CN115613149A - Superfine polyacrylonitrile fiber and preparation method thereof - Google Patents
Superfine polyacrylonitrile fiber and preparation method thereof Download PDFInfo
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- CN115613149A CN115613149A CN202211173816.5A CN202211173816A CN115613149A CN 115613149 A CN115613149 A CN 115613149A CN 202211173816 A CN202211173816 A CN 202211173816A CN 115613149 A CN115613149 A CN 115613149A
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- polyacrylonitrile
- polyvinyl alcohol
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- 229920002239 polyacrylonitrile Polymers 0.000 title claims abstract description 135
- 239000000835 fiber Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 91
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 91
- 238000009987 spinning Methods 0.000 claims description 85
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 35
- 239000002131 composite material Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000015271 coagulation Effects 0.000 claims description 11
- 238000005345 coagulation Methods 0.000 claims description 11
- 229920002972 Acrylic fiber Polymers 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000002166 wet spinning Methods 0.000 claims description 9
- 238000004804 winding Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 239000013585 weight reducing agent Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000008213 purified water Substances 0.000 claims description 3
- 229920001410 Microfiber Polymers 0.000 claims 2
- 239000003658 microfiber Substances 0.000 claims 2
- 239000002657 fibrous material Substances 0.000 abstract description 2
- 230000001112 coagulating effect Effects 0.000 description 10
- 239000002994 raw material Substances 0.000 description 5
- 230000007547 defect Effects 0.000 description 3
- 238000009998 heat setting Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920000098 polyolefin Polymers 0.000 description 3
- 239000007788 liquid Substances 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- 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
-
- 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
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D10B2321/06—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention relates to the field of fiber materials, in particular to superfine polyacrylonitrile fiber and a preparation method thereof.
Description
Technical Field
The invention relates to the field of fiber materials, in particular to superfine polyacrylonitrile fiber and a preparation method thereof.
Background
The polyacrylonitrile fiber has the characteristics of good fluffiness, elasticity, heat preservation, weather resistance, sun resistance and the like, has the reputation of artificial wool, and has wide application. However, the traditional polyacrylonitrile fiber has high monofilament linear density, the fiber and the woven fabric have hard hand feeling and poor drapability, and the application to high-end clothes is difficult.
CN110055601A is a wet spinning method of polyacrylonitrile fiber and the polyacrylonitrile fiber. The main technical scheme adopted is as follows: a wet spinning method of polyacrylonitrile fibers comprises the following steps: spinning: extruding the spinning solution through a spinneret orifice of a spinneret assembly to obtain spinning trickle; solidification and forming: the spinning trickle enters a coagulating bath for coagulation and forming to obtain nascent fiber; hot drawing treatment: performing multi-stage hot drawing treatment on the nascent fiber; and (3) water washing treatment: washing the fiber after the hot drawing treatment with water; drying and heat setting treatment: and (3) drying and heat setting the fiber after washing to obtain the polyacrylonitrile fiber. The polyacrylonitrile fiber is prepared by the wet spinning method of the polyacrylonitrile fiber. The invention is mainly used for ensuring the spinnability of the spinning solution in the spinning process and improving the mechanical property of the polyacrylonitrile fiber. However, the patent is mainly a one-component solution spinning method, and the one-component solution spinning method is difficult to produce fine denier fiber.
CN103981593A discloses a method for preparing polyvinyl alcohol melt-spun superfine fiber, which comprises the steps of respectively adding polyvinyl alcohol serving as a raw material I and a polyolefin linear polymer serving as a raw material II into a two-component composite spinning machine hopper, spraying the two-component composite spinning machine hopper through a spinneret plate, and cooling melt trickle by side blowing to prepare nascent fiber; stretching the obtained nascent fiber, and then performing relaxation and heat setting to obtain the sea-island type coarse denier composite fiber of polyvinyl alcohol/polyolefin; then, the sea-phase polyolefin linear polymer is dissolved and removed by a dissolving tank containing selective solvent, the polyvinyl alcohol superfine fiber bundle is dried by a drier so as to remove the residual selective solvent in the polyvinyl alcohol superfine fiber bundle, and the drier is provided with a solvent recovery device; and winding the dried polyvinyl alcohol superfine fiber bundle to obtain the finished fiber. The invention has the advantages that: simple and convenient process, easy realization of industrialization, low production cost, energy conservation and environmental protection. But the raw material of the acrylic fiber is cheap propylene which is a byproduct of petroleum cracking: the polyacrylonitrile copolymer is not melt-spun but is melt-spun because it is decomposed without melting when heated to 230C or more.
