CN103741469A - Antibiotic finishing agent - Google Patents
Antibiotic finishing agent Download PDFInfo
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- CN103741469A CN103741469A CN201310567657.1A CN201310567657A CN103741469A CN 103741469 A CN103741469 A CN 103741469A CN 201310567657 A CN201310567657 A CN 201310567657A CN 103741469 A CN103741469 A CN 103741469A
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Abstract
The invention relates to an antibiotic finishing agent mainly used in textile coatings. A self-crosslinked organosilicon modified polymer is prepared through an emulsion polymerization method with an acrylate monomer, styrene, an organosilicon cross-linking agent and an alkenyl amine monomer as polymerization monomers and polymerizable maleic anhydride fatty alcohol polyoxyethylene ether monoester as an emulsifier, and a silver salt is added to an emulsion for a complexation reaction in order to prepare the textile finishing agent having antibiotic and antistatic functions. The finishing agent has the characteristics of good water resistance, good low temperature resistance and the like, has the durable antibiotic and antistatic functions, and can be used for the functional finishing of the textile surfaces.
Description
Technical field
The present invention relates to a kind of antibacterial finishing agent, is textiles chemical field.
Background technology
The antiseptic that textiles is used at present is generally divided into natural antibacterial agent, organic antibacterial agent and inorganic antiseptic three classes.
Inorganic antiseptic mainly refers to that metal or metal ion load that silver etc. itself is had to an antibacterial ability are scattered in making on inorganic matter carrier.Commercial inorganic antiseptic is silver-series antibacterial agent mostly at present, dispersed, the permanent timeliness of carrying silver antimicrobials in medium, in carrier from existing problems aspect animal migration and slow release.These problems are mainly because the inherent characteristics such as the absorption property of inorganic mineral carrier, specific area cause.Inorganic antibacterial preparation has outstanding durability, high security, heat resistance, broad spectrum activity, the feature such as long-lasting, is main development direction from now on.
Summary of the invention
The object of the invention is to:
(1) provide a kind of antibacterial finishing agent;
(2) provide a kind of preparation method of antibacterial finishing agent.
The present invention is take acrylate, styrene, organosilicon cross-linking agent, thiazolinyl amine monomer as polymerization single polymerization monomer, take polymerizable anhydride aliphatic alcohol polyoxyethylene ether monoesters as emulsifying agent, adopt emulsion polymerisation process to prepare self-cross linking type silicone modified polymers, then make to adding silver salt to carry out complex reaction in emulsion.Because silver ion is evenly fixed on strand by complex reaction with amino, thereby can overcome that general inorganic silver antiseptic easily moves, the defect such as not durable.In addition, be positioned at polymer micelle superficial layer and there is abundant organosilicon crosslinked functional group, crosslinked film forming in solidification process, the fastness of increase polyacrylate polymers film.Thereby the finishing agent making has good resistance to water and the feature such as low temperature resistant
For achieving the above object, product of the present invention completes by following two steps:
Unless stated otherwise, unit below is parts by mass.
The first step: polymer emulsion synthetic
Described polymer emulsion is by least comprising that acrylate, styrene, thiazolinyl amine monomer, organosilicon cross-linking agent, emulsifying agent, initator, deionized water make through emulsion polymerisation process.
In above-mentioned each component, 20～60 parts of acrylic ester monomers, 10～18 parts of styrene, 2～9 parts of organosilicon cross-linking agents, 3～7 parts of thiazolinyl amine monomers, 4～22 parts of emulsifying agents, 0.2～0.6 part of initator, 400～900 parts of deionized waters.
Described acrylic ester monomer comprises one or more the combination in acrylic acid, methacrylic acid, methyl methacrylate, hydroxy methyl methacrylate, hydroxyethyl methylacrylate, hydroxy propyl methacrylate, methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxy butyl ester, the own ester of acrylic acid hydroxyl, 2-EHA.
Described organosilicon cross-linking agent is vinyltriethoxysilane [CH
2=CHSi (OC
2h
5)
3], vinyl three (2-methoxy ethoxy) silane [CH
2=CHSi (OC
2h
4oCH
3)
3], methyl allyl acyloxypropyl trimethoxysilane [CH
2=C (CH
3) COOC
3h
6si (OCH
3)
3] in one or more.
Described thiazolinyl amine monomer comprises one or more the combination in alkenyl amine, diallylamine, triallylamine.
Described initator comprises one or more combinations in sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate, azodiisobutyronitrile, benzoyl peroxide.
