CN117286609B - Bio-based yarn and vortex spinning preparation method thereof - Google Patents

Bio-based yarn and vortex spinning preparation method thereof Download PDF

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CN117286609B
CN117286609B CN202311588689.XA CN202311588689A CN117286609B CN 117286609 B CN117286609 B CN 117286609B CN 202311588689 A CN202311588689 A CN 202311588689A CN 117286609 B CN117286609 B CN 117286609B
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spinning
bio
rpm
parts
fiber
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CN117286609A (en
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陈路
张仕成
孔国庆
徐庆红
胡宁华
李长红
孙磊
冷如波
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Wujiang Jingyi Special Fiber Co ltd
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Wujiang Jingyi Special Fiber Co ltd
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    • 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
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • 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
    • D01HSPINNING OR TWISTING
    • D01H4/00Open-end spinning machines or arrangements for imparting twist to independently moving fibres separated from slivers; Piecing arrangements therefor; Covering endless core threads with fibres by open-end spinning techniques
    • D01H4/02Open-end spinning machines or arrangements for imparting twist to independently moving fibres separated from slivers; Piecing arrangements therefor; Covering endless core threads with fibres by open-end spinning techniques imparting twist by a fluid, e.g. air vortex
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02Yarns or threads characterised by the material or by the materials from which they are made
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20Cellulose-derived artificial fibres
    • D10B2201/22Cellulose-derived artificial fibres made from cellulose solutions
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/66Disintegrating fibre-containing textile articles to obtain fibres for re-use

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a bio-based yarn and a vortex spinning preparation method thereof, wherein the bio-based yarn is obtained by introducing pretreated graphene oxide and a modifier into cellulose spinning solution and adopting a wet spinning process; and then the vortex spinning biological base yarn is prepared through the procedures of opening and picking, carding, drawing, vortex spinning, inspection, warehousing, doubling, double twisting and warehousing. Compared with the prior art, the method can realize good stretching and directional arrangement of fibers, improve spinning efficiency and yarn quality, enhance mechanical property and thermal stability of the bio-based yarn through preparation of the bio-based fibers, and improve comprehensive performance of the bio-based yarn.

Description

Bio-based yarn and vortex spinning preparation method thereof
Technical Field
The invention relates to the technical field of spinning, in particular to a bio-based yarn and a vortex spinning preparation method thereof.
Background
At present, the vortex spinning preparation method of the bio-based yarn mainly comprises the following several prior arts: in the solution spinning method, a solution of the bio-based fiber is extruded through a spinning nozzle to form fiber yarn, and then the fiber yarn is prepared into yarn through the process steps of solidification, stretching, winding and the like. In vortex spinning preparation, commonly used bio-based fiber solutions include cellulose solutions, protein solutions, polylactic acid solutions, and the like. In the melt spinning method, a bio-based polymer (such as polylactic acid, polyhydroxyalkanoate and the like) is subjected to a melting and extrusion process to form fiber filaments, and then the fiber filaments are prepared into yarns through steps of stretching, cooling, winding and the like. The method is suitable for bio-based fibers with certain meltability. Dry spinning process, extruding dry fiber bundle of biological base fiber through spinning nozzle, stretching, winding and other technological steps to prepare yarn. The method is generally applicable to biobased fibers having relatively high fiber strength and length. The wet spinning method is to extrude cellulose solution of biological base fiber through a spinning nozzle, and then to solidify, stretch and wind in a coagulating bath to prepare yarn. The method is suitable for preparing cellulose-based bio-based fibers.
The cellulose-based bio-based fiber is prepared by pretreating natural cellulose materials (such as wood pulp, cotton, etc.) in alkaline or acidic solution to remove non-cellulose components, and dissolving and regenerating the cellulose by alkali method to obtain the cellulose-based bio-based fiber. The prior art of cellulose-based bio-based fibers still has the defects of poor mechanical properties and insufficient thermal stability. Despite some drawbacks, with the continued development and improvement of technology, the performance of cellulose-based bio-based fibers is expected to be improved, further pushing the application and popularization of bio-based fibers.
The invention patent CN115161842B of Chinese patent application discloses a seaweed modified fiber blended fabric and a preparation method thereof, the seaweed modified fiber blended fabric comprises warp yarns and weft yarns, the weft yarns are blended yarns made of cotton fibers and seaweed modified cellulose fibers, the seaweed modified cellulose fibers are prepared by adding seaweed powder into a spinning solution of cellulose fibers and through a spinning process, and the blending ratio of the cotton fibers and the seaweed modified cellulose fibers in the blended yarns is 50-74%: 26-50%. According to the seaweed modified fiber blended fabric and the preparation method thereof, cotton fibers and seaweed modified cellulose fibers are blended to prepare blended yarns, and the blended yarns are used as weft yarns to weave the fabric, so that the prepared seaweed modified fiber blended fabric contains amino acids and trace elements, has antibacterial and antioxidant properties, is not influenced in the processes of use, washing and dry cleaning, and has good tensile breaking strength. But the seaweed modified fiber prepared by the invention has poor mechanical property and low thermal stability.
Disclosure of Invention
In view of the defects of poor mechanical property and low thermal stability of the bio-based yarn in the prior art, the invention aims to provide the bio-based yarn with high mechanical property and good thermal stability and the vortex spinning preparation method thereof.
