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CN113338029A - Antiviral silver-loaded fiber and preparation method thereof - Google Patents

Antiviral silver-loaded fiber and preparation method thereof Download PDF

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Publication number
CN113338029A
CN113338029A CN202110588369.9A CN202110588369A CN113338029A CN 113338029 A CN113338029 A CN 113338029A CN 202110588369 A CN202110588369 A CN 202110588369A CN 113338029 A CN113338029 A CN 113338029A
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Prior art keywords
silver
fiber
cation exchange
washing
antiviral
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CN202110588369.9A
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Inventor
郑斌
曾庆轩
李运稳
周定怀
何星存
郑波
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Guilin Zhenghan Technology Development Co ltd
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Guilin Zhenghan Technology Development Co ltd
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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
    • D06M11/58Treating 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 nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64Treating 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 nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • D06M11/65Salts of oxyacids of nitrogen
    • 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

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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)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention discloses an antivirus silver-carrying fiber and a preparation method thereof, cation exchange fiber is reacted with silver nitrate solution by adopting an ion exchange method to prepare the silver-carrying fiber, the silver content and the antivirus performance of the silver-carrying fiber are detected and analyzed, and the antivirus activity rate of the silver-carrying fiber prepared by adopting the method is 99.99 percent according to the detection result, thus the antivirus silver-carrying fiber has the antivirus performance. The antiviral silver-loaded fiber prepared by the preparation method can be used in the fields of home textiles, special clothing, medical treatment, sports, army equipment, air purification and the like. At present, a large number of products are used for producing medical masks. The preparation method of the invention not only effectively reduces the production cost, but also reduces the environmental pollution, and is suitable for popularization and application.

