CN109487554A - A kind of antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver - Google Patents
A kind of antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver Download PDFInfo
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- CN109487554A CN109487554A CN201811370444.9A CN201811370444A CN109487554A CN 109487554 A CN109487554 A CN 109487554A CN 201811370444 A CN201811370444 A CN 201811370444A CN 109487554 A CN109487554 A CN 109487554A
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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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/30—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating 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 nitrogen
- D06M13/325—Amines
- D06M13/342—Amino-carboxylic acids; Betaines; Aminosulfonic acids; Sulfo-betaines
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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Abstract
The invention discloses a kind of antibacterial cotton fabrics and preparation method thereof based on Chitosan-Thiolated Polymers in-situ reducing nano silver, Chitosan-Thiolated Polymers grafting cotton fabric is immersed in silver nitrate solution, it is slowly added to reducing agent under room temperature, the antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver can be obtained after 60-80 DEG C of reaction 30-300min.The present invention is by the Covalent bonding together (C=N) between sulfydryl (- SH) and the coordination and cotton fiber and chitosan of silver, using dialdehyde cotton fabric as substrate, in-situ preparation has the nanometer silver antimicrobial cotton fabric of excellent dispersing uniformity, antibacterial and washing fastness.
Description
Technical field
The present invention relates to a kind of antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver, metal nanometer material,
High molecular material and textile material field.
Background technique
In recent years, nanotechnology has become the forward position interdisciplinary such as physics, chemistry, biology, medicine and material science
Technology, because to the energy, medicine, electronics, aircraft industry etc. have can not estimate tremendous influence due to by researcher pass
Note.And metal nanoparticle causes due to properties such as unique physics, chemistry, optics, electricity, magnetics, calorifics, biology
Great interest, metal nanoparticle especially nano silver have huge potential using value in multiple fields, such as sense skill
Art, optical device, catalysis, biomarker, drug reprinting and treatment of cancer etc..
The preparation of traditional nano silver is divided into physical method and chemical method.Physical method is more demanding to instrument and equipment, and production takes
With valuableness.Chemical method mostly uses hydrazine hydrate, formaldehyde, polyalcohol, organic amine etc. to make reducing agent, although these reducing agents have high live
Property, but to environment nocuousness, and agglomeration easily occurs for nano silver obtained.
In recent years, the hot spot that nano silver is increasingly becoming research, phase are prepared using green, environmentally friendly, efficient and cheap method
Than in physics, chemical method, advantageously, from a wealth of sources, reaction condition is mild, can be reacted at normal temperatures and pressures, synthesis
Nano silver particles have good biocompatibility.The green reducing agent used at present specifically includes that vitamin, citric acid
Sodium, pyrogallol, hydroquinone, tea polyphenols, glucose, fructose, sucrose, plant and pericarp extract, microorganism etc..
Chitosan is the green reducing agent and protective agent of a kind of important nano silver.Such as Zhejiang University's Zhang Yufei useization
Reduction method is learned in the chitosan-acetic acid solution of various concentration, with sodium borohydride reduction silver nitrate, is prepared for serial chitosan nano
The silver-colored solution of the rice (stability of Zhang Yufei, Li Youliang, Yao Yuan, Li Wenyu, Hu Qiaoling chitosan nano silver solution and anti-in fabric
Application [J] Chemical Journal of Chinese Universities that bacterium arranges, 2012,33 (08): 1860-1865).Wuhan Textile University Peng Junjun
Using chitin modified cotton and dacron, nanometer is prepared for by the chitosan in situ absorption of fabric surface, reduction silver ion
Silver-colored antibiotic fabric (closes in situ in the chitin modified fabric of Peng Junjun, Zhang Xin, Wu Yiming, Liu Hongling, Ran Jianhua, Li Ming, Yang Feng
At Nano silver grain [J] Chemical Journal of Chinese Universities, 2014,35 (02): 415-420).The Durability of antimicrobial effect of nano silver
(durable antibacterial properties) is an important index, including two parts: first is that nanometer silver surface
The stabilizer of modification and the binding strength of nano silver, second is that the combination between the stabilizer and textile fabric of nano silver surface modification
Fastness, the two are indispensable.But between above-mentioned document nano silver and chitosan, chitosan it is firm to lacking between fabric
Covalent bonding together.
Summary of the invention
In view of the above deficiencies, the present invention provides a kind of antibacterial cottons based on Chitosan-Thiolated Polymers in-situ reducing nano silver to knit
The preparation method of object.
