CN110373895B - Preparation method of silver-loaded antibacterial viscose fiber - Google Patents

Preparation method of silver-loaded antibacterial viscose fiber Download PDF

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CN110373895B
CN110373895B CN201910717912.3A CN201910717912A CN110373895B CN 110373895 B CN110373895 B CN 110373895B CN 201910717912 A CN201910717912 A CN 201910717912A CN 110373895 B CN110373895 B CN 110373895B
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silver
fiber
loaded
viscose fiber
soaking
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CN110373895A (en
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高晓红
孙静
方婧
蔡小斌
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Nantong 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
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • 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

Abstract

The invention discloses a preparation method of silver-loaded antibacterial viscose fiber, which comprises the following steps: step A, soaking viscose in warm water at 35-40 ℃ containing 1% of penetrating agent (JFC)The time is 10-30min, and the moisture absorption swelling fiber is obtained; step B, draining the moisture absorption swelling fiber obtained in the step A, wherein the input temperature is 70-100 ℃, and the input temperature is 0.01-3mmol.L‑1Soaking in silver nitrate solution for 30-90min, cooling to room temperature, washing with purified water, and oven drying at 60-80 deg.C to obtain silver-loaded viscose fiber; and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.5-1% of silane coupling agent at the temperature of 60-90 ℃ for 30-90min to obtain the silver-loaded antibacterial viscose fiber. The preparation method provided by the invention is simple to operate and low in cost, and the prepared antibacterial viscose fiber is soft in hand feeling, good in antibacterial effect, resistant to washing for more than 50 times, not easy to break and long in service life.

