CN112647301A - Antibacterial non-woven fabric and preparation method thereof - Google Patents
Antibacterial non-woven fabric and preparation method thereof Download PDFInfo
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- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 113
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 58
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229960003638 dopamine Drugs 0.000 claims abstract description 25
- INUNLMUAPJVRME-UHFFFAOYSA-N 3-chloropropanoyl chloride Chemical compound ClCCC(Cl)=O INUNLMUAPJVRME-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920001690 polydopamine Polymers 0.000 claims abstract description 21
- 125000002603 chloroethyl group Chemical group [H]C([*])([H])C([H])([H])Cl 0.000 claims abstract description 14
- 239000012670 alkaline solution Substances 0.000 claims abstract description 7
- 238000010534 nucleophilic substitution reaction Methods 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000007112 amidation reaction Methods 0.000 claims abstract description 5
- 230000032050 esterification Effects 0.000 claims abstract description 5
- 238000005886 esterification reaction Methods 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- YCFQZBVUTQXHCS-UHFFFAOYSA-N [6-(methylamino)pyridin-3-yl]boronic acid Chemical compound CNC1=CC=C(B(O)O)C=N1 YCFQZBVUTQXHCS-UHFFFAOYSA-N 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000004743 Polypropylene Substances 0.000 claims description 12
- -1 polypropylene Polymers 0.000 claims description 12
- 229920001155 polypropylene Polymers 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 229940017219 methyl propionate Drugs 0.000 abstract description 2
- 150000003863 ammonium salts Chemical class 0.000 abstract 1
- 150000007942 carboxylates Chemical group 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 23
- 238000005406 washing Methods 0.000 description 15
- 230000010355 oscillation Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 238000001291 vacuum drying Methods 0.000 description 12
- 241000894006 Bacteria Species 0.000 description 6
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 229960001149 dopamine hydrochloride Drugs 0.000 description 6
- 239000007983 Tris buffer Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241000222122 Candida albicans Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 229940095731 candida albicans Drugs 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 206010011409 Cross infection Diseases 0.000 description 1
- 241000192125 Firmicutes Species 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical group CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- 206010029803 Nosocomial infection Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating 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
- D06M11/32—Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
- D06M13/21—Halogenated carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/213—Perfluoroalkyl carboxylic acids; Anhydrides, halides or salts thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides an antibacterial non-woven fabric and a preparation method thereof, wherein the preparation method of the antibacterial non-woven fabric comprises the following steps: immersing the non-woven fabric into a dopamine solution for oxidation self-polymerization to obtain the non-woven fabric with the surface coated with a poly dopamine layer; immersing the non-woven fabric with the surface coated with the polydopamine layer into a 3-chloropropionyl chloride solution for esterification or amidation reaction to obtain a non-woven fabric with the surface grafted with chloroethyl; immersing the non-woven fabric with the chloroethyl grafted on the surface into a 3- (dimethylamino) methyl propionate solution for nucleophilic substitution reaction to obtain a quaternized non-woven fabric; and (3) immersing the quaternized non-woven fabric into an alkaline solution for hydrolysis reaction to obtain the non-woven fabric with a zwitterion structure, namely the antibacterial non-woven fabric. According to the antibacterial non-woven fabric and the preparation method thereof, zwitterions with ammonium salt and carboxylate structures are grafted on the surface of the non-woven fabric through a molecular bonding technology, so that the non-woven fabric is endowed with more excellent antibacterial performance.
Description
Technical Field
The invention relates to the technical field of functional non-woven fabrics, in particular to an antibacterial non-woven fabric and a preparation method thereof.
Background
The polypropylene non-woven fabric is a novel fabric product formed without spinning and weaving, has the advantages of wide source, simple process flow, low cost, good mechanical property, relatively stable physicochemical property and the like, and is widely applied to the fields of clothing textile industry, medical protective articles, industrial matrix materials and the like.
Although polypropylene non-woven fabrics produced by different processes have excellent effects in improving sanitary environment and facilitating use. However, human skin and clothes are places where bacteria grow, and the bacteria continuously propagate by taking human excrement such as urea in sweat as a nutrient source and simultaneously discharge ammonia with strong odor. Especially in hospitals, stations, markets, cinemas, public transport vehicles and other places, and living goods easy to breed bacteria, such as: the use of the common polypropylene non-woven fabric can not effectively avoid the propagation infection and cross infection of bacteria.
