CN115467083A - Degradable antibacterial non-woven fabric and preparation method thereof - Google Patents
Degradable antibacterial non-woven fabric and preparation method thereof Download PDFInfo
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- CN115467083A CN115467083A CN202211198190.3A CN202211198190A CN115467083A CN 115467083 A CN115467083 A CN 115467083A CN 202211198190 A CN202211198190 A CN 202211198190A CN 115467083 A CN115467083 A CN 115467083A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 229
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 50
- -1 polypropylene Polymers 0.000 claims abstract description 88
- 239000000843 powder Substances 0.000 claims abstract description 84
- 239000004743 Polypropylene Substances 0.000 claims abstract description 83
- 229920001155 polypropylene Polymers 0.000 claims abstract description 83
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 81
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 61
- 239000004626 polylactic acid Substances 0.000 claims abstract description 61
- 238000007664 blowing Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 34
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- 238000000498 ball milling Methods 0.000 claims description 93
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 60
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- 241000588724 Escherichia coli Species 0.000 description 3
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- 235000006251 pelargonidin Nutrition 0.000 description 2
- XVFMGWDSJLBXDZ-UHFFFAOYSA-O pelargonidin Chemical compound C1=CC(O)=CC=C1C(C(=C1)O)=[O+]C2=C1C(O)=CC(O)=C2 XVFMGWDSJLBXDZ-UHFFFAOYSA-O 0.000 description 2
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- SNPLKNRPJHDVJA-ZETCQYMHSA-N D-panthenol Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCCO SNPLKNRPJHDVJA-ZETCQYMHSA-N 0.000 description 1
- GCPYCNBGGPHOBD-UHFFFAOYSA-N Delphinidin Natural products OC1=Cc2c(O)cc(O)cc2OC1=C3C=C(O)C(=O)C(=C3)O GCPYCNBGGPHOBD-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
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- 229920002907 Guar gum Polymers 0.000 description 1
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 239000006067 antibiotic powder Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- JKHRCGUTYDNCLE-UHFFFAOYSA-O delphinidin Chemical compound [O+]=1C2=CC(O)=CC(O)=C2C=C(O)C=1C1=CC(O)=C(O)C(O)=C1 JKHRCGUTYDNCLE-UHFFFAOYSA-O 0.000 description 1
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- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 description 1
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- URXQDXAVUYKSCK-UHFFFAOYSA-N hexadecyl(dimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[NH+](C)C URXQDXAVUYKSCK-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/4291—Olefin series
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4326—Condensation or reaction polymers
- D04H1/435—Polyesters
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a degradable antibacterial non-woven fabric and a preparation method thereof. The invention mixes the polypropylene plastic master batch, the polylactic acid plastic master batch and a small amount of proper antibacterial powder, granulates under proper conditions, adds the obtained antibacterial master batch into the polypropylene cellulose in a small amount, and then melts and sprays under proper conditions, thereby forming the specific antibacterial non-woven fabric process. In addition, the addition of the small amount of the antibacterial powder can also promote the degradation of plastics. Particularly, the invention improves the toughness of the obtained non-woven fabric by integrally adjusting the proportion of the polypropylene master batch, the polylactic acid master batch and the antibacterial powder and the proportion of the antibacterial master batch and the polypropylene cellulose and matching with the conditions of granulation and melt-blowing.
Description
Technical Field
The invention relates to the technical field of medical material preparation, in particular to a degradable antibacterial non-woven fabric and a preparation method thereof.
Background
The non-woven fabric has the advantages of light weight, good air permeability, moisture resistance, no stimulation, low toxicity, easy degradation, low price and the like, and is widely applied to the preparation of baby diapers, masks, protective clothing, operating gowns, operating drapes and the like. Although the non-woven fabric is spread over the aspects of our lives, most of the antibacterial performance needs to be improved. Therefore, it is important to provide a non-woven fabric having antibacterial properties for the purpose of life health and safety of people.
Conventional antibacterial nonwoven fabrics include, for example: the preparation method of the nano-silver antibacterial non-woven fabric disclosed in the Chinese patent application CN14758613A comprises the steps of uniformly stirring nano-silver powder and polypropylene fibers in a certain proportion, melting the polypropylene fibers mixed with the nano-silver into a liquid mixture through an extruding machine, and carrying out melt-blowing on the liquid mixture through a melt-blowing injection molding machine to obtain the antibacterial non-woven fabric. The antibacterial nano-silver non-woven fabric has stronger antibacterial property, but the amount of the nano-silver antibacterial agent is too much, so that the antibacterial non-woven fabric is hard to be produced in a land for enterprises to produce the antibacterial non-woven fabric in batches.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
It is a primary object of embodiments of the present invention to provide an antibacterial nonwoven fabric having a superior antibacterial effect with a small amount of an appropriate kind of antibacterial ingredient.
In a first aspect of the present invention, there is provided a method for preparing a degradable antibacterial non-woven fabric, the method comprising the steps of:
mixing antibacterial colloid and a filler, stirring, infiltrating the filler with the antibacterial colloid, and performing ball milling and drying on the obtained mixture to prepare antibacterial powder;
mixing the antibacterial powder, the polypropylene master batch and the polylactic acid master batch, stirring and granulating to prepare antibacterial master batch;
mixing the antibacterial master batches and polypropylene cellulose, and melt-blowing to prepare degradable antibacterial non-woven fabric;
wherein, the first and the second end of the pipe are connected with each other,
the antibacterial colloid comprises anthocyanin-modified nano-gold particles, the average particle size of the nano-gold particles is 3nm-5nm, the polydispersity index is 0.01-0.2, and the particle size of particles in a product obtained by ball milling is 50nm-300nm;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (10-50): (0.001-0.35);
the mass ratio of the antibacterial master batch to the polypropylene cellulose is 1: (45-55);
the granulation conditions include: the temperature is 135-255 ℃, and the pressure is 2.5kg/cm 2 -7.5kg/cm 2 ；
The conditions for melt blowing include: the temperature is 145-235 ℃, and the pressure is 3.5kg/cm 2 -8kg/cm 2 。
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The filler is selected from one or more of nano hydroxyapatite, montmorillonite and starch;
(2) One or more of zirconia balls and agate balls are adopted for ball milling;
(3) The viscosity average molecular weight of the polypropylene master batch is 9-14 ten thousand daltons;
(4) The viscosity average molecular weight of the polylactic acid master batch is 14-18 ten thousand daltons; and the combination of (a) and (b),
(5) The viscosity average molecular weight of the polypropylene cellulose is 10-30 ten thousand daltons.
