being 500 DEG C obtained by the present embodiment
Electron microscope picture), understood according in Fig. 1, titanium oxide meso-porous nano fibre diameter is 100~200nm, and fiber surface is thick
Rough, fiber two ends can see obvious alveolate texture.
Embodiment two：The preparation of titanium oxide meso-porous nano fiber
S1：The preparation of spinning precursor solution：
S11, take 0.8g polyvinylpyrrolidones (PVP；Mx=1,300,000) add 4ml absolute ethyl alcohol in mix, then
At room temperature magnetic agitation 5h until polyvinylpyrrolidone be dissolved completely in absolute ethyl alcohol, obtain PVP solution for standby；
S12,2.5ml butyl titanates are slowly dropped into the mixed solution of 2.5ml absolute ethyl alcohols and 2ml glacial acetic acid, stirred
2h is well mixed, standby；
S13, the solution for preparing step S11, S12 add the paraffin oil of 2.0ml, magnetic agitation under room temperature condition after mixing
2h, obtains spinning precursor solution；
In S2, the spinning precursor solution injection outer shaft syringe for preparing step S1, injection 4ml stones in interior axle syringe
Wax oil, adjusting electrospinning conditions is：Apply the DC voltage of 15KV, and nozzle diameter is 0.2mm, nozzle and receiver spacing
From being set to 12cm, outer shaft fltting speed 100um/min, interior axle fltting speed is 12um/min, 25 DEG C of temperature, and relative humidity is
50%, spinning time 15min, obtain the uniform butyl titanate nanofiber of spinning；
S3：It is positioned in the middle of two pieces of iron plates after first butyl titanate nanofiber prepared by step S2 is cut out so that cut out
Butyl titanate nanofiber be wrapped between two panels iron plate；The iron plate that butyl titanate nanofiber will be placed with again is put into height
500 DEG C, 600 DEG C (equal scanning electron microscope diagram when 500 DEG C, 600 DEG C are warming up to), and liter are heated in warm stove respectively
Warm speed is 4 DEG C/min, and soaking time is 3h, is annealed naturally, to obtain titanium oxide meso-porous nano fiber.
(Fig. 2 is that annealing temperature is 500 DEG C to titanium oxide meso-porous nano fiber such as Fig. 2, the Fig. 3 obtained by the present embodiment
When scanning electron microscope diagram, Fig. 3 is scanning electron microscope diagram when annealing temperature is 600 DEG C), can according to Fig. 2, Fig. 3
Know, titanium oxide meso-porous nano fibre diameter is 100~200nm, fiber surface forms Openworks shape, and fiber two ends can be seen substantially
Hollow form structure.
Embodiment three：The preparation of titanium oxide composite reactive carbon nanofibers
S1：The preparation of spinning precursor solution：
S11, take 0.6g polyvinylpyrrolidones (PVP；Mx=1,300,000) add 4ml absolute ethyl alcohol in mix, then
At room temperature magnetic agitation 4h until polyvinylpyrrolidone be dissolved completely in absolute ethyl alcohol, obtain PVP solution for standby；
S12,2ml butyl titanates are slowly dropped into the mixed solution of 2ml absolute ethyl alcohols and 2ml glacial acetic acid, stir 1.5h
It is well mixed, it is standby；
S13, the solution for preparing step S11, S12 add the paraffin oil of 1.5ml, magnetic agitation under room temperature condition after mixing
2.5h, obtains spinning precursor solution；
S2, the spinning precursor solution for preparing step S1 inject interior axle syringe, outer shaft syringe as outer shaft solution
The mixed solution of interior perfusion 5ml paraffin oils and 0.1g activated carbons, adjusting electrospinning conditions is：Apply the DC voltage of 15KV,
And nozzle diameter is that distance is set to 12cm, outer shaft fltting speed 12um/min, interior axle propulsion between 0.2mm, nozzle and receiver
Speed is 90um/min, 20 DEG C of temperature, and relative humidity is 24%, spinning time 12min, obtains the uniform butyl titanate of spinning and receives
Rice fiber；
S3：It is positioned in the middle of two pieces of iron plates after first butyl titanate nanofiber prepared by step S2 is cut out so that cut out
Butyl titanate nanofiber be wrapped between two panels iron plate；The iron plate that butyl titanate nanofiber will be placed with again is put into height
600 DEG C are heated in warm stove respectively, and heating rate is 4 DEG C/min, soaking time is 3h, is annealed naturally, to obtain titanium
Oxide mesoporous nanofiber.
The titanium oxide composite activated carbon meso-porous nano fiber such as Fig. 4 obtained by the present embodiment is that annealing temperature is 600
DEG C when scanning electron microscope diagram, shown in figure titanium oxide composite activated carbon meso-porous nano fiber a diameter of 100~
200nm, and fiber surface is distributed uniform activated carbon granule.
Three kinds of titanium oxide composite activated carbons of titanium oxide meso-porous nano fiber in above-described embodiment two and embodiment are situated between
Hole nanofiber is as the electrode material in ultracapacitor, and ultracapacitor to being provided with this electrode material carries out electricity
Chemical property is tested：
Tested using cyclic voltammetry (CV circulations), and sweep speed is 50mV/S, scanning voltage width is -1V~1V,
Electrode material area is 1cm*1.5cm.
