CN115161790A - Preparation method of light and warm aerogel modified fiber - Google Patents
Preparation method of light and warm aerogel modified fiber Download PDFInfo
- Publication number
- CN115161790A CN115161790A CN202210813766.6A CN202210813766A CN115161790A CN 115161790 A CN115161790 A CN 115161790A CN 202210813766 A CN202210813766 A CN 202210813766A CN 115161790 A CN115161790 A CN 115161790A
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- aerogel
- warm
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- light
- modified fiber
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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
- 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
- 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
- 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
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
Abstract
The invention discloses a preparation method of light and warm aerogel modified fibers, which comprises the following steps: s1, preparing graphene oxide fragments; s2, preparing graphene aerogel; s3, preparing the light and warm aerogel modified fiber. The thermal insulation aerogel has the advantages that the graphene oxide is adopted to modify the aerogel, so that the heat transfer speed in the aerogel can be further reduced, the overall heat storage and thermal insulation capacity is improved, meanwhile, the graphene and the carbon fibers further influence the internal void structure of the aerogel, the overall density is reduced, the thermal insulation aerogel is lighter, the fiber preparation is realized through the wet spinning with the acetonitrile composite fiber, and the thermal insulation effect is more excellent.
Description
Technical Field
The invention relates to the technical field of warm-keeping fabric research and development, and particularly relates to a preparation method of light warm-keeping aerogel modified fiber.
Background
With the improvement of the existing living standard, the requirements of people on clothes are higher and higher, only comfortable and beautiful clothes can not meet the requirements of people, the requirements of people on the warm-keeping effect of the clothes are extremely high in winter, but after the warm-keeping effect is good, the clothes are often hot, sweat on the body and feel uncomfortable after the clothes move a little, and then the cold symptom is easy to happen under the condition of low temperature in winter.
Various novel warm-keeping materials are continuously developed in the market, and various modified and compounded novel warm-keeping materials continuously appear, such as warm-keeping materials of washed cotton, shaped degreased washed cotton, down wadding, compound acupuncture, melt-blown cotton and the like. Because a single thermal insulation material often has defects, the requirements of different consumer groups are difficult to meet only by using one material, and simultaneously, the performance of the thermal insulation material is difficult to be greatly improved.
A new warm-keeping fabric obtained by compounding different materials is a trend of the development of the existing cold-proof warm-keeping fabric. The conventional method in the market at present is to add layers and thicken the textile fabric, and the textile fabric prepared by the method has poor air permeability, easy fluffing and pilling, poor elasticity, heavy weight, moisture absorption and swelling and serious electrostatic phenomenon.
Disclosure of Invention
The invention aims to provide a preparation method of a light and warm aerogel modified fiber, which improves the overall heat storage and insulation capacity while realizing lightness and thinness.
The technical purpose of the invention is realized by the following technical scheme:
the preparation method of the light and warm aerogel modified fiber is characterized by comprising the following steps of:
s1, placing a sodium nitrate reagent and graphite powder into a concentrated sulfuric acid solution for ice-bath stirring, then adding potassium permanganate powder into a mixed solution for multiple times while stirring, subsequently heating and continuously stirring until the mixture is dark brown reaction paste, adding hot water, stirring and heating, then continuously stirring, subsequently cooling to room temperature, adding a hydrogen peroxide solution, taking out and filtering the reactant after the color of the reactant is changed from dark brown to bright yellow, re-dispersing the reactant into deionized water, subsequently washing by a hydrochloric acid solution, centrifuging, taking the centrifuged precipitate, and drying to obtain graphene oxide fragments;
s2, re-dispersing the dried graphene oxide fragments in deionized water, adding carbon fibers, carrying out ultrasonic dissolution on the mixed solution, adding ascorbic acid in proportion after the carbon fibers are fully dissolved, continuously stirring to obtain a uniform stirred substance, placing the stirred substance into a heat preservation box for standing reaction, taking out the stirred substance, replacing and cleaning impurities with deionized water, and carrying out freeze drying to obtain the graphene aerogel;
and S3, melting the acetonitrile composite fibers to obtain a spinning solution, adding the graphene aerogel into the spinning solution, uniformly mixing, spraying out through a spinneret orifice, and performing fiber forming, primary fiber drafting orientation, fiber heat setting and winding to obtain the light and warm aerogel modified fibers.
