CN112251864A - Wear-resistant improved viscose composite yarn and preparation method thereof - Google Patents

Wear-resistant improved viscose composite yarn and preparation method thereof Download PDF

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Publication number
CN112251864A
CN112251864A CN202011024567.4A CN202011024567A CN112251864A CN 112251864 A CN112251864 A CN 112251864A CN 202011024567 A CN202011024567 A CN 202011024567A CN 112251864 A CN112251864 A CN 112251864A
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viscose
inorganic filler
cellulose
wear
mass
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CN112251864B (en
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郑永祥
刘伟民
方芹
陈云辉
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Jinyuan Jiangxi Textile Co ltd
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Jinyuan Jiangxi Textile Co ltd
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    • 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
    • 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
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath
    • D01F2/10Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
    • 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
    • D10B2201/24Viscose
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/06Load-responsive characteristics
    • D10B2401/061Load-responsive characteristics elastic
    • 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
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing 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

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

Abstract

The invention discloses a process for improving the wear resistance, the breaking strength and the elasticity of viscose fibers, improving the dimensional stability of viscose fiber products and relieving the wrinkle degree of the viscose fiber products by adding conventional fillers and modified fillers into viscose. The conventional filler added in the invention can effectively improve the wear resistance, breaking strength and elasticity of the viscose fiber; the wear resistance, the breaking strength and the elasticity of the viscose can be further improved by using the hydroxyl cellulose for coupling; and a small amount of hydroxyl-terminated silicone oil is coupled, so that the friction coefficient of the surface of the viscose fiber can be further reduced, and the wear resistance of the viscose fiber is improved. The viscose fiber is used as a raw material, and the wear-resistant improved viscose composite yarn can be prepared through blowing, cotton carding, drawing, roving, spinning and spooling processes, has the advantages of good wear resistance, high breaking strength and good elasticity, and can effectively improve the dimensional stability and the wrinkle resistance of the viscose fiber fabric.

Description

Wear-resistant improved viscose composite yarn and preparation method thereof
Technical Field
The invention belongs to the technical field of spinning, and particularly relates to a wear-resistant improved viscose composite yarn and a preparation method thereof.
Background
The viscose fiber is mainly prepared by using natural cellulose such as cotton linter, wood and a small amount of bamboo as raw materials, preparing dissolving pulp with high cellulose purity through a series of treatment processes such as cooking, bleaching and the like, and then performing the working sections such as dipping, squeezing, crushing, ageing, yellowing, dissolving, mixing, filtering, defoaming, filtering, spinning, post-treatment, drying, packaging and the like. The common viscose fiber has excellent wearability, is extremely similar to certain performances of natural cotton fiber, has better hygroscopicity, dyeability, antistatic property and comfortable wearing, and has the advantages which are incomparable with other chemical fibers. But it also has a number of drawbacks as a textile fiber: viscose fibers have low strength, particularly wet strength, which is usually only about one-half of dry strength; the fabric made of viscose fiber cannot be strongly rubbed and washed when being washed, and the service life is short; the shrinkage rate of the viscose fiber is high, and the appearance of the washed fabric is not ideal; viscose has poor elasticity, is easy to deform when being worn, generates wrinkles and influences the attractive appearance of fabrics. Meanwhile, the abrasion resistance of the viscose fiber is poor, so that the service life and the use range of the viscose fiber product are greatly restricted.
CN104328523A discloses a method for introducing graphene into a viscose or a viscose semi-finished product to improve the breaking strength. However, this method is extremely expensive because graphene is expensive in the range of several hundreds to several thousands yuan per gram, making it difficult to popularize on a large scale.
Therefore, the invention develops a conventional filler and a filler modification technology to improve the wear resistance, the breaking strength and the elasticity of the viscose, improve the dimensional stability of viscose products and relieve the wrinkle degree of the viscose products.
Disclosure of Invention
The invention aims to provide an improved wear-resistant viscose composite yarn and a preparation method thereof, so as to improve the wear resistance, the breaking strength and the elasticity of viscose, improve the dimensional stability of viscose products and relieve the wrinkle degree of the viscose products.
