CN114411282B - Preparation method of high-strength skin-core structure porous aerogel fiber, product and application thereof - Google Patents
Preparation method of high-strength skin-core structure porous aerogel fiber, product and application thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 91
- 239000004964 aerogel Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000012530 fluid Substances 0.000 claims abstract description 29
- 238000009987 spinning Methods 0.000 claims abstract description 20
- 239000012792 core layer Substances 0.000 claims abstract description 15
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- 238000001125 extrusion Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 230000001054 cortical effect Effects 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 239000007790 solid phase Substances 0.000 claims abstract description 6
- 239000002952 polymeric resin Substances 0.000 claims abstract description 5
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 5
- 238000007711 solidification Methods 0.000 claims abstract description 3
- 230000008023 solidification Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 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 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 230000015271 coagulation Effects 0.000 claims description 5
- 238000005345 coagulation Methods 0.000 claims description 5
- 238000004146 energy storage Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000003115 biocidal effect Effects 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000010865 sewage Substances 0.000 claims description 4
- 230000000844 anti-bacterial effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000006557 surface reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 2
- 229920001661 Chitosan Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 230000003020 moisturizing effect Effects 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 12
- 239000002657 fibrous material Substances 0.000 abstract description 5
- 238000013035 low temperature curing Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 230000001112 coagulating effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- -1 diamine compound Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000013265 porous functional material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000001891 gel spinning Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003880 polar aprotic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- DQFBYFPFKXHELB-VAWYXSNFSA-N trans-chalcone Chemical group C=1C=CC=CC=1C(=O)\C=C\C1=CC=CC=C1 DQFBYFPFKXHELB-VAWYXSNFSA-N 0.000 description 1
- 229920003176 water-insoluble polymer Polymers 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Abstract
The invention discloses a preparation method and a product of a high-strength skin-core structure porous aerogel fiber and application thereof, wherein the preparation method comprises the steps of adding high polymer resin into a solvent, and uniformly dissolving to prepare core layer fluid; adding the functional components into a high polymer solution, and uniformly dispersing to prepare a cortical fluid; defoaming sheath fluid and core fluid to prepare sheath-core spinning solution; continuously extruding the sheath-core spinning solution into a low-temperature curing system through coaxial extrusion equipment to prepare solid-phase fibers; and (3) immediately freeze-drying the solid-phase fiber after low-temperature solidification to obtain the porous aerogel fiber. The technology can prepare the fibrous material with microscopic open pore structures on the surface and inside of the fiber, and the prepared aerogel fiber ensures rich pore structures and simultaneously endows the aerogel fiber with excellent strength.
Description
Technical Field
The invention belongs to the technical field of functional fibers, and particularly relates to a preparation method and a product of a high-strength skin-core structure porous aerogel fiber and application thereof.
Background
Aerogel fibers have wide applications in the fields of energy storage sensing, heat insulation, wave absorption stealth and the like due to abundant porous structures, and the prominence of the performances of the aerogel fibers in the applications is mostly attributed to the multi-scale microporous structure on the surface of the fibers.
However, the conventional spinning technology can only form a pore structure inside the fiber, and a dense skin layer is often formed outside the fiber, which is not beneficial to the subsequent surface functionalization treatment and application of the fiber, and most aerogel fibers have lower strength, so that the wide application of the fiber is limited.
Patent CN201911221326.6 reports a preparation method of polyimide aerogel fiber, which prepares aerogel fiber with porous structure inside fiber and cortical structure on fiber surface by gel spinning technology, but the prepared aerogel fiber can not realize microporous structure inside and surface.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of the high-strength porous aerogel fiber with a sheath-core structure.