In order to achieve the above object, the present invention adopts the following technical scheme:
a vortex spinning preparation method of a bio-based yarn comprises the following steps:
step 1, opening and picking: processing the bio-based fiber by adopting a cotton opener;
step 2, carding cotton: feeding the biological base fiber subjected to opening and picking treatment into a carding machine;
step 3, drawing: feeding the combed biological base fiber into a drawing frame to obtain a cooked strip;
step 4, vortex spinning: vortex spinning the cooked strips;
step 5, checking: detecting cotton knots, semi-finished strips, finished sliver evenness, coarse and fine materials and cotton knots, performing spot check on semi-finished products or finished products in each working procedure in production, performing periodic spot check and real-time spot check, and checking whether the semi-finished products or the finished products in each working procedure meet the quality control requirement through data check analysis;
step 6, warehouse entry: warehouse entry is performed after the quality control requirement is met;
step 7, doubling: doubling the warehoused yarns, and selecting two yarns to be combined into one yarn, wherein the doubling speed is 300-500 rpm;
step 8, double twisting: the speed of the double twisting is 4000-6000 rpm, the twist is 50-100 twists/m, and the twisting direction is S;
step 9, warehouse entry: and (5) achieving the quality control requirement and warehousing.
Preferably, the rotation speed of the beater bar of the cotton opener in the step 1 is 400-450 rpm, the interval between the cotton feeding roller and the beater bar is 9-10 mm, the interval between the dust bar and the dust bar is 8-9 mm, the interval between the dust bar and the beater bar is 8-10 mm at the inlet, 18-19 mm at the outlet, the interval between the beater bar and the cotton stripping knife is 1.5-2.5 mm, and the speed of the lap roller is 10-12 rpm; the dry basis weight of the cotton rolls is 350-400 g/m, and the length of the cotton rolls is 28-35 m.
Preferably, the cotton carding process in the step 2 is configured as follows: the speed of the cylinder is 350-420 rpm, the speed of the licker-in is 750-800 rpm, the speed of the cover plate is 130-150 mm/min, the speed of the doffer is 20-24 rpm, the gauge of the cylinder and the front fixed cover plate is 0.08-0.12 mm multiplied by 0.08-0.1 mm, the gauge of the cylinder and the rear fixed cover plate is 0.08-0.12 mm multiplied by 0.1-0.14 mm, the gauge of the cylinder-licker-in is 0.05-0.08 mm, the gauge of the cylinder-doffer is 0.04-0.06 mm, the sliver outlet speed is 50-80 m/min, and the dry basis weight of the cotton sliver is 18-24 g/5m.
Preferably, three drawing steps are adopted in the step 3, and main process parameters are as follows: the head roller interval is 10-12 multiplied by 8-9 multiplied by 17-19 mm, the back zone draft multiple is 1.2-1.8 times, the total draft multiple is 4-8 times, and the total number of the combined strips is 2-8; the interval between the two doubling rollers is 10-12 multiplied by 8-9 multiplied by 17-19 mm, the draft multiple of the rear zone is 1.2-1.8 times, the total draft multiple is 4-10 times, and the doubling number is 2-8; the three combining rollers are spaced by 8-12 multiplied by 8-9 multiplied by 16-18 mm, the back zone draft multiple is 1.2-1.4 times, the total draft multiple is 4-10 times, and the combining number is 2-8.
Preferably, the vortex spinning process in the step 4 is configured as follows: the air flow temperature is controlled at 20-30 ℃, the relative humidity is controlled at 60-70%, the spinning speed is 300-360 rpm, the total draft is 150-250, the main draft is 20-40, the feeding ratio is 0.94-1.1, the crimping ratio is 0.8-1.1, and the BR initiation rate is 90-100%.
The preparation method of the bio-based fiber comprises the following steps of:
s1, adding 1800-2200 parts of 0.2-0.3 wt% graphene oxide aqueous solution into a three-necked flask, stirring at 1500-2500 rpm in a water bath at 60-80 ℃ for 15-25 min, adding 70-90 parts of 2-3 wt% ammonium persulfate aqueous solution, and stirring at 100-500 rpm for 10-30 min; then adding 180-220 parts of 3-8 wt% N-carbamoyl maleic acid aqueous solution, stirring for 0.5-2 hours at 100-500 rpm at 60-80 ℃, adding 15-25 parts of 2-3 wt% ammonium persulfate aqueous solution, stirring for 1-3 hours at 100-500 rpm at 70-90 ℃, then raising the reaction temperature to 90-98 ℃, adding 180-220 parts of 20-30 wt% ascorbic acid aqueous solution, stirring for 3-5 hours at 180-220 parts rpm, filtering, washing for 2-4 times with water and absolute ethyl alcohol, and vacuum freeze-drying for 5-20 hours to obtain pretreated graphene oxide;
s2, adding 180-220 parts of 2, 4-diamino-1, 3, 5-triazine, 100-240 parts of paraformaldehyde and 20-30 parts of formaldehyde into 300-500 parts of water, stirring at 100-500 rpm for 2-8 hours at 50-70 ℃, adding 8-12 parts of parahydroxybenzaldehyde, stirring at 100-500 rpm for 2-5 hours at 70-90 ℃, and regulating the pH to 6.5-7.5 by using triethanolamine to obtain a modifier;
s3, mixing 0.5-2 parts of the pretreated graphene oxide prepared in the step S1 with 12-20 parts of 8-12 mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 1-3 hours, wherein the ultrasonic power is 100-300W, and the ultrasonic frequency is 30-60 kHz, so as to obtain a dispersion solution; adding the dispersion solution and 2-4 parts of the modifier prepared in the step S2 into 80-120 parts of cellulose spinning solution, and stirring at 1500-2500 rpm for 0.5-2 hours at room temperature to obtain spinning solution; injecting the spinning solution into a storage tank, degassing at a vacuum degree of-0.05 to-0.1 Mpa, and adopting a wet spinning process to obtain the bio-based fiber.