Therefore, based on the above prior art, at present, the preparation of polyacrylonitrile fiber cannot be melt-spun, but only a solution spinning method is adopted, and the traditional method for preparing polyacrylonitrile fiber is mainly a one-component solution spinning method. The method is difficult to produce fine denier fiber and can not overcome the defects of hard hand feeling and poor drapability of the fabric. Although some companies use flexible groups in polyacrylonitrile to produce polyacrylonitrile fibers by copolymerization or blending with another high polymer, the effect is not ideal. Based on this, the shadow of the superfine polyacrylonitrile fiber is difficult to see in the high-end clothing market.
Therefore, how to prepare the ultrafine polyacrylonitrile fiber is a problem which needs to be solved urgently in the prior art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the superfine polyacrylonitrile fiber and the preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that the superfine polyacrylonitrile fiber is obtained by preparing polyvinyl alcohol spinning solution prepared from polyvinyl alcohol and polyacrylonitrile spinning solution prepared from polyacrylonitrile through wet spinning to prepare polyvinyl alcohol polyacrylonitrile composite fiber with a sea-island (orange petal) structure, and then drawing, reducing, washing, drying, oiling and winding the polyvinyl alcohol polyacrylonitrile composite fiber.
The monofilament linear density of the superfine polyacrylonitrile fiber is 0.08D-0.2D.
The breaking strength of the superfine polyacrylonitrile fiber is 3CN/dtex +/-0.2 CN/dtex, and the elongation at break is 35 +/-4%.
The preparation method of the superfine polyacrylonitrile fiber comprises the following steps:
(1) Heating polyvinyl alcohol and purified water to 60 ℃ to prepare a solution, so as to obtain a polyvinyl alcohol spinning solution;
(2) Preparing polyacrylonitrile and dimethyl sulfoxide (DMSO) into a solution to obtain polyacrylonitrile spinning solution;
(3) Respectively filtering the polyvinyl alcohol spinning solution obtained in the step (1) and the polyacrylonitrile spinning solution obtained in the step (2), performing vacuum defoaming, then respectively entering a feeding hole of a wet spinning machine A, B, spraying out the polyvinyl alcohol spinning solution through the same island-type (orange petal-type) composite spinneret plate, and solidifying and drafting the sprayed out composite fiber through a solidification bath to obtain the polyvinyl alcohol-polyacrylonitrile composite fiber with the island-type (orange petal-type) structure, wherein the polyvinyl alcohol is sea and the polyacrylonitrile is island;
(4) And after the polyvinyl alcohol polyacrylonitrile composite fiber is drafted for 1-N times, the drafted polyvinyl alcohol polyacrylonitrile composite fiber enters a decrement tank to reduce polyvinyl alcohol, and finally the superfine polyacrylonitrile fiber is obtained.
In the preparation method of the superfine polyacrylonitrile fiber, the mass ratio of the polyvinyl alcohol in the polyvinyl alcohol solution to the polyacrylonitrile in the polyacrylonitrile solution in the step (2) is (25-30): (75-70).
In the preparation method of the superfine polyacrylonitrile fiber, the concentration of the polyvinyl alcohol in the polyvinyl alcohol solution in the step (1) and the concentration of the polyacrylonitrile in the polyacrylonitrile solution in the step (2) are independently 6-17 wt%.
In the step (3), the flow rate ratio of the polyvinyl alcohol spinning solution to the polyacrylonitrile spinning solution is 1 (0.5-10), and the sum of the flow rates of the polyvinyl alcohol spinning solution and the polyacrylonitrile spinning solution is 0.3-6) L/h.
In the step (3), the solvent in the coagulation bath is dimethyl sulfoxide (DMSO), the concentration is 25-30%, the temperature is controlled at 30 +/-2 ℃, the coagulation time is 15min, after the coagulation is finished, the acrylic fiber enters a washing tank, and the acrylic fiber is soaked and extruded in the washing tank for multiple times, so that the DMSO residue in the fiber is less than or equal to 0.005%.
