CN104650290B - Use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method and preparation method thereof - Google Patents
Use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method and preparation method thereof Download PDFInfo
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- CN104650290B CN104650290B CN201510058729.9A CN201510058729A CN104650290B CN 104650290 B CN104650290 B CN 104650290B CN 201510058729 A CN201510058729 A CN 201510058729A CN 104650290 B CN104650290 B CN 104650290B
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- 239000002649 leather substitute Substances 0.000 title claims abstract description 36
- 239000004599 antimicrobial Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229920000642 polymer Polymers 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004220 aggregation Methods 0.000 title claims abstract description 10
- 230000002776 aggregation Effects 0.000 title claims abstract description 10
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 19
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 19
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000002421 anti-septic effect Effects 0.000 claims abstract description 14
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940043237 diethanolamine Drugs 0.000 claims abstract description 7
- -1 diallyldimethylammonium chlorides Chemical class 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 235000013904 zinc acetate Nutrition 0.000 claims description 7
- 125000005395 methacrylic acid group Chemical class 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 19
- 239000000835 fiber Substances 0.000 abstract description 11
- 230000000845 anti-microbial effect Effects 0.000 abstract description 4
- 241000588724 Escherichia coli Species 0.000 abstract description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 3
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000004246 zinc acetate Substances 0.000 abstract description 2
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 abstract 2
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 46
- 239000011787 zinc oxide Substances 0.000 description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- CWNOEVURTVLUNV-UHFFFAOYSA-N 2-(propoxymethyl)oxirane Chemical compound CCCOCC1CO1 CWNOEVURTVLUNV-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000007901 in situ hybridization Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Treatment And Processing Of Natural Fur Or Leather (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method and preparation method thereof.It is rarely reported at present with the research of antiseptic about synthetic leather base cloth.Zinc acetate and ethanol are mixed in water-bath of the present invention, diethanol amine is added and Nano-ZnO Sol is made in diallyldimethylammonium chloride；Allyl glycidyl ether, methacrylic acid and Nano-ZnO Sol are well mixed Nano-ZnO Sol mixed liquor is made；Diallyldimethylammonium chloride, ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming are mixed in water-bath, ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor is added dropwise, stirring reaction, insulation cooling produces superfine fiber synthetic leather base cloth antiseptic.N in the complex antimicrobials of the present invention+It can be good at improving the anti-microbial property of synthetic leather base cloth with the synergy of nano zine oxide, applied in superfine fiber synthetic leather base cloth, to the antibiotic rate of Escherichia coli and staphylococcus aureus up to more than 99%.
Description
Technical field
The present invention relates to a kind of preparation method of use for synthetic leather antiseptic, and in particular to a kind of conjunction based on situ aggregation method
Finished leather polymer nanocomposite ZnO complex antimicrobials and preparation method thereof.
Background technology
Synthetic leather is widely used in making footwear, boots, case and bag and ball etc., but it contains nutrition necessary to bacterium, mould
Material, under the conditions of suitable temperature and humidity, bacterium and mould will on synthetic leather amount reproduction, cause microbial resistance
It can decline.Properties influence of the base fabric on synthetic leather is most important.Therefore, excellent long-acting synthetic leather base cloth antibacterial is studied
Material has great importance.
With going deep into that development in science and technology is studied, the research of nanometer technology and its antibacterial research in synthetic leather also result in
The concern of people.Fan Hao armies et al.（Chen Yi, Feng Ping, Fan Haojun, wait nano-TiOs2In-situ hybridization polyurethane and its antibacterial and mouldproof
Performance study [J] leather sciences and engineering, 2008,3（18）：11-15.）Do not changing the existing wet method life of Synthetic Leather
On the premise of production. art and production equipment, by hybrid inorganic-organic technology in situ by nanoscale TiO2Use for synthetic leather is introduced to gather
In urethane film.It is demonstrated experimentally that through nano-TiO2Polyurethane film after in-situ modified not only has excellent antibacterial and mouldproof
Can, its tensile strength and elongation percentage are also improved simultaneously.But the research about synthetic leather base cloth antiseptic is also rarely seen
Report.
The content of the invention
It is an object of the invention to provide a kind of use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method
And preparation method thereof, utilize N+The antibacterial of superfine fiber synthetic leather base cloth antiseptic is improved with the synergy of nano zine oxide
Performance.