Particularly, in the prior art, the medical protective non-woven fabric mostly adopts a positively charged mode to adsorb viruses and bacteria, while the antibacterial mode of the antibacterial non-woven fabric mostly adopts a dissolution type antibacterial mode, so that the dissolution speed of antibacterial active substances is high, the antibacterial active substances are easy to fall off, the safety problem is caused, and meanwhile, the service life is short.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides an antibacterial non-woven fabric and a preparation method thereof.
The invention provides an antibacterial non-woven fabric, wherein the surface of the non-woven fabric is connected with the following group structure:
preferably, the surface of the non-woven fabric is coated with a poly-dopamine layer, and the poly-dopamine layer is chemically bonded with the following group structure:
the invention provides a preparation method of an antibacterial non-woven fabric, which comprises the following steps:
s1, immersing the non-woven fabric into a dopamine solution for oxidation self-polymerization to obtain the non-woven fabric with the surface coated with the poly dopamine layer;
s2, immersing the non-woven fabric with the surface coated with the poly dopamine layer into a 3-chloropropionyl chloride solution for esterification or amidation reaction to obtain a non-woven fabric with the surface grafted with chloroethyl;
s3, immersing the non-woven fabric with the chloroethyl grafted on the surface into a methyl 3- (dimethylamino) propionate solution for nucleophilic substitution reaction to obtain a quaternized non-woven fabric;
s4, soaking the quaternized non-woven fabric into an alkaline solution for hydrolysis reaction to obtain the non-woven fabric with a zwitterion structure, namely the antibacterial non-woven fabric.
Preferably, the nonwoven fabric is a polypropylene nonwoven fabric.
Preferably, the dopamine solution is a solution comprising dopamine, ammonium persulfate and ethylenediamine;
preferably, the concentration of the dopamine in the dopamine solution is 15-35mmol/L, and the molar ratio of the dopamine to the ammonium persulfate to the ethylenediamine is 1:0.5-2: 0.5-3.
Preferably, the temperature of the oxidative self-polymerization reaction is 15-35 ℃ and the time is 0.5-1 h.
Preferably, the 3-chloropropionyl chloride solution is a solution comprising 3-chloropropionyl chloride and triethylamine;
preferably, the concentration of the 3-chloropropionyl chloride in the 3-chloropropionyl chloride solution is 0.1-0.6mol/L, and the molar ratio of the 3-chloropropionyl chloride to triethylamine is 8-12: 1.
Preferably, the esterification or amidation reaction is carried out at a temperature of 15 to 25 ℃ for a time of 20 to 24 hours.
Preferably, the concentration of the methyl 3- (dimethylamino) propionate in the methyl 3- (dimethylamino) propionate solution is 0.3-0.9 mol/L;
preferably, the temperature of the nucleophilic substitution reaction is 50-60 ℃ and the time is 6-10 h.
Preferably, the alkaline solution is a methanol solution of sodium hydroxide, and the concentration of the sodium hydroxide in the alkaline solution is 0.01-0.05 mol/L;
preferably, the temperature of the hydrolysis reaction is 30-40 ℃ and the time is 6-10 h.
In the invention, the advantage that dopamine is self-polymerized in a slightly alkaline environment to form Polydopamine (PDA) and is easy to firmly adhere to various substrate materials is firstly utilized, when the non-woven fabric is immersed in a dopamine solution, dopamine can accelerate self-polymerization on the surface of the non-woven fabric under the action of an oxidant, and finally a polydopamine layer is coated on the surface of the non-woven fabric; then, utilizing rich phenolic hydroxyl and amino contained in the polydopamine layer, the polydopamine layer can react with 3-chloropropionyl chloride under the catalysis of organic amine to generate ester or amide, so that chloroethyl groups are grafted to the surface of the polydopamine film layer; then, carrying out nucleophilic substitution reaction on the chloroethyl grafted non-woven fabric and 3- (dimethylamino) methyl propionate to obtain a quaternized non-woven fabric; finally, methyl propionate structure contained in the non-woven fabric grafted by the quaternized non-woven fabric is hydrolyzed under alkaline conditions, so that the non-woven fabric with a zwitterion structure is obtained, and finally the non-woven fabric is endowed with excellent antibacterial performance.
