CN113073423A - Method for preparing micro-nanofiber three-dimensional network by expansion method - Google Patents
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- CN113073423A CN113073423A CN202110205461.2A CN202110205461A CN113073423A CN 113073423 A CN113073423 A CN 113073423A CN 202110205461 A CN202110205461 A CN 202110205461A CN 113073423 A CN113073423 A CN 113073423A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/76—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres otherwise than in a plane, e.g. in a tubular way
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Abstract
The invention relates to a method for preparing a three-dimensional network of micro-nano fibers by an expansion method, which comprises the steps of adding an expansion medium when receiving micro-nano fibers by electrostatic spinning, and then expanding the expansion medium to prepare the three-dimensional network of the micro-nano fibers; the length-diameter ratio of the micro-nano fibers is greater than 10000; the expansion medium refers to a foaming agent which can cause volume increase through physical and chemical reaction and the volume increase is more than 20 times; the micro-nano fiber three-dimensional network is a self-locking three-dimensional network; the self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network breaks. According to the invention, the expansion medium is added when the electrostatic spinning is used for receiving the micro-nano fibers, so that the expansion medium and the high-length-diameter-ratio fibers can be uniformly mixed, the expansion medium between adjacent fibers can be in a monodisperse state through volume increase, the method is simple, and the application range is wide.
Description
Technical Field
The invention belongs to the technical field of micro-nano fibers, and relates to a method for preparing a three-dimensional network of micro-nano fibers by an expansion method.
Background
The three-dimensional micro-nano fiber scaffold has wide application prospects in the fields of biological scaffolds, tissue engineering, battery electrodes, solar cells and the like. However, the micro-nano fiber is in a two-dimensional membrane structure with high bulk density in a macroscopic view in a natural state due to low rigidity. The technical key of preparing the three-dimensional micro-nano fiber support is how to realize the three-dimensional distribution of micro-nano fibers and keep the three-dimensional structure of the micro-nano fibers. Existing strategies can be divided into three categories:
firstly, micro-nano fibers are prepared, and then the fibers are dispersed in various viscous liquids by utilizing the difference of the fibers and media in fluid shearing force through mechanical action. The viscous liquid can be a hydrogel precursor, and then the viscous liquid is crosslinked to form hydrogel, wherein the micro-nano fibers are fixed in the hydrogel under the action of hydrogen bonds and van der waals force, so that the three-dimensional distribution state of the micro-nano fibers is maintained; in addition, the viscous liquid can also be an organic solvent, after the nano fibers are dispersed, the mixed solution is freeze-dried, the organic solvent is volatilized, a three-dimensional skeleton structure of the pure micro-nano fibers is left, then the fibers are crosslinked by using a crosslinking agent, and at the moment, the fibers are mutually connected in a covalent bond mode. However, the long fibers are low in rigidity and easy to intertwine with each other, so that uniform dispersion in viscous liquid is difficult to realize, and the three-dimensional micro-nano support is mostly composed of short fibers.
And secondly, in the preparation process of the micro-nano fibers, the stacking density of the fibers is controlled through the action of external force, so that the three-dimensional nano fiber support with high porosity is prepared. However, in the micro-nano fiber support, only electrostatic action and friction action exist among fibers, entanglement interaction among the fibers is less, the structure is loose, the mechanical property is poor, and the micro-nano fiber support is difficult to serve in practical application.
Thirdly, the existing two-dimensional micro-nano fiber membrane is finished by utilizing a foaming technology. Specifically, the fiber membrane is immersed in a foaming agent solution, cohesive force among the micro-nanofibers is overcome by utilizing the power of gas expansion, the micro-nanofibers are displaced mutually, and therefore the three-dimensional nanofiber scaffold with high porosity is prepared. However, the micro-nanofiber membrane has inevitable structural defects, and the fiber displacement of the weak part of the stress is large, so that the micro-nanofiber membrane is difficult to realize uniform monodispersion and is dispersed into a multilayer fiber membrane. Furthermore, some researchers add a foaming agent into the electrostatic spinning solution to improve the foaming uniformity, but the method inevitably damages the micro-nano fibers in the foaming process, and the prepared three-dimensional scaffold fibers have poor shapes and continuity.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing a micro-nanofiber three-dimensional network by an expansion method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the steps of adding an expansion medium (added after an electrostatic spinning Taylor cone is formed, the adding method comprises but is not limited to local addition, all addition, addition at intervals and all addition in the spinning process) when micro-nanofibers are received by electrostatic spinning, and then expanding the expansion medium to prepare the micro-nanofiber three-dimensional network;
the length-diameter ratio of the micro-nano fibers is greater than 10000;
the expansion medium refers to a foaming agent which can cause volume increase through physical and chemical reaction and the volume increase is more than 20 times;
the micro-nano fiber three-dimensional network is a self-locking three-dimensional network;
the self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network breaks.