In some embodiments of the invention, the filler is montmorillonite and starch;
the ball milling conditions include: zirconium oxide balls are adopted;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (28-50): (0.001-0.3);
the granulation conditions include: the temperature is 140-240 ℃, and the pressure is 3kg/cm 2 -7kg/cm 2 ；
Conditions for melt blowing include: the temperature is 150-225 ℃, and the pressure is 4.5kg/cm 2 -7.5kg/cm 2 。
In some embodiments of the present invention, the mass ratio of the polypropylene masterbatch, the polylactic acid masterbatch and the antibacterial powder is 100: (30-50): (0.005-0.15);
the granulation conditions include: the temperature is 210-220 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 210-220 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 。
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (1-23): (1-20);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 15rpm-1200rpm,21 ℃ -85 ℃;
(3) The soaking time is 2-11 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.2-11); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 100rpm-850rpm, and the ball milling time is 0.3h-6.5h.
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (2.5-22): (1.5-15);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 150rpm-950rpm,26 ℃ -75 ℃;
(3) The soaking time is 3-10 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.3-9.5); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 120rpm-750rpm, and the ball milling time is 0.5h-5h.
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (2.5-6): (1.5-4);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 200rpm-400rpm,27 ℃ -30 ℃;
(3) The soaking time is 4-6 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.5-5.5); and (c) and (d),
(5) The rotation speed of the ball milling is 250rpm-650rpm, and the ball milling time is 1h-4h.
In some embodiments of the invention, the filler is nano-hydroxyapatite and starch;
the ball milling conditions include: agate balls are adopted;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-45): (0.001-0.25);
the granulation conditions include: the temperature is 140-220 ℃, and the pressure is 3kg/cm 2 -6kg/cm 2 ；
The conditions for melt blowing include: the temperature is 150-210 ℃, and the pressure is 4.5kg/cm 2 -6.5kg/cm 2 。
In some embodiments of the present invention, the mass ratio of the polypropylene masterbatch, the polylactic acid masterbatch and the antibacterial powder is 100: (30-45): (0.008-0.25);
the granulation conditions include: the temperature is 205-210 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 ；
The conditions for melt blowing include: the temperature is 205-210 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 。
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the nano hydroxyapatite to the starch is 1: (1-23): (1-20);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 15rpm-1200rpm,21 ℃ -85 ℃;
(3) The soaking time is 2-11 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.2-11); and (c) and (d),
(5) The rotation speed of the ball milling is 100rpm-850rpm, and the ball milling time is 0.3h-6.5h.
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1-20): (1-15);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 150rpm-800rpm,26 ℃ -70 ℃;
(3) The soaking time is 4-9 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.35-9); and (c) and (d),
(5) The rotation speed of the ball milling is 200rpm-650rpm, and the ball milling time is 1h-6h.
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1.75-3.5): (1.2-2.5);
(2) In the step of preparing the antibacterial powder, the stirring conditions comprise: 200rpm-450rpm,30 ℃ -35 ℃;
(3) The soaking time is 5-8 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (2-4); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 200rpm-350rpm, and the ball milling time is 2h-4h.
In a second aspect of the present invention, there is provided a degradable antibacterial nonwoven fabric, which is prepared by the preparation method provided in the first aspect.
Compared with the prior art, the invention has the beneficial effects that:
the invention mixes the polypropylene plastic master batch, the polylactic acid plastic master batch and a small amount of proper antibacterial powder, granulates under proper conditions, then adds the obtained antibacterial master batch into the polypropylene cellulose in a small amount, and melts and sprays under proper conditions, thereby forming the specific antibacterial non-woven fabric process.In addition, the addition of the small amount of the antibacterial powder can also promote the degradation of plastics. Particularly, the invention improves the toughness of the obtained non-woven fabric by integrally adjusting the proportion of the polypropylene master batch, the polylactic acid master batch and the antibacterial powder and the proportion of the antibacterial master batch and the polypropylene cellulose and matching with corresponding conditions of granulation and melt-blowing。
Moreover, the process of the antibacterial non-woven fabric provided by the invention has high biological safety, no matter the antibacterial component is selected, no toxic reagent is involved in the later preparation process, and the negative influence on environmental pollution is effectively avoided. In addition, the preparation process is simple and easy to operate, the dosage of the required antibacterial component is small, the cost is controllable, and the preparation method is suitable for mass production of enterprises.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application and to more fully understand the present application and the advantages thereof, the drawings that are required in the description of the embodiments will be briefly introduced below. It is obvious that the drawings in the following description are only some embodiments of the application, and that other drawings can be derived from these drawings by a person skilled in the art without inventive effort.
Fig. 1 is an electron microscope image of anthocyanin-modified gold nanoparticles (average particle size of 3nm to 5 nm) in the anthocyanin-containing antibacterial colloid prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to the drawings, embodiments and examples. It should be understood that these embodiments and examples are merely illustrative of the present invention and are not intended to limit the scope of the present invention, which is provided for the purpose of making the present disclosure more thorough and complete. It is also understood that the present invention may be embodied in many different forms and is not limited to the embodiments and examples described herein, and that various changes and modifications may be effected therein by one of ordinary skill in the art without departing from the spirit and scope of the invention and the resulting equivalents are within the scope and range of equivalents of the present application. Furthermore, in the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention, and it is to be understood that the present invention may be practiced without one or more of these details.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments and examples only and is not intended to be limiting of the invention.
Term(s) for
Unless otherwise indicated or contradicted, terms or phrases used herein have the following meanings:
as used herein, the term "and/or", "and/or" includes any and all combinations of two or more of the associated listed items, including any two or any more of the associated listed items, or all of the associated listed items.
As used herein, "one or more" means any one, any two, or any two or more of the listed items. Wherein, the 'several' means any two or more than any two.
As used herein, "a combination thereof," "any combination thereof," and the like, includes all suitable combinations of any two or more of the listed items.
In the present specification, the term "suitable" in "a suitable combination, a suitable manner," any suitable manner "and the like shall be construed to mean that the technical solution of the present invention can be implemented, the technical problem of the present invention can be solved, and the technical effect of the present invention can be achieved.