Drawings
Fig. 1 is a schematic diagram of a synthetic route of the antibacterial non-woven fabric of the present invention.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
An antibacterial non-woven fabric is prepared by the following steps:
s1, adding dopamine hydrochloride into a tris buffer solution, stirring and dissolving to prepare a dopamine solution (pH 8.5) with the concentration of 25mmol/L, and adding ammonium persulfate and ethylenediamine which are in equal molar ratio to the dopamine hydrochloride to obtain the dopamine solution; respectively ultrasonically treating polypropylene non-woven fabric in water and ethanol for 15min to remove impurities, drying, soaking the polypropylene non-woven fabric into the dopamine solution according to a bath ratio (g/mL, the same below) of 1:30, carrying out oscillation reaction in a constant-temperature water bath shaker at 25 ℃ for 40min, taking out, washing with deionized water, and carrying out vacuum drying at room temperature to obtain the non-woven fabric with the surface coated with the polydopamine layer;
s2, sequentially adding triethylamine and 3-chloropropionyl chloride into anhydrous tetrahydrofuran, stirring and dissolving, wherein the addition amount of the triethylamine is 10 mol% of the 3-chloropropionyl chloride, and preparing a solution with the concentration of the 3-chloropropionyl chloride being 0.3 mol/L; immersing the non-woven fabric with the surface coated with the poly dopamine layer into the solution according to a bath ratio of 1:20, carrying out oscillation reaction in a constant-temperature water bath shaker at 20 ℃ for 22h, taking out, sequentially washing with deionized water and ethanol, and carrying out vacuum drying at room temperature to obtain the non-woven fabric with the surface grafted with chloroethyl;
s3, adding methyl 3- (dimethylamino) propionate into absolute ethyl alcohol, stirring and dissolving to prepare a methyl 3- (dimethylamino) propionate solution with the concentration of 0.6 mol/L; immersing the non-woven fabric with the surface grafted with chloroethyl into the methyl 3- (dimethylamino) propionate solution according to a bath ratio of 1:20, performing water bath oscillation reaction at 60 ℃ for 6 hours, taking out, washing with ethanol, and performing vacuum drying at room temperature to obtain a quaternized non-woven fabric;
s4, adding sodium hydroxide into methanol, stirring and dissolving to prepare a sodium hydroxide solution with the concentration of 0.03 mol/L; and (2) immersing the quaternized non-woven fabric into the sodium hydroxide solution according to a bath ratio of 1:30, performing water bath oscillation reaction at 35 ℃ for 8 hours, taking out, washing with ethanol, and performing vacuum drying at room temperature to obtain the non-woven fabric with a zwitterion structure, namely the antibacterial non-woven fabric.
Example 2
An antibacterial non-woven fabric is prepared by the following steps:
s1, adding dopamine hydrochloride into a tris buffer solution, stirring and dissolving to prepare a dopamine solution (pH 8.5) with the concentration of 15mmol/L, and adding ammonium persulfate and ethylenediamine which are in equal molar ratio to the dopamine hydrochloride to obtain a dopamine solution; respectively ultrasonically treating polypropylene non-woven fabric in water and ethanol for 15min to remove impurities, drying, soaking the polypropylene non-woven fabric into the dopamine solution according to a bath ratio (g/mL, the same below) of 1:30, carrying out oscillation reaction in a 35 ℃ constant-temperature water bath shaking table for 30min, taking out, washing with deionized water, and carrying out vacuum drying at room temperature to obtain the non-woven fabric with the surface coated with the polydopamine layer;
s2, sequentially adding triethylamine and 3-chloropropionyl chloride into anhydrous tetrahydrofuran, stirring and dissolving, wherein the addition amount of the triethylamine is 9 mol% of the 3-chloropropionyl chloride, and preparing a solution with the concentration of the 3-chloropropionyl chloride being 0.1 mol/L; immersing the non-woven fabric with the surface coated with the poly dopamine layer into the solution according to a bath ratio of 1:20, carrying out oscillation reaction in a constant-temperature water bath shaker at 25 ℃ for 20h, taking out, sequentially washing with deionized water and ethanol, and carrying out vacuum drying at room temperature to obtain the non-woven fabric with the surface grafted with chloroethyl;
s3, adding methyl 3- (dimethylamino) propionate into absolute ethyl alcohol, stirring and dissolving to prepare a methyl 3- (dimethylamino) propionate solution with the concentration of 0.3 mol/L; immersing the non-woven fabric with the surface grafted with chloroethyl into the methyl 3- (dimethylamino) propionate solution according to a bath ratio of 1:20, carrying out water bath oscillation reaction for 10h at 50 ℃, taking out, washing with ethanol, and carrying out vacuum drying at room temperature to obtain a quaternized non-woven fabric;
s4, adding sodium hydroxide into methanol, stirring and dissolving to prepare a sodium hydroxide solution with the concentration of 0.05 mol/L; and (2) immersing the quaternized non-woven fabric into the sodium hydroxide solution according to a bath ratio of 1:30, performing water bath oscillation reaction at 30 ℃ for 10 hours, taking out, washing with ethanol, and performing vacuum drying at room temperature to obtain the non-woven fabric with a zwitterion structure, namely the antibacterial non-woven fabric.
