CN106917266B - antibacterial natural silk fiber product and preparation method thereof - Google Patents
antibacterial natural silk fiber product and preparation method thereof Download PDFInfo
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- CN106917266B CN106917266B CN201710177609.XA CN201710177609A CN106917266B CN 106917266 B CN106917266 B CN 106917266B CN 201710177609 A CN201710177609 A CN 201710177609A CN 106917266 B CN106917266 B CN 106917266B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating 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
- D06M11/83—Treating 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
Abstract
The invention discloses an antibacterial natural silk fiber product and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a formic acid solution, adding a silver salt into the formic acid solution, and stirring for dissolving; immersing a natural silk fiber product into a silver-containing hydrochloric acid solution, and reacting for a period of time; and fully washing the reacted silk fiber product, and drying to obtain the antibacterial natural silk fiber product. The invention can improve the broad-spectrum antibacterial performance of the silk fiber and the fabric thereof, and simultaneously avoid the harm to human bodies and the pollution to the environment. The preparation method is simple and easy for batch production, and the obtained antibacterial silk fiber product has excellent antibacterial property and lasting antibacterial performance.
Description
Technical Field
The invention relates to an antibacterial natural silk fiber product and a preparation method thereof, belonging to the technical field of high polymer materials.
Background
At present, the antibacterial treatment technology of textiles at home and abroad can be roughly divided into two types:Firstly, preparing antibacterial fibers, and then preparing various antibacterial fabrics;The fabric is post-treated with various antimicrobial agents to achieve antimicrobial properties.
In comparison, the fabric obtained by the first method has a lasting antibacterial effect and good washing fastness, but has the advantages of high technical content, high difficulty, wide related field, relatively complex antibacterial fiber production process and high requirement on antibacterial agents. The second method has simple processing process, but has more three wastes in production, and has poor washability and durability of antibacterial effect. But because the second method is convenient to process and has a wide range of available antibacterial agents. The antibacterial effect of the textile, whether the textile is raw fiber, yarn or fabric, or even garment, can be obtained by the after-finishing method, so that the after-finishing processing is more common in various antibacterial fabrics on the market at present.
In the prior art, the method of post-finishing processing comprises:
The antibacterial agent is fixed on the fiber surface by heat with reactive resin, such as diphenyl ether antibacterial agent like Nonstack, sanitze, etc. of Japan compressA deodorant finishing agent. It has no affinity to cellulose, and needs to be used together with 2D resin or cyanoaldehyde resin to improve its durability, and its deodorizing and antibacterial mechanism is to inhibit the functions of cell membrane and cell wall of microorganism.
The antibacterial agent is adsorbed and fixed on the surface of the fiber. Represents a commercial product such as Odoyte of cotton, both inside and outside.
The trimethoxy of the organosilicon quaternary ammonium salt is utilized to react with the hydroxyl methanol on the surface of the fiber to fix the antibacterial agent. The method is characterized in that the antibacterial agent is completely immobilized, and the antibacterial effect is determined by the contact state of the active part of the antibacterial agent and the cell surface of the bacteria. Such as Viosil, jenno, cronsil, dow, DC5700, from dow corning, usa, and the like.
Finishing by utilizing nano silver and silver-loaded zinc nano SiO2Finishing, chitosan finishing and the like to perform antibacterial after-finishing on the silk.
The antibacterial agents used in the general finishing of the post-woven fabrics mainly comprise quaternary ammonium salts, organic silicon quaternary ammonium salts, chitin, chitosan, inorganic salts, extracts of natural substances and the like, but most of the currently marketed antibacterial agents have the problems of poor antibacterial broad spectrum, poor washing resistance, unreliable safety and the like.
In the antibacterial fabric finishing agent, the silver system has stronger and wide antibacterial action, is dominant in inorganic antibacterial agents, and is a good choice for the antibacterial agent of the silk product. The current nano-silver antibacterial modification methods mainly comprise two methods: firstly, nano silver is synthesized and then decorated on the surface of a silk material; the other is to directly synthesize the nano silver on the surface of the silk material in situ. However, the two methods have the common problems that the nano silver is only adhered to the surface of the silk material, the adhesion amount is low, the adhesion fastness is poor, and the requirements of practical application cannot be met, so that the further application and popularization are greatly limited.
