CN115142260A - Antibacterial lyocell fabric and preparation method thereof - Google Patents

Antibacterial lyocell fabric and preparation method thereof Download PDF

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Publication number
CN115142260A
CN115142260A CN202210775402.3A CN202210775402A CN115142260A CN 115142260 A CN115142260 A CN 115142260A CN 202210775402 A CN202210775402 A CN 202210775402A CN 115142260 A CN115142260 A CN 115142260A
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antibacterial
lyocell fabric
preparation
lyocell
liquid
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彭雄义
蔡映杰
董雄伟
王强
李宁
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Wuhan Textile University
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Wuhan Textile University
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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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • 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
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/11Compounds containing epoxy groups or precursors 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
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • 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
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to an antibacterial lyocell fabric and a preparation method thereof, which is characterized in that the antibacterial lyocell fabric is prepared by the following method: firstly, extracting azadirachtin from chinaberry seeds; secondly, preparing the finishing liquid by the finishing liquid and epoxy chloropropane and the like; and finally, performing antibacterial finishing on the lyocell fabric in finishing liquor to obtain the antibacterial lyocell fabric. The initial bacteriostasis rate of the antibacterial Lyocell fabric prepared by the invention to escherichia coli reaches more than 98.0 percent, after 10 times of washing, the antibacterial Lyocell fabric still has strong antibacterial performance to the escherichia coli, and the bacteriostasis rate reaches more than 96.0 percent; the initial bacteriostasis rate of the antibacterial lyocell fabric to staphylococcus aureus reaches more than 98.0%, and after 10 times of washing, the antibacterial lyocell fabric still has strong antibacterial performance to staphylococcus aureus, and the bacteriostasis rate reaches more than 96.0%.

Description

Antibacterial lyocell fabric and preparation method thereof
Technical Field
The invention belongs to the technical field of fabric preparation, and particularly relates to an antibacterial lyocell fabric and a preparation method thereof.
Background
The textile is easy to absorb sweat and grease secreted by metabolism of a human body due to the loose and porous structure of the textile, a favorable place is provided for attachment and propagation of microorganisms, and some bacteria and viruses can survive on the surface of the textile for hours to days. Experiments prove that the textile is an important mode for spreading and diffusing pathogenic bacteria. Therefore, the development and application of the antibacterial and antiviral textiles have important significance.
Lyocell fiber, also known as velvet, is a novel regenerated cellulose fiber which is made of natural plant fibers and can realize industrial production, and is a brand new textile fabric. The lyocell fiber has various excellent performances of natural fiber and synthetic fiber, has strong dry and wet strength, the woven lyocell fabric has good comfort, the raw material resources are renewable, the production process is low-carbon and non-toxic, and the product can be completely degraded. Meanwhile, the lyocell fabric has excellent air permeability and dyeability, good hand feeling, pilling resistance and small shrinkage in washing.
A common commercial production method for lyocell fibers is the NMMO solvent process to regenerate cellulose fibers; the method is characterized in that N-methylmorpholine-N-oxide (NMMO) is used as a solvent to directly dissolve spinning pulp, and a dry-jet wet-spinning-prevention process is carried out to prepare regenerated cellulose fiber-lyocell fiber. The production technology has the advantages of short process flow, recyclable solvent and green and environment-friendly production process, so that the lyocell fibers are regarded as substitute products of viscose fibers.
The lyocell fabric can be applied to various fields, from industrial fabrics to coats of clothing products to home textiles, in particular to high-grade female clothing. However, lyocell fibers, like other synthetic fibers, have the drawback of being susceptible to the propagation of bacteria. If the antibacterial property is endowed to the lyocell fabric, the application range of the lyocell fabric is further expanded and developed.