In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing high-strength porous aerogel fiber with a sheath-core structure comprises the steps of,
adding high polymer resin into a solvent, and uniformly dissolving to obtain core layer fluid;
adding the functional components into a high polymer solution, and uniformly dispersing to prepare a cortical fluid;
defoaming sheath fluid and core fluid to prepare sheath-core spinning solution;
continuously extruding the sheath-core spinning solution into a low-temperature curing system through coaxial extrusion equipment to prepare solid-phase fibers;
and (3) immediately freeze-drying the solid-phase fiber after low-temperature solidification to obtain the porous aerogel fiber.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the polymer resin is water-soluble polymer or water-insoluble polymer solution, and comprises polyvinyl alcohol aqueous solution, carboxymethyl cellulose aqueous solution, chitosan acetic acid solution and polyvinyl alcohol dimethyl sulfoxide solution.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the solvent comprises N, N-dimethylformamide, and the mass concentration of the core layer fluid is 12-20%.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the functional components are added into a polymer solution, wherein the polymer solution comprises carboxymethyl cellulose solution, and the functional components comprise a conductive component, an antibacterial component, a flame-retardant component, a fragrance component, a moisturizing component and a beautifying component.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the functional component accounts for 0-80% of the mass of the sheath core layer fluid.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the mass concentration of the cortical fluid is 1-12%.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the defoaming process is 0-0.2 MPa and is constant for 2-12 h.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the sheath-core spinning solution is continuously extruded into a low-temperature curing system through coaxial extrusion equipment, wherein,
extruding the spinning solution into a low-temperature system, and condensing the water solvent in the spinning solution into a micro ice phase under the action of low temperature to solidify the fiber;
the low-temperature system is a liquid nitrogen coagulation bath or low-temperature glycol, polyethylene glycol and ethanol;
the low temperature range is-10 to-196 ℃;
the ratio of the length and the diameter of the extrusion capillary holes is 1-1000, and the extrusion speed is 0.5-8 m/min.
As a preferable scheme of the preparation method of the high-strength sheath-core structure porous aerogel fiber, the preparation method comprises the following steps: the fiber before freeze drying is low temperature frozen fiber, the freeze drying process is-40 ℃, and the vacuum is continuously pumped for 24-96 hours.
The invention further aims to overcome the defects in the prior art and provide an application of a product prepared by the preparation method of the high-strength skin-core structure porous aerogel fiber in the surface functionalization treatment of the aerogel fiber, wherein the application comprises the fields of energy storage, sensing, heat insulation, catalytic reaction, sewage treatment, wave absorption stealth, electrostatic shielding, antibiosis, flame retardance and moisture preservation.
The invention has the beneficial effects that:
(1) The aerogel fiber material with a porous structure is prepared by a liquid phase low temperature spinning technology (Liquid low temperature spinningtechnology, LLTST), and the liquid phase low temperature spinning technology is developed; the prepared aerogel fiber can be used for preparing various light and porous functional materials through chemical reaction or physical coating technology, and has wide application in the fields of energy storage, sensing, heat insulation, catalytic reaction, sewage treatment, wave absorption stealth, electrostatic shielding, antibiosis, flame retardance, moisture preservation, skin care and the like.
(2) The technology can prepare the fibrous material with microscopic open pore structures on the surface and inside of the fiber, and the prepared aerogel fiber ensures rich pore structures and simultaneously endows the aerogel fiber with excellent strength.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a SEM photograph of fibers of example 1 of the present invention.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Strength measurement of aerogel fibers of the invention: shanghai new fiber instruments company XQ-1 type single fiber strength tester, test conditions: the fiber clamping distance was 20mm, the filament clamping weight was 0.25cN, the stretching speed was 20mm/min, and the average value was obtained by 10 tests.
The raw materials in the invention are common commercial products without special description.