In the preparation method of the superfine polyacrylonitrile fiber, the drafting temperature T in the step (4) is 80-100 ℃, and the drafting multiple DR is 3-4.
In the preparation method of the superfine polyacrylonitrile fiber, the temperature of the water in the weight reduction pool in the step (4) is 90-100 ℃, and the weight reduction time is 5-8 minutes.
The invention relates to a superfine polyacrylonitrile fiber and a preparation method thereof, which have the beneficial effects that polyvinyl alcohol spinning solution and polyacrylonitrile spinning solution are respectively spun, then are sprayed out by a same sea-island (orange petal type) composite spinneret plate, and are solidified by a coagulating bath and drawn for 1-N times to obtain the sea-island (orange petal) structure polyvinyl alcohol polyacrylonitrile composite fiber, wherein the polyvinyl alcohol is sea, and the polyacrylonitrile is islands. And then the polyvinyl alcohol polyacrylonitrile composite fiber enters a decrement tank to reduce the polyvinyl alcohol, and finally the superfine polyacrylonitrile fiber with the monofilament linear density of 0.08D-0.2D is obtained.
The superfine polyacrylonitrile fiber prepared by the method has good hand feeling and drapability, and simultaneously well maintains the original excellent performance of polyacrylonitrile.
The invention controls the concentration of polyacrylonitrile in the polyacrylonitrile solution within the range of 6-17 wt%, and can avoid the influence on the spinning forming of the composite fiber caused by the too high or too low viscosity of the prepared spinning solution due to the too high or too low concentration of polyacrylonitrile.
The mass ratio of the polyvinyl alcohol in the polyvinyl alcohol solution to the polyacrylonitrile in the polyacrylonitrile solution in the step (2) is (25-30): (75 to 70). In the proportion range, the island phase is uniformly distributed in the sea phase, and if the proportion is too small, the island phase is not well distributed in the sea phase, so that the island phase is easy to adhere, and the quality of the fiber is influenced; if the ratio is too large, the island phases are well distributed in the sea phase, but the sea phase is wasted.
The concentration of the coagulating bath is 25-30%, so that the phenomenon that the exchange of DMSO and water is too fast to generate acrylic fiber surface micro defects due to too low concentration of the coagulating liquid is prevented, and the acrylic fiber coagulation speed is too slow due to too high concentration of the coagulating liquid.
In the step (4), the drafting temperature T is 80-100 ℃, and the drafting multiple DR is 3-4. Within the range, the prepared fiber has higher strength, moderate elongation, good fiber dyeing and less broken filaments; if the content exceeds the range, the prepared fiber has low strength, too short or too long elongation, and stiff silks and fuzzes are easy to generate, so that the use of the subsequent process cannot be well met.
The method provided by the invention is simple to operate, mild in reaction conditions, wide in raw material source, low in cost, green and environment-friendly, and suitable for large-scale production.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and specific embodiments.
Example 1
A superfine polyacrylonitrile fiber is prepared from polyvinyl alcohol spinning solution prepared from polyvinyl alcohol and polyacrylonitrile spinning solution prepared from polyacrylonitrile through wet spinning to obtain composite polyvinyl alcohol-polyacrylonitrile fiber with island (orange petal) structure, drafting, reducing, washing, drying, oiling and winding.
The monofilament linear density of the superfine polyacrylonitrile fiber is 0.08D-0.2D.
The breaking strength is 3CN/dtex +/-0.2 CN/dtex, and the elongation at break is 35 +/-4%.
The preparation method of the superfine polyacrylonitrile fiber comprises the following steps:
(1) Heating polyvinyl alcohol and purified water to 60 ℃ to prepare a solution, so as to obtain a polyvinyl alcohol spinning solution;
(2) Preparing polyacrylonitrile and dimethyl sulfoxide (DMSO) into a solution to obtain polyacrylonitrile spinning solution;
the step (1) and the step (2) are not divided in sequence;
(3) Respectively filtering the polyvinyl alcohol spinning solution obtained in the step (1) and the polyacrylonitrile spinning solution obtained in the step (2), performing vacuum defoaming, then respectively entering a feeding hole of a wet spinning machine A, B, spraying out the polyvinyl alcohol spinning solution through the same island-type (orange petal-type) composite spinneret plate, and solidifying and drafting the sprayed out composite fiber through a solidification bath to obtain the polyvinyl alcohol-polyacrylonitrile composite fiber with the island-type (orange petal-type) structure, wherein the polyvinyl alcohol is sea and the polyacrylonitrile is island;
(4) And after the polyvinyl alcohol polyacrylonitrile composite fiber is drafted for 1-N times, the drafted polyvinyl alcohol polyacrylonitrile composite fiber enters a decrement tank to reduce polyvinyl alcohol, and finally the superfine polyacrylonitrile fiber is obtained.
The mass ratio of the polyvinyl alcohol in the polyvinyl alcohol solution to the polyacrylonitrile in the polyacrylonitrile solution in the step (2) is (25-30): (75-70).
The concentration of the polyvinyl alcohol in the polyvinyl alcohol solution in the step (1) and the concentration of the polyacrylonitrile in the polyacrylonitrile solution in the step (2) are independently 6-17 wt%. More preferably from 7 to 16wt%.
In the step (3), the flow rate ratio of the polyvinyl alcohol spinning solution to the polyacrylonitrile spinning solution is 1 (0.5-10), and the sum of the flow rates of the polyvinyl alcohol spinning solution and the polyacrylonitrile spinning solution is 0.3-6) L/h.
In the step (3), the solvent in the coagulating bath is dimethyl sulfoxide (DMSO), the concentration is 25-30%, the temperature is controlled to be 30 +/-2 ℃, the coagulating time is 15min, after the coagulation is finished, the acrylic fiber enters a washing tank, and the acrylic fiber is soaked and extruded for multiple times in the washing tank, so that the DMSO residue in the fiber is less than or equal to 0.005%.
In the step (4), the drafting temperature T is 80-100 ℃, and the drafting multiple DR is 3-4.
The temperature of the water in the reduction pool in the step (4) is 90-100 ℃, and the reduction time is 5-8 minutes.
The invention respectively carries out spinning through polyvinyl alcohol spinning solution and polyacrylonitrile spinning solution, then the spinning solution is sprayed out by a same sea-island (orange petal type) composite spinneret plate, and the sea-island (orange petal) structure polyvinyl alcohol polyacrylonitrile composite fiber is obtained through coagulation bath coagulation and 1-N times of drafting, wherein the polyvinyl alcohol is sea and the polyacrylonitrile is islands. And then the polyvinyl alcohol polyacrylonitrile composite fiber enters a decrement tank to reduce the polyvinyl alcohol, and finally the superfine polyacrylonitrile fiber with the monofilament linear density of 0.08D-0.2D is obtained.
The spinneret orifices used for spinning are not particularly limited in the invention, and the spinneret orifices can be conventional in the field.
The present invention is not particularly limited in the manner of drawing, reducing, washing, drying and winding, and may be performed in a manner well known to those skilled in the art.
In the present invention, the raw materials used are all those conventionally commercially available in the art unless otherwise specified.
Example 2
The same parts of this embodiment as embodiment 1 are not described again, but the differences are:
the mass ratio of the polyvinyl alcohol in the polyvinyl alcohol spinning solution to the polyacrylonitrile in the polyacrylonitrile spinning solution is 25:75.
the concentration of the polyvinyl alcohol spinning solution is 10wt%; the polyvinyl alcohol dope was prepared by dissolving 25g of polyvinyl alcohol in 225g of DMSO (dimethyl sulfoxide).
The concentration of the polyacrylonitrile spinning solution is 8wt%; the polyacrylonitrile spinning solution was prepared by dissolving 20g of polyacrylonitrile in 230g of dmso (dimethyl sulfoxide).
The step (1) and the step (2) are not divided in sequence.
(3) Respectively feeding the polyvinyl alcohol spinning solution obtained in the step (1) and the polyacrylonitrile spinning solution obtained in the step (2) into a wet composite spinning machine, and finally feeding the polyvinyl alcohol spinning solution and the polyacrylonitrile spinning solution into the same island type (orange petal type) spinneret plate for spinning and coagulating bath treatment to obtain nascent fibers; and sequentially carrying out drafting, decrement, washing, drying, oiling and winding on the obtained nascent fiber to obtain the superfine polyacrylonitrile fiber.
The drafting temperature T in the step (3) is respectively one-to-one at 90 ℃, two at 93 ℃, three at 95 ℃, and the drafting times DR are respectively one-to-one at 1.4, two-to-one at 1.5 and three-to-one at 1.5.
The temperature of the water in the reduction pool in the step (3) is 90 ℃, and the reduction time is 8 minutes.
Example 3
The same parts of this embodiment as embodiment 1 are not described again, but the differences are:
the mass ratio of the polyvinyl alcohol in the polyvinyl alcohol spinning solution to the polyacrylonitrile in the polyacrylonitrile spinning solution is 28:72.
the concentration of the polyvinyl alcohol spinning solution is 10wt%; the polyvinyl alcohol dope was prepared by dissolving 25g of polyvinyl alcohol in 225g of DMSO (dimethyl sulfoxide).
The concentration of the polyacrylonitrile spinning solution is 8wt%; the polyacrylonitrile spinning solution was prepared by dissolving 20g of polyacrylonitrile in 230g of dmso (dimethyl sulfoxide).
The step (1) and the step (2) are not divided in sequence.
(3) Performing wet composite spinning on the polyvinyl alcohol spinning solution obtained in the step (1) and the polyvinyl alcohol spinning solution obtained in the step (2) respectively, and finally performing spinning and coagulating bath treatment on the same island type (orange petal type) spinneret plate to obtain nascent fibers; and sequentially carrying out drafting, decrement, washing, drying, oiling and winding on the obtained nascent fiber to obtain the superfine polyacrylonitrile fiber.
The drafting temperature T in the step (3) is respectively one draft 90 ℃, two drafts 95 ℃, three drafts 95 ℃, and the drafting times DR are respectively one draft 1.35, two drafts 1.5 and three drafts 1.5.
The temperature of the water in the reduction pool in the step (3) is 95 ℃, and the reduction time is 7 minutes.
Example 4
The same parts of this embodiment as embodiment 1 are not described again, but the differences are:
the mass ratio of the polyvinyl alcohol in the polyvinyl alcohol spinning solution to the polyacrylonitrile in the polyacrylonitrile spinning solution is 30:70.
the concentration of the polyvinyl alcohol spinning solution is 10wt%; the polyvinyl alcohol dope was prepared by dissolving 25g of polyvinyl alcohol in 225g of DMSO (dimethyl sulfoxide).
The concentration of the polyacrylonitrile spinning solution is 8wt%; the polyacrylonitrile spinning solution was prepared by dissolving 20g of polyacrylonitrile in 230g of dmso (dimethyl sulfoxide).
The step (1) and the step (2) are not divided in sequence.
(3) Performing wet composite spinning on the polyvinyl alcohol spinning solution obtained in the step (1) and the polyacrylonitrile spinning solution obtained in the step (2) respectively, and finally performing spinning and coagulating bath treatment on the polyvinyl alcohol spinning solution and the polyacrylonitrile spinning solution in the same sea-island type (orange petal type) spinneret plate to obtain nascent fibers; and sequentially carrying out drafting, decrement, washing, drying, oiling and winding on the obtained nascent fiber to obtain the superfine polyacrylonitrile fiber.
The drafting temperature T in the step (3) is respectively one-to-one at 90 ℃, two at 93 ℃, three at 95 ℃, and the drafting times DR are respectively one-to-one at 1.5, two-to-one at 1.5, and three-to-one at 1.5.
The temperature of the water in the reduction pool in the step (3) is 100 ℃, and the reduction time is 5 minutes.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and that various changes, modifications, additions and substitutions which are within the spirit and scope of the present invention and which can be made by those skilled in the art are also within the scope of the present invention.
Claims (10)
1. The superfine polyacrylonitrile fiber is characterized in that: the fiber is prepared by preparing polyvinyl alcohol polyacrylonitrile composite fiber with sea island (orange petal) structure from polyvinyl alcohol spinning solution prepared from polyvinyl alcohol and polyacrylonitrile spinning solution prepared from polyacrylonitrile by wet spinning, and then drawing, reducing, washing, drying, oiling and winding the polyvinyl alcohol polyacrylonitrile composite fiber.