Literature investigation and research show that the antibacterial performance of the lyocell fabric is widely concerned, and Chinese patent application No. 201780071701.6 discloses an antibacterial regenerated cellulose fiber and a preparation method thereof: spinning the cellulose solution through a spinneret in a regeneration bath to obtain regenerated cellulose fibres; washing the regenerated cellulose fiber; treating the regenerated cellulose fibers with a solution of a quaternary ammonium compound in a concentration range of 0.1-1.5% w/w to obtain antibacterial regenerated cellulose fibers, i.e., antibacterial lyocell fibers. However, the antibacterial agent used in the antibacterial lyocell fabric prepared by the method is single in component, and long-acting high-activity antibacterial effect cannot be realized. Therefore, it is a goal of a continuous effort to develop a lyocell fabric having excellent antibacterial properties in the fabric research field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an antibacterial lyocell fabric and a preparation method thereof.
The invention aims to provide the antibacterial lyocell fabric which has the characteristics of environmental protection, human body friendliness and the like; the fabric can be prepared by the following method: firstly, extracting azadirachtin from chinaberry seeds; secondly, preparing the finishing liquid by the finishing liquid and epoxy chloropropane; and finally, performing antibacterial finishing on the lyocell fabric in finishing liquid to obtain the antibacterial lyocell fabric.
The purpose of the invention is realized by the following technical scheme:
s1, extracting an antibacterial solution: cleaning fructus Toosendan, crushing with a crusher, distilling with water vapor, and collecting filtrate to obtain antibacterial liquid.
Preferably, the dosage ratio of the chinaberry seeds to the water vapor is as follows: 1g to (20-40) mL/min.
Preferably, the temperature of the steam distillation is 200-260 ℃ and the time is 45-60 min.
S2, preparation of finishing liquid: and (2) diluting the antibacterial liquid prepared in the step (S1) with water, regulating and controlling the pH of the diluted liquid with a NaOH aqueous solution, adding epoxy chloropropane, and uniformly stirring to prepare a finishing liquid.
Preferably, the amount of water is 200 to 400 times by volume of the antibacterial liquid.
Preferably, the mass concentration of the NaOH aqueous solution is as follows: 10 to 20 percent.
Preferably, the pH of the diluent is 11 to 12.
Preferably, the amount of the epichlorohydrin is 0.02-0.04% of the mass fraction of the diluent.
S3, antibacterial finishing: soaking the lyocell fabric into the finishing liquid prepared in the step S2, and regulating and controlling the temperature of the finishing liquid; after the reaction is finished, neutralizing the lyocell fabric, and then washing with water; and finally, drying to obtain the antibacterial lyocell fabric.
Preferably, the usage ratio of the lyocell fabric to the finishing liquid is as follows: 1g to (20-40) mL.
Preferably, the temperature of the finishing liquor is 50 to 60 ℃.
Preferably, the reaction time is 1 to 3 minutes.
The main reaction mechanism analysis of the invention is as follows: the main components of the chinaberry can be extracted by a simple water vapor extraction method. The main components of the chinaberry fruit comprise: beta-sitosterol, vanillin, benzoic acid, vanillic acid, daucosterol, alpha-D-glucopyranose; under the alkaline condition, the substances can be grafted to the lyocell fabric through the condensation reaction of epoxy chloropropane and hydroxyl on the lyocell. The beta-sitosterol, the vanillin, the benzoic acid, the vanillic acid, the daucosterol, the alpha-D-glucopyranose and the like have antibacterial properties of different degrees, so that the prepared lyocell fabric has good antibacterial property.
The invention has the following remarkable characteristics:
(1) The invention extracts antibacterial components in the chinaberry seeds, and then the antibacterial components react with the lyocell fabric to be grafted on the lyocell fabric; the inventor of the application unexpectedly finds that the antibacterial component is combined with the lyocell fabric through a chemical bond, the combination is very firm, and the antibacterial performance of the lyocell fabric is still unchanged after multiple times of washing.
(2) The effective antibacterial components in the chinaberry fruit belong to natural products, the environment is friendly, and the prepared antibacterial lyocell fabric has the characteristics of environmental protection, human body friendliness and the like.
