CN110344127A - A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre - Google Patents
A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre Download PDFInfo
- Publication number
- CN110344127A CN110344127A CN201910546552.5A CN201910546552A CN110344127A CN 110344127 A CN110344127 A CN 110344127A CN 201910546552 A CN201910546552 A CN 201910546552A CN 110344127 A CN110344127 A CN 110344127A
- Authority
- CN
- China
- Prior art keywords
- centrifugal spinning
- polyethylene glycol
- kynoar
- glycol oxide
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
-
- 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
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- 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
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention belongs to porous micro nano rice technical field of fiber preparation, in particular to a kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide (PVDF/PEO) micro/nano-fibre.This method comprises the following steps: (1) preparation of centrifugal spinning solution: Kynoar (PVDF) being mixed with polyethylene glycol oxide (PEO) the two and is dissolved in N-N dimethylformamide (DMF), acetone and water, finely dispersed centrifugal spinning solution is obtained after stirring, wherein the mass concentration of PVDF and PEO is respectively 10-12wt% and 0.2-1wt%；(2) centrifugal spinning: centrifugal spinning is carried out using centrifugal spinning solution made from step (1), obtains Kynoar/polyethylene glycol oxide (PVDF/PEO) micro/nano-fibre with porous structure.Kynoar/polyethylene glycol oxide micro/nano-fibre film appearance structure can be controlled by the content of adjusting polyethylene glycol oxide.
Description
Technical field
The invention belongs to porous micro nano rice technical field of fiber preparation, in particular to a kind of Kynoar/polyoxyethylene
The centrifugal spinning preparation method of alkene (PVDF/PEO) micro/nano-fibre.
Background technique
The method using electrostatic spinning is concentrated mainly on to the preparation of micro/nano-fibre at present, electrostatic spinning there is with
Under several inherent shortcomings limit this method business large-scale use: (1) need to apply high voltage electric field in preparation process；(2) raw
Produce low efficiency；(3) pollution that solution needs a certain proportion of solvent to generate solution with certain conductivity.Therefore at
Sheet, scale, from practical and application demand, there are also with a distance from very big in terms of controllability Study.
Centrifugal spinning overcomes the limitation that the preparation method of electrostatic spinning micro/nano-fibre is encountered, and can be with height
Speed and low cost generate micro/nano-fibre.The design is not required to apply high voltage electric field, can prepare the polymerization not constrained by conductivity
Object micro/nano-fibre, and its production efficiency greatly improves.Centrifugal spinning device structure is simple, mainly by motor, spinneret,
Stick etc. is collected to constitute.For spinneret on motor shaft, the inside is equipped with polymer solution, has spinneret orifice on spinneret.When work, electricity
Machine energization rotary spinning head makes spinneret high speed rotation, and polymer solution is at spinneret orifice since centrifugal force effect is injected in receipts
It moves to collect between collection stick and spinneret orifice and forms orderly micro/nano-fibre on stick.Polymer solution is formed at spinneret orifice
The main experienced three stages of micro/nano-fibre: 1. polymer solution need to have certain viscosity, and when rotation reaches to be formed at spinneret orifice
Taylor cone；2. polymer solution is acted on by surface tension and centrifugal force simultaneously, when centrifugal force is greater than surface tension, polymer
Stretching forms tiny micro/nano level fiber；3. fiber rotates between spinneret orifice and collection stick under the influence of centrifugal force,
Solvent volatilization during this in polymer solution obtains fiber and rotates on collection stick.
Summary of the invention
The present invention provides a kind of Kynoar/polyethylene glycol oxide (PVDF/PEO) micro/nano-fibre of porous structure
Centrifugal spinning preparation method.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre, this method include
Following steps:
(1) preparation of centrifugal spinning solution: Kynoar (PVDF) is mixed with polyethylene glycol oxide (PEO) the two and is dissolved in
In N-N dimethylformamide (DMF), acetone and water, finely dispersed centrifugal spinning solution is obtained after stirring, wherein PVDF with
The mass concentration of PEO is respectively 10-12wt% and 0.2-1wt%；
(2) centrifugal spinning: centrifugal spinning is carried out using centrifugal spinning solution made from step (1), obtains that there is porous knot
Kynoar/polyethylene glycol oxide (PVDF/PEO) micro/nano-fibre of structure.
Preparation method of the present invention is simple, can rapidly and efficiently prepare Kynoar/polyethylene glycol oxide micro/nano-fibre.