Description

Preparation method of silver-loaded antibacterial viscose fiber
Technical Field
The invention relates to the technical field of viscose fiber preparation, in particular to a preparation method of antibacterial viscose fiber.
Background
Viscose fiber is made by dissolving cellulose-containing substances such as wood, cotton linter, bagasse and the like to regenerate, belongs to regenerated cellulose fiber in chemical fiber, and has the same chemical composition as cotton fiber. The viscose fiber has good hygroscopicity, strong air permeability, free wearing and low price, and can be continuously renewed according to the fashion of clothes. The viscose staple fiber can be blended with chemical fibers such as terylene, chinlon and the like to form various yarns, can also be blended with other synthetic fibers to form a net to be processed into non-woven fabrics, and can be used for ready-made clothes, home textiles, medical materials, decorative fabrics and the like, and has extremely wide application.
With the advancement of science and technology and the improvement of the living standard of people, people are increasingly pursuing health, and fiber products are increasingly required to be colorful, beautiful and practical, and meanwhile, the fiber products also have the function of preventing the spread of infectious diseases by using antibacterial fibers.
Silver, as a precious metal, has long been known and utilized for its excellent antimicrobial properties. The nano silver combines the antibacterial property of metal silver and the unique characteristics of small-size effect, quantum size effect, surface effect, macroscopic quantum tunneling effect and the like of the nano material, the antibacterial property of the nano silver is increased by thousands of times, the particle size of the nano silver is small, the nano silver can penetrate through the cell wall of bacteria and viruses to be combined with enzymes used for respiration of cells, the cells are suffocated, genes of the bacteria and the viruses cannot be changed, and therefore the nano silver has high-efficiency and broad-spectrum antibacterial property and good drug resistance.
Chinese patent CN200410062799.3 discloses a method for preparing antibacterial viscose fiber, which comprises adding nano silver colloid aqueous solution into spinning solution, and forming by conventional wet spinning and spinning process to obtain antibacterial viscose fiber, wherein the silver-loaded antibacterial viscose fiber prepared by the process has difficulty in controlling silver loading amount, and the nano silver is easy to agglomerate and block a spinning nozzle, thereby affecting the production efficiency of the spinning process; in the prior art, silver-loaded antibiosis is realized in the post-treatment process of fabrics (fabrics and the like) after fiber processing, and the craft fabrics have poor hand feeling, poor washability and poor antibiosis effect.
Disclosure of Invention
The invention aims to provide a preparation method of silver-loaded antibacterial viscose fibers, which has simple process, silver particles are uniformly distributed on the inner and outer surfaces of the fibers, the silver particles are firmly combined with the fibers, and the fibers are soft and smooth.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in warm water containing 1 percent of JFC and at the temperature of 35-40 ℃ for 10-30min to obtain moisture absorption swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 70-100 ℃ and 0.01-3mmol.L-1Soaking in silver nitrate solution for 30-90min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 60-80 deg.C to obtain silver-loaded viscose fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.5-1% of silane coupling agent at the temperature of 60-90 ℃ for 30-90min to obtain the silver-loaded antibacterial viscose fiber.
Preferably, the moisture-absorbing swelling fibers in the step B are drained and then are placed at the temperature of 80-90 ℃ and the concentration of 0.05-2.5mmol.L-1Soaking in silver nitrate solution for 40-80 min.
Preferably, the silver-loaded viscose fiber is soaked in 0.6-0.9% of silane coupling agent, the soaking temperature is 70-80 ℃, and the soaking time is 40-80min, so that the silver-loaded antibacterial viscose fiber is obtained.
Compared with the prior art, the invention has the beneficial effects that:
1. when the moisture-absorbing swelling fiber is placed in a silver nitrate solution, under the wicking action of a viscose fiber nanometer pore canal, the silver nitrate solution slowly enters a gap of the viscose fiber, silver ions are slowly reduced into simple substance silver particles in situ under the reduction action of aldehyde groups exposed at the tail end of fiber macromolecules, and due to the limited area action of the fiber pore canal, the silver particles are uniformly distributed on the inner surface and the outer surface of the fiber, so that the agglomeration of nanometer silver is effectively prevented.
2. When the silver-carrying viscose fiber is put into the silane coupling agent, the silane coupling agent is hydrolyzed to generate silanol which respectively reacts with hydroxyl on the surface of the nano silver and hydroxyl on the viscose fiber, and simultaneously, the silanol of the silane coupling agent molecules are mutually associated and polymerized to form a film with a net structure to cover the surface of the fiber, so that the silver particles are firmly combined with the fiber, and the fiber is softer and smoother.
3. The preparation method provided by the invention is simple to operate and low in cost, and the prepared antibacterial viscose fiber is soft in hand feeling, good in antibacterial effect, resistant to washing for more than 50 times, not easy to break and long in service life.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a silver-loaded antimicrobial viscose fiber of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of a viscose fiber;
fig. 3 is a graph showing the effect of the bacteriostatic rate of the silver-loaded antibacterial viscose fiber of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
referring to fig. 1, fig. 2 and fig. 3, the present invention provides a technical solution: a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in warm water at 35 ℃ containing a proper amount of 1 percent JFC for 10min to obtain hygroscopic swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 70 ℃ and 0.01mmol.L-1Soaking in silver nitrate solution for 30min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 60 deg.C to obtain silver-loaded viscose fiber with silver loading of 0.14mg/g fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.5% of silane coupling agent at the temperature of 60 ℃ for 30min to obtain the silver-loaded antibacterial viscose fiber, wherein the bacteriostasis rate of the fiber to staphylococcus aureus is 46% and the bacteriostasis rate to escherichia coli is 48%.
Example 2:
referring to fig. 1, fig. 2 and fig. 3, the present invention provides a technical solution: a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in warm water at 40 ℃ containing 1% JFC for 30min to obtain moisture absorption swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 100 ℃ and 3mmol.L-1Soaking in silver nitrate solution for 90min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 80 deg.C to obtain silver-loaded viscose fiber with silver loading of 0.57mg/g fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 1% of silane coupling agent at 90 ℃ for 90min to obtain the silver-loaded antibacterial viscose fiber, wherein the bacteriostasis rate of the fiber to staphylococcus aureus is 70% and the bacteriostasis rate to escherichia coli is 68%.
Example 3:
referring to fig. 1, fig. 2 and fig. 3, the present invention provides a technical solution: a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in 36 ℃ warm water containing 1 percent of JFC for 15min to obtain hygroscopic swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 80 ℃ and 0.05mmol.L-1Soaking in silver nitrate solution for 40min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 80 deg.C to obtain silver-loaded viscose fiber with silver loading of 0.32mg/g fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.6% of silane coupling agent at 70 ℃ for 40min to obtain the silver-loaded antibacterial viscose fiber, wherein the bacteriostasis rate of the fiber to staphylococcus aureus is 53% and the bacteriostasis rate to escherichia coli is 56%.
Example 4:
referring to fig. 1, fig. 2 and fig. 3, the present invention provides a technical solution: a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in warm water containing 1 percent JFC and at 37 ℃ for 25min to obtain moisture absorption swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 90 ℃ and 2.5mmol.L-1Soaking in silver nitrate solution for 80min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 75 deg.C to obtain silver-loaded viscose fiber with silver loading of 10.79mg/g fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.9% of silane coupling agent at 80 ℃ for 80min to obtain the silver-loaded antibacterial viscose fiber, wherein the bacteriostasis rate of the fiber to staphylococcus aureus is 98%, and the bacteriostasis rate of the fiber to escherichia coli is 98%.
Example 5:
referring to fig. 1, fig. 2 and fig. 3, the present invention provides a technical solution: a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in warm water containing 1 percent JFC and at 38 ℃ for 20min to obtain hygroscopic swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 85 ℃ and 1.0mmol.L-1Soaking in silver nitrate solution for 60min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 75 deg.C to obtain silver-loaded viscose fiber with silver loading of 4.32mg/g fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.7% of silane coupling agent at the temperature of 75 ℃ for 60min to obtain the silver-loaded antibacterial viscose fiber, wherein the bacteriostasis rate of the fiber to staphylococcus aureus is 98%, and the bacteriostasis rate to escherichia coli is 100%.
Example 6:
referring to fig. 1, fig. 2 and fig. 3 provide a technical solution of the present invention: a preparation method of silver-loaded antibacterial viscose fiber comprises the following steps:
step A, soaking the viscose in warm water containing 1 percent JFC and at the temperature of 39 ℃ for 20min to obtain moisture absorption swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 85 ℃ and 0.20mmol.L-1Soaking in silver nitrate solution for 75min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 75 deg.C to obtain silver-loaded viscose fiber with silver loading of 0.86mg/g fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.7% of silane coupling agent at 75 ℃ for 60min to obtain the silver-loaded antibacterial viscose fiber, wherein the bacteriostasis rate of the fiber to staphylococcus aureus is 99% and the bacteriostasis rate to escherichia coli is 100%.
In conclusion, various reagents used in the invention can be obtained commercially, the raw materials are wide in source and low in price, and the reagents can stably exist at normal temperature and normal pressure, are convenient to operate and treat and do not need special treatment.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (1)