The technical solution adopted in the present invention is：
The preparation method of use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method, it is characterised in that：
Realized by following steps：
Step one：Prepare Nano-ZnO Sol：
By warming-in-water to 60 DEG C, 0.658-1.317g zinc acetates and 100ml ethanol are added in 150ml there-necked flasks,
Rotating speed is adjusted to 400rpm, stirs 10min；
12.615g diethanol amine is added, 10min is stirred；
2.425g diallyldimethylammonium chlorides are added, 10min is stirred, 2h is incubated, is cooled to room temperature, nanometer is made
ZnO colloidal sols；
Step 2：Prepare complex antimicrobials：
2.4g ammonium persulfates are added in 38.4g water ammonium persulfate aqueous solution is made；
0.675g sodium hydrogensulfites are added in 10g water aqueous solution of sodium bisulfite is made；
Nano-ZnO Sol made from 1.8g allyl glycidyl ethers, 2.46g methacrylic acids and step one is mixed equal
It is even that Nano-ZnO Sol mixed liquor is made；
Water-bath is warming up to 80 DEG C, 97g diallyldimethylammonium chlorides, 1/3 over cure are added in there-necked flask
Sour aqueous ammonium and aqueous solution of sodium bisulfite bottoming, the ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor of dropwise addition 2/3,
Rotating speed 350rpm, starts after stirring, 45min, completion of dropping, is incubated 4h, is cooled to room temperature, stops stirring, produces superfine fibre
Synthetic leather base cloth antiseptic.
The preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method is made as mentioned
Antiseptic.
The present invention has advantages below：
The present invention prepares nano-ZnO using sol-gal process, with dimethyl diallyl ammonium chloride, methacrylic acid, alkene
Propyl glycidyl ether, zinc acetate are raw material, polymer matrix/nano-ZnO composite material antiseptic are prepared by in-situ method, by it
Applied in superfine fiber synthetic leather base cloth.N in the composite+It can be good at improving with the synergy of nano zine oxide
The anti-microbial property of synthetic leather base cloth.The synthetic leather antiseptic according to said method prepared is applied in superfine fiber synthetic leather base cloth, right
The antibiotic rate of Escherichia coli and staphylococcus aureus is up to more than 99%.
Embodiment
With reference to embodiment, the present invention will be described in detail.
The preparation side of use for synthetic leather polymer nanocomposite ZnO complex antimicrobials of the present invention based on situ aggregation method
Method, nano-ZnO is prepared using sol-gal process, and then by in-situ method by itself and dimethyl diallyl ammonium chloride, pi-allyl
Glycidol ether, methacrylic acid prepare polymer matrix/nano-zinc oxide composite material, and plan utilizes N+With the association of nano zine oxide
Same-action improves the anti-microbial property of synthetic leather base cloth.Specifically include following steps：
Step one：Prepare Nano-ZnO Sol：
By warming-in-water to 60 DEG C, 0.658-1.317g zinc acetates and 100ml ethanol are added in 150ml there-necked flasks,
Rotating speed is adjusted to 400rpm, stirs 10min；
12.615g diethanol amine is added, 10min is stirred；
2.425g diallyldimethylammonium chlorides are added, 10min is stirred, 2h is incubated, is cooled to room temperature, nanometer is made
ZnO colloidal sols；
Step 2：Prepare complex antimicrobials：
2.4g ammonium persulfates are added in 38.4g water ammonium persulfate aqueous solution is made；
0.675g sodium hydrogensulfites are added in 10g water aqueous solution of sodium bisulfite is made；
Nano-ZnO Sol made from 1.8g allyl glycidyl ethers, 2.46g methacrylic acids and step one is mixed equal
It is even that Nano-ZnO Sol mixed liquor is made；
Water-bath is warming up to 80 DEG C, 97g diallyldimethylammonium chlorides, 1/3 over cure are added in there-necked flask
Sour aqueous ammonium and aqueous solution of sodium bisulfite bottoming, the ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor of dropwise addition 2/3,
Rotating speed 350rpm, starts after stirring, 45min, completion of dropping, is incubated 4h, is cooled to room temperature, stops stirring, produces superfine fibre
Synthetic leather base cloth antiseptic.
