CN104650290A - Polymer nano ZnO compound antibacterial agent for synthetic leathers based on in-situ polymerization process and preparation method of polymer nano ZnO compound antibacterial agent - Google Patents
Polymer nano ZnO compound antibacterial agent for synthetic leathers based on in-situ polymerization process and preparation method of polymer nano ZnO compound antibacterial agent Download PDFInfo
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- CN104650290A CN104650290A CN201510058729.9A CN201510058729A CN104650290A CN 104650290 A CN104650290 A CN 104650290A CN 201510058729 A CN201510058729 A CN 201510058729A CN 104650290 A CN104650290 A CN 104650290A
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- 229920000642 polymer Polymers 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003242 anti bacterial agent Substances 0.000 title abstract description 9
- 238000011065 in-situ storage Methods 0.000 title abstract description 5
- -1 ZnO compound Chemical class 0.000 title abstract 4
- 238000006116 polymerization reaction Methods 0.000 title abstract 2
- 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 46
- 239000002649 leather substitute Substances 0.000 claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000000835 fiber Substances 0.000 claims abstract description 12
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004246 zinc acetate Substances 0.000 claims abstract description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004599 antimicrobial Substances 0.000 claims description 15
- 239000004744 fabric Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 12
- LSWYGACWGAICNM-UHFFFAOYSA-N 2-(prop-2-enoxymethyl)oxirane Chemical compound C=CCOCC1CO1 LSWYGACWGAICNM-UHFFFAOYSA-N 0.000 claims description 8
- 238000004220 aggregation Methods 0.000 claims description 8
- 230000002776 aggregation Effects 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000002114 nanocomposite Substances 0.000 claims description 8
- 239000004160 Ammonium persulphate Substances 0.000 claims description 6
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 5
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 3
- 150000001875 compounds Chemical class 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
- 241000588724 Escherichia coli Species 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 229940079827 sodium hydrogen sulfite Drugs 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 41
- 239000011787 zinc oxide Substances 0.000 description 35
- 241000894006 Bacteria Species 0.000 description 4
- 230000000845 anti-microbial effect Effects 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000003115 biocidal effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 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
- 230000000968 intestinal effect Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007901 in situ hybridization Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920006264 polyurethane film Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a polymer nano ZnO compound antibacterial agent for synthetic leathers based on an in-situ polymerization process and a preparation method of the polymer nano ZnO compound antibacterial agent. Studies relative to an antibacterial agent for synthetic leather base cloths have been rarely reported at present. The preparation method comprises the following steps: mixing zinc acetate and ethanol in water bath, and adding diethanolamine and diallyldimethylammonium chloride to prepare a nano ZnO sol; uniformly mixing allyl glycidyl ether, methacrylic acid and the nano ZnO sol to prepare a nano ZnO sol mixed solution; and mixing diallyldimethylammonium chloride, an ammonium persulfate aqueous solution and a sodium hydrogen sulfite aqueous solution in the water bath for bottoming, dropwise adding the ammonium persulfate aqueous solution and the nano ZnO sol mixed solution, performing stirring reaction, and performing heat preservation and cooling to obtain the antibacterial agent for superfine fiber synthetic leather base cloths. According to the compound antibacterial agent disclosed by the invention, the antibacterial properties of the synthetic leather base cloths can be well improved by virtue of the synergistic effects of N<+> and nano ZnO; and the compound antibacterial agent can be applied to the superfine fiber synthetic leather base cloths, and ensures that the antibacterial rate on escherichia coli and staphylococcus aureus can reach more than 99%.
Description
Technical field
the present invention relates to a kind of preparation method of use for synthetic leather antiseptic-germicide, be specifically related to a kind of use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method and preparation method thereof.
Background technology
Synthetic leather is widely used in making footwear, boots, case and bag and ball etc., but it contains bacterium, the necessary nutritive substance of mould, under suitable temperature and humidity condition, bacterium and mould will on synthetic leather amount reproduction, cause microbial resistance to decline.The properties impact of Ji Bu on synthetic leather is most important.Therefore, study excellent long-acting synthetic leather base cloth anti-biotic material to have great importance.