Fig. 5 is CV loop test results, and titanium oxide meso-porous nano fiber obtained in as shown by data and titanium oxide are compound
Activated carbon meso-porous nano fiber enhances the electric double layer capacitance effect of electrode material, with specific capacitance higher and good follows
Ring charging-discharging performances, as can be seen from the figure titanium oxide nanofiber occur redox peaks between 0.05V~0.2V, but
Increase with scanning voltage, current value declines, electric double layer capacitance effect does not embody；
The porosity of electrode material is also enhanced simultaneously, is observed according in Fig. 5, be not decreased obviously after redox peaks
Gesture, 40% is increased compared to titanium oxide nanofiber specific capacitance, and activated carbon can improve electrode material electric conductivity, therefore with titanyl
The fake capacitance and electric double layer capacitance of electrode material prepared by compound composite activated carbon meso-porous nano fiber have certain enhancing, its ratio
Electric capacity is 4mA/cm2；Have extended cycle life, loop test 6 hours, its capacity attenuation is less than 15%.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (8)
1. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning, it is characterised in that：Including as follows
Step
S1：The preparation of spinning precursor solution：With polyvinylpyrrolidone, paraffin oil, butyl titanate, glacial acetic acid and anhydrous second
Alcohol prepares precursor solution for raw material；
S2：By coaxial electrostatic spinning technique, spinning precursor solution prepared by step S1 is poured into outer shaft syringe, it is interior
Perfusion paraffin oil prepares butyl titanate nanofiber in axle syringe, or spinning precursor solution prepared by step S1 is filled
Note in interior axle syringe, outer shaft perfusion paraffin oil and the mixed solution of activated carbon, obtain butyl titanate composite activated carbon Nanowire
Dimension；
S3：By step S2 prepare nanofiber be put into annealing furnace, after being made annealing treatment can acquisition titanium oxide it is mesoporous
Nanofiber or titanium oxide composite reactive carbon nanofibers.
2. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning according to claim 1, its
It is characterised by：Step S1 is comprised the following steps：
S11,0.5g~0.8g polyvinylpyrrolidones are mixed with 3ml~4ml absolute ethyl alcohols, at ambient temperature magnetic agitation
Until polyvinylpyrrolidone is dissolved completely in absolute ethyl alcohol, it is standby；
S12,1.5ml~2.5ml butyl titanates are dropped to the mixed of 2ml~3ml glacial acetic acid and 1.5ml~2.5ml absolute ethyl alcohols
Close in liquid, stir 1~2h, it is standby；
S13, the solution for preparing step S11, S12 are mixed after mixing with 1.0ml~2.0ml paraffin oils, stir 2~3h,
Just spinning precursor solution is obtained.
3. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning according to claim 1, its
It is characterised by：In step S2, prepare during butyl titanate nanofiber, 2~4ml paraffin oils are irrigated in interior axle syringe.
4. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning according to claim 1, its
It is characterised by：In step S2, the spinning process condition for preparing butyl titanate nanofiber is：The DC voltage of 10~15KV, and
Nozzle diameter is that distance is set to 12~15cm between 0.2~0.5mm, nozzle and receiver, outer shaft fltting speed is 80~
120um/min, interior axle fltting speed is 10~12um/min, and temperature is 18~25 DEG C, and relative humidity is 24%~50%, spinning
10~15min of time.
5. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning according to claim 1, its
It is characterised by：In step S2, prepare during butyl titanate composite reactive carbon nanofibers, outer shaft irrigates 5ml~7ml paraffin oils
With the mixed solution of 0.1g~0.3g activated carbons.
6. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning according to claim 1, its
It is characterised by：In step S2, the spinning process condition for preparing butyl titanate composite reactive carbon nanofibers is：10~15KV's is straight
Stream voltage, and nozzle diameter is that distance is set to 12~15cm between 0.2~0.5mm, nozzle and receiver, outer shaft fltting speed is
10~12um/min, interior axle fltting speed is 80~120um/min, and temperature is 18~25 DEG C, and relative humidity is 24%~50%,
10~15min of spinning time.
7. a kind of titanium oxide meso-porous nano fiber producing processes based on coaxial electrostatic spinning according to claim 1, its
It is characterised by：In step S3, placed after first cutting out butyl titanate nanofiber or butyl titanate composite reactive carbon nanofibers
In the middle of two pieces of iron plates so that the nanofiber cut out is wrapped between two panels iron plate, then the iron of nanofiber will be placed with
Piece is heated to 500~700 DEG C in being put into high temperature furnace, and heating rate is 3~5 DEG C/min, and soaking time is 3~5h.
8. a kind of ultracapacitor, the titanium oxide meso-porous nano fiber prepared with any methods described of such as claim 1 to 8,
Or titanium oxide composite reactive carbon nanofibers are used as the electrode material of ultracapacitor.
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| CN201710039169.1A CN106929948A (en) | 2017-01-19 | 2017-01-19 | A kind of titanium oxide meso-porous nano fiber producing processes and its application based on coaxial electrostatic spinning |
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| CN201710039169.1A CN106929948A (en) | 2017-01-19 | 2017-01-19 | A kind of titanium oxide meso-porous nano fiber producing processes and its application based on coaxial electrostatic spinning |
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| CN111330624A (en) * | 2020-03-25 | 2020-06-26 | 陕西科技大学 | One-step method for preparing hierarchical mesoporous-porous TiO2/g-C3N4Nanofiber photocatalytic material |
| CN113529197A (en) * | 2020-04-22 | 2021-10-22 | 中化(宁波)润沃膜科技有限公司 | Polyvinylpyrrolidone hollow nanofiber and preparation method thereof |
| CN115778827A (en) * | 2023-02-02 | 2023-03-14 | 广东碧茜生物科技有限公司 | high-VC-loading core/shell type nanofiber mask and preparation method and application thereof |
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Application publication date: 20170707 |