Embodiment 1：
Step one：Prepare Nano-ZnO Sol：
By warming-in-water to 60 DEG C, 0.658g zinc acetates and 100ml ethanol are added in 150ml there-necked flasks, rotating speed is adjusted
To 400rpm, 10min is stirred；
12.615g diethanol amine is added, 10min is stirred；
2.425g diallyldimethylammonium chlorides are added, 10min is stirred, 2h is incubated, is cooled to room temperature, nanometer is made
ZnO colloidal sols；
Step 2：Prepare complex antimicrobials：
2.4g ammonium persulfates are added in 38.4g water ammonium persulfate aqueous solution is made；
0.675g sodium hydrogensulfites are added in 10g water aqueous solution of sodium bisulfite is made；
Nano-ZnO Sol made from 1.8g allyl glycidyl ethers, 2.46g methacrylic acids and step one is mixed equal
It is even that Nano-ZnO Sol mixed liquor is made；
Water-bath is warming up to 80 DEG C, 97g diallyldimethylammonium chlorides, 1/3 over cure are added in there-necked flask
Sour aqueous ammonium and aqueous solution of sodium bisulfite bottoming, the ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor of dropwise addition 2/3,
Rotating speed 350rpm, starts after stirring, 45min, completion of dropping, is incubated 4h, is cooled to room temperature, stops stirring, produces superfine fibre
Synthetic leather base cloth antiseptic.
Embodiment 2：
Step one：Prepare Nano-ZnO Sol：
By warming-in-water to 60 DEG C, 0.988g zinc acetates and 100ml ethanol are added in 150ml there-necked flasks, rotating speed is adjusted
To 400rpm, 10min is stirred；
12.615g diethanol amine is added, 10min is stirred；
2.425g diallyldimethylammonium chlorides are added, 10min is stirred, 2h is incubated, is cooled to room temperature, nanometer is made
ZnO colloidal sols；
Step 2：Prepare complex antimicrobials：
2.4g ammonium persulfates are added in 38.4g water ammonium persulfate aqueous solution is made；
0.675g sodium hydrogensulfites are added in 10g water aqueous solution of sodium bisulfite is made；
Nano-ZnO Sol made from 1.8g allyl glycidyl ethers, 2.46g methacrylic acids and step one is mixed equal
It is even that Nano-ZnO Sol mixed liquor is made；
Water-bath is warming up to 80 DEG C, 97g diallyldimethylammonium chlorides, 1/3 over cure are added in there-necked flask
Sour aqueous ammonium and aqueous solution of sodium bisulfite bottoming, the ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor of dropwise addition 2/3,
Rotating speed 350rpm, starts after stirring, 45min, completion of dropping, is incubated 4h, is cooled to room temperature, stops stirring, produces superfine fibre
Synthetic leather base cloth antiseptic.
Embodiment 3：
Step one：Prepare Nano-ZnO Sol：
By warming-in-water to 60 DEG C, 1.317g zinc acetates and 100ml ethanol are added in 150ml there-necked flasks, rotating speed is adjusted
To 400rpm, 10min is stirred；
12.615g diethanol amine is added, 10min is stirred；
2.425g diallyldimethylammonium chlorides are added, 10min is stirred, 2h is incubated, is cooled to room temperature, nanometer is made
ZnO colloidal sols；
Step 2：Prepare complex antimicrobials：
2.4g ammonium persulfates are added in 38.4g water ammonium persulfate aqueous solution is made；
0.675g sodium hydrogensulfites are added in 10g water aqueous solution of sodium bisulfite is made；
Nano-ZnO Sol made from 1.8g allyl glycidyl ethers, 2.46g methacrylic acids and step one is mixed equal
It is even that Nano-ZnO Sol mixed liquor is made；
Water-bath is warming up to 80 DEG C, 97g diallyldimethylammonium chlorides, 1/3 over cure are added in there-necked flask
Sour aqueous ammonium and aqueous solution of sodium bisulfite bottoming, the ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor of dropwise addition 2/3,
Rotating speed 350rpm, starts after stirring, 45min, completion of dropping, is incubated 4h, is cooled to room temperature, stops stirring, produces superfine fibre
Synthetic leather base cloth antiseptic.
