CN117143390B - Bionic micro-nanofiber aerogel and preparation method thereof - Google Patents
Bionic micro-nanofiber aerogel and preparation method thereof Download PDFInfo
- Publication number
- CN117143390B CN117143390B CN202311422370.XA CN202311422370A CN117143390B CN 117143390 B CN117143390 B CN 117143390B CN 202311422370 A CN202311422370 A CN 202311422370A CN 117143390 B CN117143390 B CN 117143390B
- Authority
- CN
- China
- Prior art keywords
- bmi
- pmia
- pai
- nanofiber
- dispersion liquid
- 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.)
- Active
Links
- 239000002121 nanofiber Substances 0.000 title claims abstract description 170
- 239000004964 aerogel Substances 0.000 title claims abstract description 81
- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229920000889 poly(m-phenylene isophthalamide) Polymers 0.000 claims abstract description 109
- 239000006185 dispersion Substances 0.000 claims abstract description 101
- 229920001410 Microfiber Polymers 0.000 claims abstract description 69
- 239000003658 microfiber Substances 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 34
- 230000008569 process Effects 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000007710 freezing Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 40
- 239000002904 solvent Substances 0.000 claims description 28
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 238000010041 electrostatic spinning Methods 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 230000003592 biomimetic effect Effects 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 abstract description 15
- 238000009413 insulation Methods 0.000 abstract description 8
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 description 135
- 229920003192 poly(bis maleimide) Polymers 0.000 description 135
- 229920002312 polyamide-imide Polymers 0.000 description 91
- 239000004962 Polyamide-imide Substances 0.000 description 90
- 239000004760 aramid Substances 0.000 description 32
- 229920003235 aromatic polyamide Polymers 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 24
- 229920006231 aramid fiber Polymers 0.000 description 8
- 239000012634 fragment Substances 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 5
- 238000001523 electrospinning Methods 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 238000000265 homogenisation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000012827 research and development Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007970 homogeneous dispersion Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 244000223014 Syzygium aromaticum Species 0.000 description 2
- 235000016639 Syzygium aromaticum Nutrition 0.000 description 2
- 239000005456 alcohol based solvent Substances 0.000 description 2
- 238000012669 compression test Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 210000003462 vein Anatomy 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 241000219138 Luffa Species 0.000 description 1
- 235000003956 Luffa Nutrition 0.000 description 1
- 244000280244 Luffa acutangula Species 0.000 description 1
- 235000009814 Luffa aegyptiaca Nutrition 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920001872 Spider silk Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229920005570 flexible polymer Polymers 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a bionic micro-nanofiber aerogel and a preparation method thereof, wherein PMIA/BMI nanofibers and PAI/BMI microfibers are used as raw materials to prepare mixed dispersion liquid, and the mixed dispersion liquid is subjected to quick freezing, vacuum freeze drying and heat treatment to obtain the bionic micro-nanofiber aerogel; the mass ratio of PMIA to PAI in the mixed dispersion was 1:3-3:1, a step of; wherein, the mixed dispersion liquid is prepared by respectively preparing PMIA/BMI nanofiber dispersion liquid and PAI/BMI micron fiber dispersion liquid, and then mixing the two; or is prepared by adding PAI/BMI micro-fibers into PMIA/BMI nano-fiber dispersion liquid and then homogenizing and dispersing. The bionic micro-nanofiber aerogel prepared by the invention has super elasticity, excellent heat insulation, high temperature resistance and flame retardance; the preparation method has simple process, green and environment-friendly performance and low cost.
Description
Technical Field
The invention relates to the field of aerogel materials, in particular to meta-aramid/polyamide imide micro-nanofiber aerogel with a bionic structure and a preparation method thereof.
Background
The meta-aramid (PMIA) fiber material has the advantages of high temperature resistance, softness, light weight, electric insulation, high strength and the like, and is widely applied to the fields of high-temperature smoke filtration, electric insulation, flame retardance, heat insulation and the like. It is notable that meta-aramid (PMIA) as a flexible polymer has a breaking strength higher than that of common polyester, cotton, nylon, etc., and has a large elongation, soft hand feeling, good spinnability, excellent flame retardance, high temperature resistance, and excellent durability, and can be considered as a raw material for preparing aerogel with soft and comfortable properties and thermal properties. CN114481680A is prepared into an ultrafine meta-aramid fiber film and a sponge by a solution blowing gas spinning method, and the prepared ultrafine meta-aramid fiber film and sponge are desalted and dealkalized, suspension slurry is prepared, and vacuum freeze-drying is carried out to obtain ultrafine meta-aramid aerogel; the prepared superfine meta-aramid aerogel keeps a fluffy structure and has good heat insulation performance, but has weaker microstructure, easy compression deformation and poorer elasticity.
Disclosure of Invention
Aiming at the defects in the prior art, the invention discloses a bionic micro-nanofiber aerogel and a preparation method thereof, wherein the preparation method combines electrostatic spinning, homogeneous dispersion, freeze drying and heat treatment, and the prepared meta-aramid/polyamide imide micro-nanofiber aerogel with a semi-interpenetrating bionic structure has excellent heat insulation performance, superelasticity, high temperature resistance and flame retardance.