The invention adopts the technical scheme that a wear-resistant improved viscose fiber is prepared by the following steps:
(1) preparation of viscose
A. Alkaline impregnation
Taking pulp as a raw material, and carrying out alkali impregnation treatment to obtain cellulose sulfonate;
B. aging to the age
B, ageing the cellulose sulfonate obtained in the step A;
C. yellowing of
B, yellowing the aged cellulose sulfonate obtained in the step B;
D. dissolution
C, dissolving the cellulose sulfonate subjected to yellowing treatment obtained in the step C to obtain viscose;
(2) preparation of filler dispersion slurry
Selecting an inorganic filler with the particle size of 100-200 nm, taking the viscose prepared in the step (1) with the mass of 5-10 times of that of the inorganic filler, and uniformly dispersing the viscose by a sand mill to obtain filler dispersion slurry;
(3) mixing
Adding the filler dispersion slurry prepared in the step (2) into the viscose prepared in the step (1), and uniformly dispersing;
(4) defoaming, aging and filtering
Defoaming and curing the viscose obtained in the step (3), and then filtering to obtain a pre-spinning viscose solution with the alpha cellulose content of 9.2-9.5%, the sodium hydroxide content of 5.8-6.0%, the viscosity of 48-52 seconds and the curing degree of 4.9-5.3 mL;
(5) spinning and aftertreatment
Preparing the viscose fiber product by conventional spinning, desulfurizing, washing, oiling and drying processes of the viscose liquid before spinning obtained in the step (4);
the concentration of the dipping alkali used in the alkali dipping in the step A is 260-270 g/L, the dipping temperature is controlled to be 40-42 ℃, and the dipping time is 80-90 minutes;
the temperature of the ageing in the step B is controlled to be 40-42 ℃, and the ageing time is 100-120 minutes;
the adding amount of the etiolation CS2 in the step C is 34-36% of that of the methylcellulose;
and the step D of dissolving is to add demineralized water at the temperature of 8-12 ℃ for full dissolving and grinding.
In order to further improve the dispersibility of the inorganic filler and the performance of the viscose, and relieve brittleness caused by the addition of the inorganic filler, the inorganic filler in the step (2) is modified as follows:
i: dispersing hydroxyl cellulose in pure water with the mass being 10-20 times of 60-70 ℃ to obtain hydroxyl cellulose dispersion liquid;
II: dispersing inorganic filler in 0.1% dilute hydrochloric acid with the mass being 1-3 times of that of the inorganic filler, uniformly stirring, standing and activating for 20-30 minutes to obtain activated inorganic filler liquid;
III: adding an activated inorganic filler liquid into a hydroxy cellulose dispersion liquid with the mass 3-5 times that of the activated inorganic filler liquid, uniformly dispersing, adding a silane coupling agent with the mass 1-3% of that of the inorganic filler, uniformly stirring, and reacting for 2-4 h;
IV: and (4) after the reaction is finished, carrying out reduced pressure dehydration on the reaction liquid to 1/4-1/3 of the total mass, and then mixing in the step (3).
Further, hydroxyl-terminated silicone oil microemulsion can be added in the step III:
adding a hydroxyl cellulose dispersion liquid with the mass 3-5 times of that of the activated inorganic filler liquid, adding 1% of hydroxyl-terminated silicone oil microemulsion with the mass 1/15-1/10 of the inorganic filler, uniformly dispersing, adding a silane coupling agent with the mass 1-3% of that of the inorganic filler, uniformly stirring, and reacting for 2-4 h.
Further, the inorganic filler in the step (2) is one or more of nano ceramic powder and nano alumina.
Further, in the viscose obtained by mixing in the step (3), the mass of the inorganic filler is 0.8-1.2% of that of alpha-cellulose in the viscose.
Further, the hydroxy cellulose is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose and hydroxypropyl methylcellulose.
Further, the silane coupling agent is one or more of KH550, KH560 and KH 570.
Further, after the inorganic filler is modified, the spinning and the post-treatment in the step (5) can use a two-bath method for spinning, and the two-bath method is beneficial to stretching of molecular chains of hydroxyl cellulose and hydroxyl-terminated silicone oil coupled with the inorganic filler, improving the binding force of the inorganic filler and viscose, improving the elasticity and the breaking strength and reducing the surface friction coefficient.
The viscose fiber prepared by the method can be used for directly producing viscose yarns and can also be used for producing viscose composite yarns.
The wear-resistant improved viscose fiber is used as a raw material, and the wear-resistant improved viscose composite yarn can be prepared through blowing, cotton carding, drawing, roving, spinning and spooling.