Micro/nano-fibre material is high due to having many advantages, such as small fibre diameter, large specific surface area, porosity, and is widely used in a group weaver
The fields such as engineering support, drug delivery, filter medium, artificial blood vessel, biochip, micro-/ nano sensor, optics, composite material.
Micro/nano-fibre film obtains the concern of numerous researchers because of the significant micro-/ nano scale effect of micro/nano-fibre.It is passed through in low-carbon
Under Ji, environmental protection, social safety and human health time equivalence require, fiber/fabric is higher towards technology content, by resource shadow
The research and development and industrialization direction for ringing the new and high technologies fibrous materials such as smaller differential, high-performance, functionality develop.
The method using electrostatic spinning is concentrated mainly on to the preparation of micro/nano-fibre film at present, cost, scale, can
Control in terms of Journal of Sex Research that there are also with a distance from very big from practical and application demand.Therefore, controllable, the rule to realize micro/nano-fibre film
Modelling preparation, needs to explore suitable new technology and method, reduces cost, expands scale, improves preparation controllability.And based on tool
There is the centrifugal spinning technology of industrial applications prospect, is a kind of water-saving, energy saving, green non-pollution technique, it can be with polymer, pottery
Porcelain, composite material are that raw material prepares micro/nano-fibre.The yield of data with existing display centrifugation spinning technique micro/nano-fibre is at least
Two orders of magnitude can be promoted than electrostatic spinning.Centrifugal spinning is that a new road has been opened up in the preparation of micro/nano-fibre, is had
Preferable development prospect.
Preferably, the mass ratio of DMF, the summation of acetone and water are 48-52 in the dicyandiamide solution of DMF, acetone and water:
3。
Preferably, the mass concentration of PEO is 0.4-0.8wt% in centrifugal spinning solution.
Preferably, Kynoar (PVDF) molal weight MW=600000g/mol, chain structure formula are as follows:Polyethylene glycol oxide (PEO) molal weight MW=2000000g/mol, chain structure formula are as follows:
Preferably, step (1) the centrifugal spinning solution the preparation method is as follows: by 1g Kynoar (PVDF) with
0.06g polyethylene glycol oxide (PEO) is placed in 20ml sample bottle, and 5.9g acetone, 2.53g DMF and 0.51g are pipetted into sample bottle
Water seals sample bottle preservative film, raw material band and sealed membrane, is heated to 40-50 DEG C of stirring 12 hours or more, obtains centrifugation and spin
Silk solution.
Preferably, the centrifugal spinning device that centrifugal spinning uses includes motor, spinneret and collects stick, spinneret is installed
At the top of the shaft of motor and it is driven by a motor rotation, there is the cavity for accommodating spinning solution in spinneret, be equipped at the top of spinneret
Liquid injection port, spinneret side wall are equipped with the spinneret orifice being connected to the cavity, collect stick around the circle setting of spinneret one.Centrifugal spinning
When, spinneret is driven by a motor rotation, and spinning solution is sprayed from the spinneret orifice of spinneret, moves between spinneret orifice and collection stick
It is stretched, while solvent volatilizees, forms fiber, receive to obtain tunica fibrosa by collecting stick.Motor speed is generally 5000-
15000rpm/min.Preferably, spinneret and collecting distance controlling between stick and in 10cm ± 2cm, the diameter of spinneret orifice being
0.4mm-0.6mm.Preferably, collecting stick using spinneret is that axis is centrosymmetric distribution, it is a for 6-12 to collect the number of stick.Make
To be preferred, spinneret is made of spinning shell and circular seal ring, and spinning shell is the cylinder-like structure of bottom opening, outside spinning
The bottom end of shell extends outward to form annular edge, and step is arranged in the middle part on annular edge, and the circular seal ring makes with step cooperation
The opening of spinning shell seals, and the bottom of circular seal ring is concordant with the annular bottom plane on edge.Preferably, spinneret by
Polytetrafluoroethylene (PTFE) is made.Preferably, spinneret and the difference in height for collecting stick top are 1-2cm.Preferably, spinneret orifice is located at
Position of the spinneret bottom surface at top surface 2/3, and it is symmetrical arranged 6-8 in the same plane.Preferably, in annular along upper
Horizontally disposed a pair of blade.Formed when spinning upward air-flow make spun fiber collect collecting stick top half and
Do not deposit to bottom.
Preferably, spinning revolving speed is adjusted to 12000rpm/min, spinneret orifice of the spinning solution from spinneret when centrifugal spinning
Middle ejection forms fiber, receives to obtain fiber by collecting stick.