In order to achieve the technical aim, in one aspect, the invention provides a preparation method of bionic micro-nanofiber aerogel, which takes PMIA/BMI nanofiber and PAI/BMI nanofiber as raw materials to prepare mixed dispersion liquid, and the mixed dispersion liquid is subjected to quick freezing, vacuum freeze drying and heat treatment to obtain the bionic micro-nanofiber aerogel; the mass ratio of PMIA to PAI in the mixed dispersion liquid is 1:3-3:1, a step of; wherein, the mixed dispersion liquid adopts:
s1, uniformly dispersing PMIA/BMI nano-fibers in a first alcohol solvent to prepare PMIA/BMI nano-fiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in a second glycol solvent to prepare PAI/BMI microfiber dispersion; s3, mixing the PMIA/BMI nanofiber dispersion liquid and the PAI/BMI micro fiber dispersion liquid to obtain a mixed dispersion liquid;
or adopts the following steps:
s1, uniformly dispersing PMIA/BMI nano-fibers in a first alcohol solvent to prepare PMIA/BMI nano-fiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in the PMIA/BMI nanofiber dispersion liquid to prepare the mixed dispersion liquid.
In order to fully exert the excellent flexibility and thermal performance of meta-aramid, the technical scheme of the invention respectively prepares functional meta-aramid/Bismaleimide (BMI) nanofibers and functional polyamide imide (PAI)/BMI microfibers through an electrostatic spinning technology, then obtains unreinforced aerogel of micro-nanofiber aerogel through a homogenizing dispersion and freeze drying process, and then forms a semi-interpenetrating polymer network between bismaleimide and polyamide imide and between bismaleimide and meta-aramid through heat treatment, so that cross-linking structure occurs among the micro-nanofibers, and the bionic micro-nanofiber aerogel is obtained. A Scanning Electron Microscope (SEM) analysis shows that the PMIA nanofiber and the PAI microfiber respectively form a semi-interpenetrating bionic luffa structure under the action of a crosslinking agent BMI, and the PMIA/PAI micro-nanofiber are crosslinked to form a bionic clove leaf vein structure.
In the technical scheme, the high-temperature-resistant cross-linking agent bismaleimide, meta-aramid and polyamide imide are dissolved by adopting an organic solvent to prepare the corresponding spinning solution. As a further scheme, in order to improve the quality and performance of meta-aramid nanofibers and polyamide-imide microfibers prepared by electrospinning, the research and development team explores and optimizes the content of meta-aramid and bismaleimide in the prepared meta-aramid spinning solution, the content of polyamide-imide and bismaleimide in the prepared polyamide-imide spinning solution, and the types of organic solvents used.
As a further scheme, the fiber diameter of the prepared meta-aramid nanofiber is 140-514nm.
As a further scheme, the fiber diameter of the prepared polyamide-imide microfiber is 847-2081nm.
As a further approach, the research and development team explored and optimized the aspect ratio of PMIA/BMI nanofibers in the PMIA/BMI nanofiber dispersion; the aspect ratio of the PAI/BMI microfibers in the mixed dispersion was further explored and optimized.
As a further scheme, the research and development team of the invention explores and optimizes the dispersion solvent used in the step (1), wherein the first alcohol solvent and the second alcohol solvent are respectively and independently selected from tertiary butanol or tertiary butanol aqueous solution; wherein the tertiary butanol aqueous solution is tertiary butanol aqueous solution with the tertiary butanol content w being more than or equal to 20wt% and less than 100 wt%.
On the other hand, the invention provides the meta-aramid/polyamideimide micro-nanofiber aerogel with the bionic structure, which is prepared by the preparation method.
Compared with the prior art, the preparation method of the bionic micro-nanofiber aerogel introduces polyamide imide/bismaleimide microfibers into the meta-aramid nanofiber aerogel, promotes the hydrogen bonding action among the meta-aramid nanofibers and the thermal polymerization crosslinking action of the bismaleimide in the meta-aramid nanofibers and the polyamide imide microfibers through freeze drying and heat treatment processes, so that sufficient connection nodes are formed among the microfibers and the microfibers, between the microfibers and the nanofibers and between the nanofibers and the nanofibers, and a unique network structure of the prepared bionic micro-nanofiber aerogel is endowed, namely a microstructure of micro-nanofiber cross-linking and rigid-flexible coupling; the prepared bionic micro-nanofiber aerogel has ultra-light weight, super elasticity, excellent heat insulation performance, high temperature resistance and flame retardance, and widens the application range of meta-aramid nanofiber materials; the preparation method has the advantages of simple process flow, environmental protection and low cost.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is an electron microscope topography of PMIA/BMI nanofibers prepared from the spinning solutions of different PMIA concentrations of example 2;
FIG. 2 is an electron microscope topography of PAI/BMI microfibers prepared from spinning solutions of different PAI concentrations of example 3;
FIG. 3 is a graph showing the comparison of the state of the PMIA/BMI nanofiber dispersion and the mixed dispersion according to example 4 at different homogenization times;
FIG. 4 is a graph of the macro topography of the aerogels of examples 5.1-5.3, comparative examples 5.1-5.2;
FIG. 5 is a graph of the microscopic morphology of aerogels prepared in comparative example 5.1, example 5.2, and comparative example 5.2;
FIG. 6 is a graph of thermal conductivity versus the aerogels of examples 5.1-5.3, comparative examples 5.1-5.2;
FIG. 7 is a stress-strain curve for the aerogels of examples 5.1-5.3, comparative examples 5.1-5.2 at 60% strain;
FIG. 8 is a stress-strain curve of the biomimetic micro-nanofiber aerogel of example 5.2 under a range of strains;
FIG. 9 shows the fatigue resistance test results of the bionic micro-nanofiber aerogel of example 5.2;
fig. 10 shows the flame retardant performance test procedure of the bionic micro-nanofiber aerogel of example 5.2.
