CN109023560A - The device and method of hollow nanometer yarn is directly prepared based on electrostatic spinning technique one-step method - Google Patents
The device and method of hollow nanometer yarn is directly prepared based on electrostatic spinning technique one-step method Download PDFInfo
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- CN109023560A CN109023560A CN201811235323.3A CN201811235323A CN109023560A CN 109023560 A CN109023560 A CN 109023560A CN 201811235323 A CN201811235323 A CN 201811235323A CN 109023560 A CN109023560 A CN 109023560A
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- steel wire
- spinning
- funnel
- wire axle
- electric field
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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
-
- 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
- D01F1/08—Addition of substances to the spinning solution or to the melt for forming hollow filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01H—SPINNING OR TWISTING
- D01H1/00—Spinning or twisting machines in which the product is wound-up continuously
- D01H1/08—Spinning or twisting machines in which the product is wound-up continuously cup, pot or disc type, in which annular masses of yarn are formed by centrifugal action
Abstract
The present invention relates to a kind of device and method that hollow nanometer yarn is directly prepared based on electrostatic spinning technique one-step method, devices are as follows: steel wire axle is placed on spinning liquid bath, and drive rotation is connected to motor in axis;Funnel is placed in the side of spinning liquid bath 1, is located at steel wire axle and rotates ray path;Funnel lower end is equipped with collection cylinder and sink, and sink is equipped with water pump, and the outlet of water pump is connected to funnel.Under high voltage electric field effect, each drop can form taylor cone, and then form jet stream, and be finally solidified into silk in receiving end.Needle-less electrostatic spinning does not use any syringe needle, the problem of when electric field strength is more than critical value, a large amount of jet streams are directly formed from open free surface, avoid syringe needle blocking, spinning efficiency and fiber production are greatly improved, provides feasible approach for electrostatic spinning industrialization.
Description
Technical field
The invention belongs to electrostatic spinning techniques and Material Field, are related to one kind and are directly made based on electrostatic spinning technique one-step method
The device and method of standby nanometer yarn hollow out, is related to a kind of needle-less electrostatic spinning system, and in particular to one-step method is directly measured
Produce the device and method of hollowfil yarns.
Background technique
Method of electrostatic spinning is a kind of special fiber fabrication process, and polymer solution carries out jet spinning in strong electrical field.
Under electric field action, the drop at syringe needle can be become conical (i.e. " taylor cone ") from spherical shape, and be extended from conical tip at thin
Silk, after filament runs a distance in air, is finally solidified into fiber in cathode.This mode can produce nanometer to micro-
The polymer filaments of meter level diameter.Electrostatic spinning is simple with its manufacturing device, cost of spinning is cheap, it is various to spin substance classes,
The advantages that technique is controllable becomes and prepares one of main path of nano-fiber material.It is hollow that hollow Nano fiber in use is that one kind possesses
The function nano material of single-pass configuration, size are distributed between 10nm-10 μm, are indispensable in nanoscale science and technology
Material has huge potential value in thermal insulation material, sewage treatment, filtration membrane research.
Traditional method of electrostatic spinning can obtain non-woven fibrofelt, and fiber architecture is unordered, not can be carried out weaving, thus can only
It applies in comparatively narrow some fields, such as filtering material, tissue scaffold, membrane material and wound dressing etc..By pair
Electric field is constrained, or improves reception device (such as roller reception), it is also possible to obtain the fiber of certain orientation.However, by
It is too low in single fiber intensity, process operation can not be carried out, it is difficult to batch machining production, only with the continuity of some strength
Nanofiber tow uniaxially is produced, and nanofiber can really obtain practical application.Above method efficiency
Lower (consumption spinning solution is 1-3mL/h), it is difficult to obtain volume production fiber;Meanwhile it can only be by secondary for orientation fiber
Twister is just able to achieve the preparation of yarn, greatly limits the application of electrospun fibers.Therefore, it is necessary to the prior art
It is transformed, invents a kind of device based on electrostatic spinning technique one-step method volume production hollowfil yarns.
