CN107201561B - Micro-/ nano composite material coaxially sprays electrospinning method for preparing altogether - Google Patents
Micro-/ nano composite material coaxially sprays electrospinning method for preparing altogether Download PDFInfo
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- CN107201561B CN107201561B CN201710476104.3A CN201710476104A CN107201561B CN 107201561 B CN107201561 B CN 107201561B CN 201710476104 A CN201710476104 A CN 201710476104A CN 107201561 B CN107201561 B CN 107201561B
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- spinning
- spray head
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- liquid storage
- spraying
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Classifications
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
Abstract
Electrospinning method for preparing is coaxially sprayed altogether the invention discloses a kind of micro-/ nano composite material, and this method configures certain density spray coating liquor and spinning solution as needed first, and is added separately to spray accordingly in liquid storage pump and spinning liquid storage pump；Spraying liquid storage pump and spinning liquid storage pump are connect with the core spray head of Coaxial nozzle with shell spray head respectively, adjust the internal diameter ratio of core spray head and shell spray head, to guarantee the coaxial realization that spray is spun altogether；Voltage needed for regulating device receives the other factors such as distance, to guarantee that the even distribution of prepared micro/nano-fibre and micro-/ nano particle is spun in coaxial spray altogether.The method achieve by the way that coaxially spray spinning equipment prepares micro-/ nano particle and micro/nano-fibre composite material altogether.
Description
Technical field
The present invention relates to micro-/ nano field of composite material preparation more particularly to a kind of the coaxial of micro-/ nano composite material to be total to
Spray electrospinning method for preparing.
Background technique
Electrostatic spinning technique under the synergistic effect of electric field force and surface tension, is generated " Taylor circle by polymer drop
Cone ", and then jet stream is generated, into receiver board operational process, drop is divided and is stretched, and solvent volatilizees, final fine
Dimension deposits on receiver board.Traditional uniaxial electrospinning technology can only once prepare a kind of fibrous material.
Electrostatic spraying is the physical phenomenon according to electrophoresis, and the polymer drop being atomized is made to take negative electricity in high voltage electric field
Lotus, and be crushed under the action ofs electric field force, surface tension, gravity etc., and then after dividing, discrete jet stream is directionally formed,
Flow to positively charged receiving platform and deposited thereon.Traditional uniaxial spraying technology can only once prepare a kind of granular materials.
The technology of composite fibre is prepared by coaxial electrostatic spinning it has been reported that coaxial electrospray is multiple to prepare simultaneously
The technology for closing particle also has been reported that.But coaxial electrostatic spinning can only prepare composite fibre, and coaxial electrospray can only be prepared again
Particle is closed, two kinds of technologies cannot prepare micro/nano-fibre and particulate composite, and there is no utilize coaxial technology system at present
The relevant report of standby micro/nano-fibre and particulate composite method.
Summary of the invention
Based on the problems of prior art, the object of the present invention is to provide a kind of the coaxial of micro-/ nano composite material
Electrospinning method for preparing is sprayed altogether, can prepare micro/nano-fibre and particulate composite in a manner of coaxially total spray spinning.
The purpose of the present invention is what is be achieved through the following technical solutions:
What embodiment of the present invention provided a kind of micro-/ nano composite material coaxially sprays electrospinning method for preparing altogether, comprising:
Step 1: configuration can be dissolved in the Polymer Solution of solvent as spinning solution；Configuration can be dissolved in the inorganic high score of solvent
Sub- solution is as spray coating liquor；
Step 2: the spray coating liquor is added in spraying liquid storage pump, and the spinning solution is added in spinning liquid storage pump, will
Spraying liquid storage pump and spinning liquid storage pump are connect with the coaxial spinning equipment of spray altogether；
Step 3: the spinning shell spray head and spraying core of the coaxial reception distance for spraying spinning equipment altogether and Coaxial nozzle are adjusted
The internal diameter ratio of spray head forms drop below spraying core spray head, while the spinning solution of spinning shell spray head wraps spraying core spray head
Outer wall when, open high voltage power supply, adjust voltage, make spray coating liquor and spinning solution by setting flow velocity simultaneously to received diaphragm carry out
Equally distributed micro-/ nano particle and micro/nano-fibre composite material are prepared in spraying and spinning.