The production process of the wear-resistant improved viscose composite yarn specifically comprises the following steps:
(1) the blowing process adopts the process principle of 'more loosening, less beating, low falling and less falling', the beater speed of an A002 type plucker is 720r/min, the distance of the beater extending out of a rib is 2mm, and the beater speed of an FA106B cotton opener is 480 r/min;
(2) the carding process adopts an FA212A carding machine, adopts the process principle of 'light weight, low speed, tight spacing, strong carding and fiber protection', and makes 'five-blade one-standard' work (the 'five-blade one-standard' means that the teeth of a cylinder, a doffer, a cover plate, a licker-in and an additional carding piece are sharp, and the spacing is accurate and consistent), and keeps the rotating speed of the cylinder at 330r/min, the rotating speed of the licker-in at 760r/min, and the spacing between the cylinder and the cover plate is 0.20, 0.18 and 0.20 mm;
(3) in the drawing process, an FA315A drawing frame is adopted, a forward drawing process principle is adopted, and the drawing speed is controlled at 300 m/min;
(4) in the roving process, an FA415A roving frame is adopted, the principles of low speed, high twist, loose tension and stable elongation are adopted, the roller gauge is 10 × 26 × 37mm, and the spindle speed is 1000 r/min;
(5) the spinning process adopts an FA507 spinning frame, and adopts a 'two-large two-small' process (the 'two-large two-small' process means that the roving twist coefficient is large, the interval distance after spinning is large, the roving drafting is small, the interval distance after spinning is small), the roller interval is 18 x 40mm, and the spindle speed is 14000 r/min;
(6) the winding process adopts a Savio winder, and the winding linear speed is controlled at 1400 m/min.
The invention has the advantages that:
1. the conventional filler is adopted, so that the production cost of the viscose fiber can be greatly reduced, and the large-scale production is facilitated; meanwhile, the wear resistance, the breaking strength and the elasticity of the viscose fiber are improved, the size stability of a viscose fiber product is improved, the wrinkle degree of the viscose fiber product is relieved, and the service life and the attractiveness of the viscose fiber product can be greatly improved.
2. The inorganic filler is modified by the hydroxyl cellulose, so that the inorganic filler has a hyperbranched structure, the bonding force between the inorganic filler and the viscose fiber is further enhanced, and meanwhile, the long-chain molecules can effectively relieve the stress generated by adding the inorganic filler and reduce the brittleness of the inorganic filler.
3. The inorganic filler is modified by a small amount of hydroxyl-terminated silicone oil, so that the hygroscopicity of the viscose fiber and the difference of the dry and wet performances of the viscose fiber can be reduced, the surface friction coefficient of the viscose fiber is reduced, and the wear resistance of the viscose fiber is further improved.
4. After the inorganic filler is modified, the coupled long-chain molecules can be fully expanded by using a two-bath spinning method, the binding force between the inorganic filler and the viscose fiber is further improved, and the surface friction coefficient of the viscose fiber is reduced.
5. The viscose fiber prepared by the method is used as a raw material, and the wear-resistant improved viscose composite yarn can be prepared by blowing, cotton carding, drawing, roving, spinning and spooling processes, has the advantages of good wear resistance, high breaking strength and good elasticity, and can effectively improve the dimensional stability and the wrinkle resistance of viscose fiber fabrics.
Detailed Description
The pulp used in the following embodiments of the present invention is a cotton pulp raw material of the same batch, and the processes for producing viscose yarn and viscose fabric by using the prepared viscose fiber are the same in the subsequent test.
Example 1
An abrasion-resistant improved viscose fiber is prepared by the following steps:
(1) preparation of viscose
A. Alkaline impregnation
Taking pulp as a raw material, and carrying out alkali impregnation treatment to obtain cellulose sulfonate;
B. aging to the age
B, ageing the cellulose sulfonate obtained in the step A;
C. yellowing of
B, yellowing the aged cellulose sulfonate obtained in the step B;
D. dissolution
C, dissolving the cellulose sulfonate subjected to yellowing treatment obtained in the step C to obtain viscose;
(2) preparation of filler dispersion slurry
Selecting an inorganic filler with the particle size of 100nm, and modifying:
i: dispersing the hydroxy cellulose in pure water with the mass of 20 times of 60 ℃ to obtain hydroxy cellulose dispersion liquid;
II: dispersing inorganic filler in 0.1% dilute hydrochloric acid with the mass of 1 time, uniformly stirring, standing and activating for 30 minutes to obtain activated inorganic filler liquid;
III: adding an activated inorganic filler liquid into a hydroxyl cellulose dispersion liquid with the mass 5 times that of the activated inorganic filler liquid, then adding a hydroxyl-terminated silicone oil microemulsion with the mass 1% of that of 1/10% of the inorganic filler, after uniform dispersion, adding a silane coupling agent with the mass 3% of that of the inorganic filler, uniformly stirring, and reacting for 4 hours;
IV: after the reaction is finished, the reaction liquid is decompressed and dehydrated to 1/4 of the total mass, and then the step (3) can be carried out for mixing.
