CN103881035B - Antibacterial finishing agent for fabric - Google Patents
Antibacterial finishing agent for fabric Download PDFInfo
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- CN103881035B CN103881035B CN201310567946.1A CN201310567946A CN103881035B CN 103881035 B CN103881035 B CN 103881035B CN 201310567946 A CN201310567946 A CN 201310567946A CN 103881035 B CN103881035 B CN 103881035B
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Abstract
The invention relates to an antibacterial finishing agent for fabrics, which is prepared by the reaction of polymerizable polyurethane prepolymer, acrylic acid, an initiator, a silver-ammonia solution, a reducing agent and water. The finishing agent is a macromolecular emulsion which takes polyurethane as a main body and contains a proper amount of carboxyl in a molecular chain, and then the carboxyl reacts with silver ammonia solution under the action of a catalyst to obtain the antibacterial finishing agent containing silver ions on the surface of the molecular chain.
Description
Technical Field
The invention discloses a fabric antibacterial finishing agent, and belongs to the technical field of textile auxiliaries.
Technical Field
Currently, the antibacterial agents used for textiles are generally classified into three types, namely natural antibacterial agents, organic antibacterial agents and inorganic antibacterial agents.
The inorganic antibacterial agent is mainly a preparation in which metals or metal ions such as silver, copper, zinc and the like having antibacterial ability are supported on an inorganic carrier. Silver is a silver-based antimicrobial agent because silver has a sterilizing ability many times higher than that of copper and zinc. However, silver-loaded antimicrobial agents generally suffer from problems of uniform dispersion in the medium, long-term aging, and self-migration and sustained release of the antimicrobial component (silver ion) in the carrier. These problems are mainly caused by inherent properties such as adsorption property, specific surface area, and dispersibility in other host materials of the inorganic mineral carrier. The ionic antibacterial agent is mainly characterized in that metal ions with antibacterial action are loaded on a certain carrier, and the antibacterial action is achieved by slowly releasing the metal ions, but the ionic antibacterial agent has obvious defects, such as weak mildew-proof and antifungal effects, high cost, easy color change and the like.
Disclosure of Invention
In order to overcome the defects of the silver antibacterial agent, the invention provides an antibacterial finishing agent for fabric.
In order to achieve the purpose, the invention adopts the following technical scheme:
the fabric antibacterial finishing agent is characterized by being prepared by reacting 50-155 parts of polymerizable polyurethane prepolymer, 10-30 parts of acrylic acid, 1-3 parts of initiator, 15-40 parts of silver ammonia solution, 5-20 parts of reducing agent and 70-125 parts of water.
The structural formula of the polymerizable polyurethane prepolymer is shown as formula 1
In the formula 1, n = 9-22.
The reducing agent is any one or more of aldehydes, sugar containing aldehyde groups, fructose, organic salts with reducibility, hydrazine and alpha-naphthol.
The aldehyde is any one of the aldehydes shown in formula 2
In the formula 2, R is alkyl;
the saccharide containing aldehyde group is any one of glucose, maltose, rhamnose, fucose, arabinose, xylose, mannose, galactose and aldotriose; the organic salt with reducibility is any one of tartrate, trisodium citrate and sodium lactate.
The initiator is one or more of ammonium persulfate, potassium persulfate and sodium persulfate.
The preparation method of the fabric antibacterial finishing agent comprises the following steps:
(1) adding the polymerizable polyurethane prepolymer and a proper amount of water into a reaction kettle, and heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer;
(2) dripping acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, carrying out heat preservation reaction for 2h at the temperature of 80 ℃, and cooling to 40-60 ℃;
(3) slowly adding the silver-ammonia solution, uniformly stirring, then adding a reducing agent, reacting by using a silver mirror, and stirring and reacting for 1-2 hours at the water bath temperature of 40-60 ℃ to obtain the fabric antibacterial finishing agent;
the preparation method of the silver ammonia solution comprises the following steps: weighing appropriate amount of AgNO3The solution is put into a clean container, and dilute ammonia water is dripped into AgNO3The solution was shaken while dropping until the initially formed precipitate just dissolved.
The first two steps of the preparation method of the antibacterial finishing agent are emulsion polymerization reaction of polymerizable polyurethane prepolymer and acrylic acid. The polymerizable polyurethane prepolymer shown in the formula 1 contains double bonds, can perform free radical polymerization reaction, and has good surface activity and the function of stabilizing macromolecular emulsion particles in the polymerization reaction process.