(3) The antibacterial finishing process is simple, the raw material source is wide, and the antibacterial finishing process has a large-scale production prospect.
(4) The initial bacteriostasis rate of the prepared antibacterial lyocell fabric to escherichia coli reaches more than 98.0%, the antibacterial lyocell fabric still has strong antibacterial performance to escherichia coli after 10 times of washing, and the bacteriostasis rate reaches more than 96.0%; the initial bacteriostasis rate of the antibacterial lyocell fabric to staphylococcus aureus reaches more than 98.0%, and after 10 times of washing, the antibacterial lyocell fabric still has strong antibacterial performance to staphylococcus aureus, and the bacteriostasis rate reaches more than 96.0%.
Detailed Description
The examples and comparative examples described below illustrate the present invention in detail.
Example 1
In this embodiment, a preparation method of an antibacterial lyocell fabric includes the following steps:
s1, extracting an antibacterial solution: cleaning 1g of chinaberry fruit, crushing the chinaberry fruit by using a crusher, distilling the crushed chinaberry fruit by using 30mL/min of water vapor, wherein the distillation temperature is 240 ℃, the distillation time is 50min, and collecting filtrate after the distillation is finished to obtain the antibacterial liquid.
S2, preparation of finishing liquid: diluting the antibacterial liquid prepared in the step S1 by using water with the volume 300 times that of the antibacterial liquid, regulating the pH of the diluent to be 11.5 by using a NaOH aqueous solution with the mass concentration of 15%, adding epoxy chloropropane accounting for 0.03% of the mass fraction of the diluent, and uniformly stirring to prepare a finishing liquid.
S3, antibacterial finishing: soaking the lyocell fabric into the finishing liquid prepared in the step S2, wherein the usage ratio of the lyocell fabric to the finishing liquid is as follows: 1g to 30mL, regulating and controlling the temperature of finishing liquid to be 55 ℃, and controlling the reaction time to be 2 minutes; after the reaction is finished, neutralizing the lyocell fabric, and then washing with water; and finally, drying to obtain the antibacterial lyocell fabric.
Example 2
In this embodiment, a preparation method of an antibacterial lyocell fabric includes the following steps:
s1, extracting an antibacterial solution: cleaning 1g of chinaberry seeds, crushing the chinaberry seeds by using a crusher, distilling the crushed chinaberry seeds by using 20mL/min of water vapor at the distillation temperature of 200 ℃ for 45min, and collecting filtrate after the distillation is finished to obtain the antibacterial liquid.
S2, preparation of finishing liquid: diluting the antibacterial liquid prepared in the step S1 by using water with the volume of 200 times, regulating the pH of the diluent to be 11 by using a NaOH aqueous solution with the mass concentration of 10%, adding epoxy chloropropane accounting for 0.02% of the mass fraction of the diluent, and uniformly stirring to prepare a finishing liquid.
S3, antibacterial finishing: and (3) soaking the lyocell fabric into the finishing liquid prepared in the step (S2), wherein the usage ratio of the lyocell fabric to the finishing liquid is as follows: 1g to 20mL, regulating and controlling the temperature of finishing liquid to be 50 ℃, and controlling the reaction time to be 1 minute; after the reaction is finished, neutralizing the lyocell fabric, and then washing with water; and finally, drying to obtain the antibacterial lyocell fabric.
Example 3
In this embodiment, a preparation method of an antibacterial lyocell fabric includes the following steps:
s1, extracting an antibacterial solution: cleaning 1g of chinaberry seeds, crushing the chinaberry seeds by using a crusher, distilling the crushed chinaberry seeds by using water vapor of 40mL/min at the distillation temperature of 260 ℃ for 60min, and collecting filtrate after the distillation is finished to obtain the antibacterial liquid.
S2, preparation of finishing liquid: diluting the antibacterial solution prepared in step S1 with 400 times of water by volume, regulating the pH of the diluted solution to 12 by using NaOH aqueous solution with the mass concentration of 20%, adding epoxy chloropropane accounting for 0.04% of the mass fraction of the diluted solution, and uniformly stirring to prepare the finishing solution.