As seen from the above technical solution provided by the invention, the coaxial spinning of spray altogether provided in an embodiment of the present invention is standby multiple
The method of condensation material, it has the advantage that:
This method by using spinning equipment is coaxially sprayed altogether, realize by coaxially altogether spray spinning in a manner of prepare micro/nano-fibre with
Micro-/ nano particulate composite, the micro/nano-fibre and micro-/ nano particulate composite of preparation have secured with substrate bonding
And the advantages of high-specific surface area, while there is the associativity of better uniformly dispersed and fiber and particle, it can be simultaneously to base
The improvement effect of material offer reinforcing effect and specific surface area.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is the coaxial schematic device for spraying electrospinning method for preparing altogether provided in an embodiment of the present invention；
Fig. 2 is that the SEM that the coaxial total spray that the embodiment of the present invention 1 provides spins standby composite process schemes；
Fig. 3 is that the SEM that the coaxial total spray that the embodiment of the present invention 2 provides spins standby composite process schemes；
Fig. 4 is that the SEM that the coaxial total spray that the embodiment of the present invention 3 provides spins standby composite process schemes.
Specific embodiment
Below with reference to particular content of the invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts,
Belong to protection scope of the present invention.
The embodiment of the present invention provides a kind of the coaxial of micro-/ nano composite material (i.e. micron order or nanocomposite)
Electrospinning method for preparing is sprayed altogether, can prepare micro/nano-fibre and micro-/ nano particulate composite, comprising the following steps:
Step 1: configuration can be dissolved in the Polymer Solution of solvent as spinning solution；Configuration can be dissolved in the inorganic high score of solvent
Sub- solution is as spray coating liquor；
Step 2: the spray coating liquor is added in spraying liquid storage pump, and the spinning solution is added in spinning liquid storage pump, will
Spraying liquid storage pump and spinning liquid storage pump are connect with the coaxial spinning equipment of spray altogether；
Step 3: the spinning shell spray head and spraying core of the coaxial reception distance for spraying spinning equipment altogether and Coaxial nozzle are adjusted
The internal diameter ratio of spray head forms drop below spraying core spray head, while the spinning solution of spinning shell spray head wraps spraying core spray head
Outer wall when, open high voltage power supply, adjust voltage, make spray coating liquor and spinning solution by setting flow velocity simultaneously to received diaphragm carry out
Equally distributed micro-/ nano particle and micro/nano-fibre composite material are prepared in spraying and spinning.
In above-mentioned preparation method, spray coating liquor is configured by PVDF, DMF and acetone soln；
The spinning solution is configured by PVDF, DMF and acetone soln.
In above-mentioned preparation method, the PVDF mass fraction of spray coating liquor is 0.1%~100%, DMF in the spray coating liquor: acetone
Mass ratio be 3:2；
The PVDF mass fraction of the spinning solution is 0.1%~100%, DMF in the spinning solution: the mass ratio of acetone is 3:
2。
As shown in Figure 1, coaxially spray spinning equipment includes: altogether in above-mentioned preparation method
Bracket 1, spinning liquid storage pump 2, spinning shell spray head 3, spraying liquid storage pump 4, spraying core spray head 5, spinning nitrogen pressurization dress
Set 7, spraying nitrogen pressure device 8, receiving platform 6 and high voltage power supply 9；Wherein,
The spinning liquid storage pump is set on the bracket, and spinning liquid storage pump is connect with the spinning nitrogen pressure device,
The liquid outlet of spinning liquid storage pump connects the spinning shell spray head；
The spraying liquid storage pump is located in the spinning liquid storage pump, spraying liquid storage pump and the spraying nitrogen pressure device
The liquid outlet of connection, spraying liquid storage pump connects the spraying core spray head, and the spraying core spray head is located at the spinning shell spray head
Interior formation Coaxial nozzle, the Coaxial nozzle are electrically connected with the high voltage power supply cathode；
Receiving platform is located at below the Coaxial nozzle, is electrically connected with the high-voltage power cathode.
In above-mentioned preparation method, spinning shell spray head and spraying core spray head are all made of spray head made of conductive and heat-conductive metal；
The internal diameter of the spinning shell spray head is 0.1mm~100mm；
The internal diameter for spraying core spray head is 0.1mm~100mm.