Preferably, the cellulose content in the cellulose spinning solution is 7-9wt% and the sodium hydroxide concentration is 4-5wt%.
Preferably, the wet spinning process is that the spinning solution is extruded to a coagulation bath through a porous spinneret with the spinning speed of 30-40 m/min, the diameter of the spinneret is 40-55 mu m, the number of holes is 180-220, and then the fiber is washed for 0.5-2 hours in an off-line way by water with the temperature of 60-80 ℃ and is air-dried in a tension-free way.
Preferably, the coagulation bath consists of 110-120 g/L sulfuric acid, 330-350 g/L sodium sulfate and 8-12 g/L zinc sulfate.
According to the invention, an in-situ grafting polymerization method is adopted to carry out surface modification on the graphene oxide nano-sheet, the amino group of the N-carbamyl maleic acid firstly reacts with the carboxyl group and the epoxy group on the surface or the edge of the graphene oxide, and then ammonium persulfate is used as an initiator to carry out in-situ free radical polymerization of the monomer. Then, the pretreated graphene oxide is obtained by reduction with ascorbic acid. Furthermore, dispersing the pretreated graphene oxide in a solvent is critical to obtaining a uniform polymer solution. By grafting N-carbamoylmaleic acid on the surface of graphene oxide, the interaction between pretreated graphene oxide and an organic solvent can be significantly improved. The presence of N-carbamoylmaleic acid enlarges the distance between the pretreated graphene oxides, thereby avoiding agglomeration and enhancing dispersion.
In the prior art, after the cellulose spinning solution is subjected to wet spinning, the obtained fiber is in a zigzag structure, and the main reason is that the cellulose spinning solution is solidified on the surface and then solidified inside. The surface of the bio-based fiber loaded with the pretreated graphene oxide and the modifier is relatively smooth, has no microcrack, and has compact and uniform structure. The possible reasons are mainly that the pretreated graphene oxide has a good interfacial interaction with the biomass fiber matrix. Compared with pure viscose fiber, the addition of the pretreated graphene oxide improves the tensile strength of the fiber. A strong non-covalent interaction, such as hydrogen bonding, may be created between the cellulose and the pretreated graphene oxide, and the addition of the pretreated graphene oxide promotes the orientation of the cellulose molecular chains along the fiber axis. The enhancement of the mechanical properties of the fibers is mainly benefited by the uniform dispersion and arrangement of the pretreated graphene oxide in the cellulose matrix. In addition, the compatibility and strong interaction of the pretreated graphene oxide and the cellulose matrix greatly enhance the dispersibility and interfacial adhesion of the pretreated graphene oxide, thereby remarkably improving the mechanical properties of the fiber. In addition, the addition of the pretreated graphene oxide improves the thermal stability of the bio-based fiber and shows higher thermal degradation temperature. This improved thermal stability may be attributed to the pretreated graphene oxide acting as a protective layer during combustion.
Further, the modifier is successfully incorporated into the biobased fiber, and the compatibility of the modifier with cellulose is good, which is mainly benefited by hydrogen bonds formed between hydroxyl groups, thereby replacing part of the surface grooves. The addition of modifiers to the fibrous structure may serve a heat stabilizing function. This is due to the cross-linking action with the modifier and the formation of more hydrogen bonds, which enhances the tensile properties of the biobased fiber, mainly due to the cross-linking interaction of the modifier molecules entangled with the biobased fiber, which creates a polymer network with the fiber, providing the fiber with greater fineness, initial modulus and elongation at break. In addition, hydrogen bonds can be formed through hydroxyl groups and amino groups, so that the elongation of the fiber at break is improved. The crosslinking interaction mainly consists in swelling cellulose by immersing it in aqueous sodium hydroxide solution, thereby improving its compatibility with 2, 4-diamino-1, 3, 5-triazine and making it intertwined. After the modifier is added into the cellulose alkaline solution, the modifier and the cellulose are easy to crosslink to form a network structure due to a large amount of amino groups and hydroxyl groups. Part of the modifier is separated out at the structure of the surface of the fiber and is wound around the fiber, so that part of grooves on the surface of the fiber are replaced, and the mechanical property of the fiber is improved.
Compared with the prior art, the invention has the beneficial effects that:
1) The vortex spinning preparation method of the bio-based yarn adopts pretreatment equipment such as a cotton opener, a carding machine, a drawing frame and the like, effectively removes impurities and short fibers in the fibers, improves the quality and uniformity of the fibers, and thus obtains high-quality fiber raw materials.