A kind of electro-spun nanofiber yarn system disclosed in document 1 " application No. is 200810018267.8 Chinese patents "
The preparation method of system and nano-fibre yams, which, which carries out twisting to nanofiber using twist roller, becomes yarn, yarn
With certain intensity, but the system carries out Electrospun using a spinning head, and spinning efficiency is low, and fiber generates in the unit time
Low output, it is to be improved in terms of spinning efficiency.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of electrostatic spinning technique one-step method that is based on directly is made
The device and method of standby nanometer yarn hollow out, resulting hollow Nano fiber in use yarn have good mechanical property, certain
Orientation and excellent cycling processability can be directly used for thermal insulation material, the fields such as sewage treatment and filtration membrane.
Technical solution
A kind of device for directly preparing hollow nanometer yarn based on electrostatic spinning technique one-step method, it is characterised in that including
Spinning liquid bath 1, steel wire axle 2, funnel 4, collection cylinder 6, sink 7 and water pump 8;Steel wire axle 2 is placed on spinning liquid bath 1, axis and electricity
Machine connection drives rotation;Funnel 4 is placed in the side of spinning liquid bath 1, is located at steel wire axle 2 and rotates ray path;4 lower end of funnel is equipped with
Collection cylinder 6 and sink 7, sink 7 are equipped with water pump 8, and the outlet of water pump 8 is connected to funnel 4;The steel wire axle 2 includes cylinder
Shape metal shaft, two rosettes and Duo Gen stainless steel steel wire, two rosettes are fixed on cylindrical metal axis both ends, and more
Stainless steel fixation with steel wire is between two rosettes.
The more stainless steel steel wires are 18.
A method of hollow nanometer yarn being prepared using described device, it is characterised in that steps are as follows:
Step 1: polymer solution is placed in solution tank;
Step 2: applying a high voltage electric field between the steel wire axle 2 and funnel 4 of spinning liquid bath 1;
Step 3: steel wire axle 2 rotates in solution tank under motor drive, when the lower part steel of submergence in a polymer solution
When silk rotates out of liquid level, the polymer drop on steel wire is adhered under high voltage electric field effect, each drop can form Taylor
Cone, and then form jet stream and enter funnel 4, hollow nanometer yarn is obtained on collection cylinder 6.
The electric field force that the high voltage electric field is formed is just greater than Surface Tension of Liquid Drops.
Beneficial effect
It is proposed by the present invention it is a kind of based on electrostatic spinning technique one-step method directly prepare hollow nanometer yarn device and
Method, under high voltage electric field effect, each drop can form taylor cone, and then form jet stream, and finally solidify in receiving end
At silk, which can consume the spinning solution higher than 200mL per hour.Needle-less electrostatic spinning does not use any syringe needle, when
The problem of when electric field strength is more than critical value, a large amount of jet streams are directly formed from open free surface, avoid syringe needle blocking, pole
The earth improves spinning efficiency and fiber production, provides feasible approach for electrostatic spinning industrialization.Existed using different solutes
The difference of solubility in solvent, and difference in solubility is very big, forms radial solubility gradients, this fast original of sandwich layer solute volatilization
Reason, and then fiber can form hollow structure.The present invention has prepared a variety of solutes and solvent is prepared into emulsion and carries out uniaxial electrostatic
Spinning obtains doughnut.Using water pump, dynamic water circulation prepares fiber yarn system, cone vortex twisted fibers resultant yarn
Line, the water flow of the circulatory system form stable vortex in funnel, become yarn using the centripetal force twisting doughnut of vortex,
It realizes one-step method and prepares hollowfil yarns.
Detailed description of the invention
Fig. 1: the schematic diagram of apparatus of the present invention
1- spinning liquid bath, 2- steel wire axle, 3- doughnut, 4- funnel, 5- hollow yarns, 6- collection cylinder, 7- sink, 8-
Water pump.