Detailed Description
In order that the invention may be understood more fully, a more particular description of the invention will be rendered by reference to preferred embodiments thereof. It should be understood that these examples are for the purpose of more detailed description only and should not be construed as limiting the invention in any way, i.e., not limiting the scope of the invention.
Example 1
The preparation method of the meta-aramid/polyamide imide micro-nanofiber aerogel with the bionic structure comprises the steps of preparing mixed dispersion liquid by taking PMIA/BMI nanofibers and PAI/BMI microfibers as raw materials, and obtaining the bionic micro-nanofiber aerogel through quick freezing, vacuum freeze drying and heat treatment of the mixed dispersion liquid; the mass ratio of PMIA to PAI in the mixed dispersion liquid is 1:3-3:1, a step of; wherein, the mixed dispersion liquid adopts:
s1, uniformly dispersing PMIA/BMI nano-fibers in a first alcohol solvent to prepare PMIA/BMI nano-fiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in a second glycol solvent to prepare PAI/BMI microfiber dispersion; s3, mixing the PMIA/BMI nanofiber dispersion liquid and the PAI/BMI micrometer fiber dispersion liquid to obtain a mixed dispersion liquid;
or adopts the following steps:
s1, uniformly dispersing PMIA/BMI nano-fibers in a first alcohol solvent to prepare PMIA/BMI nano-fiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in the PMIA/BMI nanofiber dispersion liquid to prepare the mixed dispersion liquid.
Optionally, the mass ratio of PMIA to PAI in the mixed dispersion is 1:1.
alternatively, the PMIA/BMI nanofiber is prepared by an electrostatic spinning process, which comprises the steps of dissolving PMIA and BMI in N, N-dimethylacetamide to obtain PMIA/BMI spinning solution, and then preparing the PMIA/BMI nanofiber by an electrostatic spinning device; wherein the concentration of PMIA in the PMIA/BMI spinning solution is 12wt% to 18wt%.
Note that parameters for preparing PMIA/BMI nanofibers by using the electrospinning process were optimized in this example: the syringe can be 10ml or 20ml, and the needle can be 20G, 21G or 22G; the speed of the injection pump is 0.3-0.8ml/L, the spinning voltage is 16-25kV, the receiving distance is 14-20cm, and the rotating speed of the receiving roller is 40-100rpm.
Optionally, the diameter of the PMIA/BMI nanofiber in the PMIA/BMI nanofiber dispersion is 140-514nm.
Alternatively, the PAI/BMI microfibers are prepared by an electrospinning process comprising dissolving PAI and BMI in an organic solvent to obtain a PAI/BMI spinning solution, and then preparing the PAI/BMI microfibers by an electrospinning device; wherein the PAI concentration in the PAI/BMI spinning solution is 22wt% to 28wt%, and the organic solvent comprises dimethyl sulfoxide (DMSO), N-dimethylacetamide (DMAc), N-Dimethylformamide (DMF) or N-methylpyrrolidone (NMP).
Note that parameters for preparing PAI/BMI microfibers using the electrospinning process were optimized in this example: the syringe can be 10ml or 20ml, and the needle can be 20G, 21G or 22G; the speed of the injection pump is 0.2-0.5 ml/L, the voltage is 8.3-14.3 kV, the receiving distance is 18-22 cm, and the rotation number of the receiving roller is 60-100 rpm.
Optionally, the diameter of the microfibers in the PAI/BMI microfibers is 847-2081nm.
It should be noted that the temperature and humidity conditions of the electrostatic spinning are not limited in this embodiment, and the electrostatic spinning may be performed under the conditions of 25±5 ℃ and 25±5% of temperature and humidity.
Based on extensive research experiments, the mixed dispersion in this example may be prepared by the method one: firstly, respectively preparing PMIA/BMI nanofiber dispersion liquid and PAI/BMI micrometer fiber dispersion liquid, and then mixing the two dispersion liquids to prepare mixed dispersion liquid, namely S1, homogenizing and dispersing PMIA/BMI nanofiber in a first alcohol solvent to prepare PMIA/BMI nanofiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in a second glycol solvent to prepare PAI/BMI microfiber dispersion; s3, mixing the PMIA/BMI nanofiber dispersion liquid and the PAI/BMI micro fiber dispersion liquid to obtain a mixed dispersion liquid; a second method may also be employed: firstly preparing PMIA/BMI nanofiber dispersion liquid, then adding PAI/BMI microfibers into the PMIA/BMI nanofiber dispersion liquid for homogenizing and dispersing to prepare mixed dispersion liquid, namely S1, homogenizing and dispersing the PMIA/BMI nanofiber in a first alcohol solvent to prepare PMIA/BMI nanofiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in the PMIA/BMI nanofiber dispersion liquid to prepare the mixed dispersion liquid.
It should be noted that in this embodiment, the operation condition for homogeneously dispersing the PMIA/BMI nanofiber is not limited, and optionally, the operation of homogeneously dispersing the PMIA/BMI nanofiber dispersion liquid is performed in a homogenizing and dispersing machine, the rotation speed of the homogenizing and dispersing machine is 15000-20000 r/min, and the homogenizing time is 5-15min. In this embodiment, the operation conditions for homogeneously dispersing the PAI/BMI microfibers are not limited, and optionally, the operation of homogeneously dispersing the PAI/BMI microfiber dispersion liquid in a homogenizing and dispersing machine is performed, wherein the homogenizing time is 30-60 s, and 10000-15000 r/min.