Described emulsifying agent is one or more in maleic anhydride nine alcohol polyoxyethylene ether monoesters, maleic anhydride ten alcohol polyoxyethylene ether monoesters, maleic anhydride undecyl alcohol polyoxyethylene ether monoesters, maleic anhydride Dodecyl Polyoxyethylene Ether monoesters.This emulsifying agent is that maleic anhydride and fatty alcohol-polyoxyethylene ether are carried out single-esterification and made, because of contain can with two key groups of other monomer polymerizations, can be aggregated on macromolecular chain, therefore in emulsion, substantially do not contain small-molecular emulsifier, prepared latex particle surface ratio is " cleaning ", and the performance of polymer coating film obtains very large improvement.
The concrete steps of preparing polymer emulsion are as follows:
A, in reactor, add 4～22 parts of emulsifying agents and 300～400 parts of water, heat up, stir, treat emulsifiers dissolve, be cooled to below 50 ℃;
B, add 10～20 parts of acrylic ester monomers, 6～8 parts of styrene, 6～14 parts, acrylic acid, emulsification 30min, adds 0.1～0.3 part of initator, 10～30 parts of water-soluble solutions for initator, be warming up to 60～68 ℃ of initiation reactions, along with the carrying out of polymerisation, reaction temperature rises to 70～85 ℃ gradually, reaction time is 1～3h, and emulsion presents light blue;
After c, question response temperature in the kettle fall after rise, emulsion temperature is adjusted into 70 ℃, and is incubated 0.5h;
D, then at 70～75 ℃ of temperature, drip 10～50 parts of acrylic ester monomers, 4～10 parts of styrene, 2～9 parts of organosilicon cross-linking agents, 3～7 parts of thiazolinyl amine monomers, and 0.1～0.3 part of initator, 20～60 parts of water-soluble solutions for initator, time for adding is 1～1.5h, drips follow-up continuation of insurance temperature 1h, is cooled to below 50 ℃, by ammoniacal liquor adjusting pH value to 7, obtain silicon-containing polymer emulsion.
Second step: the complexing of silver salt
Under pH neutral, on the nitrogen-atoms in amido contained lone pair electrons can with Ag
+ion forms stable complex compound, makes Ag
+be fixed on copolymer molecule chain.
In synthetic the containing in amine copolymer thing emulsion of the first step, add 8～14 parts of silver nitrates, at 16～25 ℃, stir 1～3 hour, make amido and Ag
+fully complexing, makes and has textile finish antibacterial, antistatic property.
This finishing agent has good filming performance, silver ion is anchored on polymer by coordinate bond, avoided moving during use and weakened its antibacterial, antistatic property, thereby strengthened its endurance quality, in addition, this finishing agent adopts emulsifier-free emulsion polymerization method, makes emulsifying agent and other monomer copolymerizations and is connected on polymer molecular chain, has avoided the harmful effect of emulsifying agent to emulsion property.
Specific implementation method:
Following embodiment, only illustrates, and is not only, so all within the scope of the present invention or make within the change similar to the present invention be all contained in the present invention.
Unless stated otherwise, unit below is parts by mass.
The concrete steps of textile finish of the present invention are:
Embodiment 1
(a) by following monomer
6 parts of butyl acrylates
8 parts of methyl methacrylates
4 parts of ethyl acrylates
Be placed in 500ml reactor, stir, form polymer monomer mixed liquor A.
(b) by following component
6 parts of emulsifying agents, 360 parts of deionized waters are placed in 500ml glass, in 50 ℃ of stirring and dissolving 40min, form stable emulsifier aqueous solution B.By 0.35 part of ammonium persulfate formation solution for standby of 55 parts of deionized water dissolvings.
(c) under agitation, polymer monomer mixed liquor A is joined in emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) to being equipped with in the 1000ml four-hole boiling flask of thermometer, agitator, add above-mentioned emulsion C.Under agitation, temperature in bottle is risen to 60 ℃, add the ammonium persulfate solution of 1/3 weight with dropping funel, initiated polymerization, after temperature falls after rise in bottle, is adjusted into 70 ℃ by emulsion temperature, and is incubated 0.5h.Then at the same temperature, with 1h, drip the ammonium persulfate solution of 12 parts of butyl acrylates, 6 parts, 4 parts vinyltriethoxysilane of styrene, 3 parts of alkenyl amines, 4 parts of diallylamines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, by ammoniacal liquor adjustment pH value to 7, obtains containing amine copolymer thing emulsion.