Therefore, a simple and convenient method for preparing antibacterial natural silk fiber products is needed.
Disclosure of Invention
the invention aims to provide a preparation method of an antibacterial natural silk fiber product, endows the natural silk fiber product with new functions and expands the application field of the natural silk fiber product.
In order to achieve the aim, the specific technical scheme of the invention is that the preparation method of the antibacterial natural silk fiber product comprises the following steps of preparing formic acid solution, adding silver salt into the formic acid solution, and stirring and dissolving the mixture under the condition of keeping out of the sun to prepare treatment solution; immersing the natural silk fiber product into the treatment solution, and standing for 0.1-24 hours at 0-60 ℃ in a dark place; and then washing and drying the natural silk fiber product to obtain the antibacterial natural silk fiber product.
In the technical scheme, the formic acid solution contains one or more of water, methanol, ethanol, propanol and isopropanol.
In the technical scheme, the concentration of the formic acid is 50-98%.
In the technical scheme, the silver salt is one or more of silver nitrate, silver chloride, silver bromide and silver fluoride.
in the technical scheme, the mass concentration of the silver salt is 0.0001-10%.
in the above technical scheme, the silk is mulberry silk, tussah silk, castor-oil plant silk.
In the above technical scheme, the natural silk fiber product is cocoon silk, raw silk, degumming silk, twisted silk, braided wire, non-woven fabric, knitted fabric or braided fabric.
In the preferred technical scheme, the mass concentration of formic acid in the formic acid solution is 90-98%; in the treatment fluid, the mass concentration of silver salt is 0.001-0.1%; the standing time is 1-12 h, and the temperature is 4-24 ℃; under the optimal condition, the preparation time is short, and the obtained natural silk fiber product also has good antibacterial performance.
The invention also discloses an antibacterial natural silk fiber product prepared by the preparation method of the antibacterial natural silk fiber product and application of the antibacterial natural silk fiber product in preparation of the antibacterial silk product.
According to the technical scheme of the invention, firstly, the formic acid is utilized to swell but not dissolve the silk, silver ions dissolved in the formic acid are introduced into the silk, and uniform dispersion in the silk is realized; then, the strong reducing aldehyde group contained in the carboxylic acid formic acid is utilized to directly reduce silver ions into nano metal silver in situ in the silk, so that the uniform loading of the nano silver in the silk can be realized. However, the prior art only fixes the nano silver on the surface of the silk fiber, and has the problems of low load rate, low fixing strength and uneven dispersion. According to the invention, the fluffy and porous structures of the silk are combined, the swelling effect of formic acid is utilized to introduce silver ions into silk fibers, and the strong reducibility of formic acid is utilized to directly reduce the silver ions into nano silver in situ, so that the uniform dispersion and fixation of the nano silver are realized, and the permanent antibacterial property and the water washing resistance can be obtained.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) The method adopts an in-situ reduction method, utilizes the reducibility of a formic acid solvent and combines the fluffy and porous structure of the silk, directly reduces silver ions into metal silver particles, and introduces the silver ions into silk fibers; the method solves the defect that silver ions reduced in the prior art are only attached to the surface of silk or surface holes and cannot enter the interior of silk fibers.
(2) According to the invention, the swelling property of formic acid to silk is utilized, silver seeds are introduced into the silk, and then the in-situ reduction technology is combined, so that the generated nano silver keeps good dispersibility, and meanwhile, most of the nano silver is fixed in the silk, the antibacterial property is durable, and the problem of poor binding fastness of the antibacterial agent and the silk product is solved.
(3) The nano silver particles prepared by the method have the diameter of 10-100 nm, small particle size, uniform size and excellent antibacterial performance, especially the nano silver ions and the silk material have strong binding force, and the silk fibroin is used for adsorbing and wrapping the silver ions and then reducing the silver ions into the nano silver in situ, so that the aggregation of the nano silver is effectively avoided, and the good dispersibility of the nano silver is realized.