Herein, "preferred" merely describes a more effective embodiment or example, and it should be understood that the scope of the present invention is not limited thereto.
In the present invention, the terms "first," "second," "third," "fourth," "first class," "second class," "first segment," "second segment," and the like in the terms of "first aspect," "second aspect," "third aspect," "fourth aspect," "first class," "second class," "first segment," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or quantity or as implying any indication of the importance or quantity of the technical feature being indicated. Moreover, "first," "second," "third," "fourth," etc. are used merely as non-exhaustive lists and should not be construed as limiting the number of instances.
In the present invention, the technical features described in the open type include a closed technical solution including the listed features, and also include an open technical solution including the listed features.
In the present invention, the numerical range is defined to include both endpoints of the numerical range unless otherwise specified.
The percentage contents referred to in the present invention mean, unless otherwise specified, mass percentages for solid-liquid mixing and solid-solid mixing, and volume percentages for liquid-liquid mixing.
First aspect of the invention
The invention provides a preparation method of a degradable antibacterial non-woven fabric, which comprises the following steps:
mixing an antibacterial colloid and a filler, stirring, infiltrating the filler with the antibacterial colloid, performing ball milling on the obtained mixture, and drying to prepare antibacterial powder;
mixing the antibacterial powder, the polypropylene master batch and the polylactic acid master batch, stirring and granulating to prepare antibacterial master batch;
mixing the antibacterial master batches and polypropylene cellulose, and melt-blowing to prepare a degradable antibacterial non-woven fabric;
wherein the content of the first and second substances,
the antibacterial colloid comprises anthocyanin-modified nano-gold particles, the average particle size of the nano-gold particles is 3nm-5nm, the polydispersity index is 0.01-0.2, and the particle size of particles in a product obtained by ball milling is 50nm-300nm;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (10-50): (0.001-0.35);
the mass ratio of the antibacterial master batch to the polypropylene cellulose is 1: (45-55);
the granulation conditions include: the temperature is 135-255 ℃, and the pressure is 2.5kg/cm 2 -7.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 145-235 ℃, and the pressure is 3.5kg/cm 2 -8kg/cm 2 。
In the invention, the mass ratio of the polypropylene master batch, the polylactic acid master batch and the antibacterial powder is, for example, 100:10:0.001, 100:10:0.01, 100:10:0.1, 100:10:0.2, 100:10:0.3, 100:10:0.35, 100:20:0.001, 100:20:0.01, 100:20:0.1, 100:20:0.2, 100:20:0.3, 100:20:0.35, 100:50:0.001, 100:50:0.01, 100:50:0.1, 100:50:0.2, 100:50:0.3, 100:50:0.35.
in the invention, the mass ratio of the antibacterial master batch to the polypropylene cellulose is, for example, 1: 45. 1: 46. 1: 47. 1: 48. 1: 49. 1: 50. 1: 51. 1: 52. 1: 53. 1: 54. 1:55.
in the present invention, the temperature for granulation is, for example, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃, 190 ℃, 195 ℃, 200 ℃, 205 ℃, 210 ℃, 215 ℃, 220 ℃, 225 ℃, 230 ℃, 235 ℃, 240 ℃, 245 ℃, 250 ℃, 255 ℃. The pressure for granulation is, for example, 2.5kg/cm 2 、2.7kg/cm 2 、2.9kg/cm 2 、3.1kg/cm 2 、3.5kg/cm 2 、3.7kg/cm 2 、4.0kg/cm 2 、4.3kg/cm 2 、4.5kg/cm 2 、4.9kg/cm 2 、5.1kg/cm 2 、5.5kg/cm 2 、5.9kg/cm 2 、6.1kg/cm 2 、6.5kg/cm 2 、6.9kg/cm 2 、7.5kg/cm 2 。
In the present invention, the temperature of the melt blowing is, for example, 145 ℃, 150 ℃, 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃, 190 ℃, 195 ℃, 200 ℃, 205 ℃, 210 ℃, 215 ℃, 220 ℃, 225 ℃, 230 ℃ and 235 ℃. The pressure of the meltblowing is, for example, 3.5 kg-cm 2 、3.7kg/cm 2 、4.0kg/cm 2 、4.3kg/cm 2 、4.5kg/cm 2 、4.9kg/cm 2 、5.1kg/cm 2 、5.5kg/cm 2 、5.9kg/cm 2 、6.1kg/cm 2 、6.5kg/cm 2 、6.9kg/cm 2 、7.5kg/cm 2 、8kg/cm 2 。
In the present invention, the particle size of the filler is not particularly limited, and it is understood that a filler having an appropriate particle diameter may be selected for the convenience of the subsequent ball milling.
In some embodiments of the invention, the preparation method has one or more of the following technical features:
(1) The filler is selected from one or more of nano hydroxyapatite, montmorillonite and starch;
(2) One or more of zirconia balls and agate balls are adopted for ball milling;
(3) The viscosity average molecular weight of the polypropylene master batch is 9-14 ten thousand daltons (for example, 9 ten thousand, 10 ten thousand, 11 ten thousand, 12 ten thousand, 13 ten thousand and 14 ten thousand daltons);
(4) The viscosity-average molecular weight of the polylactic acid master batch is 14-18 ten thousand daltons (for example, 14 ten thousand, 15 ten thousand, 16 ten thousand, 17 ten thousand and 18 ten thousand daltons);
(5) The polypropylene cellulose has a viscosity average molecular weight of 10 to 30 million daltons (e.g., 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30 million daltons);
optionally, the filler is montmorillonite and starch;
the ball milling conditions include: zirconia balls are adopted;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (28-50): (0.001-0.3);
the granulation conditions include: the temperature is 140-240 ℃, and the pressure is 3kg/cm 2 -7kg/cm 2 ；
The conditions for melt blowing include: the temperature is 150-225 ℃, and the pressure is 4.5kg/cm 2 -7.5kg/cm 2 。
Preferably, the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-50): (0.005-0.15);
the granulation conditions include: the temperature is 210-220 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 210-220 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 。
Preferably, the preparation method has one or more of the technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (1-23): (1-20);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 15rpm-1200rpm,21 ℃ -85 ℃;
(3) The soaking time is 2-11 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.2-11);
(5) The rotation speed of the ball milling is 100rpm-850rpm, and the ball milling time is 0.3h-6.5h.