When the second method is adopted to prepare the mixed dispersion liquid, 10000-15000 r/min can be adopted to homogenize the PAI/BMI micro-fiber into the PMIA/BMI nano-fiber dispersion liquid for about 30-60 s, namely, lower rotating speed and homogenization time are adopted in preparation of the PMIA/BMI nano-fiber dispersion liquid, so that the mixed dispersion liquid is obtained.
It is further noted that when preparing the hybrid dispersion by method two, the PAI/BMI microfibers or fiber films may be cut into smaller film fragments (e.g., 1cm x 1cm film fragments, 1.5cm x 1.5cm film fragments, or irregularly sized film fragments, etc.), and then the film fragments may be added directly to the PMIA/BMI nanofiber dispersion for homogeneous dispersion, or the film fragments may be dispersed in a second solvent, and then mixed and homogeneously dispersed with the PMIA/BMI nanofiber dispersion.
Alternatively, the first alcohol solvent and the second alcohol solvent are respectively and independently selected from tertiary butanol or tertiary butanol aqueous solution. According to contact angle tests, the research and development team discovers that PMIA/BMI nanofibers and PAI/BMI microfibers prepared by an electrostatic spinning process have different wettability in tertiary butanol or tertiary butanol aqueous solutions with different concentrations, so that in the preparation process of a specific mixed dispersion liquid, proper first alcohol solvents and second alcohol solvents can be respectively selected for infiltrating the PMIA/BMI nanofibers and the PAI/BMI microfibers. In practical operation, the first alcohol solvent and the second alcohol solvent may be tertiary butanol, or tertiary butanol aqueous solutions with the same concentration, or tertiary butanol with different tertiary butanol contents, or tertiary butanol aqueous solutions respectively.
Optionally, the PMIA/BMI nanofibers in the PMIA/BMI nanofiber dispersion have an aspect ratio of 179.28 to 371.57.
Further alternatively, the PAI/BMI microfibers in the mixed dispersion have an aspect ratio of 16.29 to 39.52.
Optionally, the temperature of quick freezing is-25 ℃, the freezing time is 6-24h, and vacuum freeze drying is carried out after the freezing is finished; the vacuum freeze drying condition is about-40 ℃ and the freeze drying is carried out for 24-96 h under the vacuum environment of 4 Pa.
Optionally, the temperature of the heat treatment operation is 180-220 ℃, and further optionally 200 ℃; the heat treatment time is 0.5-3h.
Example 2
Based on the preparation method of the bionic micro-nanofiber aerogel shown in the embodiment 1, the embodiment explores and optimizes the addition amount of the meta-aramid spinning solution intermediate aramid. It should be noted that the specific process flow shown in this embodiment is only shown in a preferred manner, and the protection scope of the present invention is not limited thereby.
Specifically, in the embodiment, meta-aramid stock solution, bismaleimide and N, N-dimethylacetamide are sequentially added into a glass container, stirred for 3-5 hours in a water bath kettle at 50-70 ℃, then kept still for eliminating bubbles, and 4 groups of meta-aramid spinning solutions with the mass fractions of 12wt%, 14wt%, 16wt% and 18wt% of meta-aramid are obtained, and the mass fractions of bismaleimide are 2.4wt%, 2.8wt%, 3.2wt% and 3.6wt% of the 4 groups of meta-aramid spinning solutions. Optionally, the meta-aramid stock solution used in the embodiment includes N, N-dimethylacetamide and meta-aramid in a mass ratio of 80:20.
and then respectively pouring the obtained 4 groups of meta-position aramid spinning solutions with different concentrations into 10ml needle tube injectors, and carrying out electrostatic spinning by adopting a 22G needle head, wherein the parameters of the electrostatic spinning are as follows: the spinning voltage was 19kV, the receiving distance was 20cm, the number of revolutions of the collecting roller was 100rpm, the boosting speed was 0.3ml/h, and the spinning was performed at a temperature of 25.+ -. 5 ℃ and a humidity of 30.+ -. 10%.
FIG. 1 shows a scanning electron microscope image of meta-aramid nanofibers prepared using different concentrations of meta-aramid spinning solutions. The appearance of the nanofiber under the scanning electron microscope is observed through comparison: when the mass fraction of the meta-aramid fiber of the spinning solution is 12wt%, the prepared nanofiber forms beads and the fiber diameter is uneven; when the mass fraction of the meta-aramid fiber of the spinning solution is 14wt%, the prepared nanofiber has smaller diameter and no obvious entanglement phenomenon; when the mass fraction of the meta-aramid fiber of the spinning solution is 16wt%, the appearance of the prepared nanofiber is obviously improved, the diameter distribution is uniform, the thickness is moderate, and the phenomena of broken ends and entanglement are few; when the mass fraction of the spinning solution is 18wt%, the prepared nanofibers are loose in distribution and uniform in thickness. Therefore, the PMIA concentration in the PMIA/BMI spinning solution in the technical scheme of the invention can be selected to be 12-18 wt%, and further can be selected to be 14-18 wt%. The PMIA concentration in the PMIA/BMI spinning solution is further selected to be 16wt percent by comprehensively considering that the higher concentration of meta-aramid leads to higher viscosity of the spinning solution and leads to difficult extrusion during spinning operation.
