CN106676653A - Three-level coaxial electro-spinning method for loading two sheath fluids without spinnability on core fluid - Google Patents
Three-level coaxial electro-spinning method for loading two sheath fluids without spinnability on core fluid Download PDFInfo
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- CN106676653A CN106676653A CN201611021148.9A CN201611021148A CN106676653A CN 106676653 A CN106676653 A CN 106676653A CN 201611021148 A CN201611021148 A CN 201611021148A CN 106676653 A CN106676653 A CN 106676653A
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- 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
- D01D5/0015—Electro-spinning characterised by the initial state of the material
-
- 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
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- 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
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention relates to a three-level coaxial electro-spinning method for loading two sheath fluids without spinnability on a core fluid. According to the method, spinnability of the polymer core fluid is used as support, functional fluids without spinnability are loaded in an external sheath fluid surrounding manner to serve as an interlayer, pure organic solvents serve as outermost fluids, and a three-level coaxial high-voltage electrostatic spinning process is implemented. The outermost organic solvents can effectively ensure stability and continuous implementation of the three-level coaxial electro-spinning process, and high-quality core sheath structure nano-fiber products can be prepared. The functional fluids without spinnability are effectively led into the three-level coaxial electro-spinning process, and the nano-structure preparation capacity of the process is greatly extended. Besides, the method is effective in single step, prepared nano-fiber core sheath structures are clear, small in nano-fiber diameter, good in linearity and uniform in diameter distribution, and fiber surfaces are smooth. By the method, numerous functional components can be loaded on the polymer nano-fiber surfaces to obtain novel functional nano-fiber products.
Description
Technical field
The present invention relates to a kind of processing of micro Nano material, more particularly to a kind of core fluid carries two kinds can not spin outer sheath fluid
Three-level coaxial electrically spun method.
Background technology
High-voltage electrostatic spinning technology（Electrospinning）It is a kind of nano-fabrication technique of (top-down) from top to bottom, by additional
Electric field force overcomes the surface tension of liquid and viscoelastic power of shower nozzle tip drop and forms jet, in electrostatic repulsion, Coulomb force and table
Under the tension force collective effect of face, the liquid jet after being atomized is drafted thousand by high frequency flexural, drawing, division within a few tens of milliseconds
Wan Bei, nano-scale fiber is obtained through solvent volatilization or melt cooling in receiving terminal.The technical matters process is simple, manipulation is convenient,
Material ranges are extensive for selection, controllability is strong, be considered as one kind side for most possibly realizing continuous nano-fibre industrialized production
Method, preparing functional nano-fiber using the technology has good prospect.
But there are two aspect reasons to significantly limit the extensive use of the technology at present.One is an only 100 kinds left sides
Right polymer has good spinning properties, and the concentration window spun of these polymer is narrow；The second is due to making
Spinning solution is allocated with the organic solvent for being easy to volatilization, therefore there are many materials（Small molecule function ingredients including easy precipitation,
Binding agent, the protein for easily being interacted with spinneret etc.）It is very easy to block spinneret.The effective of these problems overcomes
It is possible to greatly expand the nano structural material preparative capacibility of electrospinning processes, is guided out the polymer matrix function of a series of new
Micro-nano rice product.
The content of the invention
Material limited problem when being used the present invention be directed to high-voltage electrostatic spinning technology, it is proposed that a kind of core fluid is carried
Two kinds of three-level coaxial electrically spun methods that can not spin outer sheath fluid, the method with using polymer core liquid spinnability for support, with
The mode of outer shroud sheath fluid carries the functional fluid without spinning properties for intermediate layer and pure organic solvent are outermost layer fluid, real
Apply three-level coaxial high pressure electrostatic spinning process.