2) The invention can realize good stretching and directional arrangement of the fiber and improve spinning efficiency and yarn quality by adjusting vortex spinning process parameters such as air flow temperature, relative humidity, spinning speed and the like.
3) According to the invention, through carrying out spot check and data analysis on semi-finished products or finished products in each procedure, the quality problem in the production process can be detected and corrected in time, and the spinning quality is ensured to meet the requirements.
4) The invention adopts the bio-based fiber as the raw material, and the bio-based fiber is generally renewable and biodegradable, is environment-friendly, and is beneficial to reducing the dependence on limited resources and the negative influence on the environment.
5) According to the invention, through the introduction of the pretreatment graphene oxide and the modifier, the properties of the fiber, such as the mechanical property, the thermal stability and the like of the reinforced fiber, can be improved, and the comprehensive properties of the fiber can be improved.
6) The optimized technological parameters and equipment configuration of the invention can improve the production efficiency of spinning and reduce the energy consumption and the production cost, and the vortex spinning preparation method of the bio-based yarn has obvious advantages and beneficial effects in the aspects of spinning quality, environmental protection performance, production efficiency and the like.
Detailed Description
The main material sources are as follows:
graphene oxide: shenzhen Jianzhen technologies Co., ltd., product number: NA.
Paraformaldehyde: the Jinan century reaches chemical industry Co., ltd, model: 410.
cellulose: the chemical industry limited company is also bloged in great city county, goods number: 5865124.
polyvinyl alcohol: shanghai Xinheng New Material technology Co., ltd., brand: 1788.
example 1
A vortex spinning preparation method of a bio-based yarn comprises the following steps:
step 1, opening and picking: the bio-based fiber is processed by a cotton opener, wherein the rotating speed of a beater bar of the cotton opener is 430rpm, the interval between a cotton feeding roller and the beater bar is 9.5mm, the interval between a dust rod and the dust rod is 8.5mm, the interval between the dust rod and the beater bar is 9mm at an inlet, 18.5mm at an outlet, the interval between the beater bar and a cotton stripping knife is 2mm, and the speed of a cotton roll roller is 11rpm; the dry basis weight of the cotton roll is 380g/m, and the length of the cotton roll is 32m;
step 2, carding cotton: feeding the bio-based fibers subjected to opening and picking treatment into a carding machine, wherein the carding process comprises the following steps of: the cylinder speed is 390rpm, the licker-in speed is 780rpm, the cover plate speed is 145mm/min, the doffer speed is 22rpm, the gauge of the cylinder and the front fixed cover plate is 0.1mm multiplied by 0.09mm, the gauge of the cylinder and the rear fixed cover plate is 0.10mm multiplied by 0.11mm multiplied by 0.12mm, the gauge of the cylinder-licker-in is 0.07mm, the gauge of the cylinder-doffer is 0.05mm, the doffing speed is 70m/min, and the dry quantitative of cotton sliver is 20g/5m;
step 3, drawing: the biological base fiber after cotton carding is fed into a drawing frame, three drawing steps are adopted, and the main technological parameters are as follows: the head roller interval is 11 multiplied by 8.5 multiplied by 18mm, the back zone draft multiple is 1.61 times, the total draft multiple is 6.74 times, and the number of the combined yarns is 8; the interval between the two doubling rollers is 11 multiplied by 8.5 multiplied by 18mm, the back zone draft multiple is 1.45 times, the total draft multiple is 8.05 times, and the number of the doubling rollers is 8; the three combining rollers are spaced by 10 multiplied by 8.5 multiplied by 17mm, the back zone draft multiple is 1.25 times, the total draft multiple is 6.09 times, and the combining number is 6, so that cooked strips are obtained;
step 4, vortex spinning: vortex spinning the cooked strips, wherein the vortex spinning process is configured as follows: the air flow temperature is controlled at 25 ℃, the relative humidity is controlled at 65%, the spinning speed is 340rpm, the total draft is 211, the main draft is 30, the feeding ratio is 0.96, the curling ratio is 1.015, and the BR starting rate is 100%;
step 5, checking: detecting cotton knots, semi-finished strips, finished sliver evenness, coarse and fine materials and cotton knots, performing spot check on semi-finished products or finished products in each working procedure in production, performing periodic spot check and real-time spot check, and checking whether the semi-finished products or the finished products in each working procedure meet the quality control requirement through data check analysis;
step 6, warehouse entry: warehouse entry is performed after the quality control requirement is met;
step 7, doubling: doubling the warehoused yarns, and selecting two yarns to be combined into one yarn, wherein the doubling speed is 400rpm;
step 8, double twisting: the speed of the double twisting is 5000rpm, the twist is 80 twists/m, and the twisting direction is S;
step 9, warehouse entry: and (5) achieving the quality control requirement and warehousing.