(3) Mixing
Adding the filler dispersion slurry prepared in the step (2) into the viscose prepared in the step (1), and uniformly dispersing;
(4) defoaming, aging and filtering
Defoaming and curing the viscose obtained in the step (3), and then filtering to obtain pre-spinning viscose with the alpha cellulose content of 9.2%, the sodium hydroxide content of 5.8%, the viscosity of 48 seconds and the curing degree of 4.9 mL;
(5) spinning and aftertreatment
Preparing the viscose fiber product by conventional spinning, desulfurizing, washing, oiling and drying processes of the viscose liquid before spinning obtained in the step (4);
the concentration of the impregnation alkali used in the alkali impregnation in the step A is 260g/L, the impregnation temperature is controlled to be 42 ℃, and the impregnation time is 90 minutes;
the temperature of the aging in the step B is controlled to be 42 ℃, and the aging time is 100 minutes;
the adding amount of the etiolation CS2 in the step C is 34 percent of that of the methylcellulose;
the step D dissolution is that demineralized water is added at 12 ℃ for full dissolution and grinding.
The inorganic filler in the step (2) is nano ceramic powder.
In the viscose obtained by mixing in the step (3), the mass of the inorganic filler is 0.8 percent of that of alpha-cellulose in the viscose.
The hydroxycellulose is hydroxymethylcellulose.
The silane coupling agent is KH 570.
And (4) after the inorganic filler is modified, spinning in the step (5) and spinning in a two-bath method are used for the post-treatment.
Example 2
An abrasion-resistant improved viscose fiber is prepared by the following steps:
(1) preparation of viscose
A. Alkaline impregnation
Taking pulp as a raw material, and carrying out alkali impregnation treatment to obtain cellulose sulfonate;
B. aging to the age
B, ageing the cellulose sulfonate obtained in the step A;
C. yellowing of
B, yellowing the aged cellulose sulfonate obtained in the step B;
D. dissolution
C, dissolving the cellulose sulfonate subjected to yellowing treatment obtained in the step C to obtain viscose;
(2) preparation of filler dispersion slurry
Selecting an inorganic filler with the particle size of 150nm, and modifying:
i: dispersing hydroxy cellulose in pure water with the mass 15 times of that of the pure water at 65 ℃ to obtain hydroxy cellulose dispersion liquid;
II: dispersing inorganic filler in 0.1% dilute hydrochloric acid with the mass 2 times that of the inorganic filler, uniformly stirring, standing and activating for 25 minutes to obtain activated inorganic filler liquid;
III: adding the activated inorganic filler liquid into hydroxyl cellulose dispersion liquid with the mass 4 times that of the activated inorganic filler liquid, then adding 1% hydroxyl-terminated silicone oil microemulsion with the mass of 1/12% of the inorganic filler liquid, after uniform dispersion, adding silane coupling agent with the mass of 2% of the inorganic filler liquid, uniformly stirring, and reacting for 3 hours;
IV: after the reaction is finished, the reaction liquid is decompressed and dehydrated to 1/4 of the total mass, and then the step (3) can be carried out for mixing.
(3) Mixing
Adding the filler dispersion slurry prepared in the step (2) into the viscose prepared in the step (1), and uniformly dispersing;
(4) defoaming, aging and filtering
Defoaming and curing the viscose obtained in the step (3), and then filtering to obtain pre-spinning viscose with the alpha cellulose content of 9.4%, the sodium hydroxide content of 5.9%, the viscosity of 50 seconds and the curing degree of 5.1 mL;
(5) spinning and aftertreatment
Preparing the viscose fiber product by conventional spinning, desulfurizing, washing, oiling and drying processes of the viscose liquid before spinning obtained in the step (4);
the concentration of the impregnation alkali used in the alkali impregnation in the step A is 266g/L, the impregnation temperature is controlled to be 41 ℃, and the impregnation time is 88 minutes;
the temperature of the aging in the step B is controlled to be 41 ℃, and the aging time is 115 minutes;
the adding amount of the etiolation CS2 in the step C is 35 percent of that of the methylcellulose;
the step D dissolution is that demineralized water is added at 10 ℃ for full dissolution and grinding.
The inorganic filler in the step (2) is nano ceramic powder.
In the viscose obtained by mixing in the step (3), the mass of the inorganic filler is 1.0 percent of that of alpha-cellulose in the viscose.
The hydroxycellulose is hydroxyethyl cellulose.
The silane coupling agent is KH 560.
And (4) after the inorganic filler is modified, spinning in the step (5) and spinning in a two-bath method are used for the post-treatment.