The technical scheme is that：A kind of core fluid carries two kinds of three-level coaxial electrically spun sides that can not spin outer sheath fluid
Method, specifically includes following steps：
1）Build preparation facilities：In the coaxial spinneret of three-level by three capillaries of different sizes constitute it is interior, in, outer three layers it is same
Correspondence is installed with internal layer and middle layer fluid injection on axial outlet, internal layer fluid syringe pump and middle layer fluid syringe pump
Device, internal layer and intermediate layer fluid injector are by the internal layer in high resiliency silica gel hose and the coaxial spinneret of three-level and intermediate layer
Capillary inlet is connected, on outer layer fluid syringe pump fixedly mount outer layer fluid injector directly with the coaxial spinneret of three-level
In outer capillary tube entrance be connected, high pressure generator and the connection of three-level coaxial spinneret, under the coaxial spinneret exit orifices of three-level
The fiber for holding the hardboard of useful aluminium foil parcel to make receives flat board；
2）Inner operative fluid is made into using spinnable polymer solution, is the Core support fluid of three-level coaxial electrically spun, injected
Internal layer fluid injector；
3）Intermediate layer working fluid is made into using not spinnable function ingredients solution, intermediate layer fluid injector is injected；
4）Outer operative fluid is made into using pure organic solvent, outer layer fluid injector is injected；
5）High pressure generator is opened, three kinds of flow velocitys of fluid in the coaxial spinneret of three-level are controlled respectively by three syringe pumps,
In the presence of high-pressure electrostatic, the coaxial spinneret exit orifices of three-level produce the nanofiber with core sheath structure feature, are connect by fiber
It is closed flat plate reception.
The step of feature nanofiber with core sheath structure 2）、3）With 4）Three layers of allotment of working fluid：By 15 grams
Cellulose acetate is put into 120 grams of mixed solvents, is made into the Core support fluid with favorable spinning quality, and mixed solvent is by 20
Gram DMF, 20 grams of ethanol and 80 grams of acetone are mixed；Outer operative fluid is by 20 grams of N, N- dimethyl methyls
Acid amides, 20 grams of ethanol and 80 grams of acetone are mixed；10 grams of gliadins are dissolved in the mixed solvent of 100 grams of acetic acid and ethanol,
Volume ratio acetic acid：Ethanol is 1:3, constitute middle level working fluid；
Step 5 after the allotment）Control is required：Internal layer, intermediate layer, outer layer fluid flow are respectively 0.5,0.5,2.0 mL/h,
It is 20 cm, the kV of high pressure generator voltage 18 with a distance from spinning nozzle that fiber receives flat board；Environment temperature is 24 ± 2 DEG C, environment
Humidity is 55 ± 5%.
It is described with core sheath structure feature nanofiber for medicine directly wraps up polymer fiber when the step of 2）、3）With 4）
Three layers of allotment of working fluid：15 grams of cellulose acetates are put into 120 grams of mixed solvents, are made into favorable spinning quality
Core support fluid, mixed solvent is mixed by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone；Outer layer work
Make fluid to be mixed by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone；10 grams of medicine Ketoprofens are dissolved
In the mixed solvent being made up of 80 grams of acetone and 20 grams of ethanol be middle level working fluid；
Step 5 after the allotment）Control is required：：Internal layer, intermediate layer, outer layer fluid flow are respectively 0.5,1.0,2.0 mL/h,
It is 20 cm with a distance from spinning nozzle that fiber receives flat board, and the kV of high pressure generator voltage 20, environment temperature is 24 ± 2 DEG C, environment
Humidity is 55 ± 5%.
The beneficial effects of the present invention are：Core fluid of the present invention carries two kinds of three-level coaxial electrically spuns that can not spin outer sheath fluid
Method, outer layer organic solvent can effectively ensure that three-level coaxial electrically spun technique stabilization and lasting implementation, while ensure prepare
Go out high-quality core sheath structure nanofiber product.Spinnable functional fluid is effectively introduced three-level coaxial electrically spun by the inventive method
In technique, the nanostructured preparative capacibility of the technique is greatly expanded；The method single step simultaneously is effective, the Nanowire prepared
Dimension core sheath structure is clear, nanofiber diameter is small, good linearity, diameter are evenly distributed, fiber surface is smooth.Can be with by the method
Numerous function ingredients are mounted in polymer nanofiber surface, new function nanofiber product is obtained.