In the invention, the mass ratio of the antibacterial colloid, the montmorillonite and the starch is, for example, 1:1: 1. 1:1: 5. 1:1: 10. 1:1: 15. 1:1: 20. 1:10: 1. 1:10: 5. 1:10: 10. 1:10: 15. 1:10: 20. 1:23: 1. 1:23: 5. 1:23: 10. 1:23: 15. 1:23:20.
in the present invention, in the step of preparing the antibacterial powder, the rotation speed of stirring is, for example, 15rpm, 20rpm, 50rpm, 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, 450rpm, 500rpm, 550rpm, 600rpm, 650rpm, 700rpm, 750rpm, 800rpm, 850rpm, 900rpm, 950rpm, 1000rpm, 1050rpm, 1100rpm, 1150rpm, 1200rpm. The stirring temperature is, for example, 21 ℃, 25 ℃,30 ℃, 35 ℃,40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and 85 ℃.
In the present invention, the time for the impregnation is, for example, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, and 11 hours.
In the present invention, the rotation speed of the ball mill is, for example, 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, 450rpm, 500rpm, 550rpm, 600rpm, 650rpm, 700rpm, 750rpm, 800rpm, 850rpm. The ball milling time is, for example, 0.3h, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h.
Preferably, the preparation method has one or more of the technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (2.5-22): (1.5-15);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 150rpm-950rpm,26 ℃ -75 ℃;
(3) The soaking time is 3-10 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.3-9.5);
(5) The rotation speed of the ball milling is 120rpm-750rpm, and the ball milling time is 0.5h-5h.
Preferably, the preparation method has one or more of the technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (2.5-6): (1.5-4);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 200rpm-400rpm,27 ℃ -30 ℃;
(3) The soaking time is 4-6 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.5-5.5);
(5) The rotation speed of the ball milling is 250rpm-650rpm, and the ball milling time is 1h-4h.
Optionally, the filler is nano hydroxyapatite and starch;
the ball milling conditions include: adopting agate balls;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-45): (0.001-0.25);
the granulation conditions include: the temperature is 140-220 ℃, and the pressure is 3kg/cm 2 -6kg/cm 2 ；
The conditions for melt blowing include: the temperature is 150-210 DEG CAt a pressure of 4.5kg/cm 2 -6.5kg/cm 2 。
Preferably, the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-45): (0.008-0.25);
the granulation conditions include: the temperature is 205-210 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 205-210 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 。
Preferably, the preparation method has one or more of the following technical characteristics:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1-23): (1-20);
(2) In the step of preparing the antibacterial powder, the stirring conditions comprise: 15rpm-1200rpm,21 ℃ -85 ℃;
(3) The soaking time is 2-11 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.2-11);
(5) The rotation speed of the ball milling is 100rpm-850rpm, and the ball milling time is 0.3h-6.5h.
In the invention, the mass ratio of the antibacterial colloid, the montmorillonite and the starch is, for example, 1:1: 1. 1:1: 5. 1:1: 10. 1:1: 15. 1:1: 20. 1:10: 1. 1:10: 5. 1:10: 10. 1:10: 15. 1:10: 20. 1:23: 1. 1:23: 5. 1:23: 10. 1:23: 15. 1:23:20.
in the step of preparing the antibacterial powder in the present invention, the rotation speed of stirring is, for example, 15rpm, 20rpm, 50rpm, 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, 450rpm, 500rpm, 550rpm, 600rpm, 650rpm, 700rpm, 750rpm, 800rpm, 850rpm, 900rpm, 950rpm, 1000rpm, 1050rpm, 1100rpm, 1150rpm, 1200rpm. The stirring temperature is, for example, 21 ℃, 25 ℃,30 ℃, 35 ℃,40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and 85 ℃.
In the present invention, the time for the impregnation is, for example, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h, 10h, and 11h.
In the present invention, the rotation speed of the ball mill is, for example, 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, 450rpm, 500rpm, 550rpm, 600rpm, 650rpm, 700rpm, 750rpm, 800rpm, 850rpm. The ball milling time is, for example, 0.3h, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h.
Preferably, the preparation method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1-20): (1-15);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 150rpm-800rpm,26 ℃ -70 ℃;
(3) The soaking time is 4-9 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.35-9);
(5) The rotation speed of the ball milling is 200rpm-650rpm, and the ball milling time is 1h-6h.
Preferably, the preparation method has one or more of the following technical characteristics:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1.75-3.5): (1.2-2.5);
(2) In the step of preparing the antibacterial powder, the stirring conditions comprise: 200rpm-450rpm,30 ℃ -35 ℃;
(3) The soaking time is 5-8 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (2-4);
(5) The rotation speed of the ball milling is 200rpm-350rpm, and the ball milling time is 2h-4h.
In the invention, the preparation method of the antibacterial colloid comprises the following steps:
mixing a chloroauric acid solution with a first reducing agent solution, and carrying out reduction reaction to prepare a first product;
mixing the first product with an organic solvent to prepare a second product;
mixing the second product with a surfactant to produce a third product;
mixing the third product with a second reducing agent to produce a fourth product;
and mixing the fourth product with anthocyanin, and carrying out chelation reaction to prepare the antibacterial colloid containing anthocyanin.
Optionally, the preparation method has one or more of the following technical features:
(1) The first reducing agent and the second reducing agent are independently selected from one or more of sodium citrate, ascorbic acid and sodium borohydride;
(2) The amount of the second reducing agent is 17-27% (w/v) of the volume of the second product.
In the present invention, the amount of the second reducing agent is, for example, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27% (w/v) of the volume of the second product.
Alternatively, the conditions of the chelation reaction include: the temperature is 10-42 ℃, the time is 3-9 h, and the rotating speed is 200-600 rpm.
In the present invention, the temperature of the chelation reaction is, for example, 10 ℃, 11 ℃, 12 ℃, 13 ℃, 14 ℃, 15 ℃, 16 ℃, 17 ℃, 18 ℃, 19 ℃, 20 ℃,21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃,26 ℃,27 ℃, 28 ℃, 29 ℃,30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃,40 ℃, 41 ℃ and 42 ℃. The time of the chelation reaction is, for example, 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours, 5.5 hours, 6 hours, 6.5 hours, 7 hours, 7.5 hours, 8 hours, 8.5 hours, 9 hours. The rotational speed of the chelation reaction is, for example, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, 450rpm, 500rpm, 550rpm, 600rpm.