Further, the diameter of the nanofiber prepared by the spinning solution with the mass fraction of the meta-aramid fiber of 16wt% and 18wt% is measured by the fiber diameter, so that the diameter of the nanofiber in the PMIA/BMI nanofiber is 140-514nm.
Example 3
Based on the preparation method of the bionic micro-nanofiber aerogel shown in the embodiment 1, the embodiment explores and optimizes the addition amount of PAI at the middle position of the prepared PAI/BMI spinning solution. It should be noted that the specific process flow shown in this embodiment is only shown in a preferred manner, and the protection scope of the present invention is not limited thereby.
Specifically, PAI powder with molecular weight of 200000 is adopted in a glass container during preparation, then solvent DMSO and BMI powder are added, the PAI mass is set to be 22wt%, 25wt% and 28wt%, and the BMI concentration is respectively 4.4wt%, 5wt% and 5.6wt% of PAI/BMI spinning solution with three different concentrations; and (3) stirring for 3-5 hours at the temperature of 50-80 ℃ in a constant-temperature water bath kettle after mixing to obtain the PAI/BMI spinning solution. The PAI/BMI microfibers were obtained by spinning at a spinning voltage of 11.31kV, a flow rate of 0.5ml/h, a receiving distance of 18cm, a receiving roll revolution of 60rpm, a temperature and humidity of 25℃and 30.+ -. 5%.
FIG. 2 shows a scanning electron microscope image of PAI/BMI microfibers prepared using PAI spin solutions at different concentrations, and the morphology of the microfibers was observed by contrast observation scanning electron microscope: when the PAI concentration in the spinning solution is 22wt%, the viscosity of the spinning solution is lower, the sprayed fiber is relatively thin, and the phenomenon of drop-shaped and spider silk broken ends is easy to form; with the increase of the mass fraction, the fiber can be fully stretched, when the mass fraction is 25wt%, the appearance of the PAI fiber is obviously improved, the fiber diameter distribution is uniform, the thickness is moderate, and no obvious broken ends and entanglement phenomenon exist; when the mass fraction is 28wt%, the PAI fibers are loosely distributed and have uniform thickness. Therefore, the PAI concentration in the PAI/BMI spinning solution in the technical scheme of the invention can be 22wt% to 28wt%, and further can be 25wt%.
Further, the diameter of the microfibers prepared from the spinning solution with PAI concentration of 25wt% and 28wt% is measured by the fiber diameter, and the diameter of the microfibers in the PAI/BMI microfibers is 847-2081nm.
Example 4
Based on the preparation method of the bionic micro-nanofiber aerogel shown in the embodiment 1, the embodiment explores and optimizes the length-diameter ratio of PMIA/BMI nanofibers in the PMIA/BMI nanofiber dispersion liquid and the length-diameter ratio of PAI/BMI microfibers in the mixed dispersion liquid.
In this example, PMIA/BMI nanofibers prepared from a spinning solution having a mass fraction of PMIA of 16wt% were cut into pieces of about 1X 1cm, 0.5g was placed in 100ml of a tertiary butanol aqueous solution (first alcohol solvent), and the pieces were homogeneously dispersed at a speed of 15000 to 20000r/min using a high-speed homogenizer, and the state of the dispersion at different homogeneously dispersing times was as shown in (1) to (4) in FIG. 3.
Observe the homogeneous state of PMIA/BMI nanofibers: the state of the PMIA/BMI nanofiber before homogenization is as in (1) of fig. 3; when homogenized for 6min (fig. 3 (2)), the nanofibers are completely homogenized into dispersed nanofibers, but at this time, the aspect ratio of the nanofibers is large, and entanglement occurs between the nanofibers, resulting in uneven dispersion; when homogenized for 12min (3) in fig. 3, the length-diameter ratio of the nanofiber is further reduced after high-speed homogenization, so that the entangled nanofiber is uniformly dispersed, and the length-diameter ratio range of the PMIA/BMI nanofiber is 179.28-371.57 according to the electron microscope image of 3 in fig. 3.
Further, in this example, a mixed dispersion was prepared by the method shown in method two, 0.5g of PAI/BMI microfibers prepared from a spinning solution having a PAI mass fraction of 25wt% was placed in 100ml of a tertiary butanol aqueous solution (a second type solvent), then added to the PMIA/BMI nanofiber dispersion, homogenized at a rotational speed of 10000 to 15000r/min for 60 seconds, and then the PAI/BMI microfibers were uniformly dispersed (FIG. 3 (4)), and the aspect ratio of the PAI/BMI microfibers in the mixed dispersion was 16.29 to 39.52 by an electron microscopic image; the PMIA/BMI nanofiber aspect ratio was substantially unchanged. The prepared micro-nano fiber mixed dispersion liquid is used for preparing the follow-up micro-nano fiber aerogel.
Note that the first alcohol solvent and the second alcohol solvent used in this example were both 40wt% aqueous t-butanol solutions.
Note that in this example, after the completion of the homogeneous dispersion operation, the dispersed material was transferred to a reagent bottle for photographing recording, and fig. 3 was not intended to characterize the relationship between the raw materials or the ratio of the raw materials to the solvent.
Example 5
Based on the preparation method of the bionic micro-nanofiber aerogel shown in the embodiment 1, the mass ratio of PMIA to PAI in the mixed dispersion liquid is explored and optimized.