In above-mentioned preparation method step 3, the internal diameter adjustable range of the spinning shell spray head of Coaxial nozzle be 0.1mm~
100mm, the internal diameter adjustable range of spraying core spray head are 0.1mm~100mm；
Receive the adjustable range of distance are as follows: 5~30cm；
The adjustable range of supply voltage are as follows: 0.1kV~50kV；
The flow rates for controlling spray coating liquor and spinning solution are 0.1~1000ml/h；
Received diaphragm uses UHMWPE diaphragm.
The present invention coaxially sprays spinning method compared with traditional coaxial electrostatic spinning technology prepares composite material altogether: this is coaxial altogether
Spinning method can prepare two kinds of micro/nano-fibre composite materials being evenly distributed, and coaxially spray spinning method can be prepared and is evenly distributed altogether
Micro/nano-fibre and particulate composite.Coaxially spray spinning method and the preparation of traditional coaxial electrospray technology are multiple altogether by the present invention
Condensation material is compared: this, which is coaxially total to spraying method, can prepare two kinds of micro-/ nano particulate composites being evenly distributed, and coaxial spray altogether is spun
Method can prepare the micro/nano-fibre and particulate composite being evenly distributed.
The embodiment of the present invention is specifically described in further detail below.
It is provided in an embodiment of the present invention a kind of by coaxially spraying the method for spinning standby composite material altogether, the specific steps are as follows:
Step 1: all Polymer Solutions that configuration can be dissolved in solvent make it can by adjusting the concentration of above-mentioned solution
Using as spinning solution；The inorganic and high molecular solution that configuration can be dissolved in solvent allows to make by adjusting its concentration
For electrostatic masking liquid.The electrostatic spinning liquid and electrostatic coating liquid concentration configured is respectively 0.1%~100%；
Step 2: above-mentioned spray coating liquor and spinning solution are added separately in spraying liquid storage pump and spinning liquid storage pump for use, and
It is installed in the coaxial spinning equipment of spray altogether；
Step 3: the spinning shell spray head internal diameter of the coaxial Coaxial nozzle for spraying spinning equipment altogether is adjusted between 0.1mm~100mm
With spraying core spray head internal diameter, and the reception distance for coaxially spraying spinning equipment altogether is adjusted in the range of 5~30cm, when spraying core spray
Head below formed droplet, while the spinning solution of spinning shell spray head wrap spraying core spray head outer wall when, open high voltage power supply,
Adjusting voltage range is 0.1kV~50kV, applies the pressure of 0.01MPa~20MPa to spraying liquid storage pump and spinning liquid storage pump respectively
Power adjusts the rate of spraying and spinning in 0.1~1000ml/h, and preparation has micro-/ nano particle equally distributed to a certain degree
With micro/nano-fibre composite material.
Raw material used in the embodiment of the present invention: DMF (Beijing Chemical Plant), PVDF (average molecular weight 534000, A Faai
Sha Chemical Co., Ltd.), UHMWPE diaphragm (golden power new energy), acetone (Beijing Chemical Plant).
The PVDF/DMF/ acetone soln that PVDF mass fraction is 3% and 15% is respectively configured as spray coating liquor and spinning solution,
DMF in PVDF solution: acetone=3:2；Above-mentioned solution is added separately to be sprayed accordingly with spinning liquid storage pump, passes through Fig. 1
Shown in coaxially spray spinning equipment altogether, the shell spray head internal diameter for adjusting Coaxial nozzle is 1.2mm, and core spray head internal diameter is 0.7mm, and adjusting connects
Receive distance and supply voltage, the flow velocity for controlling spray coating liquor and spinning solution is respectively 0.6ml/h and 1.3ml/h, using UHMWPE every
Film spins prepared micro/nano-fibre to coaxial spray altogether and micro-/ nano particulate composite receives.
Embodiment 1:
The PVDF/DMF/ acetone soln that PVDF mass fraction is 3% and 15% is respectively configured as spray coating liquor and spinning solution,
DMF in PVDF solution: acetone=3:2；Above-mentioned solution is added separately to be sprayed accordingly in spinning liquid storage pump, passes through Fig. 1
Shown in coaxially spray spinning equipment altogether, the shell spray head internal diameter for adjusting Coaxial nozzle is 1.2mm, and core spray head internal diameter is 0.7mm, and adjusting connects
Receiving distance be 15cm and supply voltage is 17kV, and the flow velocity of control spray coating liquor and spinning solution is respectively 0.6ml/h and 1.3ml/h,
Prepared micro/nano-fibre is spun to coaxial spray altogether using UHMWPE diaphragm and micro-/ nano particulate composite receives.From figure
As can be seen that at this time due to brownout in 2, electric field force is insufficient to allow jet stream splitting at silk, micro- in prepared composite material/
Nano particle is more, and prepared micro/nano-fibre is very little, so voltage is not suitable for the coaxial progress that spray is spun altogether.