Optionally, the anthocyanins are used in an amount of 0.05-0.5% (w/v) of the third product, e.g. 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%.
Optionally, the anthocyanins are selected from one or more of pelargonidin, delphinidin and pelargonidin.
Optionally, the preparation method has one or more of the following technical features:
(1) The mass concentration of the chloroauric acid in the chloroauric acid solution is 4.5-23 wt%;
(2) The mass concentration of the first reducing agent in the first reducing agent solution is 11.3-39.5 wt%;
(3) The volume ratio of the chloroauric acid solution to the first reducing agent solution is 1: (2-14);
(4) The first reducing agent is selected from one or more of sodium citrate, ascorbic acid and sodium borohydride.
In the present invention, the mass concentration of chloroauric acid in the chloroauric acid solution is 4.5wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12wt%, 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt%, 20wt%, 21wt%, 22wt%, 23wt%. The mass concentration of the first reducing agent in the first reducing agent solution is, for example, 11.3wt%, 12wt%, 13wt%, 14wt%, 15wt%, 18wt%, 20wt%, 22wt%, 24wt%, 26wt%, 28wt%, 30wt%, 32wt%, 34wt%, 36wt%, 38wt%, 39.5wt%. The volume ratio of the chloroauric acid solution to the first reducing agent solution is, for example, 1: 2. 1: 3. 1: 4. 1: 5. 1: 6. 1: 7. 1: 8. 1: 9. 1: 10. 1: 11. 1: 12. 1: 13. 1:14.
optionally, the preparation method has one or more of the following technical features:
(1) The organic solvent is selected from one or more of ethanol, glycerol and glycol;
(2) The amount of the organic solvent is 8% to 23% (v/v) of the volume of the first product.
In the present invention, the organic solvent is used in an amount of, for example, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23% by volume of the first product.
Optionally, the preparation method has one or more of the following technical features:
(1) The surfactant is one or more of a cationic surfactant and a nonionic surfactant;
(2) The amount of said surfactant is 0.08% to 1.2% (v/v) by volume of said second product.
In the present invention, the amount of the surfactant is 0.08%, 0.09%, 0.1%, 0.15%, 1.2% (v/v) of the volume of the second product.
Optionally, the preparation method has one or more of the following technical features:
(1) The cationic surfactant is selected from one or more of cetyl dimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl dimethyl amine oxide, cetyl trimethyl ammonium bromide, cationic panthenol, octadecyl trimethyl ammonium chloride and cationic guar gum;
(2) The nonionic surfactant is selected from one or more of fatty acid glyceride, sucrose fatty acid ester, sorbitan fatty acid, polyoxyethylene fatty acid ester and polyoxyethylene fatty alcohol ether.
Optionally, in the antibacterial colloid, the anthocyanin-modified gold nanoparticles have an average particle size of 3nm to 5nm (e.g., 3nm, 3.1nm, 3.2nm, 3.3nm, 3.4nm, 3.5nm, 3.6nm, 3.7nm, 3.8nm, 3.9nm, 4nm, 4.1nm, 4.2nm, 4.3nm, 4.4nm, 4.5nm, 4.6nm, 4.7nm, 4.8nm, 4.9nm, 5 nm), and a polydispersity index of 0.01 to 0.2.
Second aspect of the invention
The invention provides a degradable antibacterial non-woven fabric which is prepared by the preparation method provided by the first aspect.
In the following specific examples, the measurement parameters relating to the components of the raw materials, if not specified otherwise, may be subject to slight deviations within the accuracy of the weighing. Temperature and time parameters are involved to allow for acceptable deviation due to instrument test accuracy or operational accuracy.
Example 1
The embodiment provides an antibacterial colloid and a preparation method thereof, and the preparation method comprises the following steps:
s1, mixing a chloroauric acid solution with 16wt% and a sodium borohydride solution with 25wt% to obtain a first product;
s2, continuously adding 15% (v/v) of ethylene glycol into the first product to obtain a second product;
s3, adding a cationic surfactant cetyl trimethyl ammonium bromide (cetyl trimethyl ammonium bromide) with the volume of 0.6% (v/v) of that of the second product into the second product to obtain a third product;
s4, adding sodium citrate with the volume of 21.4% (w/v) of the second product into the third product to obtain a fourth product;
s5, adding grape skin red pigment with the volume of 0.8% (w/v) of that of the third product into the fourth product, and reacting to obtain an antibacterial colloid;
wherein the reaction temperature is 25 ℃, the reaction time is 5h,400rpm, and finally the antibacterial colloid containing the anthocyanin modified nano-gold particles (shown in figure 1) is obtained.
Example 2
The embodiment provides a degradable antibacterial non-woven fabric and a preparation process thereof, and the preparation process comprises the following steps:
s1: the antibacterial colloid prepared in example 1 above was added to montmorillonite and starch, wherein one antibacterial colloid: montmorillonite: the starch is 1:4:2 (mass ratio), wherein the stirring speed is 200rpm, the stirring temperature is 27 ℃, the soaking time is 4 hours, the stirring is uniform, and the soaking is carried out to obtain a mixture A;
s2: ball-milling the mixture A in the step S1 by using a wet ball-milling process, wherein the ball-milling conditions comprise that: ball milling with zirconia beads, mixture a: zirconia beads are 1:1 (mass ratio), the ball milling time is 1h, the ball milling speed is 200rpm, a mixture B containing particles with uniform size and particle size of 50nm-300nm is obtained, and the mixture B is dried to obtain antibacterial powder C.
S3: and (3) uniformly mixing the antibacterial powder C in the S2 with polypropylene (12W daltons) and polylactic acid particles (15W daltons), and stirring, wherein the weight ratio of polypropylene: polylactic acid: the antibacterial powder C is 100:35:0.005 (mass ratio), stirring speed of 200rpm, temperature of 28 deg.C, adding into a granulator to obtain antibacterial mother granule D, wherein the granulator has process parameters of 220 deg.C and 5Kg/cm 2 ；
S4: adding the antibacterial master batch D in the S3 into a common polypropylene fiber (18W daltons), and adding into a melt-blowing machine, wherein the antibacterial master batch D: the polypropylene fiber is 1:50 The technological parameters of the melt-blowing machine are 210 ℃ and 5Kg/cm < 2>, and the degradable antibacterial non-woven fabric is formed by melt-blowing, natural cooling, cutting and rolling.