As a preferred technical scheme:
according to the method for preparing the micro-nanofiber three-dimensional network by the expansion method, more than 99% of fibers in the micro-nanofiber three-dimensional network are in a monodisperse state, and the diameter of the fibers is 100 nm-10 microns. The monodisperse state is a state in which fibers are not completely juxtaposed and overlapped. The absolute monodispersed state cannot be guaranteed in practical operation, and more than 99% of the fibers of the present invention are in a monodispersed state.
According to the method for preparing the micro-nanofiber three-dimensional network by the expansion method, the ratio of the volume of the micro-nanofiber three-dimensional network to the volume of all micro-nanofibers is greater than 20: 1.
According to the method for preparing the micro-nano fiber three-dimensional network by the expansion method, the expansion medium is expanded by adopting a heating mode, a product obtained after electrostatic spinning is placed in an aqueous solution, a foaming agent is heated to rapidly generate a large amount of escaping gas, the volume of an expansion component is changed, the expansion action can overcome the friction force among micro-nano fibers to enable the micro-nano fibers to generate spatial displacement, the micro-nano fibers are gradually changed into a single dispersed state from a tightly stacked state, the three-dimensional distribution of the micro-nano fibers is finally realized, and after the expansion of the foaming agent is finished, the micro-nano fiber three-dimensional network is solidified through the interaction force (friction force, hydrogen bond and van der Waals force) of the micro-nano.
According to the method for preparing the three-dimensional network of the micro-nano fibers by the expansion method, the heating temperature is higher than or equal to the decomposition temperature of the foaming agent and lower than or equal to the glass transition temperature of the micro-nano fibers or the melting point of the micro-nano fibers.
According to the method for preparing the three-dimensional network of the micro-nanofiber by the expansion method, the heating time is 3-30 min.
According to the method for preparing the three-dimensional network of the micro-nanofiber by the expansion method, hydrogen bonds and van der Waals forces exist between the micro-nanofiber and the expansion medium.
The method for preparing the micro-nanofiber three-dimensional network by the expansion method comprises the step of preparing a micro-nanofiber three-dimensional network by using a swelling medium, wherein the swelling medium is more than one of sodium bicarbonate, ammonium bicarbonate, alum and azobisisobutyronitrile.
According to the method for preparing the three-dimensional network of the micro-nano fibers by the expansion method, the addition amount of the expansion medium is 5-20 wt% of the micro-nano fibers.
The mechanism of the three-dimensional micro-nano fiber network self-locking in the invention is as follows:
according to the invention, the expansion medium is added (instead of adding the expansion medium to the formed micro-nanofiber membrane) while the micro-nanofibers are received, so that the expansion medium and the micro-nanofibers are fully contacted and mixed, the expansion medium refers to a foaming agent which can cause volume increase through physicochemical reaction and the increase multiple is more than 20 times, and the expansion force after the expansion of the expansion medium can overcome the friction force between the micro-nanofibers, so that the fibers are subjected to spatial displacement; and the volume of the expansion medium dispersed between the adjacent micro-nano fibers is changed, so that the distance between the fibers is increased. Finally realizing the monodispersed distribution of the micro-nano fibers in a three-dimensional space to prepare a micro-nano fiber three-dimensional network.
The three-dimensional network of the micro-nano fibers prepared by using the foaming agent only has the micro-nano fibers but does not contain other media, and the final purpose is to realize the expansion of the tightly piled micro-nano fibers to form the three-dimensional micro-nano fiber network.
The degree of mutual lapping and linking of the high-length-diameter ratio fibers adopted in the invention is far higher than that of the short fibers in the prior art. In addition, the fibers are in a monodisperse state, namely, the fibers are staggered in spatial position between any two fibers, so that the overlapping and hooking effect is greatly increased. After the three-dimensional micro-nano fiber network is stressed, the high-length-diameter ratio fibers in the network are extruded and cohered mutually, so that the friction force among the fibers is further increased, the mutual slippage among the fibers is weakened, and the tensile modulus of the three-dimensional network is improved. The process is strengthened along with the improvement of the tensile deformation degree until the fiber is broken and the whole structure collapses.