Along with going deep into of development in science and technology research, the research of nanotechnology and the antibacterial research in synthetic leather thereof also result in the concern of people.The people such as Fan Haojun (Chen Yi, Feng Ping, Fan Haojun, etc. nano-TiO
2in-situ hybridization urethane and antibacterial and mouldproof performance study [J] thereof. leather science and engineering, 2008,3(18): 11-15.) under the prerequisite not changing the existing wet process technique of Synthetic Leather and production unit, by original position hybrid inorganic-organic technology by nano level TiO
2introduce in use for synthetic leather polyurethane film.Experiment proves, through nano-TiO
2polyurethane film after in-situ modified not only has excellent antibacterial and mouldproof performance, and its tensile strength and unit elongation are also improved simultaneously.But about the research also rarely seen report of synthetic leather base cloth antiseptic-germicide.
Summary of the invention
The object of this invention is 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 anti-microbial property of superfine fiber synthetic leather base cloth antiseptic-germicide is improved with the synergy of nano zine oxide.
The technical solution adopted in the present invention is:
Based on the preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials of situ aggregation method, it is characterized in that:
Realized by following steps:
Step one: prepare Nano-ZnO Sol:
By warming-in-water to 60 DEG C, in 150ml there-necked flask, add 0.658-1.317g zinc acetate and 100ml ethanol, rotating speed is adjusted to 400rpm, stirs 10min;
Add 12.615g diethanolamine, stir 10min;
Add 2.425g diallyldimethylammonium chloride, stir 10min, insulation 2h, is cooled to room temperature, obtained Nano-ZnO Sol;
Step 2: prepare complex antimicrobials:
2.4g ammonium persulphate is added in 38.4g water and makes ammonium persulfate aqueous solution;
0.675g sodium bisulfite is added in 10g water and makes aqueous solution of sodium bisulfite;
The Nano-ZnO Sol that 1.8g glycidyl allyl ether, 2.46g methacrylic acid and step one are obtained is mixed and makes Nano-ZnO Sol mixed solution;
Water-bath is warmed up to 80 DEG C, add in there-necked flask 97g diallyldimethylammonium chloride, 1/3 ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming, drip ammonium persulfate aqueous solution and the Nano-ZnO Sol mixed solution of 2/3, rotating speed 350rpm, start to stir, after 45min, dropwise, insulation 4h, is cooled to room temperature, stop stirring, obtain superfine fiber synthetic leather base cloth antiseptic-germicide.
As described in the antiseptic-germicide that obtains of the preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method.
The present invention has the following advantages:
The present invention adopts sol-gel method to prepare nano-ZnO, with dimethyl diallyl ammonium chloride, methacrylic acid, glycidyl allyl ether, zinc acetate for raw material, prepare polymer-based carbon/nano-ZnO composite material antiseptic-germicide by in-situ method, be applied in superfine fiber synthetic leather base cloth.N in this matrix material
+the anti-microbial property improving synthetic leather base cloth is can be good at the synergy of nano zine oxide.The synthetic leather antiseptic-germicide according to said method prepared is applied in superfine fiber synthetic leather base cloth, reaches more than 99% to the antibiotic rate of intestinal bacteria and streptococcus aureus.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail.
The preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials based on situ aggregation method that the present invention relates to, sol-gel method is adopted to prepare nano-ZnO, and then by in-situ method, itself and dimethyl diallyl ammonium chloride, glycidyl allyl ether, methacrylic acid are prepared polymer-based carbon/nano-zinc oxide composite material, intend utilizing N
+the anti-microbial property of synthetic leather base cloth is improved with the synergy of nano zine oxide.Specifically comprise the following steps:
Step one: prepare Nano-ZnO Sol:
By warming-in-water to 60 DEG C, in 150ml there-necked flask, add 0.658-1.317g zinc acetate and 100ml ethanol, rotating speed is adjusted to 400rpm, stirs 10min;
Add 12.615g diethanolamine, stir 10min;
Add 2.425g diallyldimethylammonium chloride, stir 10min, insulation 2h, is cooled to room temperature, obtained Nano-ZnO Sol;
Step 2: prepare complex antimicrobials:
2.4g ammonium persulphate is added in 38.4g water and makes ammonium persulfate aqueous solution;
0.675g sodium bisulfite is added in 10g water and makes aqueous solution of sodium bisulfite;
The Nano-ZnO Sol that 1.8g glycidyl allyl ether, 2.46g methacrylic acid and step one are obtained is mixed and makes Nano-ZnO Sol mixed solution;
Water-bath is warmed up to 80 DEG C, add in there-necked flask 97g diallyldimethylammonium chloride, 1/3 ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming, drip ammonium persulfate aqueous solution and the Nano-ZnO Sol mixed solution of 2/3, rotating speed 350rpm, start to stir, after 45min, dropwise, insulation 4h, is cooled to room temperature, stop stirring, obtain superfine fiber synthetic leather base cloth antiseptic-germicide.