In emulsion polymerization, a surfactant plays a very important role. Although the traditional small molecular surfactant has the most varieties and numbers, the traditional small molecular surfactant is easy to desorb and fall off under the influence of high shear force, centrifugal force and temperature because of a physical adsorption mechanism, and the traditional small molecular surfactant is easy to migrate to the surface after remaining in a product to influence the product performance. Compared with the small molecular surfactant, the relative molecular mass of the high molecular surfactant is usually more than that of the small molecular surfactant, the mobility is greatly reduced, and the polymerizable emulsifier can be bonded to the emulsion particles during emulsion polymerization to form a part of the polymer, so that desorption from the polymer particles or migration in an emulsion film is avoided, the adverse effect caused by the residue of the traditional surfactant in the polymer can be overcome, the stability of the latex can be improved, and the water resistance, the light resistance, the electric resistance, the heat resistance and the like of the polymer are improved.
The polyurethane has excellent physical and mechanical properties, temperature adaptability, organic solvent resistance and other properties, and is widely applied. The polymerizable polyurethane prepolymer and acrylic acid are used as main monomers, a polymer emulsion which takes polyurethane as a main body and contains a proper amount of carboxyl in a molecular chain is prepared through copolymerization, and then the carboxyl reacts with silver ammonia solution under the action of a catalyst to obtain the antibacterial finishing agent containing silver ions on the surface of the molecular chain.
Detailed description of the preferred embodiments
The invention is further illustrated by the following specific examples:
example 1:
a preparation method of a fabric antibacterial finishing agent comprises the following steps:
(1) adding 50 parts of polymerizable polyurethane prepolymer and 55 parts of water into a reaction kettle, heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer, and dissolving 1 part of initiator sodium persulfate by 15 parts of water for later use;
(2) dripping 10 parts of acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, reacting for 2h at the temperature of 80 ℃, and cooling to 40 ℃;
(3) slowly adding 15 parts of silver-ammonia solution, uniformly stirring, then adding 5 parts of reducing agent formaldehyde, reacting by using a silver mirror, and stirring and reacting at the water bath temperature of 40 ℃ for 1-2 hours to obtain the fabric antibacterial finishing agent;
example 2:
a preparation method of a fabric antibacterial finishing agent comprises the following steps:
(1) adding 75 parts of polymerizable polyurethane prepolymer and 70 parts of water into a reaction kettle, heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer and the water, and dissolving 1.5 parts of initiator ammonium persulfate by 15 parts of water for later use;
(2) dripping 15 parts of acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, carrying out heat preservation reaction for 2h at the temperature of 80 ℃, and cooling to 45 ℃;
(3) slowly adding 20 parts of silver-ammonia solution, uniformly stirring, then adding 8 parts of reducing agent glucose, reacting by using a silver mirror, and stirring and reacting at the water bath temperature of 45 ℃ for 1-2 hours to obtain the fabric antibacterial finishing agent;
example 3:
a preparation method of a fabric antibacterial finishing agent comprises the following steps:
(1) adding 100 parts of polymerizable polyurethane prepolymer and 85 parts of water into a reaction kettle, heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer, and dissolving 2 parts of initiator potassium persulfate by using 15 parts of water for later use;
(2) dropping 20 parts of acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, reacting for 2h at the temperature of 80 ℃, and cooling to 50 ℃;
(3) slowly adding 25 parts of silver-ammonia solution, uniformly stirring, adding 12 parts of trisodium citrate serving as a reducing agent, reacting by using a silver mirror, and stirring and reacting at the water bath temperature of 50 ℃ for 1-2 hours to obtain the fabric antibacterial finishing agent;
example 4:
a preparation method of a fabric antibacterial finishing agent comprises the following steps:
(1) adding 125 parts of polymerizable polyurethane prepolymer and 100 parts of water into a reaction kettle, heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer, and dissolving 1.5 parts of initiator potassium persulfate and 1 part of initiator sodium persulfate by 15 parts of water for later use;