Example 3
An antibacterial non-woven fabric is prepared by the following steps:
s1, adding dopamine hydrochloride into a tris buffer solution, stirring and dissolving to prepare a 35mmol/L dopamine solution (pH 8.5), and adding ammonium persulfate and ethylenediamine which are in equal molar ratio to the dopamine hydrochloride to obtain a dopamine solution; respectively ultrasonically treating polypropylene non-woven fabric in water and ethanol for 15min to remove impurities, drying, soaking the polypropylene non-woven fabric into the dopamine solution according to a bath ratio (g/mL, the same below) of 1:30, carrying out oscillation reaction in a 15-DEG C constant-temperature water bath shaking table for 60min, taking out, washing with deionized water, and carrying out vacuum drying at room temperature to obtain non-woven fabric with a surface coated with a polydopamine layer;
s2, sequentially adding triethylamine and 3-chloropropionyl chloride into anhydrous tetrahydrofuran, stirring and dissolving, wherein the addition amount of the triethylamine is 12 mol% of the 3-chloropropionyl chloride, and preparing a solution with the concentration of the 3-chloropropionyl chloride being 0.6 mol/L; immersing the non-woven fabric with the surface coated with the poly dopamine layer into the solution according to a bath ratio of 1:20, carrying out oscillation reaction in a 15-DEG C constant-temperature water bath shaker for 24 hours, taking out, sequentially washing with deionized water and ethanol, and carrying out vacuum drying at room temperature to obtain the non-woven fabric with the surface grafted with chloroethyl;
s3, adding methyl 3- (dimethylamino) propionate into absolute ethyl alcohol, stirring and dissolving to prepare a methyl 3- (dimethylamino) propionate solution with the concentration of 0.9 mol/L; immersing the non-woven fabric with the surface grafted with chloroethyl into the methyl 3- (dimethylamino) propionate solution according to a bath ratio of 1:20, performing water bath oscillation reaction at 60 ℃ for 6 hours, taking out, washing with ethanol, and performing vacuum drying at room temperature to obtain a quaternized non-woven fabric;
s4, adding sodium hydroxide into methanol, stirring and dissolving to prepare a sodium hydroxide solution with the concentration of 0.01 mol/L; and (3) immersing the quaternized non-woven fabric into the sodium hydroxide solution according to a bath ratio of 1:30, performing water bath oscillation reaction at 40 ℃ for 6 hours, taking out, washing with ethanol, and performing vacuum drying at room temperature to obtain the non-woven fabric with a zwitterion structure, namely the antibacterial non-woven fabric.
The antibacterial nonwoven fabrics obtained in examples 1 to 3 were tested for antibacterial activity, specifically, with reference to GB/T20944.3-2008 "evaluation of antibacterial activity of textile", and the test strains were staphylococcus aureus (ATCC 6538) (gram-negative bacteria), escherichia coli (ATCC 8099) (gram-positive bacteria), and candida albicans (ATCC 10231) measured by the oscillation method, and the results are shown in table 1:
table 1 antibacterial test results of antibacterial nonwoven fabric
Referring to table 1, it can be seen that the unmodified polypropylene nonwoven fabric has no inhibitory effect on staphylococcus aureus, escherichia coli and candida albicans, and the antibacterial nonwoven fabric obtained by using the method of the present invention has very excellent ability to inhibit bacterial growth.