(4) The method has wide applicability, and is suitable for degumming and unglued cocoon silks, raw silks, twisted threads, braided wires, knitted fabrics, woven fabrics, non-woven fabrics, braided fabrics and the like; the nano silver antibacterial material prepared by the invention has the advantages that the nano silver is uniformly dispersed inside and outside the material, such as the inside and the surface of the fiber, so the nano silver antibacterial material has lasting or permanent antibacterial performance.
(5) The method is simple, short in process flow and easy for mass production; especially, the treated antibacterial silver particles go deep into the fiber, the mechanical property of the fiber is not influenced, the influence of substances such as hydrochloric acid, sulfuric acid, alkali and the like on the mechanical property of the silk in the prior art is avoided, and the technical problem that the antibacterial property and the mechanical property are in reverse proportion in the prior art is solved.
Drawings
FIG. 1 is a scanning electron microscope image of untreated mulberry silk fibers (degummed silk) of example two;
FIG. 2 is a scanning electron microscope image of anti-microbial mulberry silk fibers (degummed silk) of the example;
FIG. 3 is a photograph and a scanning electron microscope image of tussah silk fibers (degummed silk) treated with the third antibiotic treatment in the example;
FIG. 4 is a photograph of the four antibacterial treated and untreated silk fabrics of the example.
Detailed Description
the invention is further described with reference to the following figures and examples:
Example one
Preparing a formic acid aqueous solution with the mass fraction of 90%, then adding silver nitrate into the formic acid aqueous solution, wherein the mass fraction of the silver nitrate is 0.001%, and magnetically stirring for 5min in a dark place to dissolve; immersing natural mulberry silk raw silk into formic acid solution, keeping away from light and standing for 1h at the temperature of 4 ℃; washing the obtained raw silk with water, and naturally drying to obtain an antibacterial silkworm raw silk product; performing an X-ray diffraction test to find that a large amount of nano silver exists in the silk, wherein the X-ray diffraction test pattern shows characteristic diffraction peaks of the nano silver at 38 degrees, 44 degrees, 64 degrees and 77 degrees, and a transmission electron microscope test also observes that the fiber section has uniform nano silver dispersion; the tensile strength of the raw silk before treatment is 380MPa, and the tensile strength of the raw silk after treatment is 372MPa, which reaches more than 96 percent before treatment.
Example two
Preparing a formic acid aqueous solution with the mass fraction of 98%, then adding silver nitrate into the formic acid aqueous solution, wherein the mass fraction of the silver nitrate is 0.01%, and magnetically stirring for 15min in a dark place to dissolve; immersing the natural degummed mulberry silk fiber into a formic acid solution, and standing for 5 hours in a dark place at the temperature of 24 ℃; fully washing the degummed mulberry silk with water, and naturally drying to obtain the antibacterial degummed mulberry silk; the tensile strength reaches more than 95 percent before treatment.
As shown in fig. 1, which is a scanning electron microscope image of untreated degummed silk, it can be seen that the surface of the silk fiber is smooth; FIG. 2 is a scanning electron microscope image of degummed mulberry silk treated with antibacterial agent, in which it can be seen that the surface of the silk has nano silver with a diameter of about 50 nm; and performing an X-ray diffraction test to find that a large amount of nano silver exists in the silk, wherein the X-ray diffraction test pattern shows characteristic diffraction peaks of the nano silver at 38 degrees, 44 degrees, 64 degrees and 77 degrees, and a transmission electron microscope test also shows that the fiber section has uniform nano silver dispersion. The invention successfully loads the silver particles on the silk fiber, most of the silver particles are in the fiber and are not easy to run off, and the antibacterial property after washing can be seen.
the antibacterial test adopts an antibacterial fabric test method in antibacterial knitwear (FZ/T73023-2006) which is a textile industry standard of the people's republic of China: the flask method was shaken.