S3, antibacterial finishing: soaking the lyocell fabric into the finishing liquid prepared in the step S2, wherein the usage ratio of the lyocell fabric to the finishing liquid is as follows: 1g to 40mL, regulating the temperature of finishing liquid to be 60 ℃, and controlling the reaction time to be 3 minutes; after the reaction is finished, neutralizing the lyocell fabric, and then washing with water; and finally, drying to obtain the antibacterial lyocell fabric.
Comparative example A
In this comparative example, the "30mL/min steam distillation" was adjusted to "3mL/min steam distillation" in step S1, and the other preparation method was carried out in the same manner as in example 1, by way of comparison with example 1.
Comparative example B
In this comparative example, the "epichlorohydrin accounting for 0.03% by mass of the diluent" was adjusted to "epichlorohydrin accounting for 0.3% by mass of the diluent" in step S2, using example 1 as a comparison, and the other production method was carried out in accordance with the production method of example 1.
Comparative example C
Using example 1 as a comparison, in this comparative example, the "lyocell face fabric to finish usage ratio in step S3 is: 1 g: 30mL is adjusted to that the usage ratio of the lyocell fabric to the finishing liquid is as follows: 1 g: 300mL ", and the other preparation was carried out in the same manner as in example 1.
And (3) testing antibacterial performance:
the antibacterial lyocell fabrics prepared in examples 1-3 and comparative examples A-C are respectively subjected to antibacterial experiments, and the specific antibacterial experiment method comprises the following steps: according to GB/T20944.1-2007 evaluation part 1 of antibacterial performance of textiles: agar plate diffusion method, the qualitative detection is carried out on the fabric by the agar diffusion method, and the antibacterial performance of the textile is evaluated according to GB/T20944.3-2008, part 3 of the evaluation of the antibacterial performance of the textile: the quantitative antibacterial performance of the fabric is measured by a vibration method, and the strains are staphylococcus aureus and escherichia coli. The qualitative detection result of the sample is expressed by the inhibition zone, the quantitative antibacterial activity is expressed by the inhibition rate, and the quantitative antibacterial activity is calculated according to the formula: the bacteriostasis rate = (1-B/A) × 100%, wherein A is the number of viable bacteria on the untreated fabric; b is the number of live bacteria on the treated fabric. The fabric to be tested is subjected to standard washing by referring to a washing method of a GB/T20944.1-2007 color fastness to washing tester, the antibacterial performance of an initial sample and a sample after 10 times of washing are tested, and the test results are shown in tables 1 and 2.
TABLE 1 inhibition of E.coli by the antibacterial lyocell fabrics prepared in examples 1-3 and comparative examples A-C
Figure BDA0003726827590000051
As can be seen from Table 1, the antibacterial lyocell fabrics prepared in examples 1 to 3 have a strong antibacterial property against Escherichia coli. The antibacterial rate of the unwashed antibacterial lyocell fabric to escherichia coli reaches more than 98.0%, after 10 times of washing, the antibacterial lyocell fabric still has strong antibacterial performance to escherichia coli, and the antibacterial rate reaches more than 96.0%. The antibacterial lyocell fabric prepared in comparative examples A-C has a significantly poorer antibacterial rate against Escherichia coli, which indicates that: the steam distillation dosage, the epichlorohydrin dosage and the dosage ratio of the lyocell fabric to the finishing liquid all have important influence on the bacteriostatic performance of the lyocell fabric.