(e) in (d) solution preparing, add 8 parts of silver nitrates, at 18 ℃, stir 2 hours, make amido and Ag
+fully complexing, makes silver-carrying antibiotic finishing agent.
Embodiment 2
(a) by following monomer
8 parts of butyl acrylates
10 parts of methyl methacrylates
3 parts of ethyl acrylates
Be placed in 500ml reactor, stir, form polymer monomer mixed liquor A.
(b) by following component
9 parts of emulsifying agents, 360 parts of deionized waters are placed in 500ml glass, in 50 ℃ of stirring and dissolving 40min, form stable emulsifier aqueous solution B.By 0.4 part of ammonium persulfate formation solution for standby of 55 parts of deionized water dissolvings.
(c) under agitation, polymer monomer mixed liquor A is joined in emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) to being equipped with in the 1000ml four-hole boiling flask of thermometer, agitator, add above-mentioned emulsion C.Under agitation, temperature in bottle is risen to 60 ℃, add the ammonium persulfate solution of 1/3 weight with dropping funel, initiated polymerization, after temperature falls after rise in bottle, is adjusted into 70 ℃ by emulsion temperature, and is incubated 0.5h.Then at the same temperature, with 1h, drip the ammonium persulfate solution of 20 parts of butyl acrylates, 8 parts, 6 parts vinyltriethoxysilane of styrene, 3 parts of alkenyl amines, 3 parts of diallylamines and 2/3 weight.After dripping, continue insulation 1.5h.Polymerized emulsion is cooled to below 50 ℃, by ammoniacal liquor adjustment pH value to 7, obtains containing amine copolymer thing emulsion.
(e) in (d) solution preparing, add 10 parts of silver nitrates, at 20 ℃, stir 2 hours, make amido and Ag
+fully complexing, makes silver-carrying antibiotic finishing agent.
Embodiment 3
(a) by following monomer
10 parts of butyl acrylates
10 parts of methyl methacrylates
8 parts of ethyl acrylates
Be placed in 500ml reactor, stir, form polymer monomer mixed liquor A.
(b) by following component
12 parts of emulsifying agents, 360 parts of deionized waters are placed in 500ml glass, in 50 ℃ of stirring and dissolving 40min, form stable emulsifier aqueous solution B.By 0.45 part of ammonium persulfate formation solution for standby of 55 parts of deionized water dissolvings.
(c) under agitation, polymer monomer mixed liquor A is joined in emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) to being equipped with in the 1000ml four-hole boiling flask of thermometer, agitator, add above-mentioned emulsion C.Under agitation, temperature in bottle is risen to 60 ℃, add the ammonium persulfate solution of 1/3 weight with dropping funel, initiated polymerization, after temperature falls after rise in bottle, is adjusted into 70 ℃ by emulsion temperature, and is incubated 0.5h.Then at the same temperature, with 1h, drip the ammonium persulfate solution of 30 parts of butyl acrylates, 8 parts, 8 parts vinyltriethoxysilane of styrene, 2 parts of alkenyl amines, 5 parts of diallylamines and 2/3 weight.After dripping, continue insulation 2h.Polymerized emulsion is cooled to below 50 ℃, by ammoniacal liquor adjustment pH value to 7, obtains containing amine copolymer thing emulsion.
(e) in (d) solution preparing, add 12 parts of silver nitrates, at 18 ℃, stir 2 hours, make amido and Ag
+fully complexing, makes silver-carrying antibiotic finishing agent.
Embodiment 4
(a) by following monomer
6 parts of butyl acrylates
12 parts of methyl methacrylates
6 parts of ethyl acrylates
Be placed in 500ml reactor, stir, form polymer monomer mixed liquor A.
(b) by following component
16 parts of emulsifying agents, 360 parts of deionized waters are placed in 500ml glass, in 50 ℃ of stirring and dissolving 40min, form stable emulsifier aqueous solution B.By 0.3 part of ammonium persulfate formation solution for standby of 55 parts of deionized water dissolvings.
(c) under agitation, polymer monomer mixed liquor A is joined in emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) to being equipped with in the 1000ml four-hole boiling flask of thermometer, agitator, add above-mentioned emulsion C.Under agitation, temperature in bottle is risen to 60 ℃, add the ammonium persulfate solution of 1/3 weight with dropping funel, initiated polymerization, after temperature falls after rise in bottle, is adjusted into 70 ℃ by emulsion temperature, and is incubated 0.5h.Then at the same temperature, with 1h, drip the ammonium persulfate solution of 40 parts of butyl acrylates, 8 parts, 3 parts vinyltriethoxysilane of styrene, 2 parts of alkenyl amines, 3 parts of diallylamines and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, by ammoniacal liquor adjustment pH value to 7, obtains containing amine copolymer thing emulsion.