A kind of porous Kynoar/polyethylene glycol oxide micro/nano-fibre, the Kynoar/polyethylene glycol oxide is micro-/are received
Rice fiber is made using method above-mentioned.
Polystyrene micro/nano-fibre film of the invention, firstly, by Kynoar (PVDF) and polyethylene glycol oxide
(PEO) it is dissolved in N-N dimethylformamide (DMF), acetone and water, finely dispersed centrifugal spinning solution is obtained after stirring, so
Centrifugal spinning solution progress centrifugal spinning is obtained afterwards.The centrifugal spinning preparation method of the micro/nano-fibre film can be used for porous
The preparation of micro/nano-fibre, has a characteristic that
1, preparation method of the present invention is easy, and reaction condition is easy to accomplish and controls；
2, Kynoar/polyethylene glycol oxide micro/nano-fibre film can be controlled by the content of adjusting polyethylene glycol oxide
Appearance structure；
3, can be by adjusting spinning parameter such as: motor speed, orifice diameter collect stick distance to regulate and control micro-/ nano
The fibre diameter of tunica fibrosa；
4, to prepare micro/nano-fibre membrane efficiency using the method for centrifugal spinning higher, has and preferably expands space.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of centrifugal spinning device of the present invention；
Fig. 2 is the structural schematic diagram of spinneret in Fig. 1；
Label declaration: 1 motor；2 spinnerets；3 collect stick；4 blades；5 fibers；6 liquid injection ports；7 spinneret orifices；8 spinning shells；
9 circular seal rings；10 annular edges；11 steps；
Fig. 3 is the SEM image (left × 500 times, right × 5000 times) of Kynoar micro/nano-fibre；
Fig. 4 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PEO content is 0.2wt% (is implemented
Example 1 is made) (left × 500 times, right × 5000 times)；
Fig. 5 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PEO content is 0.4wt% (is implemented
Example 2 is made) (left × 500 times, right × 5000 times)；
Fig. 6 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PEO content is 0.6wt% (is implemented
Example 3 is made) (left × 500 times, right × 5000 times)；
Fig. 7 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PEO content is 0.8wt% (is implemented
Example 4 is made) (left × 500 times, right × 5000 times)；
Fig. 8 is Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image (embodiment that PEO content is 1wt%
5 are made) (left × 500 times, right × 5000 times)；
Fig. 9 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PVDF content is 10wt% (is implemented
Example 6 is made) (left × 500 times, right × 5000 times)；
Figure 10 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PVDF content is 11wt% is (real
Example 7 is applied to be made) (left × 500 times, right × 5000 times)；
Figure 11 is that Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image that PVDF content is 12wt% is (real
Example 8 is applied to be made) (left × 500 times, right × 5000 times)；
Figure 12 is DMF: acetone: water=35:15:1 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 9 is made) (left × 500 times, right × 5000 times)；
Figure 13 is DMF: acetone: water=35:15:2 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 10 is made) (left × 500 times, right × 5000 times)；
Figure 14 is DMF: acetone: water=35:15:3 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 11 is made) (left × 500 times, right × 5000 times)；
Figure 15 is DMF: acetone: water=35:15:4 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 12 is made) (left × 500 times, right × 5000 times)；
Figure 16 is DMF: acetone: water=30:20:3 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 13 is made) (left × 500 times, right × 5000 times)；
Figure 17 is DMF: acetone: water=35:15:3 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 14 is made) (left × 500 times, right × 5000 times)；
Figure 18 is DMF: acetone: water=40:10:3 Kynoar/polyethylene glycol oxide micro/nano-fibre SEM image
(embodiment 15 is made) (left × 500 times, right × 5000 times).
Specific embodiment
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.It should be appreciated that this hair
Bright implementation is not limited by the following examples, and the accommodation in any form made to the present invention and/or changed will all be fallen
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
The centrifugal spinning device that following embodiment centrifugal spinning uses is as depicted in figs. 1 and 2, including motor 1, spinneret
2 are mounted at the top of the shaft of motor and are driven by a motor rotation with collection stick 3, spinneret, have receiving spinning solution in spinneret
Cavity, liquid injection port 6 is equipped at the top of spinneret, spinneret side wall is equipped with the spinneret orifice 7 be connected to the cavity, and collection stick surrounds
The circle setting of spinneret one.