Example 3
An abrasion-resistant improved viscose fiber is prepared by the following steps:
(1) preparation of viscose
A. Alkaline impregnation
Taking pulp as a raw material, and carrying out alkali impregnation treatment to obtain cellulose sulfonate;
B. aging to the age
B, ageing the cellulose sulfonate obtained in the step A;
C. yellowing of
B, yellowing the aged cellulose sulfonate obtained in the step B;
D. dissolution
C, dissolving the cellulose sulfonate subjected to yellowing treatment obtained in the step C to obtain viscose;
(2) preparation of filler dispersion slurry
Selecting an inorganic filler with the particle size of 200nm, and modifying:
i: dispersing the hydroxy cellulose in pure water with the mass 10 times of that of 70 ℃ to obtain hydroxy cellulose dispersion liquid;
II: dispersing inorganic filler in 0.1% dilute hydrochloric acid with the mass 3 times of that of the inorganic filler, uniformly stirring, standing and activating for 20 minutes to obtain activated inorganic filler liquid;
III: adding 3 times of hydroxyl cellulose dispersion liquid by mass into activated inorganic filler liquid, adding 1% of hydroxyl-terminated silicone oil microemulsion by mass of 1/15% of inorganic filler, uniformly dispersing, adding 1% of silane coupling agent by mass of inorganic filler, uniformly stirring, and reacting for 2 hours;
IV: after the reaction is finished, the reaction liquid is decompressed and dehydrated to 1/3 of the total mass, and then the step (3) can be carried out for mixing.
(3) Mixing
Adding the filler dispersion slurry prepared in the step (2) into the viscose prepared in the step (1), and uniformly dispersing;
(4) defoaming, aging and filtering
Defoaming and curing the viscose obtained in the step (3), and then filtering to obtain pre-spinning viscose with the alpha cellulose content of 9.5%, the sodium hydroxide content of 6.0%, the viscosity of 52 seconds and the curing degree of 5.3 mL;
(5) spinning and aftertreatment
Preparing the viscose fiber product by conventional spinning, desulfurizing, washing, oiling and drying processes of the viscose liquid before spinning obtained in the step (4);
the concentration of the impregnation alkali used in the step A is 270g/L, the impregnation temperature is controlled to be 40 ℃, and the impregnation time is 80 minutes;
the temperature of the aging in the step B is controlled to be 40 ℃, and the aging time is 120 minutes;
c, adding the etiolation CS2 in the step C in an amount which is 36 percent of that of the methylcellulose;
the step D dissolution is that demineralized water is added at 8 ℃ for full dissolution and grinding.
The inorganic filler in the step (2) is nano alumina.
In the viscose obtained by mixing in the step (3), the mass of the inorganic filler is 1.2% of that of alpha-cellulose in the viscose.
The hydroxycellulose is hydroxypropyl cellulose.
The silane coupling agent is KH 550.
And (4) after the inorganic filler is modified, spinning in the step (5) and spinning in a two-bath method are used for the post-treatment.
Example 4
An improved abrasion-resistant viscose fiber is prepared by the process of (2) preparing filler dispersion slurry, modifying inorganic filler without adding hydroxyl-terminated silicone oil microemulsion, and the rest is the same as example 1.
Example 5
An improved abrasion-resistant viscose fiber is prepared by the process of (2) preparing filler dispersion slurry, modifying inorganic filler without adding hydroxyl-terminated silicone oil microemulsion, and the rest is the same as example 2.
Example 6
An improved abrasion-resistant viscose fiber is prepared by the process of (2) preparing filler dispersion slurry, modifying inorganic filler without adding hydroxyl-terminated silicone oil microemulsion, and the rest is the same as example 3.
Example 7
In the preparation method, the filler dispersion slurry is prepared in the step (2), inorganic filler is not modified, the inorganic filler with the particle size of 100nm is selected, the viscose prepared in the step (1) with the mass being 10 times of that of the inorganic filler is uniformly dispersed by a sand mill, and the filler dispersion slurry is obtained; the rest is the same as example 1.
Example 8
In the preparation method, the filler dispersion slurry in the step (2) is prepared, inorganic filler is not modified, the inorganic filler with the particle size of 150nm is selected, the viscose prepared in the step (1) with the mass of 8 times of that of the inorganic filler is uniformly dispersed by a sand mill, and the filler dispersion slurry is obtained; the rest is the same as example 2.
Example 9
In the preparation method, the filler dispersion slurry is prepared in the step (2), inorganic filler is not modified, inorganic filler with the particle size of 200nm is selected, viscose prepared in the step (1) with the mass of 5 times of that of the inorganic filler is uniformly dispersed by a sand mill, and the filler dispersion slurry is obtained; the rest is the same as example 3.