Preferably, the mass-to-volume ratio of the sodium nitrate reagent, the graphite powder, the potassium permanganate and the concentrated sulfuric acid reagent in the S1 is 1g: (3 to 4) g: (10 to 15) g: (41 to 63) ml.
Preferably, after the potassium permanganate in the S1 is added, the temperature is raised to 36 to 40 ℃, and then hot water at 100 ℃ is added, stirred and raised to 98 ℃.
Preferably, the mass fraction of the hydrogen peroxide in the hydrogen peroxide solution is 30%, and the volume ratio of the concentrated sulfuric acid reagent, the hot water and the hydrogen peroxide solution is 1: (2 to 3): (0.3 to 0.6).
Preferably, the mass fraction of hydrochloric acid in the hydrochloric acid solution in the S1 is 3%, the washing and centrifuging times are 4 times, the first three times are centrifuging, then removing the lower-layer precipitate and taking the supernatant, the centrifuging speed is 1500rpm, the fourth centrifuging speed is 10000rpm, and then the lower-layer precipitate is taken.
Preferably, the mass ratio of the graphene oxide fragments, the carbon fibers and the ascorbic acid in the S2 is (30 to 40): 1: (0.1 to 0.2) and the freeze drying time is 20 to 24h.
Preferably, the mass ratio of the acetonitrile composite fibers to the graphene aerogel in the S3 is 3.
In conclusion, the invention has the following beneficial effects: according to the thermal insulation aerogel, the graphene oxide is adopted to modify the aerogel, so that the heat transfer speed in the aerogel can be further reduced, the overall heat storage and thermal insulation capacity is improved, meanwhile, the graphene and the carbon fibers further influence the internal void structure of the aerogel, the overall density is reduced, the thermal insulation aerogel is lighter, the fiber preparation is realized through the wet spinning with the acetonitrile composite fiber, and the thermal insulation effect is more excellent.
Detailed Description
The following further describes the embodiments of the present invention, which are not to be construed as limiting the invention.
Example 1
A preparation method of light and warm aerogel modified fibers comprises the following steps:
s1, taking a sodium nitrate reagent and graphite powder, placing the sodium nitrate reagent and the graphite powder in a concentrated sulfuric acid solution for ice-bath stirring, taking potassium permanganate powder, stirring and adding a small amount of the potassium permanganate powder into a mixed solution for multiple times, wherein the mass-to-volume ratio of the sodium nitrate reagent to the graphite powder to the potassium permanganate to the concentrated sulfuric acid reagent is 1g:3g:10g:41ml, heating to 36 ℃, stirring continuously until the mixture is dark brown reaction paste, adding hot water at 100 ℃, stirring, heating to 98 ℃, stirring continuously, cooling to room temperature, adding hydrogen peroxide solution, wherein the mass fraction of hydrogen peroxide in the hydrogen peroxide solution is 30%, changing the color of the reactant from tan to bright yellow, taking out and filtering, and the volume ratio of concentrated sulfuric acid reagent to hot water to the hydrogen peroxide solution is 1:2: and 0.3, dispersing in deionized water again, subsequently washing by using a hydrochloric acid solution, and centrifuging, wherein the mass fraction of hydrochloric acid in the hydrochloric acid solution is 3%, the washing and centrifuging times are 4, the first three times are centrifuging, then removing the lower-layer precipitate, taking the supernatant, the centrifuging speed is 1500rpm, the fourth centrifuging speed is 10000rpm, and taking the lower-layer precipitate after the fourth centrifuging and drying to obtain the graphene oxide fragment.
S2, dispersing the dried graphene oxide fragments in deionized water again, adding carbon fibers, carrying out ultrasonic dissolution on the mixed solution, and adding ascorbic acid in proportion after the carbon fibers are fully dissolved, wherein the mass ratio of the graphene oxide fragments to the carbon fibers to the ascorbic acid is 30:1: and 0.1, continuously stirring to obtain a uniform stirred material, placing the stirred material into an incubator for standing reaction, taking out the stirred material, replacing and cleaning impurities with deionized water, and freeze-drying for 20 hours to obtain the graphene aerogel.
And S3, melting the acetonitrile composite fibers to prepare a spinning solution, adding the graphene aerogel into the spinning solution, wherein the mass ratio of the acetonitrile composite fibers to the graphene aerogel is 3.