Example 1
The embodiment provides a preparation method of a high-strength skin-core structure porous aerogel fiber, which comprises the following steps:
(1) Adding polyvinyl alcohol 2099 resin into N, N-dimethylformamide to be dissolved uniformly, and taking the mixture as a core layer fluid material, wherein the mass concentration of the core layer fluid material is 12%;
(2) Uniformly dispersing a carboxymethyl cellulose solution with the mass concentration of 2% to serve as a cortical fluid;
(3) The sheath core layer fluid is subjected to pressure deaeration for 24 hours under the pressure of 0.2MPa for later use;
(4) Extruding the debubbled sheath-core spinning solution into ethylene glycol coagulating bath at a speed of 8m/min through capillary holes with an aspect ratio of 1 (capillary hole specification length is 0.1 mm and aperture is 0.1 mm), rapidly transferring the fiber after low-temperature coagulation into a low-temperature freeze drying system, and continuously vacuumizing in a vacuum freeze dryer at-40 ℃ for 96 hours to obtain the porous aerogel fiber.
(5) Index parameters: the strength of the aerogel fiber is 1.8cN/dtex, the surface and the inside of the fiber have uniform pore structures, and the micropore diameters are distributed between 200 and 400 nm.
SEM photograph of the fibers, see fig. 1.
Example 2
The embodiment provides a preparation method of a high-strength skin-core structure porous aerogel fiber, which comprises the following steps:
(1) Adding polyvinyl alcohol 1788 resin into dimethyl sulfoxide to be dissolved uniformly, and taking the mixture as a core layer fluid material, wherein the mass percentage concentration of the core layer fluid material is 20wt%;
(2) Preparing a composite skin fluid, wherein the mass percentage of the nano silver antibacterial component is 20%, the mass percentage of the carboxymethyl cellulose is 1%, and the water is 79%;
(3) Standing the skin-core layer fluid for 2 hours under the pressure of 0.1Mpa for later use;
(4) Extruding the sheath-core spinning solution with bubble removed into a liquid nitrogen coagulating bath at a speed of 1m/min through capillary holes with an aspect ratio of 500 (capillary hole specification length is 30 mm, and aperture is 0.06 mm), rapidly transferring the fiber after low-temperature coagulation into a low-temperature freeze drying system, and continuously vacuumizing in a vacuum freeze dryer at-40 ℃ for 48 hours to obtain porous aerogel fiber;
(5) Index parameters: the strength of the aerogel fiber is 2.4cN/dtex, the surface and the inside of the fiber have uniform pore structures, the pore diameters of the micropores are distributed between 200 nm and 600nm, and the bacteriostasis rate of the escherichia coli is 99.6%.
Example 3
The embodiment provides a preparation method of a high-strength skin-core structure porous aerogel fiber, which comprises the following steps:
(1) Adding 13% polyvinyl alcohol 2099 resin into dimethyl sulfoxide to be uniformly dissolved to be used as a core layer fluid material;
(2) Adding 2% of graphene conductive component into a polyvinyl alcohol solution, and uniformly dispersing to obtain a skin layer fluid, wherein the concentration of the polyvinyl alcohol aqueous solution is 11%wt;
(3) Standing and defoaming the sheath core layer fluid for 24 hours for later use;
(4) Extruding the sheath-core spinning solution with bubble removed into an ethanol coagulating bath at a speed of 0.8m/min through capillary holes with an aspect ratio of 1000 (capillary hole specification length of 50 mm and aperture of 0.05 mm), rapidly transferring the fiber after low-temperature coagulation into a low-temperature freeze drying system, and continuously vacuumizing in a vacuum freeze dryer at-40 ℃ for 24 hours to obtain the porous aerogel fiber.
(5) Index parameters: the strength of the aerogel fiber is 4.2cN/dtex, the surface and the inside of the fiber are both provided with uniform pore structures, the micropore diameter is distributed between 300 and 500nm, and the conductivity of the aerogel fiber is 10S/m.
Comparative example 1
The invention patent CN201911221326.6 reports a preparation method of polyimide aerogel fiber, which comprises the following steps: adding diamine containing chalcone structure and other diamine compound into polar aprotic solvent, stirring, adding dianhydride compound for polymerization reaction, spinning gel from the obtained polyimide solution, exchanging solvent from the obtained polyimide wet gel fiber, and freeze drying.