Embodiment 2:
The PVDF/DMF/ acetone soln that PVDF mass fraction is 3% and 15% is respectively configured as spray coating liquor and spinning solution,
DMF in PVDF solution: acetone=3:2.Above-mentioned solution is added separately to be sprayed accordingly in spinning liquid storage pump, passes through Fig. 1
Shown in coaxially spray spinning equipment altogether, the shell spray head internal diameter for adjusting Coaxial nozzle is 1.2mm, and core spray head internal diameter is 0.7mm, and adjusting connects
Receipts distance is 7cm and supply voltage is 23kV, and the flow velocity for controlling spray coating liquor and spinning solution is respectively 0.6ml/h and 1.3ml/h, is made
Prepared micro/nano-fibre is spun to coaxial spray altogether with UHMWPE diaphragm and micro-/ nano particulate composite receives.At this time by
Too close in reception distance, the solvent in spray coating liquor institute sprayed particle can not volatilize in time during decline, finally in lithium electricity
Pond membrane surface forms aggregate, and cannot form the intact particle of shape, so receiving distance is not suitable for what coaxial spray altogether was spun
It carries out.
Embodiment 3:
The PVDF/DMF/ acetone soln that PVDF mass fraction is 3% and 15% is respectively configured as spray coating liquor and spinning solution,
DMF in PVDF solution: acetone=3:2.Above-mentioned solution is added separately to be sprayed accordingly in spinning liquid storage pump, passes through Fig. 1
Shown in coaxially spray spinning equipment altogether, the shell spray head internal diameter for adjusting Coaxial nozzle is 1.2mm, and core spray head internal diameter is 0.7mm, and adjusting connects
Receiving distance be 15cm and supply voltage is 23kV, and the flow velocity of control spray coating liquor and spinning solution is respectively 0.6ml/h and 1.3ml/h,
Prepared micro/nano-fibre is spun to coaxial spray altogether using UHMWPE diaphragm and micro-/ nano particulate composite receives.At this time
Stable spraying and spinning are formed, and as can be seen from Figure 3 micro/nano-fibre and particle are bonded together well.
Embodiment 4:
The PVDF/DMF/ acetone soln that PVDF mass fraction is 3% and 15% is respectively configured as spray coating liquor and spinning solution,
DMF in PVDF solution: acetone=3:2.Above-mentioned solution is added separately to be sprayed accordingly in spinning liquid storage pump, passes through Fig. 1
Shown in coaxially spray spinning equipment altogether, the shell spray head internal diameter for adjusting Coaxial nozzle is 1.2mm, and core spray head internal diameter is 0.4mm, and adjusting connects
Receiving distance be 15cm and supply voltage is 23kV, and the flow velocity of control spray coating liquor and spinning solution is respectively 0.6ml/h and 1.3ml/h,
Prepared micro/nano-fibre is spun to coaxial spray altogether using UHMWPE diaphragm and micro-/ nano particulate composite receives.From figure
In 4 as can be seen that at this time since spraying nozzle internal diameter is too small, it be easy to cause spraying to be obstructed, only minimal amount of micro-/ nano particle
It is produced out.