Example 2
A preparation method of light and warm aerogel modified fibers comprises the following steps:
s1, taking a sodium nitrate reagent and graphite powder, placing the sodium nitrate reagent and the graphite powder in a concentrated sulfuric acid solution for ice bath stirring, taking potassium permanganate powder, stirring and adding a small amount of the potassium permanganate powder into a mixed solution for many times, wherein the mass-to-volume ratio of the sodium nitrate reagent to the graphite powder to the potassium permanganate to the concentrated sulfuric acid reagent is 1g:4g:12g:50ml, heating to 38 ℃, stirring continuously until the mixture is dark brown reaction paste, adding hot water at 100 ℃, stirring, heating to 98 ℃, stirring continuously, cooling to room temperature, adding hydrogen peroxide solution, wherein the mass fraction of hydrogen peroxide in the hydrogen peroxide solution is 30%, changing the color of the reactant from tan to bright yellow, taking out and filtering, and the volume ratio of concentrated sulfuric acid reagent to hot water to the hydrogen peroxide solution is 1:2: and 0.4, dispersing in deionized water again, subsequently washing by using a hydrochloric acid solution, and centrifuging, wherein the mass fraction of hydrochloric acid in the hydrochloric acid solution is 3%, the washing and centrifuging times are 4, the first three times are centrifuging, then removing the lower-layer precipitate, taking the supernatant, the centrifuging speed is 1500rpm, the fourth centrifuging speed is 10000rpm, and taking the lower-layer precipitate after the fourth centrifuging and drying to obtain the graphene oxide fragment.
S2, dispersing the dried graphene oxide fragments in deionized water again, adding carbon fibers, carrying out ultrasonic dissolution on the mixed solution, and adding ascorbic acid in proportion after the carbon fibers are fully dissolved, wherein the mass ratio of the graphene oxide fragments to the carbon fibers to the ascorbic acid is 35:1: and 0.1, continuously stirring to obtain a uniform stirred material, placing the stirred material into an incubator for standing reaction, taking out the stirred material, replacing and cleaning impurities with deionized water, and carrying out freeze drying for 224 hours to obtain the graphene aerogel.
S3, melting the acetonitrile composite fibers to prepare a spinning solution, adding the graphene aerogel into the spinning solution, uniformly mixing the acetonitrile composite fibers and the graphene aerogel in a mass ratio of 3.
Example 3
A preparation method of light and warm aerogel modified fibers comprises the following steps:
s1, taking a sodium nitrate reagent and graphite powder, placing the sodium nitrate reagent and the graphite powder in a concentrated sulfuric acid solution for ice-bath stirring, taking potassium permanganate powder, stirring and adding a small amount of the potassium permanganate powder into a mixed solution for multiple times, wherein the mass-to-volume ratio of the sodium nitrate reagent to the graphite powder to the potassium permanganate to the concentrated sulfuric acid reagent is 1g:4g:15g:63ml, subsequently heating to 40 ℃, continuously stirring until the mixture is dark brown reaction paste, adding hot water at 100 ℃, stirring, heating to 98 ℃, continuously stirring, subsequently cooling to room temperature, adding a hydrogen peroxide solution, wherein the mass fraction of hydrogen peroxide in the hydrogen peroxide solution is 30%, taking out and filtering after the color of the reactant is changed from tan to bright yellow, and the volume ratio of concentrated sulfuric acid reagent, hot water and the hydrogen peroxide solution is 1: 3): and 0.6, dispersing the mixture in deionized water again, subsequently washing the mixture by using a hydrochloric acid solution, and centrifuging the mixture, wherein the hydrochloric acid solution contains 3 mass percent of hydrochloric acid, the washing and centrifuging times are 4 times, the first three times are centrifuging, then removing lower-layer precipitates and taking supernatant, the centrifuging speed is 1500rpm, the fourth centrifuging speed is 10000rpm, and the lower-layer precipitates after the fourth centrifuging are taken and dried to obtain the graphene oxide fragments.
S2, dispersing the dried graphene oxide fragments in deionized water again, adding carbon fibers, carrying out ultrasonic dissolution on the mixed solution, adding ascorbic acid in proportion after the carbon fibers are fully dissolved, wherein the mass ratio of the graphene oxide fragments to the carbon fibers to the ascorbic acid is 40:1:0.2, continuously stirring to obtain a uniform stirred material, then placing the stirred material into an incubator for standing reaction, taking out the stirred material, replacing and cleaning impurities with deionized water, and then carrying out freeze drying for 20 to 24h to obtain the graphene aerogel.