Distance controlling is 0.4mm in 10cm ± 2cm, diameter the present embodiment of spinneret orifice between spinneret and collection stick,
0.5 or 0.6mm is adjustable in actual production.To guarantee preferably to collect tunica fibrosa, spinneret and the height for collecting stick top
Difference is 1-2cm.It is that axis is centrosymmetric distribution that stick, which is collected, using spinneret, and the number for collecting stick is 8.
Spinneret is made of polytetrafluoroethylene (PTFE).Spinneret is made of spinning shell 8 and circular seal ring 9, and spinning shell is
The cylinder-like structure of bottom opening, the bottom end of spinning shell extend outward to form annular along 10, and step is arranged in the middle part on annular edge
11, the circular seal ring and step cooperation seal the opening of spinning shell, and the bottom of circular seal ring and annular edge
Bottom plane it is concordant.Spinneret orifice is located at position of the spinneret bottom surface at top surface general 2/3, and symmetrical in the same plane
Setting 8.
A pair of of blade 4 is also set up in the horizontal direction along upper in annular.Upward air-flow is formed when spinning makes spun fiber
It collects and is collecting stick top half without depositing to bottom.
When centrifugal spinning, spinneret is driven by a motor rotation, and spinning solution is sprayed from the spinneret orifice of spinneret, in spinneret orifice
It is stretched with collecting to move between stick, while solvent volatilizees, forms fiber, receive to obtain tunica fibrosa by collecting stick.Motor
Revolving speed is generally 5000-15000rpm/min.
Compared with electrostatic spinning, centrifugal spinning equipment is simple, at low cost, can spinning solution more higher than Static Spinning silk spinning it is dense
Degree, using this centrifugal spinning device, when use, is safer, high-efficient；The yield of one-jet electrostatic spinning apparatus is 1-
100mg/ hours, two orders of magnitude at least can be improved in the productivity ratio electrostatic spinning of centrifugal spinning.
Embodiment 1
A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are same
Embodiment 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (wherein molal weight of PVDF with assay balance
MW=600000g/mol) and 0.02g polyethylene glycol oxide (PEO) (the wherein molal weight M of PEOW=2000000g/mol) it is placed in
In 20ml sample bottle, 2.54g N-N dimethylformamide (DMF), 5.93g acetone and 0.51g water, sample bottle raw material band is added dropwise
Sealing is heated to 50 DEG C, stirs 12 hours, it is molten that the finely dispersed centrifugal spinning of Kynoar/polyethylene glycol oxide is finally made
Liquid.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 2
A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are same
Embodiment 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (wherein molal weight of PVDF with assay balance
MW=600000g/mol) and 0.04g polyethylene glycol oxide (PEO) (the wherein molal weight M of PEOW=2000000g/mol) it is placed in
In 20ml sample bottle, 2.53g N-N dimethylformamide (DMF), 5.92g acetone and 0.51g water, sample bottle raw material band is added dropwise
Sealing is heated to 50 DEG C, stirs 12 hours, it is molten that the finely dispersed centrifugal spinning of Kynoar/polyethylene glycol oxide is finally made
Liquid.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 3
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, 2.53g N-N dimethylformamide (DMF), 5.9g acetone and 0.51g water, sample bottle is added dropwise and is sealed with raw material band,
50 DEG C are heated to, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 4
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.08g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 2.52g N-N dimethylformamide (DMF), 5.89g acetone and 0.51g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 5
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.1g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 2.51g N-N dimethylformamide (DMF), 5.88g acetone and 0.51g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Comparative example 1
A kind of centrifugal spinning preparation method of Kynoar micro/nano-fibre, the specific steps are as follows:
(1) 1g Kynoar (PVDF) (the wherein molal weight M of PVDF is accurately weighed with assay balanceW=
It 600000g/mol) is placed in 20ml sample bottle, 2.7g N-N dimethylformamide (DMF), 6.3g acetone is added dropwise, sample bottle is used
Raw material band sealing, is heated to 50 DEG C, stirs 12 hours, finally the obtained finely dispersed centrifugal spinning solution of Kynoar.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1 and Fig. 2, setting revolving speed is 12000rpm/min, is received
Integrate stick distance as 12cm, orifice diameter 0.4mm takes 5ml spinning solution sample in spinneret, opens motor, passes through receipts
The SEM image that collection stick obtains Kynoar micro/nano-fibre obtained is shown in Fig. 3.