The antibacterial effect test of the antibacterial silk fiber obtained in the second embodiment of the first embodiment is carried out, meanwhile, the antibacterial performance of the silk fiber without antibacterial treatment is tested, the results are shown in table 1, the results show that degummed and ungummed mulberry silk after antibacterial treatment both show excellent antibacterial performance, after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, and the antibacterial fastness is high.
TABLE 1 antibacterial Properties of Mulberry Silk fibers before and after treatment
EXAMPLE III
Preparing a formic acid ethanol solution with the mass fraction of 85%, then adding silver fluoride into the formic acid solution, wherein the mass fraction of the silver fluoride is 0.1%, and stirring for 30min to dissolve in a dark magnetic field; immersing degummed natural tussah silk into formic acid solution, keeping away from light and standing for 2h at the temperature of 14 ℃; and fully washing the degummed natural tussah silk, and naturally drying to obtain the antibacterial tussah silk fiber. As shown in fig. 3, a camera photograph and a scanning electron microscope picture of the degummed tussah silk subjected to the antibacterial treatment are shown, in the picture, the silk is yellow after the antibacterial treatment of the nano-silver, and the surface of the silk is provided with the nano-silver with the diameter of about 50 nm; performing an X-ray diffraction test to find that a large amount of nano silver exists in the silk, wherein the X-ray diffraction test pattern shows characteristic diffraction peaks of the nano silver at 38 degrees, 44 degrees, 64 degrees and 77 degrees, and a transmission electron microscope test also observes that the fiber section has uniform nano silver dispersion; the tensile strength reaches more than 95 percent before treatment; the inhibition rate of escherichia coli reaches 99.1%, the inhibition rate of bacillus subtilis reaches 98.3%, the inhibition rate of bacillus subtilis reaches 98.2%, and after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, which indicates that the antibacterial fastness is high.
Example four
Preparing a formic acid methanol solution with the mass fraction of 88%, then adding silver nitrate into the formic acid solution, wherein the mass fraction of the silver nitrate is 0.005%, and stirring for 5min to dissolve in a dark magnetic field; immersing the natural mulberry silk woven fabric into formic acid solution, and standing for 5 hours in a dark place at the temperature of 15 ℃; fully washing the obtained silk fabric, and naturally drying to obtain the antibacterial mulberry silk fabric; the inhibition rate of escherichia coli reaches 99.1%, the inhibition rate of bacillus subtilis reaches 98.3%, the inhibition rate of bacillus subtilis reaches 98.9%, and after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, which indicates that the antibacterial fastness is high. As shown in FIG. 4, the photographs of the antibacterial treated silk fabric (left) and the untreated silk fabric (right) are shown, in which the silk fabric is changed from white to yellow after the nano silver antibacterial treatment, and the transmission electron microscope test also shows that the fiber section has uniform nano silver dispersion.
EXAMPLE five
Preparing a 50% by mass formic acid aqueous solution, then adding silver chloride into the formic acid aqueous solution, wherein the mass fraction of the silver chloride is 0.001%, and stirring for 10min to dissolve in a dark magnetic field; immersing natural castor-oil plant silk raw silk into a formic acid solution, and standing for 12 hours in a dark place at the temperature of 37 ℃; fully washing the obtained raw silk, and naturally drying to obtain an antibacterial castor silkworm raw silk product; the tensile strength reaches more than 94% before treatment; the inhibition rate of escherichia coli reaches 98.4%, the inhibition rate of bacillus subtilis reaches 98.7%, the inhibition rate of bacillus subtilis reaches 98.8%, and after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, which indicates that the antibacterial fastness is high.
EXAMPLE six
Preparing a formic acid aqueous solution with the mass fraction of 30%, then adding silver nitrate into the formic acid aqueous solution, wherein the mass fraction of the silver nitrate is 0.05%, and magnetically stirring for 20min in a dark place to dissolve; immersing natural mulberry silk braided wire into formic acid solution, keeping out of the sun and standing for 24h at the temperature of 4 ℃; fully washing the obtained silk braided wire, and drying in vacuum to obtain the antibacterial mulberry silk braided wire; the inhibition rate of escherichia coli reaches 99.5%, the inhibition rate of bacillus subtilis reaches 98.6%, the inhibition rate of bacillus subtilis reaches 98.1%, and after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, which indicates that the antibacterial fastness is high.