The technical scheme is that: chitosan (1) is dissolved in 2% acetic acid solution, is configured to quality
Then dialdehyde cotton fabric is immersed in 30-300min in 60-80 DEG C of chitosan solution by the chitosan solution of score 1-10%, bath
Than 1:30, deionization is cleaned repeatedly, is dried after taking-up, obtains chitosan graft cotton fabric.(2) above-mentioned chitosan graft cotton is knitted
The sodium periodate solution that object is immersed in 1g/L is protected from light 10-30min, and 60-80 DEG C of reaction temperature, bath raio 1:30 uses deionization
Water cleans repeatedly, and drying obtains dialdehyde chitosan graft cotton fabric.(3) above-mentioned dialdehyde chitosan graft cotton fabric is immersed in matter
The cysteamine solution of score 1-10% is measured, bath raio 1:30, magnetic agitation reaction for 24 hours, is cleaned repeatedly with deionized water under room temperature, is dried
It is dry that Chitosan-Thiolated Polymers grafting cotton fabric is prepared;(4) above-mentioned Chitosan-Thiolated Polymers grafting cotton fabric is immersed in 1-100g/
In the silver nitrate solution of L, bath raio 1:30 is slowly added to reducing agent under room temperature, and the mass ratio of the reducing agent and silver nitrate is
The antibacterial cotton based on Chitosan-Thiolated Polymers in-situ reducing nano silver can be obtained after 0.5-2,60-80 DEG C of reaction 30-300min to knit
Object.
The preparation of dialdehyde cellulose is a routine techniques (Cellulose Science and technology, 2003 (03): 17-21+34;Peng
It is brave rigid, Ji Junling, Tao Yongxin, Wang Yuan, Qin Yong, Zhang Wei;Printing and dyeing, 2011,37 (08): 12-14+32;Printing and dyeing assistant, 2010,27
(12):48-49,53;Printing and dyeing, 2012,38 (14): 6-9,45;University Of Suzhou's journal (industry science version), 2007,27 (4): 19-23),
Research papers are numerous.Cellulose is that a kind of renewable resource wide, that content is big is distributed in nature, is led to by glucose residue
It crosses β-Isosorbide-5-Nitrae-glucosides key connection to form, molecular composition is (C6H12O5) n, n is the degree of polymerization.There are three in each glucose unit
Polar hydroxyl groups are respectively at 2,3,6 of glucose ring.Sodium metaperiodate selective oxidation cellulose, can aoxidize o-dihydroxy
For aldehyde radical, to obtain dialdehyde cellulose (modern textile technology, 2013,21 (05): 58-61).Pass through regulation sodium metaperiodate
Oxidization time, oxidizing temperature and oxidant concentration can control the degree of oxidation of dialdehyde cellulose.
The selective oxidation of chitosan and the selective oxidation of cellulose similar (functional material, 2014,45 (06): 6092-
6096+6101;Journal of Analytical Science, 2007 (02): 125-128;Selective oxidation chitosan derivatives prepare and in papermaking
Application [D] Southern Yangtze University, 2014;Printing and dyeing, 2012,38 (23): 1-4;Chengdu Textile higher junior college's journal, 2016,33
(04): 37-41).Silver nitrate reduction even directly can be generated Nano silver grain by the dialdehyde chitosan after sodium periodate oxidation
(Chengdu Textile higher junior college's journal, 2016,33 (04): 37-41).But in order to further increase the reduction of nano silver effect
Fruit, the present invention joined common nanometer silver reductor during reduction reaction, such as hydrazine hydrate, hydroiodic acid, sodium borohydride, dimension
Raw element C, glucose, amino acid, cyclodextrin, PAMAM, polyethyleneimine, over-branched polyamidoamine etc..
The principle of the invention lies in: first in the surface grafting chitosan of dialdehyde cotton fabric, then proceed by selectivity
Oxidation, is oxidized to dialdehyde chitosan for the chitosan that dialdehyde surface of cotton fabric is grafted.Certainly in the oxidation process of sodium metaperiodate,
The macromolecular glucose unit of cotton fabric again some be selectively oxidized.When the chitosan quilt of dialdehyde surface of cotton fabric grafting
It is oxidized to dialdehyde chitosan, the site active aldehyde radical (- CHO) is increased on the macromolecular chain of chitosan, so as to continue and half
The amino (- NH on cystamine surface2) carry out schiff base reaction, the chitosan sulfhydrylation for being finally grafted dialdehyde surface of cotton fabric.It is logical
The sulfydryl (- SH) on thio chitosan surface and the coordination of silver are crossed, silver is secured firmly to the surface of cotton fabric.