Example 10
An abrasion resistant modified viscose fiber, which is prepared by the spinning of step (5) and the post-treatment using a single bath spinning method, the rest being the same as example 2.
Example 11
A viscose fiber is prepared by the following steps:
(1) preparation of viscose
A. Alkaline impregnation
Taking pulp as a raw material, and carrying out alkali impregnation treatment to obtain cellulose sulfonate;
B. aging to the age
B, ageing the cellulose sulfonate obtained in the step A;
C. yellowing of
B, yellowing the aged cellulose sulfonate obtained in the step B;
D. dissolution
C, dissolving the cellulose sulfonate subjected to yellowing treatment obtained in the step C to obtain viscose;
(2) preparation of filler dispersion slurry
Selecting an inorganic filler with the particle size of 300nm, and modifying:
i: dispersing the hydroxy cellulose in pure water with the mass of 8 times of that of the pure water at 75 ℃ to obtain hydroxy cellulose dispersion liquid;
II: dispersing inorganic filler in 0.1% dilute hydrochloric acid with the mass 4 times that of the inorganic filler, uniformly stirring, standing and activating for 45 minutes to obtain activated inorganic filler liquid;
III: adding 6 times of hydroxyl cellulose dispersion liquid by mass into activated inorganic filler liquid, adding 1% of hydroxyl-terminated silicone oil microemulsion by mass of 1/20% of inorganic filler, uniformly dispersing, adding 4% of silane coupling agent by mass of inorganic filler, uniformly stirring, and reacting for 1.5 h;
IV: after the reaction is finished, the reaction liquid is decompressed and dehydrated to 1/5 of the total mass, and then the step (3) can be carried out for mixing.
(3) Mixing
Adding the filler dispersion slurry prepared in the step (2) into the viscose prepared in the step (1), and uniformly dispersing;
(4) defoaming, aging and filtering
Defoaming and curing the viscose obtained in the step (3), and then filtering to obtain pre-spinning viscose with the alpha cellulose content of 9.0%, the sodium hydroxide content of 5.6%, the viscosity of 46 seconds and the curing degree of 4.8 mL;
(5) spinning and aftertreatment
Preparing the viscose fiber product by conventional spinning, desulfurizing, washing, oiling and drying processes of the viscose liquid before spinning obtained in the step (4);
the concentration of the impregnation alkali used in the step A is 250g/L, the impregnation temperature is controlled to be 45 ℃, and the impregnation time is 75 minutes;
the temperature of the aging in the step B is controlled to be 45 ℃, and the aging time is 90 minutes;
c, adding the etiolation CS2 in the step C in an amount of 32% of the methylcellulose;
the step D dissolution is that demineralized water is added at 6 ℃ for full dissolution and grinding.
The inorganic filler in the step (2) is nano ceramic powder.
In the viscose obtained by mixing in the step (3), the mass of the inorganic filler is 0.6 percent of that of alpha-cellulose in the viscose.
The hydroxycellulose is hydroxyethyl cellulose.
The silane coupling agent is KH 560.
And (4) after the inorganic filler is modified, spinning in the step (5) and spinning in a two-bath method are used for the post-treatment.
Example 12
A viscose fiber is prepared by the process of step (2) preparing filler dispersion slurry, modifying inorganic filler without adding hydroxyl terminated silicone oil microemulsion, and the rest is the same as example 11.
Example 13
A viscose fiber, in its preparation method, step (2) filler disperse preparation of slurry, inorganic filler is not modified, choose the inorganic filler with particle size 300nm, pick up 4 times of the viscose that step (1) makes of its quality, disperse the homogeneous through the sand mill, get filler disperse slurry; the rest is the same as example 11.
Comparative example 1
A viscose fiber is prepared by the method without adding inorganic filler, the step (2) of preparing filler dispersion slurry and the step (3) of mixing, and the rest is the same as the example 2.
Comparative example 2
A viscose fiber, which is prepared without adding a silane coupling agent, as in example 2.
Detection and analysis:
according to the same process, the viscose fibers prepared in the above examples and comparative examples are made into viscose composite yarns according to the blowing-carding-drawing-roving-spinning-spooling process, and further spun into viscose fabrics.