Has the advantages that:
(1) according to the method for preparing the micro-nanofiber three-dimensional network by the expansion method, the prepared micro-nanofiber three-dimensional network has good mechanical properties, the degree of mutual overlapping and hooking among fibers with high length-diameter ratio is far higher than that of short fibers in the prior art, self-locking is formed, the micro-nanofiber three-dimensional network has unique tensile mechanical behavior, and the micro-nanofiber three-dimensional network has higher mechanical matching degree with biological soft tissues.
(2) According to the method for preparing the micro-nanofiber three-dimensional network by the expansion method, the monodisperse micro-nanofiber network with high porosity can be in more full contact with external media (solution, microorganisms, dust and the like), and the method has unique advantages in the aspects of drug controlled release, antibiosis and pollutant adsorption.
(3) According to the method for preparing the three-dimensional network of the micro-nano fibers by the expansion method, the expansion medium is added when the micro-nano fibers are received by electrostatic spinning, so that the expansion medium and the high-length-diameter-ratio fibers can be uniformly mixed on the fiber layer surface, the expansion medium between the adjacent fibers can be in a monodisperse state by volume increase, and the method is simple and wide in application range.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding a sodium bicarbonate foaming agent when the Polycaprolactone (PCL) micro-nano fiber with the length-diameter ratio of 1000000 and the fiber diameter of 100nm is received by electrostatic spinning; wherein the addition amount of the sodium bicarbonate foaming agent is 5 wt% of the Polycaprolactone (PCL) micro-nano fiber; the melting point of the Polycaprolactone (PCL) micro-nano fiber is 60 ℃;
(2) then, expanding the sodium bicarbonate foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 50 deg.C, and the heating time is 3 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.1% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 25: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the sodium bicarbonate foaming agent.
Example 2
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding an ammonium bicarbonate foaming agent when the polylactic acid (PLA) micro-nano fiber with the length-diameter ratio of 20000 and the fiber diameter of 5 mu m is received by electrostatic spinning; wherein the addition amount of the ammonium bicarbonate foaming agent is 10 wt% of the polylactic acid (PLA) micro-nano fiber; the glass transition temperature of the polylactic acid (PLA) micro-nano fibers is 57 ℃;
(2) then, expanding the ammonium bicarbonate foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 45 deg.C, and the heating time is 15 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.3% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 50: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the ammonium bicarbonate foaming agent.
Example 3
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding a sodium bicarbonate foaming agent when electrostatic spinning receives polylactic acid-glycolic acid copolymer (PLGA) micro-nano fibers with the length-diameter ratio of 200000 and the fiber diameter of 500 nm; wherein the addition amount of the sodium bicarbonate foaming agent is 20 wt% of polylactic acid-glycolic acid copolymer (PLGA) micro-nano fibers; the glass transition temperature of polylactic acid-glycolic acid copolymer (PLGA) micro-nano fibers is 50 ℃;
(2) then, expanding the sodium bicarbonate foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 40 deg.C, and the heating time is 30 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.6% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 100: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the sodium bicarbonate foaming agent.
Example 4
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding an ammonium bicarbonate foaming agent when the polyethylene terephthalate (PET) micro-nanofibers with the length-diameter ratio of 100000 and the fiber diameter of 1 micrometer are received by electrostatic spinning; wherein the addition amount of the ammonium bicarbonate foaming agent is 7 wt% of the polyethylene terephthalate (PET) micro-nanofiber; the glass transition temperature of the polyethylene terephthalate (PET) micro-nano fiber is 70 ℃;
(2) then, expanding the ammonium bicarbonate foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 55 deg.C, and the heating time is 7 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.1% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 35: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the ammonium bicarbonate foaming agent.
Example 5
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding an ammonium bicarbonate foaming agent when the Polycaprolactone (PCL) micro-nano fiber with the length-diameter ratio of 33333 and the fiber diameter of 3 microns is received by electrostatic spinning; wherein the addition amount of the ammonium bicarbonate foaming agent is 8 wt% of the Polycaprolactone (PCL) micro-nano fiber; the melting point of the Polycaprolactone (PCL) micro-nano fiber is 60 ℃;
(2) then, expanding the ammonium bicarbonate foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 40 deg.C, and the heating time is 10 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.2% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 40: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the ammonium bicarbonate foaming agent.
Example 6
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding foaming agent (alum and sodium bicarbonate with the mass ratio of 1: 1) when polylactic acid (PLA) micro-nano fiber with the length-diameter ratio of 25000 and the fiber diameter of 4 mu m is received by electrostatic spinning; wherein the addition amount of the foaming agent is 13 wt% of the polylactic acid (PLA) micro-nano fiber; the glass transition temperature of the polylactic acid (PLA) micro-nano fibers is 57 ℃;
(2) then, expanding the foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 50 deg.C, and the heating time is 19 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.4% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 65: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the alum foaming agent.