(2) dripping 25 parts of acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, reacting for 2h at the temperature of 80 ℃, and cooling to 55 ℃;
(3) slowly adding 35 parts of silver-ammonia solution, uniformly stirring, then adding 16 parts of reducing agent hydrazine, reacting by using a silver mirror, and stirring and reacting for 1-2 hours at the water bath temperature of 55 ℃ to obtain the fabric antibacterial finishing agent;
example 5:
a preparation method of a fabric antibacterial finishing agent comprises the following steps:
(1) 155 parts of polymerizable polyurethane prepolymer and 110 parts of water are added into a reaction kettle, the mixture is heated to 60 ℃ to be completely dissolved, and 15 parts of water is used for dissolving 3 parts of initiator ammonium persulfate for later use;
(2) dropping 30 parts of acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, reacting for 2h at the temperature of 80 ℃, and cooling to 60 ℃;
(3) slowly adding 40 parts of silver-ammonia solution, uniformly stirring, then adding 20 parts of reducing agent alpha-naphthol, reacting by using a silver mirror, and stirring and reacting at the water bath temperature of 60 ℃ for 1-2 hours to obtain the fabric antibacterial finishing agent;
example 6:
a preparation method of a fabric antibacterial finishing agent comprises the following steps:
(1) adding 135 parts of polymerizable polyurethane prepolymer and 100 parts of water into a reaction kettle, heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer, and dissolving 1.3 parts of initiator potassium persulfate and 0.9 part of initiator ammonium persulfate by using 15 parts of water for later use;
(2) dripping 22 parts of acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, reacting for 2h at the temperature of 80 ℃, and cooling to 50 ℃;
(3) slowly adding 35 parts of silver ammonia solution, uniformly stirring, then adding 8 parts of reducing agent acetaldehyde and 10 parts of aldotriose, reacting by using a silver mirror, and stirring and reacting for 1-2 hours at the water bath temperature of 50 ℃ to obtain the fabric antibacterial finishing agent.
Claims (6)
1. The fabric antibacterial finishing agent is characterized by being prepared by reacting 50-155 parts of polymerizable polyurethane prepolymer, 10-30 parts of acrylic acid, 1-3 parts of initiator, 15-40 parts of silver ammonia solution, 5-20 parts of reducing agent and 70-125 parts of water, wherein the structural formula of the polymerizable polyurethane prepolymer is shown as formula 1
In formula 1, n is 9 to 22.
2. The antimicrobial finish for fabrics according to claim 1, wherein: the reducing agent is any one or more of aldehydes, sugar containing aldehyde groups, fructose, organic salts with reducibility, hydrazine and alpha-naphthol.
3. An antimicrobial finish for fabrics according to claim 2 wherein: the aldehyde is any one of the aldehydes shown in formula 2
In the formula 2, R is alkyl;
the saccharide containing aldehyde group is any one of glucose, maltose, rhamnose, fucose, arabinose, xylose, mannose, galactose and aldotriose; the organic salt with reducibility is any one of tartrate, trisodium citrate and sodium lactate.
4. The antimicrobial finish for fabrics according to claim 1, wherein: the initiator is one or more of ammonium persulfate, potassium persulfate and sodium persulfate.
5. A method of preparing an antimicrobial finish for a fabric according to claim 1, comprising the steps of:
(1) adding the polymerizable polyurethane prepolymer and a proper amount of water into a reaction kettle, and heating to 60 ℃ to completely dissolve the polymerizable polyurethane prepolymer;
(2) dripping acrylic acid and an initiator aqueous solution within 1-2 h at the temperature of 60-75 ℃, carrying out heat preservation reaction for 2h at the temperature of 80 ℃, and cooling to 40-60 ℃;
(3) slowly adding the silver-ammonia solution, uniformly stirring, then adding a reducing agent, reacting by using a silver mirror, and stirring and reacting for 1-2 hours at the water bath temperature of 40-60 ℃ to obtain the fabric antibacterial finishing agent.
6. The method of claim 5 for preparing an antimicrobial finish for a fabric, comprising: the preparation method of the silver ammonia solution comprises the following steps: weighing appropriate amount of AgNO3The solution is put into a clean container, and dilute ammonia water is dripped into AgNO3The solution was shaken while dropping until the initially formed precipitate just dissolved.