Brief description of the drawings
Fig. 1 is the coaxial spinneret schematic diagram of three-level of the present invention；
Fig. 2 is that core fluid of the present invention carries two kinds of three-level coaxial electrically spun method implementation schematic diagrams that can not spin outer sheath fluid；
Fig. 3 is that core fluid of the present invention carries two kinds of Taylor's diagram cones that can not spin the three-level coaxial electrically spun process shooting of outer sheath fluid；
Fig. 4 is that two kinds of present invention application core fluid carrying can not spin the scanning that outer sheath fluid three-level coaxial electrically spun prepares nanofiber
Electron microscope picture；
Fig. 5 is that present invention application core fluid two kinds of three-level coaxial electrically spuns that can not spin outer sheath fluid of carrying prepare the saturating of nanofiber
Penetrate electron microscope picture.
Specific embodiment
The coaxial spinneret of three-level that the present invention is used as shown in figure 1, by of different sizes, in, outer three layers coaxial capillary
Pipe is constituted, including：Outer capillary tube 1, intermediate layer capillary 2, internal layer capillary 3, the end rubber entry joint of outer capillary tube 1
4, interior, middle capillary 2, the bulge loop joint 5 of 3 ends and for fixed adhesive epoxy resin 6.Three-level coaxial electrically spun technology reality
Installation drawing is applied as shown in Fig. 2 including the coaxial spinneret 8 of high pressure generator 7, three-level, outer layer fluid syringe pump 9, middle fluid layer body
Syringe pump 10, internal layer fluid syringe pump 11, fiber receiver board 12, ground connection 13, middle layer fluid conveying high resiliency silica gel hose 14,
Internal layer fluid conveying high resiliency silica gel hose 15.
Internal layer fluid injector 18 and centre are separately installed with internal layer fluid syringe pump 11 and central fluid syringe pump 10
Internal layer and intermediate layer working fluid are filled in layer fluid syringe 17, syringe respectively, syringe is soft by high resiliency silica gel respectively
Pipe 15 and high resiliency silica gel hose 14 are connected with internal layer capillary and intermediate layer capillary in the coaxial spinneret 8 of three-level.Outward
Installation outer layer fluid injector 16 on layer fluid syringe pump 9, the built-in outer operative fluid of syringe, the coaxial spinneret 8 of three-level
Outer capillary tube is connected directly between outer layer fluid injector.The described coaxial spinneret 8 of high pressure generator 7 and described three-level connects
Connect, the coaxial lower end of spinneret 8 of described three-level is provided with a receiver board 12, and receiver sheet 12 is provided with ground connection 13.Fiber is received
Flat board 12 is the hardboard of aluminium foil parcel.
Three layers of allotment of working fluid：15 grams of cellulose acetates are put into 120 grams of mixed solvents, are made into good spinning
The operating core fluid of silk performance.Mixed solvent is by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone mixing
Into.Outer layer solvent is mixed by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone.10 grams of gliadins are dissolved in
In the mixed solvent of 100 grams of acetic acid and ethanol（Volume ratio acetic acid：Ethanol is 1:3) intermediate layer working fluid, is constituted.
The implementation of three-level coaxial high pressure electrostatic spinning process：Above-mentioned three kinds of working fluids are respectively charged into internal layer, intermediate layer
In the syringe of outer operative fluid, each layer fluid is connected in the coaxial spinneret of three-level according to Fig. 2 shown devices, connect high
Pressure spinneret and HV generator.
Implement three-level coaxial high pressure electrostatic spinning process according to following technological parameter：Internal layer/centre/outer laminar fluid flow
It is 0.5/0.5/2.0 mL/h to measure, and receiver board is 20 cm, the kV of voltage 18 with a distance from spinning nozzle.Environment temperature is (24 ± 2)
DEG C, ambient humidity is 55 ± 5%.Fiber wraps up cardboard and is collected by the aluminium foil being grounded.In the above operating condition, to electricity
Spinning process carries out bust shot in situ, as a result as shown in figure 3, the three-layer fluid from the coaxial spinneret of three-level out is collectively forming one
Individual compound Taylor cone, the top of cone sends a straight jet.