Implementation result
Kynoar/polyethylene glycol oxide fiber surface morphology scanning electron microscopic observation
Using the table of the tunica fibrosa of ULTRA55-36-73 type field emission scanning electron microscope observation embodiment 1-5 preparation
Face pattern, the SEM image of fiber are Fig. 4-8 respectively.Comparison SEM figure can be found, compared to polyvinylidene fluoride (Fig. 3), be added
The fiber for entering PEO and water forms porous structure.Under identical spinning parameter, the PEO of different content is selected to carry out spinning, it is right
Schemed than SEM it is found that the fiber of porous surface can be made when PEO content is 0.2wt% (Fig. 4, embodiment 1 are made)；And
As the content of PEO increases, the porous structure of fiber increases；But PEO content is made when being 1wt% (Fig. 8, embodiment 5 are made)
The uneven easy entanglement of fiber and difficulty in spinning.Therefore, when PEO content is that porous Kynoar/polyoxy can be made in 0.6wt%
Change vinyl fiber, distribution of fiber diameters is more uniform and fiber surface is in porous structure.
Embodiment 6
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, 2.53g N-N dimethylformamide (DMF), 5.9g acetone and 0.51g water, sample bottle is added dropwise and is sealed with raw material band,
50 DEG C are heated to, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 7
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1.1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW
=600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (the wherein molal weight M of PEOW=2000000g/mol) it is placed in
In 20ml sample bottle, 2.53g N-N dimethylformamide (DMF), 5.89g acetone and 0.51g water, sample bottle raw material band is added dropwise
Sealing is heated to 50 DEG C, stirs 12 hours, it is molten that the finely dispersed centrifugal spinning of Kynoar/polyethylene glycol oxide is finally made
Liquid.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 8
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1.2g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW
=600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (the wherein molal weight M of PEOW=2000000g/mol) it is placed in
In 20ml sample bottle, 2.52g N-N dimethylformamide (DMF), 5.89g acetone and 0.51g water, sample bottle raw material band is added dropwise
Sealing is heated to 50 DEG C, stirs 12 hours, it is molten that the finely dispersed centrifugal spinning of Kynoar/polyethylene glycol oxide is finally made
Liquid.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Implementation result
Kynoar/polyethylene glycol oxide fiber surface morphology scanning electron microscopic observation
Using the table of the tunica fibrosa of ULTRA55-36-73 type field emission scanning electron microscope observation embodiment 6-8 preparation
Face pattern, the SEM image of fiber are Fig. 9-11 respectively.When PVDF concentration is 9% since system viscosity is too low, surface tension is too
Greatly, not easily stretchable, and whole system viscosity is too low, it is difficult at silk.When PVDF additional amount is greater than 12%, system viscosity is too high,
It can not almost be sprayed from spinneret orifice, therefore can not be at silk.SEM graph discovery is compared, with the increase of PVDF concentration, concentration of dope
Increase, system viscosity also increases, causes solution to show longer stress relaxation time, limit the volatilization of solvent, Cheng Sigeng
It is difficult.Therefore, PVDF concentration is that 10% (Fig. 9, embodiment 6 are made) is relatively mild, and the diameter and thickness of fiber are also more uniform.
Embodiment 9
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 2.63g N-N dimethylformamide (DMF), 6.14g acetone and 0.17g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 10
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 2.58g N-N dimethylformamide (DMF), 6.02g acetone and 0.34g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 11
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, 2.53g N-N dimethylformamide (DMF), 5.9g acetone and 0.51g water, sample bottle is added dropwise and is sealed with raw material band,
50 DEG C are heated to, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 12
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 2.48g N-N dimethylformamide (DMF), 5.79g acetone and 0.67g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Implementation result
Kynoar/polyethylene glycol oxide fiber surface morphology scanning electron microscopic observation
Using the table of the tunica fibrosa of ULTRA55-36-73 type field emission scanning electron microscope observation embodiment 9-12 preparation
Face pattern, the SEM image of fiber are Figure 12-15 respectively.When acetone: DMF: when water is greater than 35:15:4, too due to system viscosity
It is small, spinning solution still micro- also droplet-like after being sprayed in hole, and silk can not be drawn into.Comparison SEM figure can find increasing with dampening,
Solvent rate of volatilization reduces, and the surface tension effects time that jet stream is subject to is more abundant, and level of stretch is bigger.But due to volatilization
Property solvent reduction, cause viscosity to reduce, uniformity coefficient decline, finally make fibre matting degree become larger.Comparing SEM figure can
Know, even in fiber diameter distribution and is easier into silk when proportion is 35:15:3 (Figure 14, embodiment 11 be made).Therefore it chooses molten
Agent acetone: DMF: the proportion of water is 35:15:3.