And S3, melting the acetonitrile composite fibers to prepare a spinning solution, adding the graphene aerogel into the spinning solution, wherein the mass ratio of the acetonitrile composite fibers to the graphene aerogel is 3.
According to the thermal insulation aerogel, the graphene oxide is adopted to modify the aerogel, so that the heat transfer speed in the aerogel can be further reduced, the overall heat storage and thermal insulation capacity is improved, meanwhile, the graphene and the carbon fibers further influence the internal void structure of the aerogel, the overall density is reduced, the thermal insulation aerogel is lighter, the fiber preparation is realized through the wet spinning with the acetonitrile composite fiber, and the thermal insulation effect is more excellent.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention.
Claims (7)
1. The preparation method of the light and warm aerogel modified fiber is characterized by comprising the following steps of:
s1, placing a sodium nitrate reagent and graphite powder into a concentrated sulfuric acid solution for ice-bath stirring, then adding a small amount of potassium permanganate powder into a mixed solution while stirring for multiple times, subsequently heating up, continuously stirring until the mixture is dark brown reaction paste, adding hot water, stirring and heating, continuously stirring, subsequently cooling to room temperature, adding a hydrogen peroxide solution, taking out and filtering the reactant after the color of the reactant is changed from dark brown to bright yellow, re-dispersing the reactant into deionized water, subsequently washing by a hydrochloric acid solution, centrifuging, taking the centrifuged precipitate, and drying to obtain graphene oxide fragments;
s2, re-dispersing the dried graphene oxide fragments in deionized water, adding carbon fibers, carrying out ultrasonic dissolution on the mixed solution, adding ascorbic acid in proportion after the carbon fibers are fully dissolved, continuously stirring to obtain a uniform stirred substance, placing the stirred substance into a heat preservation box for standing reaction, taking out the stirred substance, replacing and cleaning impurities with deionized water, and carrying out freeze drying to obtain the graphene aerogel;
and S3, melting the vinyl acetate-nitrile composite fiber to prepare a spinning solution, adding the graphene aerogel into the spinning solution, uniformly mixing, spraying out through a spinneret orifice, and performing fiber forming, primary fiber drafting orientation, fiber heat setting and winding to prepare the light and warm aerogel modified fiber.
2. The preparation method of the light warm aerogel modified fiber according to claim 1, characterized by comprising the following steps: in the S1, the mass-to-volume ratio of the sodium nitrate reagent to the graphite powder to the potassium permanganate to the concentrated sulfuric acid reagent is 1g: (3 to 4) g: (10 to 15) g: (41 to 63) ml.
3. The preparation method of the light warm aerogel modified fiber according to claim 1, characterized by comprising the following steps: after the potassium permanganate in the S1 is added, the temperature is raised to 36-40 ℃, hot water at 100 ℃ is added, the mixture is stirred, and the temperature is raised to 98 ℃.
4. The preparation method of the light warm aerogel modified fiber according to claim 1, characterized by comprising the following steps: the mass fraction of hydrogen peroxide in the hydrogen peroxide solution is 30%, and the volume ratio of the concentrated sulfuric acid reagent to the hot water to the hydrogen peroxide solution is 1: (2 to 3): (0.3 to 0.6).
5. The preparation method of the light warm aerogel modified fiber according to claim 1, characterized by comprising the following steps: and in the S1, the mass fraction of hydrochloric acid in the hydrochloric acid solution is 3%, the washing and centrifuging times are 4 times, the first three times are to remove lower-layer precipitates and take upper-layer clear liquid after centrifugation, the centrifugation rotating speed is 1500rpm, the fourth centrifugation rotating speed is 10000rpm, and the lower-layer precipitates are taken.
6. The preparation method of the light and warm aerogel modified fiber according to claim 1, characterized by comprising the following steps: the mass ratio of the graphene oxide fragments, the carbon fibers and the ascorbic acid in the S2 is (30-40): 1: (0.1 to 0.2) and the freeze drying time is 20 to 24h.
7. The preparation method of the light warm aerogel modified fiber according to claim 1, characterized by comprising the following steps: in the S3, the mass ratio of the acetonitrile composite fibers to the graphene aerogel is 3.
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