Description

Antiviral silver-loaded fiber and preparation method thereof
Technical Field
The invention belongs to the technical field of silver-loaded fibers, and particularly relates to an antiviral silver-loaded fiber and a preparation method thereof.
Background
The silver-carrying fiber as a high-tech functional fiber has the functions of resisting bacteria, deodorizing, preventing electromagnetic wave radiation, resisting static electricity, regulating body temperature and the like, and has wide application prospect in the fields of home textiles, special clothing, medical treatment, sports, army equipment and the like. At present, the world carries a few brands of silver-carrying fibers, mainly including MitsuuJI, American X-STATIC, Germany SHIELDEX, and some enterprises in China are producing the silver-carrying fibers. The silver-loaded fiber is easy to have the phenomena of unstable product quality, easy shedding and oxidation of a coating and the like in the preparation process, and the problems of hard yarn hand feeling, poor fabric wearability and the like in the product development process, so that the conditions of high raw material cost and unstable product performance are caused, and the commercial application of the antibacterial product based on the silver-loaded fiber is difficult to popularize in the market.
At present, the preparation method of the silver-loaded active carbon fiber mainly comprises two methods, namely a front silver-loading technology and a rear silver-loading technology. The silver front loading technology is to load silver ions, simple substance silver or silver compounds on the surface of the fiber before the fiber is carbonized and activated. The method has the problems that silver ions in the solution are not easy to load on precursor fibers, and silver particles on the surfaces of carbon fibers are not uniformly distributed, the particle diameters are different, and the antibacterial performance is poor after carbonization and activation.
Post-silver-loading technology, namely, after the fiber is carbonized and activated, silver ions, simple substance silver or silver compounds are loaded on the surface of the activated carbon fiber by methods of spraying, dipping adsorption and the like. If an electrochemical deposition method is adopted to load nano silver on the activated carbon fiber, the adsorption capacity of the activated carbon fiber is firstly utilized to adsorb silver ions, then a cathode reduction method is adopted to reduce the silver ions into silver simple substances, and the nano silver is obtained by controlling the operation conditions and is directly fixed on the surface of the activated carbon fiber while being generated. For example, vacuum impregnation is adopted to adsorb silver nitrate solution, and thermal decomposition is carried out to prepare the silver-loaded active carbon fiber. For example, the silver-loaded activated carbon fiber is prepared by immersing or spraying a silver-containing solution and oscillating so that the nano silver particles are embedded into the activated carbon fiber. For example, the silver-loaded activated carbon fiber is prepared by adopting an ion exchange method to combine nano-scale silver and silver oxide to be implanted on the surface of the activated carbon fiber. However, the post-silver loading technique tends to have the following problems: (1) the silver has poor binding force with the activated carbon fiber, is easy to fall off in the process of water filtration and has short service life; (2) the adsorption performance of the activated carbon fiber is reduced; (3) other impurities may be introduced, which causes the safety problem when the activated carbon fiber is applied to medical dressings, and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention adopts an ion exchange method to react cation exchange fiber with silver nitrate solution to prepare silver-loaded fiber, and the silver-loaded fiber is detected and analyzed, and the detection result shows that the silver-loaded fiber has antiviral performance.
The technical scheme for realizing the purpose of the invention is as follows:
the invention relates to a preparation method of an antiviral silver-loaded fiber, which comprises a static preparation method and a dynamic preparation method, wherein the static preparation method comprises the following steps:
(1) taking cation exchange fiber, washing with deionized water, detecting pH value to be neutral by pH test paper after washing, and stopping washing;
(2) putting the cation exchange fiber washed in the step (1) into a silver nitrate solution of 10 g/L, uniformly stirring, soaking, and detecting the pH value of the solution by using pH test paper after soaking, wherein the exchange is complete when the pH = 4-5;
(3) taking out the cation exchange fiber with complete exchange from the silver nitrate solution, washing the cation exchange fiber with deionized water to be neutral, detecting the washing liquid with 5% sodium chloride solution, and finishing the washing without flocculent precipitate;
(4) and (3) spin-drying or naturally airing the washed cation exchange fiber by using a centrifugal machine, wherein the water content is 20-45%, and the silver loading amount of each gram of the cation exchange fiber is 0.05-0.2 g, so that the antiviral silver-loaded fiber is obtained.
The dynamic preparation method comprises the following steps:
(1) taking cation exchange fiber, washing with deionized water, detecting pH value to be neutral by pH test paper after washing, and stopping washing;
(2) filling the cation exchange fiber washed in the step (1) into a cation exchange column, and adding 10 g/L silver nitrate solution from top to bottom at a solution flow rate of 1BV/h-10 BV/h;