Embodiment 13
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 3.37g N-N dimethylformamide (DMF), 5.06g acetone and 0.51g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 14
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, 2.53g N-N dimethylformamide (DMF), 5.9g acetone and 0.51g water, sample bottle is added dropwise and is sealed with raw material band,
50 DEG C are heated to, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Embodiment 15
A kind of centrifugal spinning preparation method of Kynoar/polyethylene glycol oxide micro/nano-fibre, specific steps are the same as implementation
Example 1, difference are as follows: (1) accurately weigh 1g Kynoar (PVDF) (the wherein molal weight M of PVDF with assay balanceW=
600000g/mol) and 0.06g polyethylene glycol oxide (PEO) (wherein molal weight M of PEOW=2000000g/mol) it is placed in 20ml
In sample bottle, it is close that 1.69g N-N dimethylformamide (DMF), 6.75g acetone and 0.51g water, sample bottle raw material band is added dropwise
Envelope is heated to 50 DEG C, stirs 12 hours, the finely dispersed centrifugal spinning solution of Kynoar/polyethylene glycol oxide is finally made.
(2) centrifugal spinning is carried out using centrifugal spinning device shown in Fig. 1, setting revolving speed is 12000rpm/min, collects stick
Distance is 12cm, orifice diameter 0.4mm, takes 5ml spinning solution sample in spinneret, opens motor, by collecting stick
Obtain porous Kynoar/polyethylene glycol oxide micro/nano-fibre.
Implementation result
Kynoar/polyethylene glycol oxide fiber surface morphology scanning electron microscopic observation
Using the ULTRA55-36-73 type field emission scanning electron microscope observation embodiment 13-15 tunica fibrosa prepared
Surface topography, the SEM image of fiber are Figure 16-18 respectively.When the amount of solvent acetone is greater than 80% (with solvent total amount for 100%)
When, since system viscosity is too small, spinning solution is still droplet-like after spinneret orifice ejection, and can not be drawn into silk.If reducing third again
The ratio of ketone will make system viscosity is too big also can not be at silk.In all solvent ratios, work as DMF: acetone: water 30:
It, can be preferably at silk when 20:3,35:15:3/40:10:3.Compare subtracting with strong volatile solvent acetone known to SEM figure
Few, jet stream increases in spinning process, and uniformity coefficient decline finally makes fibre matting degree become larger, between fiber and fiber more
It is easy to intertwine with each other.Therefore, solvent burden ratio selects DMF: acetone: water is preferable for 35:15:3.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (9)
1. a kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre, it is characterised in that should
Method includes the following steps:
(1) preparation of centrifugal spinning solution: Kynoar (PVDF) is mixed with polyethylene glycol oxide (PEO) the two and is dissolved in N-N
In dimethylformamide (DMF), acetone and water, finely dispersed centrifugal spinning solution is obtained after stirring, wherein PVDF and PEO
Mass concentration is respectively 10-12wt% and 0.2-1wt%；
(2) centrifugal spinning: centrifugal spinning is carried out using centrifugal spinning solution made from step (1), obtains that there is porous structure
Kynoar/polyethylene glycol oxide (PVDF/PEO) micro/nano-fibre.
2. centrifugal spinning preparation method according to claim 1, it is characterised in that: the dicyandiamide solution of DMF, acetone and water
In, the mass ratio of DMF, the summation of acetone and water are 48-52:3.
3. centrifugal spinning preparation method according to claim 1, it is characterised in that: the quality of PEO in centrifugal spinning solution
Concentration is 0.4-0.8wt%.
4. centrifugal spinning preparation method according to claim 1, it is characterised in that: step (1) the centrifugal spinning solution
Specifically the preparation method is as follows: Kynoar and polyethylene glycol oxide are placed in sample bottle, N-N dimethyl is added into sample bottle
Formamide, acetone and water, the mass ratio of N-N dimethylformamide, acetone and water is 15:35:3, and sample bottle raw material band is close
Envelope is heated to 50-55 DEG C of stirring 24 hours or more, obtains centrifugal spinning solution.
5. centrifugal spinning preparation method according to claim 1, it is characterised in that: polyethylene glycol oxide (PEO) molal weight MW
=2000000g/mol, chain structure formula are as follows:Kynoar (PVDF) molal weight MW=
600000g/mol, chain structure formula are as follows:
6. centrifugal spinning preparation method according to claim 1, it is characterised in that: in centrifugal spinning solution, PVDF content
It is 0.6wt for 10wt%, PEO content.