1. A preparation method of silver-loaded antibacterial viscose fiber is characterized by comprising the following steps: the method comprises the following steps:
step A, soaking the viscose in warm water containing 1 percent of JFC and at the temperature of 35-40 ℃ for 10-30min to obtain moisture absorption swelling fibers;
step B, draining the moisture absorption swelling fiber obtained in the step A, and placing the moisture absorption swelling fiber at the temperature of 85-90 ℃ and 0.2-2.5mmol.L-1Soaking in silver nitrate solution for 60-80min, cooling to room temperature, washing with pure water at room temperature, and oven drying at 60-80 deg.C to obtain silver-loaded viscose fiber;
and step C, soaking the silver-loaded viscose fiber obtained in the step B in 0.7-0.9% of silane coupling agent at the temperature of 75-80 ℃ for 60-80min to obtain the silver-loaded antibacterial viscose fiber.
CN201910717912.3A 2019-08-05 2019-08-05 Preparation method of silver-loaded antibacterial viscose fiber Active CN110373895B (en)

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CN113235197B (en) * 2021-04-30 2022-11-08 浙江世纪晨星纤维科技有限公司 Preparation process of rayon yarn
CN114395835A (en) * 2022-03-03 2022-04-26 苏州市星京泽纤维科技有限公司 Functional vortex spinning core-spun yarn and preparation method thereof
CN115595786A (en) * 2022-11-11 2023-01-13 南通大学(Cn) Preparation method of copper-loaded antibacterial viscose fiber

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US20100215894A1 (en) * 2009-02-02 2010-08-26 INVISTA North America S.ar.I Compositions of surface modified nanoparticles
CN103147289B (en) * 2012-04-24 2015-06-03 南通大学 In-situ complexing method for preparing antibacterial fabric by simple steps
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