TABLE 2 bacteriostasis rates of the antibacterial lyocell fabrics prepared in examples 1-3 and comparative examples A-C against Staphylococcus aureus
Figure BDA0003726827590000052
As can be seen from table 2, the antibacterial lyocell fabrics prepared in examples 1 to 3 have strong antibacterial properties against staphylococcus aureus. The antibacterial rate of the unwashed antibacterial lyocell fabric to staphylococcus aureus reaches more than 98.0%, after 10 times of washing, the antibacterial lyocell fabric still has strong antibacterial performance to staphylococcus aureus, and the antibacterial rate reaches more than 96.0%. The antibacterial ratio of the antibacterial lyocell fabric prepared in comparative examples A-C to Staphylococcus aureus is obviously poor, which shows that: the usage amount of steam distillation, the usage amount of epichlorohydrin and the usage amount ratio of the lyocell fabric to the finishing liquid all have important influence on the antibacterial performance of the lyocell fabric.
Through research on the antibacterial rate of the antibacterial lyocell fabric on staphylococcus aureus and escherichia coli, the antibacterial lyocell fabric prepared by the method has strong antibacterial performance.

Claims (10)

1. The preparation method of the antibacterial lyocell fabric is characterized by comprising the following steps of:
s1, extracting an antibacterial solution: cleaning fructus Toosendan, crushing with a crusher, distilling the crushed fructus Toosendan with water vapor, and collecting filtrate to obtain antibacterial liquid;
s2, preparation of finishing liquid: diluting the antibacterial liquid prepared in the step S1 with water, regulating and controlling the pH of the diluted liquid with a NaOH aqueous solution, adding epoxy chloropropane, and uniformly stirring to prepare a finishing liquid;
s3, antibacterial finishing: soaking the lyocell fabric into the finishing liquid prepared in the step S2, and regulating and controlling the temperature of the finishing liquid; after the reaction is finished, neutralizing the lyocell fabric, and then washing with water; and finally, rolling to obtain the antibacterial lyocell fabric.
2. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the dosage ratio of the chinaberry seeds to the water vapor in the step S1 is 1g to (20-40) mL/min.
3. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the temperature of the steam distillation in the step S1 is 200-260 ℃ and the time is 45-60 min.
4. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the water consumption in the step S2 is 200-400 times of the volume of the antibacterial liquid; the mass concentration of the NaOH aqueous solution is 10-20%.
5. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the pH of the diluent in the step S2 is 11-12.
6. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the consumption of the epichlorohydrin in the step S2 is 0.02-0.04% by mass of the diluent.
7. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the usage ratio of the lyocell to the finishing liquid in the step S3 is 1g to (20-40) mL.
8. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the temperature of the finishing liquid in the step S3 is 50-60 ℃.
9. The preparation method of the antibacterial lyocell fabric according to claim 1, wherein the reaction time in the step S3 is 1-3 minutes.
10. An antibacterial lyocell fabric, characterized in that it is produced by the method of any one of claims 1 to 9.
CN202210775402.3A 2022-07-01 2022-07-01 Antibacterial lyocell fabric and preparation method thereof Pending CN115142260A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101158114A (en) * 2007-11-22 2008-04-09 大连工业大学 Chitosan durable antibiotic tidying method for Cashmere (wool) fabric
CN102605630A (en) * 2012-04-06 2012-07-25 南通市嘉宇斯纺织集团有限公司 Traditional Chinese medicine inclusion compound with antibacterial effect and textile finishing method of traditional Chinese medicine inclusion compound
CN102940687A (en) * 2011-12-12 2013-02-27 苏州大学 Szechwan Chinaberry fruit extract and application thereof
CN105918357A (en) * 2016-06-27 2016-09-07 莫芳英 Natural plant bactericide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101158114A (en) * 2007-11-22 2008-04-09 大连工业大学 Chitosan durable antibiotic tidying method for Cashmere (wool) fabric
CN102940687A (en) * 2011-12-12 2013-02-27 苏州大学 Szechwan Chinaberry fruit extract and application thereof
CN102605630A (en) * 2012-04-06 2012-07-25 南通市嘉宇斯纺织集团有限公司 Traditional Chinese medicine inclusion compound with antibacterial effect and textile finishing method of traditional Chinese medicine inclusion compound
CN105918357A (en) * 2016-06-27 2016-09-07 莫芳英 Natural plant bactericide

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