The present invention has the advantages that the present invention by chitosan sulfydryl (- SH) and silver coordination and cotton fiber and
Covalent bonding together (C=N) between chitosan, using dialdehyde cotton fabric as substrate, in-situ preparation has excellent be uniformly dispersed
The nanometer silver antimicrobial cotton fabric of property, antibacterial and washing fastness.Chitosan plays the role of similar double-sided adhesive, by nano-Ag particles jail
It is sticked to the surface of cotton fabric firmly.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.
Embodiment 1:(1) chitosan is dissolved in 2% acetic acid solution, it is configured to the chitosan solution of mass fraction 1%, then
Dialdehyde cotton fabric is immersed in 30min in 60 DEG C of chitosan solution, bath raio 1:30, deionization is cleaned repeatedly, is dried after taking-up,
Obtain chitosan graft cotton fabric.(2) sodium periodate solution that above-mentioned chitosan graft cotton fabric is immersed in 1g/L is protected from light instead
10min is answered, 60 DEG C of reaction temperature, bath raio 1:30 is cleaned repeatedly with deionized water, and drying obtains dialdehyde chitosan graft cotton and knits
Object.(3) above-mentioned dialdehyde chitosan graft cotton fabric is immersed in the cysteamine solution of mass fraction 1%, bath raio 1:30, under room temperature
Magnetic agitation is reacted for 24 hours, is cleaned repeatedly with deionized water, and Chitosan-Thiolated Polymers grafting cotton fabric is prepared in drying;It (4) will be upper
It states Chitosan-Thiolated Polymers grafting cotton fabric to be immersed in the silver nitrate solution of 10g/L, bath raio 1:30, is slowly added to be hydrated under room temperature
The mass ratio of hydrazine, the hydrazine hydrate and silver nitrate is can be obtained after being 0.5,60 DEG C of reaction 30min based on Chitosan-Thiolated Polymers original
The antibacterial cotton fabric of position reducing nano-silver.
Embodiment 2:(1) chitosan is dissolved in 2% acetic acid solution, it is configured to the chitosan solution of mass fraction 5%, then
Dialdehyde cotton fabric is immersed in 60min in 70 DEG C of chitosan solution, bath raio 1:30, deionization is cleaned repeatedly, is dried after taking-up,
Obtain chitosan graft cotton fabric.(2) sodium periodate solution that above-mentioned chitosan graft cotton fabric is immersed in 1g/L is protected from light instead
20min is answered, 70 DEG C of reaction temperature, bath raio 1:30 is cleaned repeatedly with deionized water, and drying obtains dialdehyde chitosan graft cotton and knits
Object.(3) above-mentioned dialdehyde chitosan graft cotton fabric is immersed in the cysteamine solution of mass fraction 5%, bath raio 1:30, under room temperature
Magnetic agitation is reacted for 24 hours, is cleaned repeatedly with deionized water, and Chitosan-Thiolated Polymers grafting cotton fabric is prepared in drying;It (4) will be upper
It states Chitosan-Thiolated Polymers grafting cotton fabric to be immersed in the silver nitrate solution of 20g/L, bath raio 1:30, is slowly added to boron hydrogen under room temperature
The mass ratio of change sodium, the sodium borohydride and silver nitrate can be obtained after being 1,70 DEG C of reaction 60min based on Chitosan-Thiolated Polymers
The antibacterial cotton fabric of in-situ reducing nano silver.
Embodiment 3:(1) chitosan is dissolved in 2% acetic acid solution, it is configured to the chitosan solution of mass fraction 10%, so
Dialdehyde cotton fabric is immersed in 300min in 80 DEG C of chitosan solution, bath raio 1:30 afterwards, deionization is cleaned repeatedly, dried after taking-up
It is dry, obtain chitosan graft cotton fabric.(2) sodium periodate solution that above-mentioned chitosan graft cotton fabric is immersed in 1g/L is protected from light
30min is reacted, 80 DEG C of reaction temperature, bath raio 1:30 is cleaned repeatedly with deionized water, and drying obtains dialdehyde chitosan graft cotton and knits
Object.(3) above-mentioned dialdehyde chitosan graft cotton fabric is immersed in the cysteamine solution of mass fraction 10%, bath raio 1:30, under room temperature
Magnetic agitation is reacted for 24 hours, is cleaned repeatedly with deionized water, and Chitosan-Thiolated Polymers grafting cotton fabric is prepared in drying;It (4) will be upper
It states Chitosan-Thiolated Polymers grafting cotton fabric to be immersed in the silver nitrate solution of 100g/L, bath raio 1:30, is slowly added to gather under room temperature
The mass ratio of aziridine, the polyethyleneimine and silver nitrate can be obtained after being 2,80 DEG C of reaction 300min based on sulfhydrylation
The antibacterial cotton fabric of chitosan in situ reducing nano-silver.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.Here all embodiments can not be exhaustive.It is all to belong to this hair
Bright technical solution changes and variations that derived from are still in the scope of protection of the present invention.