1. Testing the breaking strength and the breaking elongation of the viscose fiber at the normal temperature of 25 ℃ according to the determination (CRE method) of single yarn breaking strength and breaking elongation of the textile reeled yarn of GB/T3916-2013, and recording the diameter, the quality and the length; placing the mixture into a constant temperature and humidity box, balancing the mixture for 6 hours at 25 ℃ and RH95%, taking out the mixture to measure the diameter change rate, the water absorption rate, the shrinkage rate, the wet fracture strength and the elongation at break, and calculating the difference between the dry state and the wet state:
diameter change rate = (wet diameter/dry diameter-1) × 100%;
water absorption = (wet mass/dry mass-1) × 100%;
shrinkage = (1-wet length/dry length) × 100%;
degree of difference in dry-wet fracture strength = (1-wet fracture strength/dry fracture strength) × 100%;
the difference in dry and wet elongation at break = (wet elongation at break/dry elongation at break-1) × 100%;
2. because the evaluation method of the wrinkle degree is extremely complex and has defects, the viscose yarn is stretched by 10 percent in a pulling mode, then is recovered, is repeatedly stretched for 100 times, and then obtains the stretching deformation ratio, so as to represent the wrinkle resistance of the viscose yarn, and the higher the stretching deformation ratio is, the worse the wrinkle resistance is.
Stretch deformation ratio = (length after stretching/length before stretching-1) × 100%;
3. determination of abrasion resistance of fabrics according to GB/T21196.3-2007 Martindall method part 3: the method comprises the following steps of (1) testing the wear resistance of the viscose fabric, wherein the modification and evaluation indexes are the percentage of friction mass loss:
percent friction mass loss = (1-mass after friction/mass before friction) × 100%;
the friction coefficient is tested by adopting an MXD-02 friction coefficient tester according to a GB 10006-1988 plastic film and sheet friction coefficient test method.
Figure DEST_PATH_IMAGE001
As can be seen from the above table, the addition of the conventional filler in the invention can effectively improve the breaking strength of the viscose fiber. After the hydroxyl-terminated cellulose is coupled, the breaking strength and the breaking elongation are both greatly improved; the addition of the hydroxyl-terminated silicone oil modified inorganic filler further improves the breaking strength and the elongation at break, and simultaneously reduces the difference of dry-wet performance.
Figure 443798DEST_PATH_IMAGE002
As can be seen from the table above, the addition of the conventional filler can reduce the water absorption and the shrinkage, and is beneficial to the dimensional stability; the tensile deformation ratio is reduced, and the anti-wrinkle performance is favorably improved; and the wear resistance is enhanced. After the hydroxyl-terminated cellulose is coupled, the water absorption rate and the water shrinkage rate can be further reduced, the wear resistance is improved, and the tensile deformation ratio is greatly reduced; the water absorption, the shrinkage and the friction coefficient are further greatly reduced by adding the hydroxyl-terminated silicone oil modified inorganic filler, and the dimensional stability, the wrinkle resistance and the wear resistance are enhanced. The viscose fiber prepared by the method is used as a raw material, and the wear-resistant improved viscose composite yarn can be prepared by blowing, cotton carding, drawing, roving, spinning and spooling processes, has the advantages of good wear resistance, high breaking strength and good elasticity, and can effectively improve the dimensional stability and the wrinkle resistance of viscose fiber fabrics.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.

Claims (10)

1. An improved viscose fiber with wear resistance, which is characterized in that: the preparation method of the wear-resistant improved viscose fiber comprises the following steps:
(1) preparation of viscose
A. Alkaline impregnation
Taking pulp as a raw material, and carrying out alkali impregnation treatment to obtain cellulose sulfonate;
B. aging to the age
B, ageing the cellulose sulfonate obtained in the step A;
C. yellowing of
B, yellowing the aged cellulose sulfonate obtained in the step B;
D. dissolution
C, dissolving the cellulose sulfonate subjected to yellowing treatment obtained in the step C to obtain viscose;
(2) preparation of filler dispersion slurry
Selecting an inorganic filler with the particle size of 100-200 nm, taking the viscose prepared in the step (1) with the mass of 5-10 times of that of the inorganic filler, and uniformly dispersing the viscose by a sand mill to obtain filler dispersion slurry;
(3) mixing
Adding the filler dispersion slurry prepared in the step (2) into the viscose prepared in the step (1), and uniformly dispersing;
(4) defoaming, aging and filtering
Defoaming and curing the viscose obtained in the step (3), and then filtering to obtain a pre-spinning viscose solution with the alpha cellulose content of 9.2-9.5%, the sodium hydroxide content of 5.8-6.0%, the viscosity of 48-52 seconds and the curing degree of 4.9-5.3 mL;
(5) spinning and aftertreatment
Preparing the viscose fiber product by conventional spinning, desulfurizing, washing, oiling and drying processes of the viscose liquid before spinning obtained in the step (4);
the concentration of the dipping alkali used in the alkali dipping in the step A is 260-270 g/L, the dipping temperature is controlled to be 40-42 ℃, and the dipping time is 80-90 minutes;
the temperature of the ageing in the step B is controlled to be 40-42 ℃, and the ageing time is 100-120 minutes;
the adding amount of the etiolation CS2 in the step C is 34-36% of that of the methylcellulose;
and the step D of dissolving is to add demineralized water at the temperature of 8-12 ℃ for full dissolving and grinding.