Example 7
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding azodiisobutyronitrile foaming agent when the polylactic acid-glycolic acid copolymer (PLGA) micro-nano fiber with the length-diameter ratio of 14286 and the fiber diameter of 7 mu m is received by electrostatic spinning; wherein the addition amount of the azodiisobutyronitrile foaming agent is 15 wt% of polylactic acid-glycolic acid copolymer (PLGA) micro-nano fibers; the glass transition temperature of polylactic acid-glycolic acid copolymer (PLGA) micro-nano fibers is 50 ℃;
(2) then, expanding the azodiisobutyronitrile foaming agent in a heating mode to prepare a micro-nano fiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 40 deg.C, and the heating time is 23 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.5% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 75: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the azodiisobutyronitrile foaming agent.
Example 8
A method for preparing a micro-nanofiber three-dimensional network by an expansion method comprises the following specific steps:
(1) adding foaming agents (alum and azodiisobutyronitrile in a mass ratio of 1: 1) when electrostatic spinning receives polyethylene terephthalate (PET) micro-nanofibers with an aspect ratio of 20000 and a fiber diameter of 5 micrometers; wherein the addition amount of the foaming agent is 18 wt% of polyethylene terephthalate (PET) micro-nano fibers; the glass transition temperature of the polyethylene terephthalate (PET) micro-nano fiber is 70 ℃;
(2) then, expanding the foaming agent in a heating mode to prepare a micro-nanofiber three-dimensional network with a self-locking three-dimensional network; wherein the heating temperature is 55 deg.C, and the heating time is 27 min.
The self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network is broken; 99.6% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the monodisperse state refers to a state that the fibers are not completely overlapped in parallel; the ratio of the volume of the micro-nano fiber three-dimensional network to the volume of all micro-nano fibers is 90: 1; hydrogen bonds and van der waals forces exist between the micro-nano fibers and the foaming agent.
Claims (9)
1. A method for preparing a micro-nanofiber three-dimensional network by an expansion method is characterized by comprising the following steps: adding an expansion medium when the micro-nano fibers are received by electrostatic spinning, and then expanding the expansion medium to prepare a three-dimensional network of the micro-nano fibers;
the length-diameter ratio of the micro-nano fibers is greater than 10000;
the expansion medium refers to a foaming agent which can cause volume increase through physical and chemical reaction and the volume increase is more than 20 times;
the micro-nano fiber three-dimensional network is a self-locking three-dimensional network;
the self-locking three-dimensional network means that the tensile modulus of the three-dimensional network increases along with the increase of tensile strain under the tensile condition until the three-dimensional network breaks.
2. The method for preparing the micro-nano fiber three-dimensional network by the expansion method according to claim 1, wherein more than 99% of fibers in the micro-nano fiber three-dimensional network are in a monodisperse state, and the diameter of the fibers is 100 nm-10 μm.
3. The method for preparing the micro-nanofiber three-dimensional network according to claim 1, wherein the ratio of the volume of the micro-nanofiber three-dimensional network to the volume of all micro-nanofibers is greater than 20: 1.
4. The method for preparing the three-dimensional network of the micro-nano fibers by the expansion method according to claim 1, wherein the expansion medium is expanded by heating.
5. The method for preparing the three-dimensional network of the micro-nano fibers by the expansion method according to claim 4, wherein the heating temperature is not lower than the decomposition temperature of the foaming agent and not higher than the glass transition temperature of the micro-nano fibers or the melting point of the micro-nano fibers.
6. The method for preparing the three-dimensional network of the micro-nano fibers by the expansion method according to claim 5, wherein the heating time is 3-30 min.
7. The method for preparing the three-dimensional network of the micro-nano fibers by the expansion method according to claim 1, wherein hydrogen bonds and van der waals forces exist between the micro-nano fibers and the expansion medium.
8. The method for preparing the three-dimensional network of the micro-nano fibers by the expansion method according to claim 1, wherein the expansion medium is more than one of sodium bicarbonate, ammonium bicarbonate, alum and azobisisobutyronitrile.
9. The method for preparing the three-dimensional network of the micro-nano fibers through the expansion method according to claim 1, wherein the addition amount of the expansion medium is 5-20 wt% of the micro-nano fibers.
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Application publication date: 20210706 |