Embodiment 1:
Step one: prepare Nano-ZnO Sol:
By warming-in-water to 60 DEG C, in 150ml there-necked flask, add 0.658g zinc acetate and 100ml ethanol, rotating speed is adjusted to 400rpm, stirs 10min;
Add 12.615g diethanolamine, stir 10min;
Add 2.425g diallyldimethylammonium chloride, stir 10min, insulation 2h, is cooled to room temperature, obtained Nano-ZnO Sol;
Step 2: prepare complex antimicrobials:
2.4g ammonium persulphate is added in 38.4g water and makes ammonium persulfate aqueous solution;
0.675g sodium bisulfite is added in 10g water and makes aqueous solution of sodium bisulfite;
The Nano-ZnO Sol that 1.8g glycidyl allyl ether, 2.46g methacrylic acid and step one are obtained is mixed and makes Nano-ZnO Sol mixed solution;
Water-bath is warmed up to 80 DEG C, add in there-necked flask 97g diallyldimethylammonium chloride, 1/3 ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming, drip ammonium persulfate aqueous solution and the Nano-ZnO Sol mixed solution of 2/3, rotating speed 350rpm, start to stir, after 45min, dropwise, insulation 4h, is cooled to room temperature, stop stirring, obtain superfine fiber synthetic leather base cloth antiseptic-germicide.
Embodiment 2:
Step one: prepare Nano-ZnO Sol:
By warming-in-water to 60 DEG C, in 150ml there-necked flask, add 0.988g zinc acetate and 100ml ethanol, rotating speed is adjusted to 400rpm, stirs 10min;
Add 12.615g diethanolamine, stir 10min;
Add 2.425g diallyldimethylammonium chloride, stir 10min, insulation 2h, is cooled to room temperature, obtained Nano-ZnO Sol;
Step 2: prepare complex antimicrobials:
2.4g ammonium persulphate is added in 38.4g water and makes ammonium persulfate aqueous solution;
0.675g sodium bisulfite is added in 10g water and makes aqueous solution of sodium bisulfite;
The Nano-ZnO Sol that 1.8g glycidyl allyl ether, 2.46g methacrylic acid and step one are obtained is mixed and makes Nano-ZnO Sol mixed solution;
Water-bath is warmed up to 80 DEG C, add in there-necked flask 97g diallyldimethylammonium chloride, 1/3 ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming, drip ammonium persulfate aqueous solution and the Nano-ZnO Sol mixed solution of 2/3, rotating speed 350rpm, start to stir, after 45min, dropwise, insulation 4h, is cooled to room temperature, stop stirring, obtain superfine fiber synthetic leather base cloth antiseptic-germicide.
Embodiment 3:
Step one: prepare Nano-ZnO Sol:
By warming-in-water to 60 DEG C, in 150ml there-necked flask, add 1.317g zinc acetate and 100ml ethanol, rotating speed is adjusted to 400rpm, stirs 10min;
Add 12.615g diethanolamine, stir 10min;
Add 2.425g diallyldimethylammonium chloride, stir 10min, insulation 2h, is cooled to room temperature, obtained Nano-ZnO Sol;
Step 2: prepare complex antimicrobials:
2.4g ammonium persulphate is added in 38.4g water and makes ammonium persulfate aqueous solution;
0.675g sodium bisulfite is added in 10g water and makes aqueous solution of sodium bisulfite;
The Nano-ZnO Sol that 1.8g glycidyl allyl ether, 2.46g methacrylic acid and step one are obtained is mixed and makes Nano-ZnO Sol mixed solution;
Water-bath is warmed up to 80 DEG C, add in there-necked flask 97g diallyldimethylammonium chloride, 1/3 ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming, drip ammonium persulfate aqueous solution and the Nano-ZnO Sol mixed solution of 2/3, rotating speed 350rpm, start to stir, after 45min, dropwise, insulation 4h, is cooled to room temperature, stop stirring, obtain superfine fiber synthetic leather base cloth antiseptic-germicide.