(e) in (d) solution preparing, add 13 parts of silver nitrates, at 18 ℃, stir 2 hours, make the abundant complexing of amido and Ag+, make silver-carrying antibiotic finishing agent.
Embodiment 5
(a) by following monomer
6 parts of butyl acrylates
10 parts of methyl methacrylates
14 parts of ethyl acrylates
Be placed in 500ml reactor, stir, form polymer monomer mixed liquor A.
(b) by following component
20 parts of emulsifying agents, 360 parts of deionized waters are placed in 500ml glass, in 50 ℃ of stirring and dissolving 40min, form stable emulsifier aqueous solution B.By 0.25 part of ammonium persulfate formation solution for standby of 55 parts of deionized water dissolvings.
(c) under agitation, polymer monomer mixed liquor A is joined in emulsifier aqueous solution B, form the emulsion C of polymer monomer.
(d) to being equipped with in the 1000ml four-hole boiling flask of thermometer, agitator, add above-mentioned emulsion C.Under agitation, temperature in bottle is risen to 60 ℃, add the ammonium persulfate solution of 1/3 weight with dropping funel, initiated polymerization, after temperature falls after rise in bottle, is adjusted into 70 ℃ by emulsion temperature, and is incubated 0.5h.Then at the same temperature, with 1h, drip the ammonium persulfate solution of 50 parts of butyl acrylates, 10 parts, 5 parts vinyltriethoxysilane of styrene, 4 parts of alkenyl amines, 1 part of diallylamine and 2/3 weight.After dripping, continue insulation 1h.Polymerized emulsion is cooled to below 50 ℃, by ammoniacal liquor adjustment pH value to 7, obtains containing amine copolymer thing emulsion.
(e) in (d) solution preparing, add 14 parts of silver nitrates, at 18 ℃, stir 2 hours, make amido and Ag
+fully complexing, makes silver-carrying antibiotic finishing agent.
Claims (8)
1. an antibacterial finishing agent, is characterized in that: this finishing agent is mainly made through complex reaction by polymer emulsion and silver salt; Described polymer emulsion is formed through emulsion polymerisation by acrylic ester monomer, styrene, organosilicon cross-linking agent, thiazolinyl amine monomer, emulsifying agent, initator and water, and described silver salt is silver nitrate.
2. a kind of antibacterial finishing agent according to claim 1, is characterized in that: described emulsifying agent is one or more in maleic anhydride nine alcohol polyoxyethylene ether monoesters, maleic anhydride ten alcohol polyoxyethylene ether monoesters, maleic anhydride undecyl alcohol polyoxyethylene ether monoesters, maleic anhydride Dodecyl Polyoxyethylene Ether monoesters.
3. a kind of antibacterial finishing agent according to claim 1, is characterized in that: described initator comprises one or more combinations in sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate, azodiisobutyronitrile, benzoyl peroxide.
4. a kind of antibacterial finishing agent according to claim 1, is characterized in that: thiazolinyl amine monomer comprises one or more the combination in alkenyl amine, diallylamine, triallylamine.
5. a kind of antibacterial finishing agent according to claim 1, is characterized in that: described acrylic ester monomer is selected from Isooctyl acrylate monomer, butyl acrylate, ethyl acrylate one or more in methyl methacrylate, methyl acrylate.
6. a kind of antibacterial finishing agent according to claim 1, is characterized in that: described organosilicon cross-linking agent is vinyltriethoxysilane [CH
2=CHSi (OC
2h
5)
3], vinyl three (2-methoxy ethoxy) silane [CH
2=CHSi (OC
2h
4oCH
3)
3], methyl allyl acyloxypropyl trimethoxysilane [CH
2=C (CH
3) COOC
3h
6si (OCH
3)
3] in one or more.
7. a kind of antibacterial finishing agent according to claim 1, it is characterized in that: 20～60 parts of acrylic ester monomers, 10～18 parts of styrene, 2～9 parts of organosilicon cross-linking agents, 3～7 parts of thiazolinyl amine monomers, 4～22 parts of emulsifying agents, water is deionized water, 400～900 parts, and 0.2～0.6 part of initator, the consumption of silver nitrate is 8～14 parts by part, and unit is parts by mass.