Specifically, this example uses the method shown in method one to prepare a mixed dispersion:
s1, uniformly dispersing 0.5g PMIA/BMI nanofiber prepared from a spinning solution with the mass fraction of PMIA of 16wt% in 100ml of 40wt% tertiary butanol aqueous solution to obtain PMIA/BMI nanofiber dispersion.
S2, uniformly dispersing 0.5g of PAI/BMI microfibers prepared from the spinning solution with the mass fraction of PAI of 22wt% in 100ml of 40wt% tertiary butanol aqueous solution to obtain PAI/BMI microfiber dispersion.
S3, using the volume ratio of the two dispersions as variables, mixed dispersions (marked as comparative examples 5.1, 5.2, 5.3 and 5.2) of PMIA/BMI nanofiber dispersion and PAI/BMI microfiber dispersion with the volume ratio of 100:0, 75:25, 50:50, 25:75 and 0:100 are respectively prepared.
10ml of the mixed dispersion of the above examples and comparative examples was placed in a cylindrical mold having a diameter of 3cm, frozen at-25℃for 6 hours, then vacuum-dried by a freeze dryer for 48 hours, and heat-treated at 200℃for 2 hours to give the micro-nanofiber super-elasticity.
FIG. 4 shows the macroscopic morphologies of the aerogels prepared in examples 5.1-5.3, and comparative examples 5.1-5.2. As can be seen from FIG. 4, although the shrinkage of the resulting aerogel was different due to the difference in mass ratio of PMIA to PAI in the mixed dispersion by the same process and heat treatment, the PAI/BMI nanofiber had better high temperature resistance than the PMIA/BMI nanofiber, and the PMIA/BMI nanofiber aerogel (comparative example 5.1) had more significant shrinkage while the PAI nanofiber aerogel (comparative example 5.2) had no significant shrinkage under heat treatment at 200 ℃.
Fig. 5 shows the microstructure and crosslinked structure of aerogels prepared in comparative example 5.1, example 5.2, and comparative example 5.2. The microstructure and cross-linked structure are affected by at least 3 factors:
1) In the aerogel preparation process shown in the embodiment, tertiary butanol aqueous solution is used as PAI/PMIA micro-nano fiber dispersion liquid, ice crystals are formed in all directions by the tertiary butanol aqueous solution during quick freezing, and then the ice crystals are sublimated through vacuum drying to form a large number of secondary holes;
2) As shown in comparative example 5.1 of fig. 5, after the fibers of the secondary pore walls are subjected to heat treatment, BMI monomer small molecules in the PMIA/BMI nanofiber undergo polymerization reaction, and a crosslinked structure is formed on the surface between the nanofibers, so that not only the secondary pore walls are reinforced, but also macroscopic superelasticity of the PMIA/BMI nanofiber aerogel is provided. Correspondingly, as shown in comparative example 5.2 of fig. 5, the PAI/BMI microfibers form a semi-interpenetrating polymer network and a crosslinked structure under heat treatment, reinforcing the secondary pore walls of the PAI/BMI microfiber aerogel; in examples 5.1-5.3, a biomimetic loofah structure was formed.
3) As shown in example 5.2 of FIG. 5, a crosslinked structure occurred between PMIA/PAI micro-nanofibers. As the meta-aramid fiber has a flexible molecular chain performance due to a special molecular structure, as the rigidity of the micro-fiber is far higher than that of the nano-fiber, the development team of the invention is inspired by the thick and thin veins of the clove leaf to prepare the PMIA/PAI micro-nano fiber, and compared with the PMIA nano fiber, the bionic micro-nano fiber aerogel shown in the embodiment 5.2 forms a rigid and flexible coupling structure, and has better mechanical property, thereby widening the application scene and the field of the meta-aramid fiber nano fiber material.
The thermal conductivity of the aerogels of examples 5.1 to 5.3 and comparative examples 5.1 to 5.2 was further tested in this example, specifically, 5501 probe model was selected for the thermal constant analyzer model (Hot Disk TPS 3500), and the thermal conductivity of the aerogel was measured at room temperature (25 ℃).
As shown in fig. 6, the aerogels of comparative example 5.1 and example 5.1 have higher thermal conductivity, 34.26 and 33.87 mW/m-K, respectively, and their high thermal conductivity is due to excessive aggregation of PMIA nanofibers, and it is seen in connection with fig. 4 that the shrinkage of both is significantly greater than other aerogels, which may be the main cause of their higher thermal conductivity. It is noted that, instead of the lower content of PMIA nanofibers in the aerogel, the lower the thermal conductivity, when the micro-nanofiber mass ratio is 1: the aerogel of example 5.2 had a moderate pore size and a small shrinkage, and a thermal conductivity of 31.73 mW/mK, i.e., a better insulation performance.
This example further tests the mechanical properties of the aerogels of examples 5.1-5.3, comparative examples 5.1-5.2.
Specifically, a series of compression tests were performed in this example. FIG. 7 shows stress-strain curves for the aerogels of examples 5.1-5.3, and comparative examples 5.1-5.2 at 60% strain. The results show that the stress of the bionic micro-nanofiber aerogels of examples 5.1-5.3 is greater than that of the aerogels of comparative examples 5.1 and 5.2, and the stress of the bionic micro-nanofiber aerogel of example 5.2 is the largest.