Utilize the complex antimicrobials that aforesaid method is obtained, N wherein
+with nano zine oxide, there is synergy, can be good at the anti-microbial property improving synthetic leather base cloth, be applied in superfine fiber synthetic leather base cloth, more than 99% is reached to the antibiotic rate of intestinal bacteria and streptococcus aureus.
Content of the present invention is not limited to cited by embodiment, and the conversion of those of ordinary skill in the art by reading specification sheets of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.
Claims (2)
1., based on the preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials of situ aggregation method, it is characterized in that:
Realized by following steps:
Step one: prepare Nano-ZnO Sol:
By warming-in-water to 60 DEG C, in 150ml there-necked flask, add 0.658-1.317g zinc acetate and 100ml ethanol, rotating speed is adjusted to 400rpm, stirs 10min;
Add 12.615g diethanolamine, stir 10min;
Add 2.425g diallyldimethylammonium chloride, stir 10min, insulation 2h, is cooled to room temperature, obtained Nano-ZnO Sol;
Step 2: prepare complex antimicrobials:
2.4g ammonium persulphate is added in 38.4g water and makes ammonium persulfate aqueous solution;
0.675g sodium bisulfite is added in 10g water and makes aqueous solution of sodium bisulfite;
The Nano-ZnO Sol that 1.8g glycidyl allyl ether, 2.46g methacrylic acid and step one are obtained is mixed and makes Nano-ZnO Sol mixed solution;
Water-bath is warmed up to 80 DEG C, add in there-necked flask 97g diallyldimethylammonium chloride, 1/3 ammonium persulfate aqueous solution and aqueous solution of sodium bisulfite bottoming, drip ammonium persulfate aqueous solution and the Nano-ZnO Sol mixed solution of 2/3, rotating speed 350rpm, start to stir, after 45min, dropwise, insulation 4h, is cooled to room temperature, stop stirring, obtain superfine fiber synthetic leather base cloth antiseptic-germicide.
2. as claimed in claim 1 based on the antiseptic-germicide that the preparation method of the use for synthetic leather polymer nanocomposite ZnO complex antimicrobials of situ aggregation method obtains.
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Cited By (7)
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CN105648745A (en) * | 2016-04-01 | 2016-06-08 | 陕西科技大学 | Polymer-based cerium-doped nano zinc oxide compound antibacterial agent for fabric 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 |
CN107287900A (en) * | 2017-07-20 | 2017-10-24 | 科凯精细化工(上海)有限公司 | The preparation method of composite antibacterial finishing agent |
CN107287899A (en) * | 2017-07-20 | 2017-10-24 | 科凯精细化工(上海)有限公司 | The antibiotic finishing method of bafta |
CN113981680A (en) * | 2021-11-16 | 2022-01-28 | 青岛大学 | Washable antibacterial fabric and preparation method thereof |
CN115226708A (en) * | 2022-06-01 | 2022-10-25 | 珠海量致科技有限公司 | Zinc oxide dispersion liquid for antibiosis, preparation method and application thereof |
CN117779442A (en) * | 2024-02-27 | 2024-03-29 | 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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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 |
CN107287900A (en) * | 2017-07-20 | 2017-10-24 | 科凯精细化工(上海)有限公司 | The preparation method of composite antibacterial finishing agent |
CN107287899A (en) * | 2017-07-20 | 2017-10-24 | 科凯精细化工(上海)有限公司 | The antibiotic finishing method of bafta |
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 |
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 |
CN113981680A (en) * | 2021-11-16 | 2022-01-28 | 青岛大学 | Washable antibacterial fabric and preparation method thereof |
CN113981680B (en) * | 2021-11-16 | 2023-12-26 | 青岛大学 | Washable antibacterial fabric and preparation method thereof |
CN115226708A (en) * | 2022-06-01 | 2022-10-25 | 珠海量致科技有限公司 | Zinc oxide dispersion liquid for antibiosis, preparation method and application thereof |
CN117779442A (en) * | 2024-02-27 | 2024-03-29 | 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 |
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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