Specific embodiment
Now in conjunction with embodiment, attached drawing, the invention will be further described:
The technical solution adopted by the present invention to solve the technical problems: one-step method directly prepares hollow Nano fiber in use yarn
Mass production device, it includes:
Cylindrical metal axis both ends are fixed on two rosettes, and are driven by a motor and are rotated with disk, along circle
Disk circumferencial direction fixes 18 stainless steel steel wires, constituent part unit steel wire axle, which is fixed on solution tank, when
When steel wire axle is driven by a motor slow rotation, lower part steel wire can be submerged by the polymer solution in solution tank, rotate out of liquid level
Afterwards, since solution surface tension acts on, many polymer drops can be adhered on steel wire, each drop is equivalent to a spinning needle
Head, which improves jet stream quantity.Under high voltage electric field effect, each drop can form taylor cone, and then form jet stream,
And it finally is solidified into silk in receiving end, which can consume the spinning solution higher than 200mL per hour.Needle-less electrostatic spinning
Without using any syringe needle, when electric field strength is more than critical value, a large amount of jet streams are directly formed from open free surface, are avoided
The problem of syringe needle blocks, greatly improves spinning efficiency and fiber production, provides feasible way for electrostatic spinning industrialization
Diameter.
Specific method embodiment:
Embodiment 1:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 5wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 10wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 80%.
Embodiment 2:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 5wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 15wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high voltage electric field, and loads high-pressure electrostatic 5KV, steel by overall solution volume 200mL
Silk axis is rotated with the speed of 30r/min, and steel wire axle constantly emits nanofibers, acts on through water flow vortex twisting in funnel, is leaked
Collect hollowfil yarns in bucket lower section.
After tested, hollowfil yarns are prepared into good orientation, and yield is high, core material PVA removal
Rate mean value is 85%.
Embodiment 3:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 5wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 20wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 90%.
Embodiment 4:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 6wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 10wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 90%.
Embodiment 5:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 6wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 15wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 100%.
Embodiment 6:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 6wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 20wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 90%.
Embodiment 7:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 7wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 10wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 80%.
Embodiment 8:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 7wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 15wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 85%.
Embodiment 9:
It chooses polyvinyl alcohol (PVA, MW=72000) and is dissolved in distilled water 7wt% and the (Nylon 6, Mw=of nylon 6
35000) formic acid 20wt% is dissolved in as spinning solution, is respectively placed on magnetic stirring apparatus and is stirred at room temperature 4 hours and 5 small
When, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic by overall solution volume 200mL
5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through in funnel
Water flow vortex twisting effect, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVA removal
Rate mean value is 90%.
Embodiment 10:
It chooses polyvinylpyrrolidone (PVP, MW=1300000) and positive silane ethyl ester (TEOS, MW=208.33) is poly-
Close object, TEOS and ethyl alcohol mix and insoluble with PVP, and PVP and TEOS are dissolved in ethanol solution, electric in TEOS/PVP mixed solution
Ethyl alcohol volatilizees rapidly during spinning, while being formed radially raised concentration gradient from inside to outside in fiber.TEOS is in ethanol
Solubility is higher, distribution gradient, and gathers in centre, and with the continuous volatilization of ethyl alcohol, phase occurs in uncured fiber
Separation obtains the fiber of hollow structure after TEOS volatilization completely.Configuration solution is placed on magnetic stirring apparatus at room temperature
Spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load height by stirring 4 hours, overall solution volume 200mL
Electrostatic 5KV is pressed, steel wire axle is rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, is passed through
The twisting of water flow vortex acts in funnel, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material TEOS removal
Rate mean value is 100%.
Embodiment 11:
4.04g ferric nitrate (Fe (NO is weighed respectively3)3·9H2O, MW=404) and 1.21g copper nitrate (Cu (NO3)2·
3H2O, MW=242) it is added in 2.5ml ethyl alcohol and 7.5ml water, then by 6.5g polyvinylpyrrolidone (PVP, MW=
1300000) it is added to the solution for being formed in said mixture and there is certain viscosity.Configuration solution is placed on magnetic stirring apparatus
It stirs 4 hours, overall solution volume 200mL at room temperature, spinning solution is placed in spinning liquid bath, open high-voltage generator, and
High-pressure electrostatic 5KV is loaded, steel wire axle is rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launches nanometer
Fiber acts on through water flow vortex twisting in funnel, can form fibre bundle, and the rotating cylinder being placed in below funnel collects silvalin
Line.