Examples 5.1-5.3 bionic micro-nanofiber aerogels when subjected to compressive loading, the resulting cross-linking points between PMIA/BMI nanofibers, between PMIA/BMI nanofibers and PAI/BMI microfibers, between PAI/BMI microfibers, impart high PMIA-50 stress. Although the PAI/BMI microfibers were rigid, since the aspect ratio of the PAI/BMI microfibers was much lower than that of the PMIA/BMI nanofibers, the adjacent PAI microfibers had fewer cross-links when cross-linked, and low cross-linking was detrimental to stress transfer resulting in lower stress in the aerogel of comparative example 5.2. In addition, since the shrinkage of the aerogel of comparative example 5.1 was higher than that of the aerogel of comparative example 5.2, the maximum stress of comparative example 5.1 was slightly higher than that of the aerogel of comparative example 5.2.
This example further tested the elasticity of the biomimetic micro-nanofiber aerogel of example 5.2.
Specifically, fig. 8 shows a stress-strain relationship curve of the bionic micro-nanofiber aerogel of example 5.2 under a series of strains ranging from 40% to 80%. The maximum stress was 0.388kPa when the strain was 40%, and 2.052kPa when the strain was 80%; when epsilon (strain) is less than or equal to 18 percent, the elastic region is a linear elastic region; when 18 < epsilon is less than or equal to 60 percent, the platform area is formed; when epsilon > 60%, the stress value increases rapidly with increasing strain, which is a dense region. Notably, the biomimetic micro-nanofiber aerogel of example 5.2 was compressed at 80% strain, and was almost restored to the original height after the external force was removed, showing excellent superelastic properties.
This example further tested the fatigue resistance of the bionic micro-nanofiber aerogel of example 5.2.
Specifically, fig. 9 shows the results of 1000 load-unload fatigue-resistant compression tests on the bionic micro-nanofiber aerogel of example 5.2: when the strain is 50%, the loading rate is 12mm/min, only 12.5% plastic deformation is generated after 1000 compression, the maximum stress retention rate is 84.21%, and the bionic micro-nano fiber aerogel has good compression recovery performance and can be used for a long time.
This example further tested the flame retardant properties of the biomimetic micro-nanofiber aerogel of example 5.2.
The specific flame retardant performance demonstration process is shown in fig. 10: the bionic micro-nanofiber aerogel of example 5.2 did not burn when contacted with high temperature flame, exhibiting excellent flame retardant properties; in addition, the bionic micro-nano fiber aerogel in the embodiment 5.2 shows rapid self-extinguishing performance after being separated from flame, and can effectively avoid fire hazard in practical application.
It should be noted that the above description of the present invention is further detailed in connection with specific embodiments, and it should not be construed that the present invention is limited to the specific embodiments; the data illustrated in this embodiment is not limited to this embodiment, but only shows one specific working condition. It will be apparent to those skilled in the art that several simple modifications and adaptations of the invention can be made without departing from the spirit of the invention and are intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the bionic micro-nanofiber aerogel is characterized by taking PMIA/BMI nanofibers and PAI/BMI microfibers as raw materials to prepare mixed dispersion liquid, and obtaining the bionic micro-nanofiber aerogel through quick freezing, vacuum freeze drying and heat treatment of the mixed dispersion liquid; the mass ratio of PMIA to PAI in the mixed dispersion liquid is 1:3-3:1, a step of; wherein, the mixed dispersion liquid adopts:
s1, uniformly dispersing PMIA/BMI nano-fibers in a first alcohol solvent to prepare PMIA/BMI nano-fiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in a second glycol solvent to prepare PAI/BMI microfiber dispersion; s3, mixing the PMIA/BMI nanofiber dispersion liquid and the PAI/BMI micro fiber dispersion liquid to obtain a mixed dispersion liquid;
or adopts the following steps:
s1, uniformly dispersing PMIA/BMI nano-fibers in a first alcohol solvent to prepare PMIA/BMI nano-fiber dispersion liquid; s2, uniformly dispersing the PAI/BMI microfibers in the PMIA/BMI nanofiber dispersion liquid to prepare the mixed dispersion liquid.
2. The method for preparing the bionic micro-nanofiber aerogel according to claim 1, wherein the mass ratio of PMIA to PAI in the mixed dispersion liquid is 1:1.
3. the method for preparing the bionic micro-nanofiber aerogel according to claim 1, wherein the PMIA/BMI nanofiber is prepared by an electrostatic spinning process, comprising dissolving PMIA and BMI in N, N-dimethylacetamide to obtain a PMIA/BMI spinning solution, and then preparing the PMIA/BMI nanofiber by an electrostatic spinning device; wherein the concentration of PMIA in the PMIA/BMI spinning solution is 12wt% to 18wt%.
4. The method for preparing the bionic micro-nanofiber aerogel according to claim 1, wherein the PAI/BMI microfiber is prepared by an electrostatic spinning process, comprising dissolving PAI and BMI in an organic solvent to obtain a PAI/BMI spinning solution, and then preparing the PAI/BMI microfiber by an electrostatic spinning device; wherein the PAI concentration in the PAI/BMI spinning solution is 22-28 wt%, and the organic solvent comprises dimethyl sulfoxide, N-dimethylformamide, N-methylpyrrolidone or N, N-dimethylacetamide.
5. The method for preparing a bionic micro-nanofiber aerogel according to claim 1, wherein the diameter of the nanofiber in the PMIA/BMI nanofiber is 140-514nm.
6. The method for preparing the bionic micro-nanofiber aerogel according to claim 1, wherein the diameter of the micro-fibers in the PAI/BMI micro-fibers is 847-2081nm.