(3) after the silver nitrate solution is added, adding deionized water from top to bottom to wash the silver nitrate solution to be neutral, wherein the flow rate is 1BV/h-10BV/h, detecting the washing solution by using a 5% sodium chloride solution, and finishing washing without flocculent precipitates;
(4) and (3) taking out the washed cation exchange fiber from the cation exchange column, and drying the cation exchange fiber by a centrifugal machine or naturally airing the cation exchange fiber, wherein the water content is 20-45%, and the silver-carrying amount of each gram of the cation exchange fiber is 0.05-0.2 g by detection, so that the antiviral silver-carrying fiber is obtained.
In the static and dynamic preparation method, the cation exchange fiber in the step (1) is a hydrogen type and strong acid cation exchange fiber.
In the static and dynamic preparation methods, the mass ratio of the cation exchange fiber in the step (2) to the silver nitrate solution is 2.5-10: 1.
In the static and dynamic preparation methods, the preferable mass ratio of the cation exchange fiber and the silver nitrate solution in the step (2) is 10: 1.
The invention also aims to provide the antiviral silver-loaded fiber prepared by the static and dynamic preparation methods, and the silver content, the antiviral property and the like of the antiviral silver-loaded fiber are detected and analyzed, so that a foundation is laid for the popularization and the application of the novel silver-loaded live fiber.
The antiviral silver-loaded fiber prepared by the preparation method can be used in the fields of home textiles, special clothing, medical treatment, sports, army equipment, air purification and the like. At present, a large number of products are used for producing medical masks.
The preparation method of the invention not only effectively reduces the production cost, but also reduces the environmental pollution, and is suitable for popularization and application.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited thereto.
Example 1
The preparation method of the antiviral silver-loaded fiber comprises the following steps:
(1) taking hydrogen type and strong acid cation exchange fibers, washing with deionized water, detecting the pH value to be neutral by using pH test paper after washing, and stopping washing;
(2) putting the cation exchange fiber washed in the step (1) into a silver nitrate solution of 10 g/L, uniformly stirring, soaking, and detecting the pH value of the solution by using pH test paper after soaking, wherein the exchange is complete when the pH = 4-5;
the mass ratio of the cation exchange fiber to the silver nitrate solution is 10: 1;
(3) taking out the cation exchange fiber with complete exchange from the silver nitrate solution, washing the cation exchange fiber with deionized water to be neutral, detecting the washing liquid with 5% sodium chloride solution, and detecting whether flocculent precipitate exists or not, wherein silver nitrate residue does not exist, and washing is finished;
(4) and (3) spin-drying or naturally airing the washed cation exchange fiber by using a centrifugal machine, wherein the water content is 20-45%, and the silver loading amount of each gram of the cation exchange fiber is 0.05-0.2 g, so that the antiviral silver-loaded fiber is obtained.
Example 2
The preparation method of the antiviral silver-loaded fiber comprises the following steps:
(1) taking hydrogen type and strong acid cation exchange fibers, washing with deionized water, detecting the pH value to be neutral by using pH test paper after washing, and stopping washing;
(2) filling the cation exchange fiber washed in the step (1) into a cation exchange column, and adding 10 g/L silver nitrate solution from top to bottom at a solution flow rate of 1BV/h-10 BV/h;
the mass ratio of the cation exchange fiber to the silver nitrate solution is 10: 1;
(3) after the silver nitrate solution is added, adding deionized water from top to bottom to wash until the solution is neutral, wherein the flow rate is 1BV/h-10BV/h, detecting the washing solution by using a 5% sodium chloride solution, and finishing washing without flocculent precipitate;
(4) and (3) taking out the washed cation exchange fiber from the cation exchange column, and drying the cation exchange fiber by a centrifugal machine or naturally airing the cation exchange fiber, wherein the water content is 20-45%, and the silver-carrying amount of each gram of the cation exchange fiber is 0.05-0.2 g by detection, so that the antiviral silver-carrying fiber is obtained.
Examples of the experiments
The silver-loaded fibers prepared in examples 1 and 2 were tested and analyzed:
1. silver content testing of silver-loaded fibers
Referring to EPA3052:1996, the content of silver in the silver-loaded activated carbon fiber was analyzed by ICP-OES, and as a result, the silver-loaded fibers prepared in examples 1 and 2 satisfied the use requirement that the silver-loaded amount per gram of the cation exchange fiber was 0.2 g.
2. Antiviral Activity test of silver-carrying fiber
At 18.03.2021, the applicant sent 60 g of prepared silver-loaded fiber to the Guangdong province microbiological analysis and detection center for detection, and the results of 2 hours of antiviral tests are shown in Table 1:
Figure DEST_PATH_IMAGE001
antiviral test 24 hour results, see table 2:
Figure 624584DEST_PATH_IMAGE002
according to the detection result, the antiviral activity rate of the silver-loaded fiber prepared by the method is 99.99%, and the silver-loaded fiber prepared by the method is a silver-loaded fiber with antiviral property.