After tested, it is prepared into CuFe2O4Hollowfil yarns have good orientation, and yield is higher, core material
PVP removal rate mean value is 95%.
Embodiment 12:
Choose polyvinylpyrrolidone (PVP, MW=1300000) and polyvinyl acetate (PVAc, MW=200000)
Polymer is dissolved in respectively in ethyl acetate and n-butyl alcohol solvent, and configuration solution is placed on magnetic stirring apparatus and is stirred at room temperature
It mixes 4 hours, overall solution volume 200mL, spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high pressure
Electrostatic 5KV, steel wire axle are rotated with the speed of 30r/min, and the drop on steel wire axle constantly forms and launch nanofiber, through leaking
The twisting of water flow vortex acts in bucket, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material PVAc removal
Rate mean value is 98%.
Embodiment 13:
Choosing polymer polyethylene base pyrrolidones (PVP, MW=1300000) and being dissolved in purity is 99% methylene chloride
(DCM, MW=84.93) prepares the solution of wt=4%, and the TiO of mass ratio 10:1 is added into solution system2It is configured to final
Electrospun solution, solution will be prepared and be placed on magnetic stirring apparatus and be stirred at room temperature 4 hours, overall solution volume 200mL, will
Spinning solution is placed in spinning liquid bath, opens high-voltage generator, and load high-pressure electrostatic 5KV, steel wire axle is with the speed of 30r/min
Rotation, and the CO of purity 99% is constantly passed through above spinning night slot2Gas, the drop on steel wire axle constantly form and launch
Nanofiber acts on through water flow vortex twisting in funnel, can form fibre bundle, and the rotating cylinder being placed in below funnel collects fiber
Yarn.
After tested, hollowfil yarns are prepared into good orientation, and yield is higher, core material DCM removal
Rate mean value is 95%.
Claims (4)
1. a kind of device for directly preparing hollow nanometer yarn based on electrostatic spinning technique one-step method, it is characterised in that including spinning
Silk liquid bath (1), steel wire axle (2), funnel (4), collection cylinder (6), sink (7) and water pump (8);Steel wire axle (2) is placed in spinning solution
On slot (1), drive rotation is connected to motor in axis;Funnel (4) is placed in the side of spinning liquid bath (1), is located at steel wire axle (2) rotary irradiating
Thread path;Funnel (4) lower end is equipped with collection cylinder (6) and sink (7), and sink (7) is equipped with water pump (8), the outlet of water pump (8)
It is connected to funnel (4);The steel wire axle (2) includes cylindrical metal axis, two rosettes and Duo Gen stainless steel steel wire, and two
Rosette is fixed on cylindrical metal axis both ends, and more stainless steel fixations with steel wire are between two rosettes.
2. the device of hollow nanometer yarn is directly prepared based on electrostatic spinning technique one-step method according to claim 1,
Be characterized in that: the more stainless steel steel wires are 18.
3. a kind of method for preparing hollow nanometer yarn using claim 1 described device, it is characterised in that steps are as follows:
Step 1: polymer solution is placed in solution tank;
Step 2: applying a high voltage electric field between the steel wire axle (2) and funnel (4) of spinning liquid bath (1);
Step 3: steel wire axle (2) rotates in solution tank under motor drive, when the lower part steel wire of submergence in a polymer solution
When rotating out of liquid level, the polymer drop on steel wire is adhered under high voltage electric field effect, each drop can form taylor cone,
And then form jet stream and enter funnel (4), hollow nanometer yarn is obtained on collection cylinder (6).
4. according to the method described in claim 3, it is characterized by: the electric field force that the high voltage electric field is formed is just greater than drop
Surface tension.
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CN110886024A (en) * | 2019-11-06 | 2020-03-17 | 南京工业职业技术学院 | Electrostatic spinning device for preparing composite fibers |
CN113061997A (en) * | 2021-03-25 | 2021-07-02 | 大连工业大学 | Preparation method of guar gum nano-fiber |
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CN113061997A (en) * | 2021-03-25 | 2021-07-02 | 大连工业大学 | Preparation method of guar gum nano-fiber |
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