The antibacterial nonwoven fabrics obtained in examples 1-3 were subjected to a water washing resistance test, specifically, the antibacterial nonwoven fabrics were washed with water for 50 times, dried, and then tested with reference to FZ/T73023 and 2006(2012) 'antibacterial knitwear', and the results are shown in table 2:
TABLE 2 washing fastness test results of antibacterial non-woven fabric
Referring to table 2, it can be seen that the antibacterial performance of the antibacterial non-woven fabric obtained by the present invention is not affected after washing.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The antibacterial non-woven fabric is characterized in that the surface of the non-woven fabric is connected with the following group structure:
2. the antibacterial non-woven fabric according to claim 1, wherein a polydopamine layer is coated on the surface of the non-woven fabric, and the following group structures are chemically bonded on the polydopamine layer:
3. a method for preparing the antibacterial non-woven fabric according to any one of claims 1 to 2, which comprises the following steps:
s1, immersing the non-woven fabric into a dopamine solution for oxidation self-polymerization to obtain the non-woven fabric with the surface coated with the poly dopamine layer;
s2, immersing the non-woven fabric with the surface coated with the poly dopamine layer into a 3-chloropropionyl chloride solution for esterification or amidation reaction to obtain a non-woven fabric with the surface grafted with chloroethyl;
s3, immersing the non-woven fabric with the chloroethyl grafted on the surface into a methyl 3- (dimethylamino) propionate solution for nucleophilic substitution reaction to obtain a quaternized non-woven fabric;
s4, soaking the quaternized non-woven fabric into an alkaline solution for hydrolysis reaction to obtain the non-woven fabric with a zwitterion structure, namely the antibacterial non-woven fabric.
4. The method of manufacturing an antibacterial nonwoven fabric according to claim 3, wherein the nonwoven fabric is a polypropylene nonwoven fabric.
5. The method for preparing the antibacterial non-woven fabric according to claim 3 or 4, wherein the dopamine solution is a solution comprising dopamine, ammonium persulfate and ethylenediamine;
preferably, the concentration of the dopamine in the dopamine solution is 15-35mmol/L, and the molar ratio of the dopamine to the ammonium persulfate to the ethylenediamine is 1:0.5-2: 0.5-3.
6. The method for preparing the antibacterial non-woven fabric according to any one of claims 3 to 5, wherein the temperature of the oxidative self-polymerization reaction is 15 to 35 ℃ and the time is 0.5 to 1 hour.
7. The method for preparing an antibacterial nonwoven fabric according to any one of claims 3 to 6, wherein the 3-chloropropionyl chloride solution is a solution comprising 3-chloropropionyl chloride and triethylamine;
preferably, the concentration of the 3-chloropropionyl chloride in the 3-chloropropionyl chloride solution is 0.1-0.6mol/L, and the molar ratio of the 3-chloropropionyl chloride to triethylamine is 8-12: 1.
8. The method for preparing the antibacterial non-woven fabric according to any one of claims 3 to 7, wherein the temperature of the esterification or amidation reaction is 15 to 25 ℃ and the time is 20 to 24 hours.
9. The method for producing an antibacterial nonwoven fabric according to any one of claims 3 to 8, wherein the concentration of methyl 3- (dimethylamino) propionate in the methyl 3- (dimethylamino) propionate solution is 0.3 to 0.9 mol/L;
preferably, the temperature of the nucleophilic substitution reaction is 50-60 ℃ and the time is 6-10 h.
10. The method for preparing the antibacterial non-woven fabric according to any one of claims 3 to 9, wherein the alkaline solution is a methanol solution of sodium hydroxide, and the concentration of the sodium hydroxide in the alkaline solution is 0.01 to 0.05 mol/L;
preferably, the temperature of the hydrolysis reaction is 30-40 ℃ and the time is 6-10 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114345140A (en) * | 2022-02-17 | 2022-04-15 | 天津工业大学 | Preparation method of high-performance composite nanofiltration membrane with interlayer structure |
| CN115125730A (en) * | 2022-08-01 | 2022-09-30 | 湖南佑华医疗用品有限公司 | Isolation clothes with high protective performance and preparation method thereof |
| CN115624646A (en) * | 2022-10-25 | 2023-01-20 | 维达纸业(浙江)有限公司 | Antibacterial liquid-absorbing non-woven material for hygienic products |
-
2020
- 2020-12-18 CN CN202011506594.5A patent/CN112647301A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114345140A (en) * | 2022-02-17 | 2022-04-15 | 天津工业大学 | Preparation method of high-performance composite nanofiltration membrane with interlayer structure |
| CN115125730A (en) * | 2022-08-01 | 2022-09-30 | 湖南佑华医疗用品有限公司 | Isolation clothes with high protective performance and preparation method thereof |
| CN115624646A (en) * | 2022-10-25 | 2023-01-20 | 维达纸业(浙江)有限公司 | Antibacterial liquid-absorbing non-woven material for hygienic products |
| CN115624646B (en) * | 2022-10-25 | 2023-09-05 | 维达纸业(浙江)有限公司 | Antibacterial liquid-absorbing nonwoven material for sanitary products |
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