EXAMPLE seven
Preparing 58% formic acid isopropanol solution, adding silver iodide into the formic acid solution, wherein the mass fraction of the silver iodide is 0.0008%, and stirring magnetically for 5min in a dark place to dissolve; immersing the natural mulberry silk knitted fabric into formic acid solution, and standing for 15h in a dark place at the temperature of 15 ℃; fully washing the obtained silk knitted fabric, naturally drying to obtain the antibacterial mulberry silk knitted fabric, and observing the fiber section by a transmission electron microscope test to have uniform nano silver dispersion; the inhibition rate of escherichia coli reaches 98.5%, the inhibition rate of bacillus subtilis reaches 98.4%, the inhibition rate of bacillus subtilis reaches 98.7%, and after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, which indicates that the antibacterial fastness is high.
Example eight
Preparing a formic acid aqueous solution with the mass fraction of 95%, then adding silver nitrate into the formic acid aqueous solution, wherein the mass fraction of the silver nitrate is 0.01%, and magnetically stirring for 5min in a dark place to dissolve; immersing degummed natural mulberry silk into formic acid solution, keeping away from light and standing for 10h at the temperature of 15 ℃; fully washing the obtained silk, and naturally drying to obtain the antibacterial mulberry silk; the tensile strength reaches more than 97 percent before treatment; the inhibition rate of escherichia coli reaches 99.8%, the inhibition rate of bacillus subtilis reaches 99.4%, the inhibition rate of bacillus subtilis reaches 99.1%, and after 50 times of standard washing, the antibacterial silk still keeps more than 80% of antibacterial effect, which indicates that the antibacterial fastness is high.
Claims (2)
1. a preparation method of an antibacterial natural silk fiber product is characterized by comprising the following steps of preparing formic acid solution, adding silver salt into the formic acid solution, and stirring and dissolving the mixture under the condition of keeping out of the sun to prepare treatment solution; immersing the natural silk fiber product into the treatment solution, and standing for 1-12 h at 4-24 ℃ in a dark place; then washing and drying the natural silk fiber product to obtain an antibacterial natural silk fiber product; the formic acid solution contains one or more of water, methanol, ethanol, propanol and isopropanol; the silver salt is one or more of silver nitrate, silver chloride, silver bromide and silver fluoride; in the formic acid solution, the mass concentration of formic acid is 90-98%; in the treatment fluid, the mass concentration of the silver salt is 0.001-0.1%.
2. The method for preparing natural silk fiber product with antibacterial effect according to claim 1, wherein the silk is one or more selected from mulberry silk, tussah silk, and castor-oil plant silk.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022029769A1 (en) * | 2020-08-06 | 2022-02-10 | Security Matters Ltd. | Marking silk products |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105256544A (en) * | 2015-10-28 | 2016-01-20 | 南通纺织丝绸产业技术研究院 | High-performance natural silk fiber and preparation method thereof |
| CN105723027A (en) * | 2013-09-23 | 2016-06-29 | 特殊纤维及材料有限公司 | Cellulose fibres |
| CN106243377A (en) * | 2016-08-19 | 2016-12-21 | 苏州大学 | A kind of porous silk fibrous material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105723027A (en) * | 2013-09-23 | 2016-06-29 | 特殊纤维及材料有限公司 | Cellulose fibres |
| CN105256544A (en) * | 2015-10-28 | 2016-01-20 | 南通纺织丝绸产业技术研究院 | High-performance natural silk fiber and preparation method thereof |
| CN106243377A (en) * | 2016-08-19 | 2016-12-21 | 苏州大学 | A kind of porous silk fibrous material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022029769A1 (en) * | 2020-08-06 | 2022-02-10 | Security Matters Ltd. | Marking silk products |
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