The preparation method of the bio-based fiber comprises the following steps:
s1, 2000g of 0.25wt% graphene oxide aqueous solution is added into a three-necked flask, then stirred at 2000rpm in a water bath at 70 ℃ for 20min, 80g of 2.5wt% ammonium persulfate aqueous solution is added, and stirred at 200rpm for 20min; subsequently, 200g of 5wt% N-carbamoylmaleic acid aqueous solution was added, stirred at 200rpm at 70℃for 1 hour, 20g of 2.5wt% ammonium persulfate aqueous solution was added, stirred at 200rpm at 80℃for 2 hours, then the reaction temperature was increased to 95℃and 200g of 25wt% ascorbic acid aqueous solution was added, stirred at 200rpm for 4 hours, filtered, washed with water and absolute ethanol for 3 times, and vacuum freeze-dried for 12 hours to obtain pretreated graphene oxide;
s2, 200g of 2, 4-diamino-1, 3, 5-triazine, 120g of paraformaldehyde and 24g of formaldehyde are added into 400g of water, stirred at 200rpm at 60 ℃ for 6 hours, 10g of p-hydroxybenzaldehyde is added, stirred at 200rpm at 80 ℃ for 3 hours, and the pH is adjusted to 7 by triethanolamine to obtain a modifier;
s3, mixing 1g of the pretreated graphene oxide prepared in the step S1 with 14g of 10mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 2 hours, wherein the ultrasonic power is 200W, and the ultrasonic frequency is 40kHz, so as to obtain a dispersion solution; adding the dispersion solution and 3g of the modifier prepared in the step S2 into 100g of cellulose spinning solution, and stirring for 1h at 2000rpm at room temperature to obtain spinning solution, wherein the cellulose content in the cellulose spinning solution is 8wt% and the sodium hydroxide concentration is 4.5wt%; injecting the spinning solution into a storage tank, degassing under the vacuum degree of-0.08 Mpa, adopting a wet spinning process, extruding the spinning solution into a coagulation bath through a porous spinning nozzle with the concentration of 48mL/min, wherein the coagulation bath consists of 115g/L sulfuric acid, 340g/L sodium sulfate and 10g/L zinc sulfate, the spinning speed is 35m/min, the diameter of the spinning nozzle is 50 mu m, the number of pores is 200, washing the fiber for 1h in an off-line way by using 70 ℃ water, and carrying out tension-free air drying to obtain the bio-based fiber.
Comparative example 1
The vortex spinning preparation of bio-based yarn was essentially the same as example 1, the only difference being that: the preparation methods of the bio-based fibers are different.
The preparation method of the bio-based fiber comprises the following steps:
s1, 2000g of 0.25wt% graphene oxide aqueous solution is added into a three-necked flask, then stirred at 2000rpm in a water bath at 70 ℃ for 20min, 80g of 2.5wt% ammonium persulfate aqueous solution is added, and stirred at 200rpm for 20min; subsequently, 200g of 5wt% acrylamide aqueous solution was added, stirred at 200rpm at 70℃for 1 hour, 20g of 2.5wt% ammonium persulfate aqueous solution was added, stirred at 200rpm at 80℃for 2 hours, then the reaction temperature was increased to 95℃and 200g of 25wt% ascorbic acid aqueous solution was added, stirred at 200rpm for 4 hours, filtered, washed with water and absolute ethanol for 3 times, and vacuum freeze-dried for 12 hours to obtain pretreated graphene oxide;
s2, 200g of 2, 4-diamino-1, 3, 5-triazine, 120g of paraformaldehyde and 24g of formaldehyde are added into 400g of water, stirred at 200rpm at 60 ℃ for 6 hours, 10g of p-hydroxybenzaldehyde is added, stirred at 200rpm at 80 ℃ for 3 hours, and the pH is adjusted to 7 by triethanolamine to obtain a modifier;
s3, mixing 1g of the pretreated graphene oxide prepared in the step S1 with 14g of 10mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 2 hours, wherein the ultrasonic power is 200W, and the ultrasonic frequency is 40kHz, so as to obtain a dispersion solution; adding the dispersion solution and 3g of the modifier prepared in the step S2 into 100g of cellulose spinning solution, and stirring for 1h at 2000rpm at room temperature to obtain spinning solution, wherein the cellulose content in the cellulose spinning solution is 8wt% and the sodium hydroxide concentration is 4.5wt%; injecting the spinning solution into a storage tank, degassing under the vacuum degree of-0.08 Mpa, adopting a wet spinning process, extruding the spinning solution into a coagulation bath through a porous spinning nozzle with the concentration of 48mL/min, wherein the coagulation bath consists of 115g/L sulfuric acid, 340g/L sodium sulfate and 10g/L zinc sulfate, the spinning speed is 35m/min, the diameter of the spinning nozzle is 50 mu m, the number of pores is 200, washing the fiber for 1h in an off-line way by using 70 ℃ water, and carrying out tension-free air drying to obtain the bio-based fiber.
Comparative example 2
The vortex spinning preparation of bio-based yarn was essentially the same as example 1, the only difference being that: the preparation methods of the bio-based fibers are different.