7. centrifugal spinning preparation method according to claim 1, it is characterised in that: the centrifugal spinning dress that centrifugal spinning uses
It sets including motor, spinneret and collects stick, spinneret is mounted on the shaft top of motor and is driven by a motor rotation, in spinneret
With the cavity for accommodating spinning solution, liquid injection port is equipped at the top of spinneret, spinneret side wall is equipped with the spinneret being connected to the cavity
Stick is collected around the circle setting of spinneret one in hole.
8. centrifugal spinning preparation method according to claim 7, it is characterised in that: when centrifugal spinning, by spinning revolving speed tune
To 12000rpm/min, spinning solution is sprayed from the spinneret orifice of spinneret forms fiber, receives to obtain tunica fibrosa by collecting stick.
9. porous Kynoar/polyethylene glycol oxide micro/nano-fibre made from a kind of method described in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910546552.5A CN110344127A (en) | 2019-06-23 | 2019-06-23 | A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910546552.5A CN110344127A (en) | 2019-06-23 | 2019-06-23 | A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110344127A true CN110344127A (en) | 2019-10-18 |
Family
ID=68182774
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910546552.5A Pending CN110344127A (en) | 2019-06-23 | 2019-06-23 | A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110344127A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111005082A (en) * | 2019-12-17 | 2020-04-14 | 东华大学 | Whole-body porous polycaprolactone fiber and preparation method thereof |
| CN114316438A (en) * | 2022-01-07 | 2022-04-12 | 仲恺农业工程学院 | Natural fiber reinforced porous composite material |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053778A (en) * | 2007-05-16 | 2007-10-17 | 天津工业大学 | Method for making poly-meta-fluoethylene hollow fibre porous membrane and products thereof |
| CN101603245A (en) * | 2009-07-06 | 2009-12-16 | 东华大学 | A kind of preparation method of high elasticity super hydrophobic high temperature nano silicon dioxide fibrous membrane |
| CN102527262A (en) * | 2011-12-09 | 2012-07-04 | 西安建筑科技大学 | Method for preparing chemically perforated polyvinylidene fluoride hollow fiber ultrafiltration membrane |
| CN104289042A (en) * | 2014-09-05 | 2015-01-21 | 东华大学 | Electrospinning nano-fiber electret filtering material and its preparation method |
| CN104878456A (en) * | 2015-05-26 | 2015-09-02 | 青岛大学 | Magnetic spinning device and method using device for manufacturing micro-nano-meter fibers |
| CN104900913A (en) * | 2015-05-12 | 2015-09-09 | 江苏科技大学 | Preparation method of porous fiber gel polymer electrolyte |
| CN105386153A (en) * | 2015-11-24 | 2016-03-09 | 浙江理工大学 | Preparation method for ethyl cellulose micro-nanofibers |
| CN108823790A (en) * | 2018-07-01 | 2018-11-16 | 浙江理工大学 | Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof |
| CN108842223A (en) * | 2018-07-04 | 2018-11-20 | 四川大学 | A kind of preparation method of polyvinylidene fluoride nanometer fabric nonwoven cloth |
| US20190145022A1 (en) * | 2017-11-15 | 2019-05-16 | Rowan University | Devices and methods for producing aligned nanofibers |
| CN109830630A (en) * | 2018-12-29 | 2019-05-31 | 深圳中兴新材技术股份有限公司 | Coating diaphragm with hierarchical porous structure and its preparation method and application |
-
2019
- 2019-06-23 CN CN201910546552.5A patent/CN110344127A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053778A (en) * | 2007-05-16 | 2007-10-17 | 天津工业大学 | Method for making poly-meta-fluoethylene hollow fibre porous membrane and products thereof |
| CN101603245A (en) * | 2009-07-06 | 2009-12-16 | 东华大学 | A kind of preparation method of high elasticity super hydrophobic high temperature nano silicon dioxide fibrous membrane |
| CN102527262A (en) * | 2011-12-09 | 2012-07-04 | 西安建筑科技大学 | Method for preparing chemically perforated polyvinylidene fluoride hollow fiber ultrafiltration membrane |
| CN104289042A (en) * | 2014-09-05 | 2015-01-21 | 东华大学 | Electrospinning nano-fiber electret filtering material and its preparation method |
| CN104900913A (en) * | 2015-05-12 | 2015-09-09 | 江苏科技大学 | Preparation method of porous fiber gel polymer electrolyte |