Preparation method of the invention is by the way that coaxially spray spinning mode prepares micro/nano-fibre and micro-/ nano Particles dispersed material altogether
Material, prepared micro/nano-fibre and micro-/ nano particulate composite, which have, bonds secured and high-specific surface area spy with substrate
Point, while there is the associativity of better uniformly dispersed and fiber and particle, can simultaneously to substrate provide reinforcing effect with
The improvement effect of specific surface area.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (6)
1. a kind of micro-/ nano composite material coaxially sprays electrospinning method for preparing altogether characterized by comprising
Step 1: configuration can be dissolved in the Polymer Solution of solvent as spinning solution；The inorganic polymer that configuration can be dissolved in solvent is molten
Liquid is as spray coating liquor；
Step 2: the spray coating liquor is added in spraying liquid storage pump, and the spinning solution is added in spinning liquid storage pump, will be sprayed
Liquid storage pump and spinning liquid storage pump are connect with the coaxial spinning equipment of spray altogether；
Step 3: the spinning shell spray head and spraying core spray head of the coaxial reception distance for spraying spinning equipment altogether and Coaxial nozzle are adjusted
Internal diameter ratio, form drop below spraying core spray head, while the spinning solution of spinning shell spray head wraps the outer of spraying core spray head
When wall, high voltage power supply is opened, adjusts voltage, sprays spray coating liquor and spinning solution to received diaphragm simultaneously by setting flow velocity
Equally distributed micro-/ nano particle and micro/nano-fibre composite material are prepared with spinning.
2. micro-/ nano composite material according to claim 1 coaxially sprays electrospinning method for preparing altogether, which is characterized in that described
Spray coating liquor is configured by PVDF, DMF and acetone soln；
The spinning solution is configured by PVDF, DMF and acetone soln.
3. micro-/ nano composite material according to claim 2 coaxially sprays electrospinning method for preparing altogether, which is characterized in that described
The PVDF mass fraction of spray coating liquor is 0.1%~100%, DMF in the spray coating liquor: the mass ratio of acetone is 3:2；
The PVDF mass fraction of the spinning solution is 0.1%~100%, DMF in the spinning solution: the mass ratio of acetone is 3:2.
4. micro-/ nano composite material according to any one of claims 1 to 3 coaxially sprays electrospinning method for preparing, feature altogether
It is, the coaxial spinning equipment of spray altogether includes:
Bracket, spinning liquid storage pump, spinning shell spray head, spraying liquid storage pump, spraying core spray head, spinning nitrogen pressure device, spraying nitrogen
Gas pressurizing device, receiving platform and high voltage power supply；Wherein,
The spinning liquid storage pump is set on the bracket, and spinning liquid storage pump is connect with the spinning nitrogen pressure device, the spinning
The liquid outlet of silk liquid storage pump connects the spinning shell spray head；
The spraying liquid storage pump is located in the spinning liquid storage pump, and spraying liquid storage pump connects with the spraying nitrogen pressure device
It connects, the liquid outlet of spraying liquid storage pump connects the spraying core spray head, and the spraying core spray head is located in the spinning shell spray head
Coaxial nozzle is formed, which is electrically connected with the high voltage power supply cathode；
Receiving platform is located at below the Coaxial nozzle, is electrically connected with the high-voltage power cathode.
5. micro-/ nano composite material according to any one of claims 1 to 3 coaxially sprays electrospinning method for preparing, feature altogether
It is, the spinning shell spray head and spraying core spray head are all made of spray head made of conductive and heat-conductive metal；
The internal diameter of the spinning shell spray head is 0.1mm~100mm；
The internal diameter for spraying core spray head is 0.1mm~100mm.
6. micro-/ nano composite material according to any one of claims 1 to 3 coaxially sprays electrospinning method for preparing, feature altogether
It is, in the method step 3, the internal diameter adjustable range of the spinning shell spray head of Coaxial nozzle is 0.1mm~100mm, sprays core
The internal diameter adjustable range of spray head is 0.1mm~100mm；
Receive the adjustable range of distance are as follows: 5~30cm；
The adjustable range of supply voltage are as follows: 0.1kV~50kV；
The flow rates for controlling spray coating liquor and spinning solution are 0.1~1000ml/h；
Received diaphragm uses UHMWPE diaphragm.
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| CN108878736A (en) * | 2018-06-12 | 2018-11-23 | 北京石油化工学院 | A kind of device and method that coaxial spray altogether spins standby lithium ion composite diaphragm |
| CN111359452B (en) * | 2020-03-18 | 2021-11-12 | 北京化工大学 | Structure-enhanced hydrotalcite-immobilized composite fiber membrane, and preparation method and application thereof |
| CN111690993A (en) * | 2020-06-24 | 2020-09-22 | 湖南工程学院 | Coaxial injection needle tube for electrostatic spinning |
| CN115275509A (en) * | 2021-04-30 | 2022-11-01 | 中国石油化工股份有限公司 | Fiber diaphragm and preparation method and application thereof |
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