7. The method for preparing a bionic micro-nanofiber aerogel according to claim 1, wherein the length-diameter ratio of the PMIA/BMI nanofiber in the PMIA/BMI nanofiber dispersion liquid is 179.28-371.57.
8. The method for preparing a bionic micro-nanofiber aerogel according to claim 7, wherein the aspect ratio of PAI/BMI microfibers in the mixed dispersion is 16.29-39.52.
9. The method for preparing a bionic micro-nanofiber aerogel according to claim 1, wherein the first alcohol solvent and the second alcohol solvent are respectively and independently selected from tertiary butanol or tertiary butanol aqueous solution.
10. A biomimetic micro-nanofiber aerogel prepared by the method of any one of claims 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311422370.XA CN117143390B (en) | 2023-10-31 | 2023-10-31 | Bionic micro-nanofiber aerogel and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311422370.XA CN117143390B (en) | 2023-10-31 | 2023-10-31 | Bionic micro-nanofiber aerogel and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117143390A CN117143390A (en) | 2023-12-01 |
| CN117143390B true CN117143390B (en) | 2024-01-26 |
Family
ID=88912435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311422370.XA Active CN117143390B (en) | 2023-10-31 | 2023-10-31 | Bionic micro-nanofiber aerogel and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117143390B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2933477A1 (en) * | 2013-12-23 | 2015-08-06 | Cytec Industries Inc. | Carbon fibers and high performance fibers for composite applications |
| CN107099117A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of fibre-reinforced aerogel-polymer composites and preparation method thereof |
| CN111116974A (en) * | 2019-12-30 | 2020-05-08 | 东华大学 | Nylon nanofiber aerogel material for air filtration and preparation method thereof |
| CN114350010A (en) * | 2022-01-19 | 2022-04-15 | 中原工学院 | Nanofiber-reinforced polyimide composite aerogel with semi-interpenetrating network structure and preparation method thereof |
-
2023
- 2023-10-31 CN CN202311422370.XA patent/CN117143390B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2933477A1 (en) * | 2013-12-23 | 2015-08-06 | Cytec Industries Inc. | Carbon fibers and high performance fibers for composite applications |
| CN107099117A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of fibre-reinforced aerogel-polymer composites and preparation method thereof |
| CN111116974A (en) * | 2019-12-30 | 2020-05-08 | 东华大学 | Nylon nanofiber aerogel material for air filtration and preparation method thereof |
| CN114350010A (en) * | 2022-01-19 | 2022-04-15 | 中原工学院 | Nanofiber-reinforced polyimide composite aerogel with semi-interpenetrating network structure and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117143390A (en) | 2023-12-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6205351B2 (en) | Process for the production of lignin-containing precursor fibers and also carbon fibers | |
| Zhang et al. | Achieving all-polylactide fibers with significantly enhanced heat resistance and tensile strength via in situ formation of nanofibrilized stereocomplex polylactide | |
| JP4647680B2 (en) | Easy-dyeing meta-type wholly aromatic polyamide fiber | |
| Yao et al. | Morphology and properties of cellulose/silk fibroin blend fiber prepared with 1-butyl-3-methylimidazolium chloride as solvent | |
| CN111235943B (en) | Preparation method of heterocyclic aramid paper | |
| JP2007262589A (en) | Easily-dyeable meta aromatic amide fiber and method for producing the same | |
| Zhang et al. | Fabrication of a high-toughness polyurethane/fibroin composite without interfacial treatment and its toughening mechanism | |
| CN117143390B (en) | Bionic micro-nanofiber aerogel and preparation method thereof | |
| JP2009120976A (en) | Easily dyeable meta-type wholly aromatic polyamide fiber | |
| Wu et al. | Cellulose/aromatic polysulfonamide blended fibers with improved properties | |
| CN107435171B (en) | A kind of preparation method of cross-linked structure orientation filling enhancing chemical fibre | |
| Fukae et al. | Gel-spinning and drawing of gelatin | |
| Mao et al. | Effects of coagulation conditions on properties of multifilament fibers based on dissolution of cellulose in NaOH/urea aqueous solution | |
| CN113718369B (en) | Method for constructing ultra-light polyurethane aerogel fiber through polymer nanofiber | |
| WO2021255957A1 (en) | Method for producing polyamide 4 fiber | |
| Wang et al. | Effect of the draw ratio in dry jet-wet spinning on aromatic copolysulfonamide fibers | |
| Guo et al. | Mechanical enhancement of bi-phasic electrospun nanofibrous films by optimizing composition and configuration | |
| KR102586543B1 (en) | Meta aramid spun yarn having improved physical properties and fabric using the same | |
| JP2013112919A (en) | Para-type wholly aromatic polyamide fiber | |
| KR100499221B1 (en) | Cellulose/Polyvinyl alcohol conjugated fiber | |
| CN117127281A (en) | Bacterial cellulose/polyurethane composite aerogel fiber and preparation method and application thereof | |
| Liu et al. | Effects of superfine silk protein powders on mechanical properties of wet‐spun polyurethane fibers | |
| Zhang et al. | Preparation and properties of novel regenerated cellulose fibers via direct dissolution of cellulose in lioh complex aqueous solution | |
| Lacy et al. | Degradation and Mechanical Behavior of Fish Gelatin/Polycaprolactone AC Electrospun Nanofibrous Meshes | |
| CN117904892A (en) | Preparation method of aramid micro-nano fiber and application of aramid micro-nano fiber in aramid paper |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |