CN111826739A - Preparation method of anti-pilling elastic fiber material - Google Patents

Preparation method of anti-pilling elastic fiber material Download PDF

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CN111826739A
CN111826739A CN202010593708.8A CN202010593708A CN111826739A CN 111826739 A CN111826739 A CN 111826739A CN 202010593708 A CN202010593708 A CN 202010593708A CN 111826739 A CN111826739 A CN 111826739A
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CN111826739B (en
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史强文
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Wuxi Hongdou Sports Technology Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/15Proteins or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35Abrasion, pilling or fibrillation resistance

Abstract

The invention relates to a preparation method of an anti-pilling elastic fiber material, and belongs to the technical field of textile fabrics. According to the technical scheme, the nano gel material is matched with the silk protein dialysate, so that the bonding fastness of the fiber and the finishing agent is effectively improved, the directional friction effect of the polyester fiber in the using process is reduced, the directional friction effect of the polyester fiber is further improved in the using process, silk fibroin is used as the finishing agent material, the anti-pilling performance of the material is further improved through film forming, meanwhile, the low-temperature sol coating is carried out, the structural anti-pilling performance of the material is firstly improved, meanwhile, the polyester fiber is rapidly cooled, and the prepared polyester fiber is good in stability, good in elasticity and excellent in mechanical property.

Description

Preparation method of anti-pilling elastic fiber material
Technical Field
The invention relates to a preparation method of an anti-pilling elastic fiber material, and belongs to the technical field of textile fabrics.
Background
The elastic polyester fiber family comprises stretch yarn, PBT fiber, PTT fiber, polyether fiber, composite polyester fiber (PET/PTT, PET/PBT, modified PET/conventional PET, etc.). Although all of the polyester groups are different from each other in the mechanism of elasticity. Usually, a pre-oriented yarn or a fully drawn yarn is processed into a yarn with a small spring-like crimp by twisting deformation or twisting-shaping-untwisting process. The elasticity of the yarn is not strong, the tension is preferably small when the yarn is processed at high temperature, and the time cannot be long, because the elasticity of the textile is greatly reduced along with the loosening or disappearance of the spring form. The macromolecular chains in the crystal region of the PBT polymer are in a planar zigzag shape and are not completely unfolded, 4 methylene flexible groups are arranged in each PBT macromolecular repeating unit, and in the process of strain caused by stress action, reversible conversion from an a crystal form to a p crystal form is generated in the lattice structure of the PBT polymer. The reversible structural change endows the PBT fiber with excellent elastic performance. In addition, PBT can also be used in other fields, such as a nano coating material obtained by compounding with an inorganic oxide, and the like, compared with an even number of methylene units in the chemical structures of PET and PBT, PTT has 3 methylene units between terephthalic acid units, and the odd number of methylene units in the chemical structures can generate an odd carbon effect among macromolecular chains.
Disclosure of Invention
The invention aims to provide an anti-pilling elastic fiber material and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the anti-pilling elastic fiber material is prepared by stretching a modified polyester spinning material and then carrying out low-temperature finishing by using a finishing agent, wherein the modified polyester is prepared by taking purified terephthalic acid and ethylene glycol as raw materials, adding deionized water, carbon nano tubes, tetrabutyl titanate and a catalyst and carrying out vacuum polycondensation, the finishing agent is prepared by dissolving ethanol, calcium chloride and degummed silk and then carrying out dialysis treatment, adding nano titanium dioxide sol and sodium sulfite and then carrying out dispersion grinding.
The preparation steps of the modified polyester are as follows: s1: respectively taking deionized water, carbon nano tubes and tetrabutyl titanate, stirring and mixing, placing in a three-neck flask, heating by a programmed temperature and reacting while keeping the temperature to obtain modified slurry; s2: and respectively putting the catalyst, ethylene glycol, the modified slurry and the purified terephthalic acid into a reaction kettle, stirring and mixing, introducing nitrogen to remove air, vacuumizing and pressurizing by introducing nitrogen again in the nitrogen atmosphere, carrying out heat preservation reaction and vacuumizing treatment, carrying out heat preservation polycondensation, standing and cooling to room temperature to obtain the modified polyester particles.
The preparation method of the anti-pilling elastic fiber material comprises the following specific preparation steps: (1) respectively placing ethanol solution, calcium chloride and degummed silk into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into a dialysis bag, performing dialysis treatment to obtain dialysis modified solution, adding tetrabutyl titanate into acetic acid solution, stirring and mixing to obtain nano sol solution, then respectively placing the nano sol solution, the dialysis modified solution and sodium sulfite solution into a mortar, grinding, dispersing and collecting dispersed slurry, passing the dispersed slurry through a screen, collecting the mixed slurry, standing and aging to obtain sol modified solution; (2) respectively taking deionized water, carbon nano tubes and tetrabutyl titanate, stirring, mixing, placing in a three-neck flask, heating by temperature programming, carrying out heat preservation reaction to obtain modified slurry, then respectively taking a catalyst, ethylene glycol, the modified slurry and purified terephthalic acid, placing in a reaction kettle, stirring, mixing, introducing nitrogen to remove air, vacuumizing and then pressurizing by nitrogen under the atmosphere of nitrogen, carrying out heat preservation reaction, carrying out vacuum treatment, carrying out heat preservation polycondensation, standing and cooling to room temperature to obtain modified polyester particles; the water content of the slices is lower through low-temperature long-time drying, and the temperature control in the spinning process is facilitated; (3) drying the modified polyester particles at low temperature, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, adjusting the spinning temperature, carrying out traction and stretching treatment, collecting spinning fibers, carrying out low-temperature finishing on the spinning fibers by using a sol modification solution, drying the spinning fibers to constant weight, standing and cooling the spinning fibers to room temperature, thus obtaining the anti-pilling elastic fiber material.
The catalyst is ethylene glycol titanium.
The low-temperature finishing temperature is 0-5 ℃; the polyester fiber is rapidly cooled, the melt can be rapidly cooled, the internal micro-crystalline structure is changed, the strength of a single fiber is increased, the strength of the obtained fiber web is also increased, other qualities are correspondingly improved, and the prepared polyester fiber is good in stability, good in elasticity and excellent in mechanical property.
And the vacuum treatment and the heat preservation polycondensation are carried out for 25-30 min at the temperature of 220-250 ℃, the vacuum pumping is carried out until the pressure is 40-50 Pa, and the heat preservation polycondensation is carried out for 2-3 h.
The traction multiplying power of the traction and stretching treatment is 3.2-3.5; optimize the draw ratio and improve the tensile rate, improve and draw the in-process, the macromolecule shortens orientation time under the tensile tension effect, come insufficient orientation, cause strand silk intensity to descend, the phenomenon that the extension is prolonged, rethread high-speed forced air cooling handles spinning fibre, make polyester fiber cool down rapidly, reduce the inside macromolecule of solution that takes place on traditional curtain net under the high temperature no tension state and separate and straighten, separate orientation and the decrystallization motion, the polyester fiber stability that makes the preparation is good, and elasticity is good, and mechanical properties is excellent.
The spinning temperature is 280-285 ℃; the spinning temperature is optimized, so that the spinning fiber structure is excellent.
Compared with the prior art, the invention has the beneficial effects that: (1) the technical scheme of the invention adopts the nanometer gel material to be matched with the fibroin dialysate, the fibroin has good film forming property on the fiber surface, the polyester fiber surface with damaged scale layers is repaired, the fiber surface is smoother, the coefficients of forward and reverse friction are obviously reduced, the directional friction effect on the fiber surface is greatly reduced, the balling-up performance of the clothing fiber material is improved, and meanwhile, the nanometer gel material has the function of forming crystalline TiO2 at a lower temperature through spontaneous crystallization of an inorganic product, so that the nanometer titanium dioxide gel is taken as a matrix gel material and is combined with C-O, -O-C-O, -COH, -COOH and CH2-OH groups contained on the fiber material surface, and the groups and titanium dioxide finishing liquid generate chemical reaction in active groups, thereby effectively improving the combination fastness of the fibers and the finishing agent, the bonding strength between the finishing agent material and the fibers is effectively improved, then the polyester fiber material is repaired by the fibroin, the directional friction effect of the polyester fibers in the using process is reduced, the directional friction effect of the polyester fibers in the using process is further improved, and the silk fibroin is used as the finishing agent material to further form a film and improve the anti-pilling performance of the material;
(2) according to the technical scheme, the carbon nanotube material is added, so that the rigidity of a molecular chain can be improved and the free volume of a matrix can be reduced due to the fact that the carbon nanotube has high rigidity when the polyurethane material is prepared, gaps among the molecular chains are reduced, small molecule permeation is blocked, the structural strength and the mechanical property of the polyester material are improved, and then the polyester particles with high viscosity are prepared by polycondensation and serve as polyester stretch yarn products, so that the production cost is low, the elasticity and the hand feeling of the polyester fabric can be improved, the products are resistant to chlorine bleaching, and the chemical stability is excellent;
(3) through the coating of the low-temperature sol, the structural anti-pilling performance of the material is improved, meanwhile, the polyester fiber is rapidly cooled, so that a molten melt can be rapidly cooled, the internal micro-crystalline structure is changed, the strength of a single fiber is increased, the strength of an obtained fiber web is also increased, other qualities are correspondingly improved, and the prepared polyester fiber is good in stability, elasticity and mechanical property.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Respectively weighing 25-30 parts by weight of 15% ethanol solution, 3-5 parts by weight of calcium chloride and 3-5 parts by weight of degummed silk, placing the materials into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into dialysis bags, respectively placing the dialysis bags with molecular weights of 3500, 7000 and 14000 for dialysis treatment in sequence, and collecting to obtain dialysis modified solution; adding tetrabutyl titanate into 50% acetic acid solution by mass ratio of 1:20, stirring and mixing to obtain a nano sol solution, respectively weighing 45-50 parts of nano sol solution, 25-30 parts of dialysis modified solution and 6-8 parts of sodium sulfite solution with mass fraction of 5% in a mortar by weight, grinding, dispersing and collecting dispersed slurry, passing the dispersed slurry through a 0.25-0.28 mu m screen, filtering and collecting the mixed slurry, and standing and aging for 6-8 hours to obtain sol modified solution; respectively weighing 45-50 parts by weight of deionized water, 6-8 parts by weight of carbon nano tubes and 10-15 parts by weight of tetrabutyl titanate, stirring, mixing, placing in a three-neck flask, heating to 150-160 ℃ at a speed of 5 ℃/min, and carrying out heat preservation reaction for 3-5 hours to obtain modified slurry; respectively weighing 1-2 parts by weight of catalyst, 10-20 parts by weight of ethylene glycol, 6-8 parts by weight of modified slurry and 35-40 parts by weight of purified terephthalic acid, placing the materials into a reaction kettle, stirring and mixing the materials, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 45-50 mL/min, vacuumizing the reaction kettle to 450-500 Pa under the nitrogen atmosphere, then introducing the nitrogen to the reaction kettle according to the proportion of 45-50 mL/min, introducing the nitrogen to pressurize to 2-3 kPa, then carrying out heat preservation reaction at 220-250 ℃ for 25-30 min, vacuumizing the reaction kettle to 40-50 Pa, carrying out heat preservation polycondensation for 2-3 h, standing and cooling the reaction product to room temperature to obtain modified polyester particles; placing the modified polyester particles at 100-110 ℃ for heat preservation and drying for 6-8 h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 280-285 ℃, performing traction and stretching treatment under the traction and stretching ratio of 3.2-3.5, collecting spinning fibers, cooling the spinning fibers in sol modification liquid at 0-5 ℃ for 3-5 s at the speed of 10m/s, drying at 100-110 ℃ to constant weight, standing and cooling to room temperature, and thus obtaining the anti-spherical-rising elastic fiber material.
Example 1
Respectively weighing 25 parts by weight of 15% ethanol solution, 3 parts by weight of calcium chloride and 3 parts by weight of degummed silk, placing the materials into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into dialysis bags, respectively placing the dialysis bags with molecular weights of 3500, 7000 and 14000 in sequence for dialysis treatment, and collecting to obtain dialysis modified solution; adding tetrabutyl titanate into 50% acetic acid solution in parts by mass according to the mass ratio of 1:20, stirring and mixing to obtain a nano sol solution, respectively weighing 45 parts of the nano sol solution, 25 parts of dialysis modified solution and 6 parts of sodium sulfite solution with the mass fraction of 5% in a mortar in parts by weight, grinding, dispersing and collecting dispersed slurry, passing the dispersed slurry through a 0.25 mu m screen, filtering and collecting the mixed slurry, standing and aging for 6 hours to obtain sol modified solution; respectively weighing 45 parts of deionized water, 6 parts of carbon nano tube and 10 parts of tetrabutyl titanate according to parts by weight, stirring, mixing, placing in a three-neck flask, heating to 150 ℃ at the speed of 5 ℃/min, and carrying out heat preservation reaction for 3 hours to obtain modified slurry; respectively weighing 1 part of catalyst, 10 parts of ethylene glycol, 6 parts of modified slurry and 35 parts of purified terephthalic acid in parts by weight, placing the mixture in a reaction kettle, stirring and mixing the mixture, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 45mL/min, vacuumizing the mixture to 450Pa in the nitrogen atmosphere, introducing the nitrogen into the reaction kettle according to the ratio of 45mL/min, introducing the nitrogen to pressurize the mixture to 2kPa, carrying out heat preservation reaction at 220 ℃ for 25min, vacuumizing the mixture to 40Pa, carrying out heat preservation polycondensation for 2-3 h, standing the mixture and cooling the mixture to room temperature to obtain modified polyester particles; placing the modified polyester particles at 100 ℃ for heat preservation and drying for 6h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 280 ℃, carrying out traction and stretching treatment at a traction and stretching ratio of 3.2, collecting spinning fibers, cooling the spinning fibers in sol modification liquid at 0 ℃ for 3s at a speed of 10m/s, drying to constant weight at 100 ℃, standing and cooling to room temperature, thus obtaining the anti-pilling elastic fiber material.
Example 2
Respectively weighing 27 parts by weight of 15% ethanol solution, 4 parts by weight of calcium chloride and 4 parts by weight of degummed silk, placing the 15% ethanol solution, the 4 parts by weight of calcium chloride and the 4 parts by weight of degummed silk into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into dialysis bags, respectively placing the dialysis bags with molecular weights of 3500, 7000 and 14000 in sequence for dialysis treatment, and collecting to obtain dialysis modified solution; adding tetrabutyl titanate into 50% acetic acid solution in parts by mass according to the mass ratio of 1:20, stirring and mixing to obtain a nano sol solution, respectively weighing 47 parts of nano sol solution, 27 parts of dialysis modified solution and 7 parts of sodium sulfite solution with the mass fraction of 5% in a mortar, grinding and dispersing and collecting dispersed slurry, passing the dispersed slurry through a 0.27 mu m screen, filtering and collecting the mixed slurry, and standing and aging for 7 hours to obtain sol modified solution; respectively weighing 47 parts of deionized water, 7 parts of carbon nano tube and 12 parts of tetrabutyl titanate by weight, stirring, mixing, placing in a three-neck flask, heating to 155 ℃ at the speed of 5 ℃/min, and carrying out heat preservation reaction for 4 hours to obtain modified slurry; respectively weighing 1 part of catalyst, 15 parts of ethylene glycol, 7 parts of modified slurry and 37 parts of purified terephthalic acid in parts by weight, placing the mixture in a reaction kettle, stirring and mixing the mixture, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 47mL/min, vacuumizing the reaction kettle to 475Pa in the nitrogen atmosphere, introducing the nitrogen into the reaction kettle according to the volume of 47mL/min, introducing the nitrogen to pressurize to 2kPa, then carrying out heat preservation reaction at 235 ℃ for 27min, vacuumizing the reaction kettle to 42Pa, carrying out heat preservation polycondensation for 2h, standing and cooling the reaction kettle to room temperature to obtain modified polyester particles; placing the modified polyester particles at 105 ℃ for heat preservation and drying for 7h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 282 ℃, carrying out traction and stretching treatment at a traction and stretching ratio of 3.4, collecting spinning fibers, cooling the spinning fibers in sol modification liquid at 3 ℃ for 4s at a speed of 10m/s, drying to constant weight at 105 ℃, standing and cooling to room temperature, thus obtaining the anti-pilling elastic fiber material.
Example 3
Respectively weighing 30 parts by weight of 15% ethanol solution, 5 parts by weight of calcium chloride and 5 parts by weight of degummed silk, placing the materials into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into dialysis bags, respectively placing the dialysis bags with molecular weights of 3500, 7000 and 14000 in sequence for dialysis treatment, and collecting to obtain dialysis modified solution; adding tetrabutyl titanate into 50 mass parts of 50% acetic acid solution according to a mass ratio of 1:20, stirring and mixing to obtain a nano sol solution, respectively weighing 50 weight parts of nano sol solution, 30 weight parts of dialysis modified solution and 8 weight parts of 5 mass% sodium sulfite solution, placing the nano sol solution, 30 weight parts of dialysis modified solution and 8 weight parts of 5 mass% sodium sulfite solution into a mortar, grinding and dispersing and collecting dispersed slurry, passing the dispersed slurry through a 0.28 mu m screen, filtering and collecting mixed slurry, and standing and aging for 8 hours to obtain sol modified solution; respectively weighing 50 parts by weight of deionized water, 8 parts by weight of carbon nano tube and 15 parts by weight of tetrabutyl titanate, stirring, mixing, placing in a three-neck flask, heating to 160 ℃ at a speed of 5 ℃/min, and carrying out heat preservation reaction for 5 hours to obtain modified slurry; respectively weighing 2 parts of catalyst, 20 parts of ethylene glycol, 8 parts of modified slurry and 40 parts of purified terephthalic acid in parts by weight, placing the mixture in a reaction kettle, stirring and mixing the mixture, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 50mL/min, vacuumizing the reaction kettle to 500Pa in the nitrogen atmosphere, introducing the nitrogen into the reaction kettle according to the ratio of 50mL/min, introducing the nitrogen to pressurize the nitrogen to 3kPa, then carrying out heat preservation reaction at 250 ℃ for 30min, vacuumizing the reaction kettle to 50Pa, carrying out heat preservation polycondensation for 3h, standing the reaction kettle and cooling the reaction kettle to room temperature to obtain modified polyester particles; placing the modified polyester particles at 110 ℃ for heat preservation and drying for 8h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 285 ℃, carrying out traction and stretching treatment at a traction and stretching ratio of 3.5, collecting spinning fibers, cooling the spinning fibers in sol modification liquid at 5 ℃ for 5s at a speed of 10m/s, drying to constant weight at 110 ℃, standing and cooling to room temperature, thus obtaining the anti-pilling elastic fiber material.
Example 4
Respectively weighing 27 parts by weight of 15% ethanol solution, 4 parts by weight of calcium chloride and 4 parts by weight of degummed silk, placing the 15% ethanol solution, the 4 parts by weight of calcium chloride and the 4 parts by weight of degummed silk into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into dialysis bags, respectively placing the dialysis bags with molecular weights of 3500, 7000 and 14000 in sequence for dialysis treatment, and collecting to obtain dialysis modified solution; adding tetrabutyl titanate into 50% acetic acid solution in parts by mass according to the mass ratio of 1:20, stirring and mixing to obtain a nano sol solution, respectively weighing 47 parts of nano sol solution, 27 parts of dialysis modified solution and 7 parts of sodium sulfite solution with the mass fraction of 5% in a mortar, grinding and dispersing and collecting dispersed slurry, passing the dispersed slurry through a 0.27 mu m screen, filtering and collecting the mixed slurry, and standing and aging for 7 hours to obtain sol modified solution; respectively weighing 1 part of catalyst, 12 parts of ethylene glycol and 37 parts of purified terephthalic acid in parts by weight, placing the mixture in a reaction kettle, stirring and mixing the mixture, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 47mL/min, vacuumizing the reaction kettle to 475Pa in the nitrogen atmosphere, introducing the nitrogen into the reaction kettle according to the nitrogen concentration of 47mL/min, introducing the nitrogen to pressurize to 2kPa, then carrying out heat preservation reaction at 235 ℃ for 27min, vacuumizing the reaction kettle to 45Pa, carrying out heat preservation polycondensation for 2h, standing the reaction kettle and cooling the reaction kettle to room temperature to obtain modified polyester particles; placing the modified polyester particles at 105 ℃ for heat preservation and drying for 7h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 282 ℃, carrying out traction and stretching treatment at a traction and stretching ratio of 3.4, collecting spinning fibers, cooling the spinning fibers in sol modification liquid at 3 ℃ for 4s at a speed of 10m/s, drying to constant weight at 100-110 ℃, standing and cooling to room temperature, thus obtaining the anti-pilling elastic fiber material.
Example 5
Respectively weighing 1 part of catalyst, 12 parts of ethylene glycol and 37 parts of purified terephthalic acid in parts by weight, placing the mixture in a reaction kettle, stirring and mixing the mixture, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 47mL/min, vacuumizing the reaction kettle to 475Pa in the nitrogen atmosphere, introducing the nitrogen into the reaction kettle according to the nitrogen concentration of 47mL/min, introducing the nitrogen to pressurize to 2kPa, then carrying out heat preservation reaction at 235 ℃ for 27min, vacuumizing the reaction kettle to 45Pa, carrying out heat preservation polycondensation for 2h, standing the reaction kettle and cooling the reaction kettle to room temperature to obtain modified polyester particles; and (2) placing the modified polyester particles at 105 ℃ for heat preservation and drying for 7h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 282 ℃, carrying out traction and stretching treatment at a traction and stretching ratio of 3.4, collecting spinning fibers, drying at 100-110 ℃ to constant weight, standing and cooling to room temperature, and thus obtaining the anti-pilling elastic fiber material.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
The performance tests of the embodiment 1, the embodiment 2, the embodiment 3, the embodiment 4 and the embodiment 5 are performed, the embodiment 4 is a composite polyester fiber prepared without adding carbon nanotubes, the embodiment 5 is a polyester fiber prepared without adopting a low-temperature finishing technical scheme, and the mechanical strength is specifically tested as follows:
and (3) testing mechanical properties: YG061 electronic yarn stretching instrument. The parameters are set according to GB/T14344-2003 Standard "test methods for tensile Properties of synthetic filaments". The test is carried out under the conditions of constant temperature and constant humidity, the temperature is (20.0 +/-2.0) ° C, and the relative humidity is (65 +/-2)%.
Specific test results are shown in table 1.
TABLE 1 comparison of Properties
Figure DEST_PATH_IMAGE001
(1) Comparing examples 1, 2, 3, 4 and 5 of the present invention, the fracture strength and fracture productivity of example 5 are far less than those of examples 1, 2 and 3, which shows that in the technical scheme of the present invention, by low temperature sol coating, the structural anti-pilling performance of the material is firstly improved, and simultaneously the polyester fiber is rapidly cooled, so that the molten melt can be rapidly cooled, the internal micro-crystalline structure will be changed, the strength of the single fiber will be increased, the strength of the obtained fiber web will be increased, other qualities will be correspondingly improved, and the prepared polyester fiber has good stability, good elasticity and excellent mechanical properties.
(2) Comparing example 1, example 2, example 3, example 4 and example 5 of the present invention, the elongation at break and the breaking strength in example 4 are significantly reduced, because the carbon nanotube material is added to make the polyurethane material in the preparation process, because the carbon nanotube has greater rigidity, the introduction into the polyester molecular chain can increase the rigidity of the molecular chain and reduce the free volume of the matrix, thereby reducing the gaps between the molecular chains, playing a role in blocking the permeation of small molecules and improving the structural strength and mechanical properties of the polyester material, and then the melt high viscosity polyester particles prepared by polycondensation are used as polyester stretch yarn products, which has low production cost, can improve the elasticity and hand feeling of the polyester fabric, and the products are resistant to chlorine bleaching, and have excellent chemical stability.
(3) By observing the directional friction coefficient of the embodiment 5 and other embodiments, the friction coefficient of the embodiment 5 is obviously increased, which shows that the technical scheme that the directional friction effect of the polyester fiber is reduced in the using process by adopting the nano gel material to be matched with the silk protein dialysate, the directional friction effect of the polyester fiber is further improved in the using process, and the silk protein is used as a finishing agent material to further form a film to improve the anti-pilling performance of the material is established.

Claims (1)

1. The preparation method of the anti-pilling elastic fiber material is characterized by comprising the following specific preparation steps:
(1) respectively weighing 30 parts by weight of 15% ethanol solution, 5 parts by weight of calcium chloride and 5 parts by weight of degummed silk, placing the materials into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into dialysis bags, respectively placing the dialysis bags with molecular weights of 3500, 7000 and 14000 in sequence for dialysis treatment, and collecting to obtain dialysis modified solution; adding tetrabutyl titanate into 50 mass parts of 50% acetic acid solution according to a mass ratio of 1:20, stirring and mixing to obtain a nano sol solution, respectively weighing 50 weight parts of nano sol solution, 30 weight parts of dialysis modified solution and 8 weight parts of 5 mass% sodium sulfite solution, placing the nano sol solution, 30 weight parts of dialysis modified solution and 8 weight parts of 5 mass% sodium sulfite solution into a mortar, grinding and dispersing and collecting dispersed slurry, passing the dispersed slurry through a 0.28 mu m screen, filtering and collecting mixed slurry, and standing and aging for 8 hours to obtain sol modified solution;
(2) respectively weighing 50 parts by weight of deionized water, 8 parts by weight of carbon nano tube and 15 parts by weight of tetrabutyl titanate, stirring, mixing, placing in a three-neck flask, heating to 160 ℃ at a speed of 5 ℃/min, and carrying out heat preservation reaction for 5 hours to obtain modified slurry; respectively weighing 2 parts of catalyst, 20 parts of ethylene glycol, 8 parts of modified slurry and 40 parts of purified terephthalic acid in parts by weight, placing the mixture in a reaction kettle, stirring and mixing the mixture, introducing nitrogen to remove air, controlling the introduction rate of the nitrogen to be 50mL/min, vacuumizing the reaction kettle to 500Pa in the nitrogen atmosphere, introducing the nitrogen into the reaction kettle according to the ratio of 50mL/min, introducing the nitrogen to pressurize the nitrogen to 3kPa, then carrying out heat preservation reaction at 250 ℃ for 30min, vacuumizing the reaction kettle to 50Pa, carrying out heat preservation polycondensation for 3h, standing the reaction kettle and cooling the reaction kettle to room temperature to obtain modified polyester particles;
(3) placing the modified polyester particles at 110 ℃ for heat preservation and drying for 8h, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, controlling the spinning temperature of the spinning device to be 285 ℃, carrying out traction and stretching treatment at a traction and stretching ratio of 3.5, collecting spinning fibers, cooling the spinning fibers in sol modification liquid at 5 ℃ for 5s at a speed of 10m/s, drying to constant weight at 110 ℃, standing and cooling to room temperature, thus obtaining the anti-pilling elastic fiber material.
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