The prepared aerogel fiber has uniform pore structure inside the fiber, but a layer of compact skin exists on the surface of the fiber. Meanwhile, compared with the loose porous fiber inside the fiber, the strength of the loose porous fiber is lower, and the loose porous fiber is practically applied. First, compared with the comparative patent, the aerogel fiber prepared by the present invention has a pore structure inside and on the surface.
The aerogel fiber material with a porous structure is prepared by a liquid phase low temperature spinning technology (Liquid low temperature spinning technology, LLTST), and the liquid phase low temperature spinning technology is developed; the prepared aerogel fiber can be used for preparing various light and porous functional materials through chemical reaction or physical coating technology, and has wide application in the fields of energy storage, sensing, heat insulation, catalytic reaction, sewage treatment, wave absorption stealth, electrostatic shielding, antibiosis, flame retardance, moisture preservation, skin care and the like. The technology can prepare the fibrous material with microscopic open pore structures on the surface and inside of the fiber, and the prepared aerogel fiber ensures rich pore structures and simultaneously endows the aerogel fiber with excellent strength.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (5)
1. A preparation method of a high-strength skin-core structure porous functional aerogel fiber is characterized by comprising the following steps: comprising the steps of (a) a step of,
adding high polymer resin into a solvent, and uniformly dissolving to obtain core layer fluid, wherein the high polymer resin comprises a polyvinyl alcohol aqueous solution, a carboxymethyl cellulose aqueous solution, a chitosan acetic acid solution and a polyvinyl alcohol dimethyl sulfoxide solution, the solvent comprises N, N-dimethylformamide, and the mass concentration of the core layer fluid is 12-20%;
adding functional components into a polymer solution, and uniformly dispersing to obtain a cortical fluid, wherein the polymer solution comprises a carboxymethyl cellulose solution, and the mass concentration of the cortical fluid is 1-12%;
defoaming sheath fluid and core fluid to prepare sheath-core spinning solution;
extruding the sheath-core spinning solution into a low-temperature system through coaxial extrusion equipment, and condensing a water solvent in the spinning solution into a micro ice phase under the action of low temperature to solidify the fiber to obtain a solid-phase fiber;
the low-temperature system is a liquid nitrogen coagulation bath or low-temperature glycol, polyethylene glycol and ethanol;
the low temperature range is-10 to-196 ℃;
the ratio of the length and the diameter of the extrusion capillary holes is 1-1000, and the extrusion speed is 0.5-8 m/min;
and immediately freeze-drying the solid phase fiber after low-temperature solidification to obtain the porous aerogel fiber, wherein the freeze-drying temperature is-40 ℃, and continuously vacuumizing for 24-96 hours.
2. The method for preparing the high-strength sheath-core structured porous functional aerogel fiber according to claim 1, wherein the method comprises the following steps: the functional components are added into the polymer solution, wherein the functional components comprise a conductive component, an antibacterial component, a flame retardant component, a fragrance component, a moisturizing component and a beautifying component.
3. The method for preparing the high-strength sheath-core structured porous functional aerogel fiber according to claim 2, wherein the method comprises the following steps: the functional component accounts for 0-80% of the mass of the sheath core layer fluid.
4. The method for preparing the high-strength sheath-core structured porous functional aerogel fiber according to claim 1, wherein the method comprises the following steps: and the defoaming process is 0-0.2 MPa and is constant for 2-12 h.
5. The application of the product prepared by the preparation method of any one of claims 1-4 in the surface functionalization treatment of aerogel fibers is characterized in that: the method is applied to the fields of energy storage, sensing, heat insulation, catalytic reaction, sewage treatment, wave absorption stealth, electrostatic shielding, antibiosis, flame retardance, moisture preservation and skin care.
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| CN101617074A (en) * | 2007-02-23 | 2009-12-30 | 3M创新有限公司 | Polymer fiber and preparation method thereof |
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