| CN104878456A (en) * | 2015-05-26 | 2015-09-02 | 青岛大学 | Magnetic spinning device and method using device for manufacturing micro-nano-meter fibers |
| CN105386153A (en) * | 2015-11-24 | 2016-03-09 | 浙江理工大学 | Preparation method for ethyl cellulose micro-nanofibers |
| US20190145022A1 (en) * | 2017-11-15 | 2019-05-16 | Rowan University | Devices and methods for producing aligned nanofibers |
| CN108823790A (en) * | 2018-07-01 | 2018-11-16 | 浙江理工大学 | Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof |
| CN108842223A (en) * | 2018-07-04 | 2018-11-20 | 四川大学 | A kind of preparation method of polyvinylidene fluoride nanometer fabric nonwoven cloth |
| CN109830630A (en) * | 2018-12-29 | 2019-05-31 | 深圳中兴新材技术股份有限公司 | Coating diaphragm with hierarchical porous structure and its preparation method and application |
Non-Patent Citations (3)
| Title |
|---|
| 杨海贞等: "静电纺丝制备聚氧化乙烯复合纳米纤维的研究进展", 《高分子通报》 * |
| 陈冠荣: "《化工百科全书 第9卷 聚合机理和方法——空间化学》", 30 June 1995, 化学工业出版社 * |
| 黄策等: "《微孔滤膜及其应用》", 31 December 1980, 上海科学技术文献出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111005082A (en) * | 2019-12-17 | 2020-04-14 | 东华大学 | Whole-body porous polycaprolactone fiber and preparation method thereof |
| CN114316438A (en) * | 2022-01-07 | 2022-04-12 | 仲恺农业工程学院 | Natural fiber reinforced porous composite material |
| CN114316438B (en) * | 2022-01-07 | 2022-08-05 | 仲恺农业工程学院 | Natural fiber reinforced porous composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105543990B (en) | A kind of centrifugal spinning preparation method of micron or nano fibrous membrane | |
| CN106835304B (en) | A kind of electrostatic spinning-electrical painting device and its application | |
| CN101476167B (en) | Electro-spinning nano fibre nonwoven production apparatus | |
| CN105926162B (en) | A kind of method that electrostatic spinning prepares porous structure nanofiber | |
| CN108589048A (en) | Orientation capillary power drive is prepared using electrostatic spinning large area efficiently to catchment the methods of hydrophobic/hydrophilic Janus composite cellulosic membranes | |
| CN108823790A (en) | Centrifugal spinning porous micro nano rice tunica fibrosa and preparation method thereof | |
| CN105350093B (en) | A kind of negative pressure array centrifuges pneumoelectric device for spinning | |
| CN1367276A (en) | Method for producing fine fibrous polymer fabric | |
| CN105350089B (en) | A kind of pneumoelectric collected based on negative pressure spins three-dimensional rack preparation method and device | |
| CN105780152A (en) | Airflow bundling rotating twisting nanometer twisted thread preparation device and process | |
| CN106119996B (en) | The more fluid jet nozzles of coaxial electrically spun for preparing composite cellulosic membrane | |
| CN206015157U (en) | A kind of many fluid jet nozzles of the coaxial electrically spun for preparing composite cellulosic membrane | |
| CN106367819B (en) | A kind of preparation facilities of function nano line | |
| CN110344127A (en) | A kind of centrifugal spinning preparation method of porous Kynoar/polyethylene glycol oxide micro/nano-fibre | |
| Chen et al. | Bubble rupture in bubble electrospinning | |
| CN101857976A (en) | Device for preparing nano fibers with ordered arrangement and cross structures | |
| CN110373766A (en) | A kind of plasma wind disappears the device and operating method of electrostatic | |
| EP3191631A1 (en) | Device and method for preparing continuous nanofibrous yarns and bundles from electrospun fibers and fibrils | |
| CN108842195A (en) | A kind of electrostatic spinning apparatus and method based on bernoulli principle | |
| CN109537073A (en) | It is a kind of to blow the device and method that spinning technique preparation aligns fiber using solution | |
| CN103088444B (en) | A kind of method and device improving the many jets of electrostatic spinning | |
| Karakaş et al. | Polyurethane nanofibers obtained by electrospinning process | |
| Figen | History, basics, and parameters of electrospinning technique | |
| CN106048749B (en) | A kind of linear channel-shaped needle-free electrostatic spinning apparatus and spinning process | |
| CN105350090B (en) | A kind of negative pressure bubble electrostatic spinning apparatus |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191018 |