Claims (6)

1. The preparation method of the antiviral silver-loaded fiber is characterized by comprising the following steps: (1) taking cation exchange fiber, washing with deionized water, detecting pH value to be neutral by pH test paper after washing, and stopping washing;
(2) putting the cation exchange fiber washed in the step (1) into a silver nitrate solution of 10 g/L, uniformly stirring, soaking, and detecting the pH value of the solution by using pH test paper after soaking, wherein the exchange is complete when the pH = 4-5;
(3) taking out the cation exchange fiber with complete exchange from the silver nitrate solution, washing the cation exchange fiber with deionized water to be neutral, detecting the washing liquid with 5% sodium chloride solution, and finishing the washing without flocculent precipitate;
(4) and (3) spin-drying or naturally airing the washed cation exchange fiber by using a centrifugal machine, wherein the water content is 20-45%, and the silver loading amount of each gram of the cation exchange fiber is 0.05-0.2 g, so that the antiviral silver-loaded fiber is obtained.
2. The preparation method of the antiviral silver-loaded fiber is characterized by comprising the following steps: (1) taking cation exchange fiber, washing with deionized water, detecting pH value to be neutral by pH test paper after washing, and stopping washing;
(2) filling the cation exchange fiber washed in the step (1) into a cation exchange column, and adding 10 g/L silver nitrate solution from top to bottom at a solution flow rate of 1BV/h-10 BV/h;
(3) after the silver nitrate solution is added, adding deionized water from top to bottom to wash the silver nitrate solution to be neutral, wherein the flow rate is 1BV/h-10BV/h, detecting the washing solution by using a 5% sodium chloride solution, and finishing washing without flocculent precipitates;
(4) and (3) taking out the washed cation exchange fiber from the cation exchange column, and drying the cation exchange fiber by a centrifugal machine or naturally airing the cation exchange fiber, wherein the water content is 20-45%, and the silver-carrying amount of each gram of the cation exchange fiber is 0.05-0.2 g by detection, so that the antiviral silver-carrying fiber is obtained.
3. The method for producing an antiviral silver-loaded fiber according to any one of claims 1 to 2, characterized in that: the cation exchange fiber in the step (1) is a hydrogen type and strong acid cation exchange fiber.
4. The method for producing an antiviral silver-loaded fiber according to any one of claims 1 to 2, characterized in that: the mass ratio of the cation exchange fiber in the step (2) to the silver nitrate solution is 2.5-10: 1.
5. The method of preparing an antiviral silver-loaded fiber as in claim 4, wherein: the mass ratio of the cation exchange fiber in the step (2) to the silver nitrate solution is 10: 1.
6. An antiviral silver-loaded fiber produced by the production method according to any one of claims 1 to 2.
CN202110588369.9A 2021-05-28 2021-05-28 Antiviral silver-loaded fiber and preparation method thereof Pending CN113338029A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06200472A (en) * 1992-12-28 1994-07-19 Suntory Ltd Antimicrobial fiber, its production and material made of fiber
WO1996000321A1 (en) * 1994-06-24 1996-01-04 Suntory Limited Antibacterial fiber, textile and water-treating element using the fiber and method of producing the same
CN1609336A (en) * 2003-10-21 2005-04-27 北京服装学院 Antiviral fibre and producing method and use thereof
CN101182689A (en) * 2007-12-14 2008-05-21 华南理工大学 Inorganic silver-impregnated zeolite antibiotic papers and method of producing the same
CN101812801A (en) * 2009-12-23 2010-08-25 中国船舶重工集团公司第七一八研究所 Antibacterial functional fibers
CN105750560A (en) * 2016-03-16 2016-07-13 张家港耐尔纳米科技有限公司 Silver-bearing antibacterial solution and preparation method thereof
CN106538519A (en) * 2016-11-01 2017-03-29 山东理工大学 A kind of method that ion exchange prepares silver molecular sieve high-efficient antibacterial agent admittedly

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06200472A (en) * 1992-12-28 1994-07-19 Suntory Ltd Antimicrobial fiber, its production and material made of fiber
WO1996000321A1 (en) * 1994-06-24 1996-01-04 Suntory Limited Antibacterial fiber, textile and water-treating element using the fiber and method of producing the same
CN1609336A (en) * 2003-10-21 2005-04-27 北京服装学院 Antiviral fibre and producing method and use thereof
CN101182689A (en) * 2007-12-14 2008-05-21 华南理工大学 Inorganic silver-impregnated zeolite antibiotic papers and method of producing the same
CN101812801A (en) * 2009-12-23 2010-08-25 中国船舶重工集团公司第七一八研究所 Antibacterial functional fibers
CN105750560A (en) * 2016-03-16 2016-07-13 张家港耐尔纳米科技有限公司 Silver-bearing antibacterial solution and preparation method thereof
CN106538519A (en) * 2016-11-01 2017-03-29 山东理工大学 A kind of method that ion exchange prepares silver molecular sieve high-efficient antibacterial agent admittedly

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
崔峰涛: "《让科技引导绿色生活》", 30 September 2013, pages: 90 - 91 *
聂梅生, 中国建筑工业出版社, pages: 700 - 701 *

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