The analysis and characterization of nanofiber：Using field scan Electronic Speculum（FESEM）Seen after surface metal spraying is carried out to prepared fiber
Examine, as a result as shown in Figure 4.Prepared fiber is presented good linear condition, does not have bead structure, fiber surface light
Sliding, fiber accumulations are uniform.A diameter of 470 ± 50 nm, than more uniform, concentration is compared in diameter distribution for distribution.
Using high-resolution projection electron microscope（TEM）Prepared fibrous inner structure is observed, as a result such as Fig. 5 institutes
Show, the core sheath structure of nanofiber is clear.
It is prepared by the core sheath structure that medicine directly wraps up polymer fiber：15 grams of cellulose acetates are put into 120 grams of mixing molten
In agent, the operating core fluid with favorable spinning quality is made into.Mixed solvent is by 20 grams of DMFs, 20 grams of second
Alcohol and 80 grams of acetone are mixed.Outer layer solvent is by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone mixing
Into.10 grams of medicine Ketoprofens are dissolved in the mixed solvent being made up of 80 grams of acetone and 20 grams of ethanol and constitute intermediate layer workflow
Body.
Above-mentioned three kinds of working fluids are respectively charged into the syringe of internal layer, intermediate layer and outer operative fluid, according to reality
Apply example 1 and connect each layer fluid in the coaxial spinneret of three-level, connect high-pressure spinning head and HV generator.According to following work
Skill conditional parameter implements three-level coaxial high pressure electrostatic spinning process：Internal layer/centre/outer layer fluid flow is 0.5/1.0/2.0
ML/h, receiver board is 20 cm, the kV of voltage 20 with a distance from spinning nozzle.Environment temperature be (24 ± 2) DEG C, ambient humidity be 55 ±
5%.Fiber wraps up cardboard and is collected by the aluminium foil being grounded.In the above operating condition, Ketoprofen can effectively be prevented in electricity
Spinning process is separated out and blocks spinneret, is prepared fiber surface and is wrapped up one layer of core sheath structure nanofiber of small-molecule drug.
Claims (3)
1. a kind of core fluid carries two kinds of three-level coaxial electrically spun methods that can not spin outer sheath fluid, it is characterised in that specifically include
Following steps：
1）Build preparation facilities：In the coaxial spinneret of three-level by three capillaries of different sizes constitute it is interior, in, outer three layers it is same
Correspondence is installed with internal layer and middle layer fluid injection on axial outlet, internal layer fluid syringe pump and middle layer fluid syringe pump
Device, internal layer and intermediate layer fluid injector are by the internal layer in high resiliency silica gel hose and the coaxial spinneret of three-level and intermediate layer
Capillary inlet is connected, on outer layer fluid syringe pump fixedly mount outer layer fluid injector directly with the coaxial spinneret of three-level
In outer capillary tube entrance be connected, high pressure generator and the connection of three-level coaxial spinneret, under the coaxial spinneret exit orifices of three-level
The fiber for holding the hardboard of useful aluminium foil parcel to make receives flat board；
2）Inner operative fluid is made into using spinnable polymer solution, is the Core support fluid of three-level coaxial electrically spun, injected
Internal layer fluid injector；
3）Intermediate layer working fluid is made into using not spinnable function ingredients solution, intermediate layer fluid injector is injected；
4）Outer operative fluid is made into using pure organic solvent, outer layer fluid injector is injected；
5）High pressure generator is opened, three kinds of flow velocitys of fluid in the coaxial spinneret of three-level are controlled respectively by three syringe pumps,
In the presence of high-pressure electrostatic, the coaxial spinneret exit orifices of three-level produce the nanofiber with core sheath structure feature, are connect by fiber
It is closed flat plate reception.