Utilize complex antimicrobials made from the above method, N therein+There is synergy with nano zine oxide, can be very
The anti-microbial property of good raising synthetic leather base cloth, is applied in superfine fiber synthetic leather base cloth, to Escherichia coli and golden yellow
The staphylococcic antibiotic rate of color is up to more than 99%.
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And any equivalent conversion taken technical solution of the present invention, it is claim of the invention and is covered.
Claims (2)
1. the preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method, it is characterised in that：
Realized by following steps：
Step one：Prepare Nano-ZnO Sol：
By warming-in-water to 60 DEG C, 0.658-1.317g zinc acetates and 100ml ethanol, rotating speed are added in 150ml there-necked flasks
400rpm is adjusted to, 10min is stirred；
12.615g diethanol amine is added, 10min is stirred；
2.425g diallyldimethylammonium chlorides are added, 10min is stirred, 2h is incubated, is cooled to room temperature, nano-ZnO are made molten
Glue；
Step 2：Prepare complex antimicrobials：
2.4g ammonium persulfates are added in 38.4g water ammonium persulfate aqueous solution is made；
0.675g sodium hydrogensulfites are added in 10g water aqueous solution of sodium bisulfite is made；
By the well mixed system of Nano-ZnO Sol made from 1.8g allyl glycidyl ethers, 2.46g methacrylic acids and step one
Into Nano-ZnO Sol mixed liquor；
Water-bath is warming up to 80 DEG C, 97g diallyldimethylammonium chlorides, 1/3 ammonium persulfate are added in there-necked flask
The aqueous solution and aqueous solution of sodium bisulfite bottoming, the ammonium persulfate aqueous solution and Nano-ZnO Sol mixed liquor of dropwise addition 2/3, rotating speed
350rpm, starts after stirring, 45min, completion of dropping, is incubated 4h, is cooled to room temperature, stops stirring, produces use for synthetic leather polymerization
Thing nano-ZnO complex antimicrobials.
2. the preparation of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials as claimed in claim 1 based on situ aggregation method
Antiseptic made from method.
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| CN105648745B (en) * | 2016-04-01 | 2018-04-17 | 陕西科技大学 | Fabric polymer matrix cerium-doped nanometer zinc oxide composite antibiosis agent and preparation method thereof |
| CN106283617A (en) * | 2016-09-13 | 2017-01-04 | 陕西科技大学 | Bafta polymer/Ag dopen Nano ZnO long acting antibiotic mildew-proofing finishing agent and preparation method thereof |
| CN107287900B (en) * | 2017-07-20 | 2019-08-13 | 科凯精细化工（上海）有限公司 | The preparation method of composite antibacterial finishing agent |
| CN107287899B (en) * | 2017-07-20 | 2019-08-13 | 科凯精细化工（上海）有限公司 | The antibiotic finishing method of cotton fabric |
| CN113981680B (en) * | 2021-11-16 | 2023-12-26 | 青岛大学 | Washable antibacterial fabric and preparation method thereof |
| CN115226708B (en) * | 2022-06-01 | 2023-08-01 | 珠海量致科技有限公司 | Zinc oxide dispersion liquid for antibiosis and preparation method and application thereof |
| CN117779442B (en) * | 2024-02-27 | 2024-05-03 | 广东七彩飞霞针织实业有限公司 | Antibacterial cellulose fiber loaded with nano ZnO, preparation method thereof and application thereof in knitted fabric |
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| CN101864022B (en) * | 2010-06-17 | 2012-11-07 | 陕西科技大学 | Method for preparing vinyl polymer/inorganic nanoparticle composite tanning agent by in-situ cyclopolymerization method |
| CN102787497B (en) * | 2012-09-05 | 2014-05-14 | 陕西科技大学 | Method for preparing novel quaternary ammonium salt copolymer/nanometer ZnO composite antimicrobial for fabric |
| CN103074455B (en) * | 2013-01-16 | 2014-12-10 | 陕西科技大学 | Method for preparing multifunctional polymer-based nanometer ZnO composite tanning agent |
| CN103130957B (en) * | 2013-03-15 | 2015-04-22 | 陕西科技大学 | Method for preparing polymer/nano ZnO composite antimicrobial for textiles through in-situ polymerization method |
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Granted publication date: 20170718 |