Example 3
The embodiment provides a degradable antibacterial non-woven fabric and a preparation process thereof, and the preparation process comprises the following steps:
s1: the antibacterial colloid prepared in example 1 above was added to montmorillonite and starch, wherein the antibacterial colloid: montmorillonite: the starch is 2:6:3 (mass ratio), the stirring speed is 250rpm, the stirring temperature is 30 ℃, the soaking time is 5 hours, the stirring is uniform, and the soaking is carried out to obtain a mixture A;
s2: ball-milling the mixture A in the S1 by using a wet ball-milling process, wherein the ball-milling conditions comprise that: ball milling with zirconia beads, mixture a: zirconia beads were 1:2 (mass ratio), the ball milling time is 1.5h, the ball milling speed is 250rpm, a mixture B containing particles with uniform size and particle size of 50nm-300nm is obtained, and the mixture B is dried to obtain the antibacterial powder C.
S3: and (3) uniformly mixing the antibacterial powder in the S2 with polypropylene (12W daltons) and polylactic acid particles (15W daltons), and stirring, wherein the weight ratio of polypropylene: polylactic acid: the antibacterial powder C is 100:40:0.008 (mass ratio), stirring speed of 250rpm, temperature of 30 deg.C, adding into a granulator to prepare antibacterial masterbatch D, wherein the granulator has process parameters of 210 deg.C and 5Kg/cm 2 ；
S4: adding the antibacterial master batch D in the S3 into a polypropylene fiber (18W daltons), and adding into a melt-blowing machine, wherein the weight ratio of the antibacterial master batch D: the polypropylene fiber is 1:50 (mass ratio), the technological parameters of the melt-blowing machine are 220 ℃ and 5Kg/cm 2 The degradable antibacterial non-woven fabric is formed by melt-blowing, natural cooling, cutting and rolling.
Example 4
The embodiment provides a degradable antibacterial non-woven fabric and a preparation process thereof, and the preparation process comprises the following steps:
s1: the antibacterial colloid prepared in the above example 1 was added to nano hydroxyapatite and starch, wherein the antibacterial colloid: nano hydroxyapatite with starch of 3:6:4 (mass ratio), wherein the stirring speed is 200rpm, the stirring temperature is 30 ℃, the soaking time is 5 hours, the stirring is uniform, and the soaking is carried out to obtain a mixture A;
s2: ball-milling the mixture A in the S1 by using a wet ball-milling process, wherein the ball-milling conditions comprise that: ball milling with agate beads, mixture a: agate beads are 1:2 (mass ratio), the ball milling time is 2h, the ball milling rotating speed is 250rpm, a mixture B containing particles with uniform size and particle diameter between 50nm and 300nm is obtained, and the mixture B is dried to obtain the antibacterial powder C.
S3: and (3) uniformly mixing the antibacterial powder C in the S2 with polypropylene (12W daltons) and polylactic acid particles (15W daltons), and stirring, wherein the weight ratio of polypropylene: polylactic acid: the antibacterial powder C is 100:40:0.015 stirring speed of 300rpm, temperature of 30 ℃, adding granulating agent to prepare the antibacterial master batch D, wherein the technological parameters of the granulating agent are 210 ℃ and 5Kg/cm 2 ；
S4: adding the antibacterial master batch D in the S3 into a common polypropylene fiber (18W Dalton) and adding into a melt-blowing machine, wherein the antibacterial master batch D: the polypropylene fiber is 1:50 The process parameters of the melt-blowing machine are 205 ℃ and 5Kg/cm 2 The degradable antibacterial non-woven fabric is formed by melt-blowing, natural cooling, cutting and rolling.
Example 5
The embodiment provides a degradable antibacterial non-woven fabric and a preparation process thereof, and the preparation process comprises the following steps:
s1: the antibacterial colloid prepared in the above example 1 was added to nano hydroxyapatite and starch, wherein the antibacterial colloid: nano hydroxyapatite with starch of 4:7:5 (mass ratio), wherein the stirring speed is 300rpm, the stirring temperature is 35 ℃, the soaking time is 8 hours, the stirring is uniform, and the soaking is carried out to obtain a mixture A;
s2: ball-milling the mixture A in the S1 by using a wet ball-milling process, wherein the ball-milling conditions comprise that: ball milling with agate beads, mixture a: agate beads are 1:3 (mass ratio), the ball milling time is 3h, the ball milling rotating speed is 300rpm, a mixture B containing particles with uniform size and particle diameter between 50nm and 300nm is obtained, and the mixture B is dried to obtain the antibacterial powder C.
S3: and (3) uniformly mixing the antibacterial powder C in the S2 with polypropylene (12W daltons) and polylactic acid particles (15W daltons), and stirring, wherein the weight ratio of polypropylene: polylactic acid: the antibacterial powder C is 100:40:0.02 stirring at 350rpm and 32 deg.C, adding into a granulator to prepare antibacterial masterbatch D, wherein the granulator has process parameters of 210 deg.C and 5Kg/cm 2 ；
S4: adding the antibacterial master batch D in the S3 into a common polypropylene fiber (18W) and adding the mixture into a melt-blowing machine, wherein the antibacterial master batch D: the polypropylene fiber is 1:50 (mass ratio), the process parameter of the melt-blowing machine is 205 ℃, and 5Kg/cm 2 The degradable antibacterial non-woven fabric is formed by melt-blowing, natural cooling, cutting and rolling.
Example 6
This embodiment is a modification of embodiment 4, and includes, in relation to the modification of embodiment 4:
in the step S1:
1. the mass ratio of the antibacterial colloid to the nano hydroxyapatite to the starch is 1:1:20;
2. in the step of preparing the antibacterial powder, the stirring conditions include: 15rpm,85 ℃;
3. the soaking time is 2h.
In the step S2:
1. the mass ratio of the mixture A to the zirconia balls is 1:0.2;
2. the rotation speed of the ball milling is 100rpm, and the ball milling time is 6.5h.
In the step S3:
1. the mass ratio of the polypropylene (12W), the polylactic acid particles (15W) and the antibacterial powder is 100:30:0.001;
2. the granulation conditions include: the temperature was 140 ℃ and the pressure was 3kg/cm 2 ；
3. The conditions for melt blowing include: the temperature is 150 ℃ and the pressure is 4.5kg/cm 2 。
The rest is the same as example 4.