2. core fluid carries two kinds of three-level coaxial electrically spun methods that can not spin outer sheath fluid, its feature according to claim 1
It is, 2 the step of the feature nanofiber with core sheath structure）、3）With 4）Three layers of allotment of working fluid：By 15 grams of acetic acid
Cellulose is put into 120 grams of mixed solvents, is made into the Core support fluid with favorable spinning quality, mixed solvent by 20 grams of N,
Dinethylformamide, 20 grams of ethanol and 80 grams of acetone are mixed；Outer operative fluid by 20 grams of DMFs,
20 grams of ethanol and 80 grams of acetone are mixed；10 grams of gliadins are dissolved in the mixed solvent of 100 grams of acetic acid and ethanol, volume ratio
Acetic acid：Ethanol is 1:3, constitute middle level working fluid；
Step 5 after the allotment）Control is required：Internal layer, intermediate layer, outer layer fluid flow are respectively 0.5,0.5,2.0 mL/h,
It is 20 cm, the kV of high pressure generator voltage 18 with a distance from spinning nozzle that fiber receives flat board；Environment temperature is 24 ± 2 DEG C, environment
Humidity is 55 ± 5%.
3. core fluid carries two kinds of three-level coaxial electrically spun methods that can not spin outer sheath fluid, its feature according to claim 1
Be, it is described with core sheath structure feature nanofiber for medicine directly wraps up polymer fiber when the step of 2）、3）With 4）Three
The allotment of layer working fluid：15 grams of cellulose acetates are put into 120 grams of mixed solvents, are made into in favorable spinning quality
Core supports fluid, mixed solvent to be mixed by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone；Outer operative
Fluid is mixed by 20 grams of DMFs, 20 grams of ethanol and 80 grams of acetone；10 grams of medicine Ketoprofens are dissolved in
The mixed solvent being made up of 80 grams of acetone and 20 grams of ethanol is middle level working fluid；
Step 5 after the allotment）Control is required：Internal layer, intermediate layer, outer layer fluid flow are respectively 0.5,1.0,2.0 mL/h,
It is 20 cm with a distance from spinning nozzle that fiber receives flat board, and the kV of high pressure generator voltage 20, environment temperature is 24 ± 2 DEG C, environment
Humidity is 55 ± 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611021148.9A CN106676653B (en) | 2016-11-21 | 2016-11-21 | Core fluid carries two kinds of three-level coaxial electrically spun methods that can not spin outer sheath fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611021148.9A CN106676653B (en) | 2016-11-21 | 2016-11-21 | Core fluid carries two kinds of three-level coaxial electrically spun methods that can not spin outer sheath fluid |
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| CN106676653A true CN106676653A (en) | 2017-05-17 |
| CN106676653B CN106676653B (en) | 2019-05-24 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757502A (en) * | 2017-01-06 | 2017-05-31 | 上海理工大学 | A kind of electro spinning nano fiber for radially isolating distribution characteristics with medicine and preparation method thereof |
| CN109295511A (en) * | 2018-09-26 | 2019-02-01 | 上海理工大学 | Detachable Coaxial nozzle, the preparation method of electric spinning equipment and core sheath nanofiber |
| CN110004506A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院长春应用化学研究所 | A kind of micro-fluidic device for spinning and method |
| CN113897691A (en) * | 2021-11-16 | 2022-01-07 | 上海理工大学 | Preparation method of bead nanofiber with composite structure |
| CN114351284A (en) * | 2022-01-18 | 2022-04-15 | 上海理工大学 | Method for preparing porous nano polymer fiber through improved coaxial electrospinning process |
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| CN109295511A (en) * | 2018-09-26 | 2019-02-01 | 上海理工大学 | Detachable Coaxial nozzle, the preparation method of electric spinning equipment and core sheath nanofiber |
| CN110004506A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院长春应用化学研究所 | A kind of micro-fluidic device for spinning and method |
| CN113897691A (en) * | 2021-11-16 | 2022-01-07 | 上海理工大学 | Preparation method of bead nanofiber with composite structure |
| CN114351284A (en) * | 2022-01-18 | 2022-04-15 | 上海理工大学 | Method for preparing porous nano polymer fiber through improved coaxial electrospinning process |
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