8. a preparation method for antibacterial finishing agent, is characterized in that, preparation process is:
A, in reactor, add 4～22 parts of emulsifying agents and 300～400 parts of water, be warming up to 50 ℃ of left and right, stir, treat emulsifiers dissolve;
B, add 20～100 parts of polymer monomers, emulsification 40min, adds 0.1～0.3 part of initator, is warming up to 60～75 ℃ of initiation reactions, and the reaction time is 1～2h;
After c, question response temperature in the kettle fall after rise, emulsion temperature is adjusted into 70～82 ℃, and is incubated 0.5h;
D, then at 70～85 ℃ of temperature, drip 20～150 parts of polymer monomers, and 0.1～0.5 part of initator, time for adding is 1～1.5h, drip follow-up continuation of insurance temperature 2～6h, be cooled to below 40 ℃, with filtering, obtain organic-silicon-modified fluorinated acrylate polymer emulsion.
E, in (d) solution preparing, add 8～14 parts of silver nitrates, at 16～25 ℃, stir 1～3 hour, make amido and Ag
+fully complexing, makes silver-carrying antibiotic finishing agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310567657.1A CN103741469A (en) | 2013-11-08 | 2013-11-08 | Antibiotic finishing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310567657.1A CN103741469A (en) | 2013-11-08 | 2013-11-08 | Antibiotic finishing agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103741469A true CN103741469A (en) | 2014-04-23 |
Family
ID=50498529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310567657.1A Pending CN103741469A (en) | 2013-11-08 | 2013-11-08 | Antibiotic finishing agent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104328657A (en) * | 2014-10-20 | 2015-02-04 | 苏州庄爵服饰有限公司 | Antibacterial finishing method used for clothes |
| CN104328656A (en) * | 2014-10-20 | 2015-02-04 | 苏州庄爵服饰有限公司 | Antibacterial finishing method used for clothes |
| CN106120337A (en) * | 2016-07-01 | 2016-11-16 | 潘明华 | A kind of environment-friendly type stiffening agent and preparation method thereof |
| CN107164961A (en) * | 2017-06-23 | 2017-09-15 | 华娜 | A kind of antibacterial finishing agent used for textiles and its production and use |
| CN114525680A (en) * | 2022-03-29 | 2022-05-24 | 清远市宏图助剂有限公司 | Multifunctional refining agent |
| CN114634590A (en) * | 2022-03-28 | 2022-06-17 | 太原工业学院 | Synthetic method of organic-inorganic composite material |
| CN116217787A (en) * | 2023-03-01 | 2023-06-06 | 安徽博瑞克科技有限公司 | Silver ion polymer for mildew prevention and sterilization and preparation method thereof |
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| CN101544718A (en) * | 2009-05-06 | 2009-09-30 | 河北科技大学 | Method for preparing antibacterial composite material with nano silver particles evenly dispersed in polymeric matrix |
| CN101768866A (en) * | 2010-02-05 | 2010-07-07 | 洪桂焕 | High-molecular microsphere silver-carrying antibacterial finishing agent and preparation method thereof |
| CN102121195A (en) * | 2010-12-30 | 2011-07-13 | 洪桂焕 | Antibacterial finishing agent and preparation method 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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| CN1461755A (en) * | 2002-05-31 | 2003-12-17 | 中国科学院化学研究所 | Preparation method of polymer/inorganic nanometer ontibacterial composition aqueous microemulsion |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104328657A (en) * | 2014-10-20 | 2015-02-04 | 苏州庄爵服饰有限公司 | Antibacterial finishing method used for clothes |
| CN104328656A (en) * | 2014-10-20 | 2015-02-04 | 苏州庄爵服饰有限公司 | Antibacterial finishing method used for clothes |
| CN104328657B (en) * | 2014-10-20 | 2016-08-31 | 苏州庄爵服饰有限公司 | Antibiotic finishing method for clothes |
| CN106120337A (en) * | 2016-07-01 | 2016-11-16 | 潘明华 | A kind of environment-friendly type stiffening agent and preparation method thereof |
| CN107164961A (en) * | 2017-06-23 | 2017-09-15 | 华娜 | A kind of antibacterial finishing agent used for textiles and its production and use |
| CN114634590A (en) * | 2022-03-28 | 2022-06-17 | 太原工业学院 | Synthetic method of organic-inorganic composite material |
| CN114525680A (en) * | 2022-03-29 | 2022-05-24 | 清远市宏图助剂有限公司 | Multifunctional refining agent |
| CN116217787A (en) * | 2023-03-01 | 2023-06-06 | 安徽博瑞克科技有限公司 | Silver ion polymer for mildew prevention and sterilization 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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