2. The polyacrylonitrile microfiber according to claim 1, wherein the polyacrylonitrile microfiber has a filament linear density of 0.08D to 0.2D.
3. The ultrafine polyacrylonitrile fiber according to claim 1, wherein the breaking strength is 3 CN/dtex. + -. 0.2CN/dtex, and the elongation at break is 35. + -. 4%.
4. The method for preparing the ultrafine polyacrylonitrile fiber according to any one of claims 1 to 3, wherein: the method comprises the following steps:
(1) Heating polyvinyl alcohol and purified water to 60 ℃ to prepare a solution, so as to obtain a polyvinyl alcohol spinning solution;
(2) Preparing polyacrylonitrile and dimethyl sulfoxide (DMSO) into a solution to obtain a polyacrylonitrile spinning solution;
(3) Respectively filtering the polyvinyl alcohol spinning solution obtained in the step (1) and the polyacrylonitrile spinning solution obtained in the step (2), performing vacuum defoaming, then respectively entering a feeding hole of a wet spinning machine A, B, spraying out the polyvinyl alcohol spinning solution through the same island-type (orange petal-type) composite spinneret plate, and solidifying and drafting the sprayed out composite fiber through a solidification bath to obtain the polyvinyl alcohol-polyacrylonitrile composite fiber with the island-type (orange petal-type) structure, wherein the polyvinyl alcohol is sea and the polyacrylonitrile is island;
(4) And after the polyvinyl alcohol polyacrylonitrile composite fiber is drafted for 1-N times, the drafted polyvinyl alcohol polyacrylonitrile composite fiber enters a decrement tank to reduce polyvinyl alcohol, and finally the superfine polyacrylonitrile fiber is obtained.
5. The method for preparing the ultrafine polyacrylonitrile fiber according to the claim 4, wherein the mass ratio of the polyvinyl alcohol in the polyvinyl alcohol solution to the polyacrylonitrile in the polyacrylonitrile solution in the step (2) is (25-30): (75-70).
6. The method as claimed in claim 5, wherein the concentration of the polyvinyl alcohol in the polyvinyl alcohol solution of the step (1) and the concentration of the polyacrylonitrile in the polyacrylonitrile solution of the step (2) are independently 6 to 17wt%.
7. The method for preparing the ultrafine polyacrylonitrile fiber according to claim 6, wherein the flow rate ratio of the polyvinyl alcohol spinning solution to the polyacrylonitrile spinning solution in the step (3) is 1 (0.5-10), and the sum of the flow rates of the polyvinyl alcohol spinning solution and the polyacrylonitrile spinning solution is (0.3-6) L/h.
8. The method for preparing the ultrafine polyacrylonitrile fiber according to the claim 7, wherein in the step (3), the solvent in the coagulation bath is dimethyl sulfoxide (DMSO), the concentration is 25-30%, the temperature is controlled at 30 degrees +/-2 degrees, the coagulation time is 15min, after the coagulation is completed, the acrylic fiber enters a water washing tank, and the acrylic fiber is soaked and extruded in the water washing tank for multiple times, so that the DMSO residue in the fiber is less than or equal to 0.005%.
9. The method for preparing ultrafine polyacrylonitrile fiber according to claim 7, wherein in the step (4), the drawing temperature T is 80-100 ℃ and the drawing multiple DR is 3-4.
10. The method for preparing the ultrafine polyacrylonitrile fiber according to the claim 9, wherein the temperature of the water in the weight reduction pool in the step (4) is 90 ℃ to 100 ℃, and the weight reduction time is 5 to 8 minutes.
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Effective date of registration: 20231225 Address after: 315475 Jianmin Village, Xiaocao'e Town, Yuyao City, Ningbo City, Zhejiang Province Applicant after: Ningbo Hengqide Chemical Fiber Technology Co.,Ltd. Address before: 251507 North side of Kaiyuan Street (Linpan Section), Linyi County, Dezhou City, Shandong Province West side of Linpan Middle School Applicant before: SHANDONG KEBEIER NONWOVEN MATERIALS TECHNOLOGY Co.,Ltd. |