2. An abrasion resistant modified viscose fiber according to claim 1 wherein: the inorganic filler in the step (2) is modified as follows:
i: dispersing hydroxyl cellulose in pure water with the mass being 10-20 times of 60-70 ℃ to obtain hydroxyl cellulose dispersion liquid;
II: dispersing inorganic filler in 0.1% dilute hydrochloric acid with the mass being 1-3 times of that of the inorganic filler, uniformly stirring, standing and activating for 20-30 minutes to obtain activated inorganic filler liquid;
III: adding an activated inorganic filler liquid into a hydroxy cellulose dispersion liquid with the mass 3-5 times that of the activated inorganic filler liquid, uniformly dispersing, adding a silane coupling agent with the mass 1-3% of that of the inorganic filler, uniformly stirring, and reacting for 2-4 h;
IV: and (4) after the reaction is finished, carrying out reduced pressure dehydration on the reaction liquid to 1/4-1/3 of the total mass, and then mixing in the step (3).
3. A wear-resistant improved viscose fiber according to claim 2, wherein: and step III, adding a hydroxyl silicone oil microemulsion for coupling:
adding a hydroxyl cellulose dispersion liquid with the mass 3-5 times of that of the activated inorganic filler liquid, adding 1% of hydroxyl-terminated silicone oil microemulsion with the mass 1/15-1/10 of the inorganic filler, uniformly dispersing, adding a silane coupling agent with the mass 1-3% of that of the inorganic filler, uniformly stirring, and reacting for 2-4 h.
4. A wear-resistant improved viscose fiber according to any one of claims 1 to 3, wherein: the inorganic filler in the step (2) is one or more of nano ceramic powder and nano alumina.
5. A wear-resistant improved viscose fiber according to any one of claims 1 to 3, wherein: in the viscose obtained by mixing in the step (3), the mass of the inorganic filler is 0.8-1.2% of that of alpha-cellulose in the viscose.
6. A wear-resistant improved viscose fiber according to any one of claims 2 to 3, wherein: the hydroxy cellulose is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, and hypromellose.
7. A wear-resistant improved viscose fiber according to any one of claims 2 to 3, wherein: the silane coupling agent is one or more of KH550, KH560 and KH 570.
8. A wear-resistant improved viscose fiber according to any one of claims 2 to 3, wherein: and (4) after the inorganic filler is modified, spinning in the step (5) and spinning in a two-bath method are used for the post-treatment.
9. The utility model provides a wear-resisting improved generation viscose composite yarn which characterized in that: the wear-resistant modified viscose fiber of any one of claims 1 to 3 is used as a raw material and is prepared through blowing, carding, drawing, roving, spinning and spooling processes.
10. A wear-resistant improved viscose composite yarn according to claim 9, wherein:
the preparation process specifically comprises the following steps:
(1) the blowing process adopts the process principle of 'more loosening, less beating, low falling and less falling', the beating speed of an A002 type plucker beater is 720r/min, the distance of the beater extending out of a rib is 2mm, and the rotating speed of the beating hand of an FA106B cotton opener is 480 r/min;
(2) the carding process adopts an FA212A carding machine, adopts the process principle of 'light basis weight, slow speed, tight spacing, strong carding and fiber protection', and makes 'five-front one-standard' work, and keeps the rotating speed of a cylinder at 330r/min, the rotating speed of a licker-in at 760r/min, and the spacing between the cylinder and a cover plate at 0.20, 0.18 and 0.20 mm;
(3) in the drawing process, an FA315A drawing frame is adopted, a forward drawing process principle is adopted, and the drawing speed is controlled at 300 m/min;
(4) in the roving process, an FA415A roving machine is adopted, the principles of low speed, high twist, loose tension and stable elongation are adopted, the roller gauge is 10 × 26 × 37mm, and the spindle speed is 1000 r/min;
(5) the spinning process adopts an FA507 spinning frame, adopts a two-large two-small process, the roller gauge is 18 x 40mm, and the spindle speed is 14000 r/min;
(6) the spooling process adopts a Savio spooling machine, and the spooling linear speed is controlled at 1400 m/min.
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