Example 7
This embodiment is a modification of embodiment 4, and includes, in relation to the modification of embodiment 4:
in the step S1:
1. the mass ratio of the antibacterial colloid to the nano hydroxyapatite to the starch is 1:23:1;
2. in the step of preparing the antibacterial powder, the stirring conditions include: 1200rpm,21 ℃;
3. the soaking time was 11h.
In the step S2:
1. the mass ratio of the mixture A to the zirconia balls is 1:11;
2. the rotation speed of the ball milling is 850rpm, and the ball milling time is 0.3h.
In the step S3:
1. the mass ratio of the polypropylene (12W), the polylactic acid particles (15W) and the antibacterial powder is 100:45:0.25;
2. the granulation conditions include: the temperature is 220 ℃ and the pressure is 6kg/cm 2 ；
3. Conditions for melt blowing include: the temperature was 210 ℃ and the pressure was 6.5kg/cm 2 。
The rest is the same as example 4.
Example 8
This embodiment is a modification of embodiment 2, and includes, in relation to the modification of embodiment 2:
in the step S1:
1. the mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1:23:1;
2. in the step of preparing the antibacterial powder, the stirring conditions include: 15rpm,21 ℃;
3. the soaking time is 2h.
In the step S2:
1. the mass ratio of the mixture A to the zirconia balls is 1:0.2;
2. the rotation speed of the ball milling is 100rpm, and the ball milling time is 0.3h.
In the step S3:
1. the mass ratio of the polypropylene (12W), the polylactic acid particles (15W) and the antibacterial powder is 100:28:0.3;
2. the granulation conditions include: the temperature is 140 ℃ and the pressure is 3kg/cm 2 ；
3. Melt blownThe conditions of (a) include: the temperature is 150 ℃ and the pressure is 4.5kg/cm 2 。
The rest is the same as example 2.
Example 9
This embodiment is a modification of embodiment 2, and includes, in relation to the modification of embodiment 2:
in the step S1:
1. the mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1:1:20;
2. in the step of preparing the antibacterial powder, the stirring conditions comprise: 1200rpm,85 ℃;
3. the soaking time is 11h.
In the step S2:
1. the mass ratio of the mixture A to the zirconia balls is 1:11;
2. the rotation speed of the ball milling is 850rpm, and the ball milling time is 6.5h.
In the step S3:
1. the mass ratio of the polypropylene (12W), the polylactic acid particles (15W) and the antibacterial powder is 100:50:0.001;
2. the granulation conditions include: the temperature is 240 ℃ and the pressure is 7kg/cm 2 ；
3. Conditions for melt blowing include: the temperature is 225 ℃ and the pressure is 7.5kg/cm 2 。
The rest is the same as example 2.
Comparative example 1
The comparative example provides a non-woven fabric and a preparation method thereof, comprising the following steps:
s1: the polypropylene fiber (18W) is added into a melt-blown machine, and the technological parameter of the melt-blown machine is preferably 205 ℃ and 5Kg/cm 2 Melt-blowing, natural cooling, cutting and rolling to obtain non-woven fabric.
Comparative example 2 (example 4 is comparative example)
The comparative example provides a non-woven fabric and a preparation process thereof, and the preparation process comprises the following steps:
s1: adding deionized water into the nano hydroxyapatite, wherein the weight ratio of deionized water: starch of the nano hydroxyapatite is 3:6:4 (mass ratio), wherein the stirring speed is 200rpm, the stirring temperature is 30 ℃, the soaking time is 5 hours, the stirring is uniform, and the soaking is carried out to obtain a mixture A';
s2: ball-milling the mixture A' in the S1 by using a wet ball-milling process, wherein the ball-milling conditions comprise that: ball milling with agate beads, mixture a': agate beads are 1:2 (mass ratio), the ball milling time is 2h, the ball milling rotating speed is 250rpm, a mixture B 'containing particles with uniform size and the particle diameter of 50nm-300nm is obtained, and the mixture B' is dried to obtain the powder C.
S3: and (3) uniformly mixing the powder C in the S2 with polypropylene (12W) and polylactic acid particles (15W), and stirring, wherein the weight ratio of polypropylene: polylactic acid: the powder C is 100:40:0.015 stirring speed of 300rpm, temperature of 30 ℃, adding a granulator to prepare master batch D', wherein the technological parameters of the granulator are 210 ℃ and 5Kg/cm 2 ；
S4: adding the master batch D 'in the S3 into the common polypropylene fiber (18W) according to a certain proportion, and adding the mixture into a melt-blowing machine, wherein the master batch D': the polypropylene fiber is 1:50 The process parameters of the melt-blowing machine are 205 ℃ and 5Kg/cm 2 The non-woven fabric is prepared by melt-blowing, natural cooling, cutting and rolling.
Comparative example 3
This comparative example is that of example 2, the main differences with respect to example 2 including the different conditions of granulation, in particular:
the granulation conditions include: the temperature is 260 ℃ and the pressure is 9kg/cm 2 。
Comparative example 4
This comparative example is that of example 2, the main differences with respect to example 2 including the different conditions of melt blowing, specifically:
conditions for melt blowing include: the temperature is 240 ℃ and the pressure is 3kg/cm 2 。
Comparative example 5
The comparative example is the comparative example of example 2, and the main differences relative to example 2 include different proportions of polypropylene master batch, polylactic acid master batch and antibacterial powder, specifically: the mass ratio of the polypropylene (12W), the polylactic acid particles (15W) and the antibacterial powder is 100:55:21.
comparative example 6
The comparative example is the comparative example of example 2, and the main differences relative to example 2 include the different mixture ratio of the antibacterial master batch and the polypropylene fiber (18W), specifically: the mass ratio of the antibacterial master batch to the polypropylene cellulose is 1:99.
1. detection of antibacterial Properties
At present, the antibacterial performance of the non-woven fabric is evaluated by referring to a method specified in national recommended standard WS/T650-2019 & ltantibacterial and bacteriostatic effect evaluation method & gt, and staphylococcus aureus and escherichia coli are used as index bacteria. If the bacteriostatic rate is not less than 50% -90%, judging that the bacteriostatic action is available; if the bacteriostatic rate is not less than 90%, the antibacterial effect is judged to be strong.
(one) test strains: staphylococcus aureus ATCC6538, escherichia coli 8099.