The preparation method of the bio-based fiber comprises the following steps:
s1, 200g of 2, 4-diamino-1, 3, 5-triazine, 120g of paraformaldehyde and 24g of formaldehyde are added into 400g of water, stirred at 200rpm at 60 ℃ for 6 hours, 10g of p-hydroxybenzaldehyde is added, stirred at 200rpm at 80 ℃ for 3 hours, and the pH is adjusted to 7 by triethanolamine to obtain a modifier;
s2, mixing 1g of graphene oxide with 14g of 10mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 2 hours, wherein the ultrasonic power is 200W, and the ultrasonic frequency is 40kHz, so as to obtain a dispersion solution; adding the dispersion solution and 3g of the modifier prepared in the step S1 into 100g of cellulose spinning solution, and stirring for 1h at 2000rpm at room temperature to obtain spinning solution, wherein the cellulose content in the cellulose spinning solution is 8wt% and the sodium hydroxide concentration is 4.5wt%; injecting the spinning solution into a storage tank, degassing under the vacuum degree of-0.08 Mpa, adopting a wet spinning process, extruding the spinning solution into a coagulation bath through a porous spinning nozzle with the concentration of 48mL/min, wherein the coagulation bath consists of 115g/L sulfuric acid, 340g/L sodium sulfate and 10g/L zinc sulfate, the spinning speed is 35m/min, the diameter of the spinning nozzle is 50 mu m, the number of pores is 200, washing the fiber for 1h in an off-line way by using 70 ℃ water, and carrying out tension-free air drying to obtain the bio-based fiber.
Comparative example 3
The vortex spinning preparation of bio-based yarn was essentially the same as example 1, the only difference being that: the preparation methods of the bio-based fibers are different.
The preparation method of the bio-based fiber comprises the following steps:
s1, 2000g of 0.25wt% graphene oxide aqueous solution is added into a three-necked flask, then stirred at 2000rpm in a water bath at 70 ℃ for 20min, 80g of 2.5wt% ammonium persulfate aqueous solution is added, and stirred at 200rpm for 20min; subsequently, 200g of 5wt% N-carbamoylmaleic acid aqueous solution was added, stirred at 200rpm at 70℃for 1 hour, 20g of 2.5wt% ammonium persulfate aqueous solution was added, stirred at 200rpm at 80℃for 2 hours, then the reaction temperature was increased to 95℃and 200g of 25wt% ascorbic acid aqueous solution was added, stirred at 200rpm for 4 hours, filtered, washed with water and absolute ethanol for 3 times, and vacuum freeze-dried for 12 hours to obtain pretreated graphene oxide;
s2, mixing 1g of the pretreated graphene oxide prepared in the step S1 with 14g of 10mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 2 hours, wherein the ultrasonic power is 200W, and the ultrasonic frequency is 40kHz, so as to obtain a dispersion solution; adding the dispersion solution into 100g of cellulose spinning solution, and stirring for 1h at 2000rpm at room temperature to obtain spinning solution, wherein the cellulose content in the cellulose spinning solution is 8wt% and the sodium hydroxide concentration is 4.5wt%; injecting the spinning solution into a storage tank, degassing under the vacuum degree of-0.08 Mpa, adopting a wet spinning process, extruding the spinning solution into a coagulation bath through a porous spinning nozzle with the concentration of 48mL/min, wherein the coagulation bath consists of 115g/L sulfuric acid, 340g/L sodium sulfate and 10g/L zinc sulfate, the spinning speed is 35m/min, the diameter of the spinning nozzle is 50 mu m, the number of pores is 200, washing the fiber for 1h in an off-line way by using 70 ℃ water, and carrying out tension-free air drying to obtain the bio-based fiber.
Comparative example 4
The vortex spinning preparation of bio-based yarn was essentially the same as example 1, the only difference being that: the preparation methods of the bio-based fibers are different.
The preparation method of the bio-based fiber comprises the following steps:
mixing 1g of graphene oxide with 14g of 10mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 2 hours with ultrasonic power of 200W and ultrasonic frequency of 40kHz to obtain a dispersion solution; adding the dispersion solution into 100g of cellulose spinning solution, and stirring for 1h at 2000rpm at room temperature to obtain spinning solution, wherein the cellulose content in the cellulose spinning solution is 8wt% and the sodium hydroxide concentration is 4.5wt%; injecting the spinning solution into a storage tank, degassing under the vacuum degree of-0.08 Mpa, adopting a wet spinning process, extruding the spinning solution into a coagulation bath through a porous spinning nozzle with the concentration of 48mL/min, wherein the coagulation bath consists of 115g/L sulfuric acid, 340g/L sodium sulfate and 10g/L zinc sulfate, the spinning speed is 35m/min, the diameter of the spinning nozzle is 50 mu m, the number of pores is 200, washing the fiber for 1h in an off-line way by using 70 ℃ water, and carrying out tension-free air drying to obtain the bio-based fiber.
Test example 1
Tensile Property test
The bio-based vortex spun yarns prepared in the examples and comparative examples of the present invention were tested using an electronic single yarn brute force apparatus YG061F, stretching speed: 500mm/min; sample length: 500mm; test temperature: 20 ℃ +/-2; humidity: 60% + -2. 30 experiments were performed for each sample and the average was taken. The test results are shown in Table 1.
TABLE 1 tensile Property test results
Test example 2
Thermal stability test
The bio-based vortex spinning yarn prepared in the examples and comparative examples of the present invention was dried, and 7mg was precisely weighed and kneaded into pellets, and flattened to prepare samples. Under the protection of nitrogen atmosphere, heating at a heating rate of 5 ℃/min, and using a Switzerland-tolidol DTG-60H type differential heat-thermogravimetric analyzer to carry out analysis and test, wherein the temperature is 20-600 ℃; the temperature at which the heat loss rate was 50% was recorded. The test results are shown in Table 2.