Claims (3)
1. a kind of preparation method of the antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver, which is characterized in that
(1) chitosan is dissolved in 2% acetic acid solution, is configured to the chitosan solution of mass fraction 1-10%, then by dialdehyde cotton
Fabric is immersed in 30-300min in 60-80 DEG C of chitosan solution, bath raio 1:30, and deionization is cleaned repeatedly, dried after taking-up,
Obtain chitosan graft cotton fabric;
(2) sodium periodate solution that above-mentioned chitosan graft cotton fabric is immersed in 1g/L is protected from light 10-30min, reaction temperature
60-80 DEG C, bath raio 1:30 of degree, is cleaned repeatedly with deionized water, and drying obtains dialdehyde chitosan graft cotton fabric;
(3) above-mentioned dialdehyde chitosan graft cotton fabric is immersed in the cysteamine solution of mass fraction 1-10%, bath raio 1:30, often
The lower magnetic agitation reaction of temperature for 24 hours, is cleaned repeatedly with deionized water, and Chitosan-Thiolated Polymers grafting cotton fabric is prepared in drying;
(4) above-mentioned Chitosan-Thiolated Polymers grafting cotton fabric is immersed in the silver nitrate solution of 1-100g/L, bath raio 1:30, room temperature
Under be slowly added to reducing agent, the mass ratio of the reducing agent and silver nitrate is 0.5-2, after 60-80 DEG C of reaction 30-300min
Obtain the antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver.
2. a kind of preparation of antibacterial cotton fabric based on Chitosan-Thiolated Polymers in-situ reducing nano silver according to claim 1
Method, which is characterized in that the reducing agent is hydrazine hydrate, hydroiodic acid, sodium borohydride, vitamin C, glucose, amino acid, ring paste
One of essence, PAMAM, polyethyleneimine, over-branched polyamidoamine are a variety of.
3. being knitted by a kind of antibacterial cotton based on Chitosan-Thiolated Polymers in-situ reducing nano silver that claim 1 preparation method obtains
Object.
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CN110373899A (en) * | 2019-06-27 | 2019-10-25 | 浙江理工大学 | A kind of washable antibacterial cotton fabric and preparation method thereof |
CN110625132A (en) * | 2019-09-05 | 2019-12-31 | 浙江科曼奇生物科技股份有限公司 | Sulfhydrylation amphiphilic carbon residue/nano-silver compound, preparation method thereof and antibacterial leather |
CN111155309A (en) * | 2019-12-31 | 2020-05-15 | 宜禾股份有限公司 | Preparation process of electromagnetic shielding fiber for preparing protective clothing |
CN111334053A (en) * | 2020-04-24 | 2020-06-26 | 刘平弟 | Antibacterial material of nano-silver covalent grafting halogenated hydantoin-based chitosan and preparation method thereof |
CN111551536A (en) * | 2020-06-05 | 2020-08-18 | 广东石油化工学院 | Preparation method and application of SERS (surface enhanced Raman Scattering) probe based on electrostatic assembly and in-situ reduction |
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CN114086405B (en) * | 2021-12-22 | 2024-02-13 | 中纺院(浙江)技术研究院有限公司 | Biological reducing agent and method for applying biological reducing agent to plant indigo dyed yarns |
CN115852674A (en) * | 2022-11-08 | 2023-03-28 | 江南大学 | Fiber product for realizing photo-thermal rapid sterilization based on in-situ deposited nanoparticles and finishing method thereof |
CN115852674B (en) * | 2022-11-08 | 2023-11-28 | 江南大学 | Fiber product for realizing photo-thermal rapid sterilization based on in-situ deposited nano particles and finishing method thereof |
CN117802801A (en) * | 2023-12-29 | 2024-04-02 | 绍兴迈宝科技有限公司 | Preparation method and application of oxidized chitosan amino-terminated hyperbranched compound grafted cellulose fabric |
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