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| CN201310567946.1A CN103881035B (en) | 2013-11-08 | 2013-11-08 | Antibacterial finishing agent for fabric |
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| CN201310567946.1A CN103881035B (en) | 2013-11-08 | 2013-11-08 | Antibacterial finishing agent for fabric |
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| CN103881035B true CN103881035B (en) | 2021-09-07 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104264485B (en) * | 2014-09-18 | 2017-01-11 | 张伟 | Preparation method of medical bandage coated with polyurethane resin prepolymer |
| CN114685714B (en) * | 2020-12-29 | 2023-09-22 | 上海朗亿功能材料有限公司 | Modified polymer, antibacterial composition, preparation method, textile finishing and application |
| CN113389053A (en) * | 2021-08-11 | 2021-09-14 | 武自萌 | Production method of anti-mildew fabric |
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| CN1442572A (en) * | 2002-03-01 | 2003-09-17 | 日清纺织株式会社 | Fibre fabric having antibacterial property |
| CN1614136A (en) * | 2004-09-15 | 2005-05-11 | 姚华珍 | Microbe-proof cloth and production thereof |
| CN1720132A (en) * | 2002-11-29 | 2006-01-11 | 美利肯公司 | Fabrics having a topically applied silver-based finish with a cross-linked binder system for improved wash durability |
| CN102182069A (en) * | 2010-12-30 | 2011-09-14 | 洪桂焕 | Silver-carried antibacterial finishing agent and preparation method thereof |
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| JPH09309930A (en) * | 1996-05-21 | 1997-12-02 | Kyoeisha Chem Co Ltd | Aqueous acrylic resin for glass fiber sizing |
| CN101759841B (en) * | 2010-01-08 | 2016-03-02 | 合肥聚合辐化技术有限公司 | Core-shell type aqueous polyurethane-acrylic ester emulsion original position radiation polymerization method |
| CN101781851B (en) * | 2010-02-05 | 2011-12-28 | 绍兴县荣利达纺织科技有限公司 | Polyurethane antibiotic soft coating agent and method for preparing same |
| CN102165960B (en) * | 2010-11-29 | 2013-07-03 | 南开大学 | Preparation method of nano silver antibacterial mother liquor through two-step polymerization |
| CN102050929B (en) * | 2010-12-08 | 2012-07-25 | 江苏日出化工有限公司 | Elastic emulsion prepared from water-soluble polyurethane and acrylic acid by hybrid polymerization |
| CN102121195A (en) * | 2010-12-30 | 2011-07-13 | 洪桂焕 | Antibacterial finishing agent and preparation method thereof |
| CN102162194A (en) * | 2010-12-30 | 2011-08-24 | 洪桂焕 | Textile finishing agent and preparation method thereof |
| CN103315001A (en) * | 2013-05-23 | 2013-09-25 | 厦门大学 | Antibacterial composite material with silver loaded on polymer nanosphere surfaces and preparation method for antibacterial composite material |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010036912A1 (en) * | 1998-10-22 | 2001-11-01 | Shulman Jan Edward | Method of promoting soil release from fabrics |
| CN1442572A (en) * | 2002-03-01 | 2003-09-17 | 日清纺织株式会社 | Fibre fabric having antibacterial property |
| CN1720132A (en) * | 2002-11-29 | 2006-01-11 | 美利肯公司 | Fabrics having a topically applied silver-based finish with a cross-linked binder system for improved wash durability |
| CN1614136A (en) * | 2004-09-15 | 2005-05-11 | 姚华珍 | Microbe-proof cloth and production thereof |
| CN102182069A (en) * | 2010-12-30 | 2011-09-14 | 洪桂焕 | Silver-carried antibacterial finishing agent and preparation method thereof |
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Addressee: SHAOXING DINGXIANG TEXTILE TRADING CO., LTD. Document name: Notification of Patent Invention Entering into Substantive Examination Stage |
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Effective date of registration: 20180411 Address after: 312030 Zhejiang Province, Shaoxing city Keqiao District Ye Xi Lu Mei Yuan District 19 Building 501 room Applicant after: Gu Xiangjun Address before: Shaoxing City, Zhejiang province 312000 Ring Road No. 508 Applicant before: SHAOXING DINGXIANG TEXTILE TRADING CO., LTD. |
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Effective date of registration: 20210819 Address after: Room 703, 245 Jiachuan Road, Xuhui District, Shanghai 200237 Applicant after: SHANGHAI HIGOAL NEW MATERIAL SCIENCE & TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: 312030 Room 501, building 19, Meiyuan community, Yexi Road, Keqiao District, Shaoxing City, Zhejiang Province Applicant before: Gu Xiangjun |
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