TABLE 2 thermal stability test results
The reason why the biomass fiber vortex spun yarn prepared in the embodiment 1 of the invention has higher tensile property and thermal stability is probably that the biomass fiber vortex spun yarn is prepared by adopting the bio-based fiber as the raw material through the procedures of opening and picking, carding, drawing, vortex spinning, inspection, warehousing, doubling, double twisting and warehousing. The preparation method of the biomass fiber comprises the steps of stirring graphene oxide aqueous solution at a high temperature, adding ammonium persulfate and stirring; adding an N-carbamyl maleic acid aqueous solution, stirring at a high temperature, adding an ammonium persulfate aqueous solution, stirring at a high temperature, increasing the temperature, adding an ascorbic acid aqueous solution, stirring, filtering, washing, and performing vacuum freeze drying to obtain pretreated graphene oxide; adding 2, 4-diamino-1, 3, 5-triazine, paraformaldehyde and formaldehyde into water, stirring at high temperature, adding p-hydroxybenzaldehyde, stirring at high temperature, and regulating pH with triethanolamine to obtain a modifier; mixing pretreated graphene oxide with a polyvinyl alcohol aqueous solution, and performing ultrasonic treatment to obtain a dispersion solution; adding the dispersion solution and the modifier into the cellulose spinning solution, and stirring to obtain a spinning solution; degassing, adopting a wet spinning process, washing and air-drying to obtain the bio-based fiber.
Example 1 and comparative example 1, in which N-carbamoylmaleic acid was used to modify the pretreated graphene oxide, the use of N-carbamoylmaleic acid modified graphene oxide can improve the tensile properties of the fiber as compared to biobased fibers prepared using acrylamide. N-carbamoylmaleic acid has good hydrophilicity and gelation, and can enhance the structural strength and tensile properties of the fiber. And may provide better thermal stability. This makes the fiber more resistant to high temperature environments and maintains its structural and performance stability.
Example 1 compared to comparative example 2, the preparation step in example 1 involved the introduction of pretreated graphene oxide, whereas comparative example 2 directly uses graphene oxide to prepare the fiber. The pretreated graphene oxide introduced in example 1 has the characteristics of high strength and high rigidity, and can increase the strength and rigidity of the fiber. This may make the biobased vortex spun yarn prepared in example 1 perform better in terms of tensile properties. The dispersibility of the pretreated graphene oxide is better, and better thermal stability can be obtained.
Compared with example 1 and comparative example 3, the biobased fiber prepared by mixing the modifier with the pretreated graphene oxide may have advantages of tensile properties and thermal stability compared with the biobased fiber prepared without the modifier, and the modifier is compounded with cellulose molecules in the cellulose spinning solution and forms a crosslinked structure. The cross-linked structure can increase the interaction force between cellulose molecules and improve the strength and rigidity of cellulose, thereby improving the tensile property of the bio-based fiber. And the crosslinked structure can slow down the degradation rate of cellulose at high temperature and improve the thermal stability of the bio-based fiber.

Claims (9)

1. The preparation method of the vortex spinning of the bio-based yarn is characterized by comprising the following steps of:
step 1, opening and picking: processing the bio-based fiber by adopting a cotton opener;
step 2, carding cotton: feeding the biological base fiber subjected to opening and picking treatment into a carding machine;
step 3, drawing: feeding the combed biological base fiber into a drawing frame to obtain a cooked strip;
step 4, vortex spinning: vortex spinning the cooked strips;
step 5, checking: detecting cotton knots, semi-finished strips, finished sliver evenness, coarse and fine materials and cotton knots, performing spot check on semi-finished products or finished products in each working procedure in production, performing periodic spot check and real-time spot check, and checking whether the semi-finished products or the finished products in each working procedure meet the quality control requirement through data check analysis;
step 6, warehouse entry: warehouse entry is performed after the quality control requirement is met;
step 7, doubling: doubling the warehoused yarns, and selecting two yarns to be combined into one yarn, wherein the doubling speed is 300-500 rpm;
step 8, double twisting: the speed of the double twisting is 4000-6000 rpm, the twist is 50-100 twists/m, and the twisting direction is S;
step 9, warehouse entry: warehouse entry is performed after the quality control requirement is met;
the preparation method of the bio-based fiber comprises the following steps of:
s1, adding 1800-2200 parts of 0.2-0.3 wt% graphene oxide aqueous solution into a three-necked flask, stirring at 1500-2500 rpm in a water bath at 60-80 ℃ for 15-25 min, adding 70-90 parts of 2-3 wt% ammonium persulfate aqueous solution, and stirring at 100-500 rpm for 10-30 min; then adding 180-220 parts of 3-8 wt% N-carbamoyl maleic acid aqueous solution, stirring for 0.5-2 hours at 100-500 rpm at 60-80 ℃, adding 15-25 parts of 2-3 wt% ammonium persulfate aqueous solution, stirring for 1-3 hours at 100-500 rpm at 70-90 ℃, then raising the reaction temperature to 90-98 ℃, adding 180-220 parts of 20-30 wt% ascorbic acid aqueous solution, stirring for 3-5 hours at 180-220 parts rpm, filtering, washing for 2-4 times with water and absolute ethyl alcohol, and vacuum freeze-drying for 5-20 hours to obtain pretreated graphene oxide;
s2, adding 180-220 parts of 2, 4-diamino-1, 3, 5-triazine, 100-240 parts of paraformaldehyde and 20-30 parts of formaldehyde into 300-500 parts of water, stirring at 100-500 rpm for 2-8 hours at 50-70 ℃, adding 8-12 parts of parahydroxybenzaldehyde, stirring at 100-500 rpm for 2-5 hours at 70-90 ℃, and regulating the pH to 6.5-7.5 by using triethanolamine to obtain a modifier;
s3, mixing 0.5-2 parts of the pretreated graphene oxide prepared in the step S1 with 12-20 parts of 8-12 mg/mL polyvinyl alcohol aqueous solution, and carrying out ultrasonic treatment for 1-3 hours, wherein the ultrasonic power is 100-300W, and the ultrasonic frequency is 30-60 kHz, so as to obtain a dispersion solution; adding the dispersion solution and 2-4 parts of the modifier prepared in the step S2 into 80-120 parts of cellulose spinning solution, and stirring at 1500-2500 rpm for 0.5-2 hours at room temperature to obtain spinning solution; injecting the spinning solution into a storage tank, degassing at a vacuum degree of-0.05 to-0.1 Mpa, and adopting a wet spinning process to obtain the bio-based fiber.
2. The vortex spinning preparation method of the bio-based yarn according to claim 1, wherein the rotating speed of a beater bar of the opener in the step 1 is 400-450 rpm, the interval between a cotton feeding roller and the beater bar is 9-10 mm, the interval between a dust bar and the dust bar is 8-9 mm, the interval between the dust bar and the beater bar is 8-10 mm at an inlet, the interval between the dust bar and the beater bar is 18-19 mm at an outlet, the interval between the beater bar and a cotton stripping knife is 1.5-2.5 mm, and the speed of a cotton roll roller is 10-12 rpm; the dry basis weight of the cotton rolls is 350-400 g/m, and the length of the cotton rolls is 28-35 m.
3. The method of claim 1, wherein the carding process in step 2 is configured to: the speed of the cylinder is 350-420 rpm, the speed of the licker-in is 750-800 rpm, the speed of the cover plate is 130-150 mm/min, the speed of the doffer is 20-24 rpm, the gauge of the cylinder and the front fixed cover plate is 0.08-0.12 mm multiplied by 0.08-0.1 mm, the gauge of the cylinder and the rear fixed cover plate is 0.08-0.12 mm multiplied by 0.1-0.14 mm, the gauge of the cylinder-licker-in is 0.05-0.08 mm, the gauge of the cylinder-doffer is 0.04-0.06 mm, the sliver outlet speed is 50-80 m/min, and the dry basis weight of the cotton sliver is 18-24 g/5m.
4. The method for preparing a biobased yarn by vortex spinning according to claim 1, wherein three drawing steps are adopted in the step 3, and the main process parameters are as follows: the head roller interval is 10-12 multiplied by 8-9 multiplied by 17-19 mm, the back zone draft multiple is 1.2-1.8 times, the total draft multiple is 4-8 times, and the total number of the combined strips is 2-8; the interval between the two doubling rollers is 10-12 multiplied by 8-9 multiplied by 17-19 mm, the draft multiple of the rear zone is 1.2-1.8 times, the total draft multiple is 4-10 times, and the doubling number is 2-8; the three combining rollers are spaced by 8-12 multiplied by 8-9 multiplied by 16-18 mm, the back zone draft multiple is 1.2-1.4 times, the total draft multiple is 4-10 times, and the combining number is 2-8.
5. The method of claim 1, wherein the vortex spinning process in step 4 is configured to: the air flow temperature is controlled at 20-30 ℃, the relative humidity is controlled at 60-70%, the spinning speed is 300-360 rpm, the total draft is 150-250, the main draft is 20-40, the feeding ratio is 0.8-1.1, the crimping ratio is 0.94-1.1, and the BR initiation rate is 90-100%.
6. The method for preparing the bio-based yarn by vortex spinning according to claim 1, wherein the cellulose content in the cellulose spinning solution is 7-9wt% and the sodium hydroxide concentration is 4-5wt%.
7. The method for preparing the bio-based yarn by vortex spinning according to claim 1, wherein the wet spinning process is to extrude spinning solution into a coagulation bath through a porous spinning nozzle with the spinning speed of 30-40 m/min, the spinning nozzle diameter of 40-55 μm and the pore number of 180-220, and then to wash the fiber for 0.5-2 hours in an off-line manner with water at the temperature of 60-80 ℃ and air-dry the fiber in a tension-free manner.
8. A method of vortex spinning a biobased yarn according to claim 7 wherein: the coagulation bath consists of 110-120 g/L sulfuric acid, 330-350 g/L sodium sulfate and 8-12 g/L zinc sulfate.
9. A biobased yarn prepared by the method of any one of claims 1-8.
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