(II) a test step:
s1, taking fresh slant culture for 24h in each experiment, washing with PBS, and diluting with PBS about 1.0X 10 5 CFU/mL～1.0×10 6 CFU/mL, preparing into bacterial suspension for later use;
s2, sample treatment: the sample and the reference sample are respectively cut into sample pieces of 20mm × 20mm under aseptic conditions by using a sterilizing scissors for standby, and the control sample (the sample which is the same material as the sample but does not contain the bacteriostatic component) is sterilized in a steam sterilizing pot at (121 + -2) DEG C for 15min or more before being infected with bacteria.
S3, test sample group: taking a sterile plate, taking 2 test pieces by using sterile tweezers, not overlapping, putting the test pieces in a water bath at 20 +/-1 ℃ for 5min, dropwise adding 0.1mL of test bacterial suspension on each sample piece, immediately counting, respectively clamping and taking a bacterial staining sample piece and adding 5.0mL of PBS test tube after 1h, uniformly mixing, shaking and eluting, respectively absorbing 1.0mL of sample liquid, determining the number of surviving bacteria according to a viable bacteria culture counting method, and inoculating 2 plates in each tube of sample liquid. If the number of colonies growing on the plate is large, viable bacteria culture counting can be carried out after 10 times of serial dilution;
s4: positive control: the sample is replaced by 2 reference samples, and the operation is the same as S3, the recovered bacteria amount is 1.0
10 4 CFU/mL～9.0×10 4 CFU/sheet;
s5: negative control: dropwise adding 0.1mL of bacterial suspension into the PBS and the culture medium in the same batch;
s6: culturing: all test samples, positive control samples and negative control samples are cultured at the temperature of (36 +/-1) DEG C, bacterial propagules are cultured for 48h, the test is repeated for 3 times, and the average bacteriostasis rate is calculated.
TABLE 1
(III) test results:
as can be seen from table 1, in examples 1 to 4, the addition of one of the anthocyanin-nanogold antibacterial powders resulted in the production of the anthocyanin-nanogold antibacterial nonwoven fabrics having an inhibitory (antibacterial) rate of 90% or more against escherichia coli and staphylococcus aureus. In contrast, in comparative example 1, no anthocyanin-nanogold antibacterial powder is added, and the non-woven fabric is prepared by using the common polypropylene and adopting the same process and conditions, so that the antibacterial rate is not greater than or equal to 50%, and the non-woven fabric has no (antibacterial) effect. In examples 6 to 9, the addition of the auxiliary materials was excessive, and the prepared antibacterial powders were diluted to a concentration equivalent to that in examples 1 to 4, so that in example 7, the effect of loading the nano-hydroxyapatite was better than that of starch in examples 6 to 9, but the degradability of the starch was better than that of the nano-hydroxyapatite. Comparative example 5 has very good antibacterial property due to the addition of a large amount of antibacterial powder, and comparative example 6 has no antibacterial property due to the addition of a very small amount of antibacterial mother particles. Therefore, in order to obtain the anthocyanin-nano gold antibacterial non-woven fabric, a certain amount of anthocyanin-nano gold antibacterial powder is required to be added.
2. Experimental testing of biodegradability
The degradation rate of the film is tested by reference to biodegradable plastic test standard JISK 6950-94:
(1) Taking from natural soil: loose farmland, pH value of 6-8, humidity more than 80%,30Kg for standby;
(2) Samples of 5cm × 5cm (3 pieces per sample, mass m) prepared for sample example 2, example 3, example 4, example 5, comparative example 1, comparative example 2 were sampled 0 ) Respectively placing the samples in 50cm multiplied by 50cm soil pits under the same room temperature environment, wherein the distance between the samples and the soil is 5cm;
(3) The experiment was carried out in the open air for 3 months;
(4) After 3 months, the mixture is taken out, washed by water and absolute ethyl alcohol, dried and weighed (m) 1 ) And calculating an average value: soil burying biodegradation rate (%) = [ (m) 0 -m 1 )/m 0 ]×100％。
TABLE 2
| m0(g) | m1(g) | Biodegradation Rate (%) for soil burying | |
| Example 2 | 10.0 | 7.84 | 21.6％ |
| Example 3 | 10.0 | 7.25 | 27.5％ |
| Example 4 | 10.0 | 6.54 | 34.6％ |
| Example 5 | 10.0 | 5.21 | 47.9％ |
| Example 6 | 10.0 | 7.46 | 25.4％ |
| Example 7 | 10.0 | 4.76 | 52.4％ |
| Example 8 | 10.0 | 8.24 | 17.6％ |
| Example 9 | 10.0 | 4.28 | 57.2％ |
| Comparative example 1 | 10.0 | 9.32 | 6.8％ |
| Comparative example 2 | 10.0 | 6.78 | 32.2％ |
| Comparative example 3 | / | / | / |
| Comparative example 4 | / | / | / |
| Comparative example 5 | 10.0 | 2.77 | 72.3％ |
| Comparative example 6 | 10.0 | 8.67 | 13.3％ |
From the above-mentioned criteria, comparative degradability 5> 9> 7> 5> 4 ≈ 2> 3> 6> 2> 8> 6> 1, the most degradability of 5 is found, the degradation rate reaches 72.3% in 3 months, mainly because more than half of polylactic acid and a large amount of submicron inorganic nanoparticles are added for filling, under the action of microorganism, the inorganic ions uniformly dispersed in the polymer can assist the microorganism to rapidly decompose the non-woven fabric, therefore, the more inorganic submicron particles are added to the polymer, the faster the degradation speed is; the more polylactic acid is added to the nonwoven fabric, the faster the degradation rate is. Therefore, the degradation speed of the example 4 is similar to that of the comparative example 2 due to the addition of the inorganic nanoparticles and the amount of the polylactic acid. On the premise of not influencing the mechanical properties of the non-woven fabric, the properties of the non-woven fabric are modified, and experimental data results show that the polypropylene non-woven fabric without any additive is difficult to degrade, and the non-woven fabric prepared finally has better degradability as the addition amount of the inorganic nanoparticles is increased and the addition proportion of polylactic acid in the polymer is increased. Compared with the comparative examples in examples 1 to 4, the anthocyanin-nanogold antibacterial non-woven fabric prepared by the invention not only has good antibacterial property, but also has good degradability, and is a sustainable and environment-friendly material.
Test results of nonwoven fabrics:
TABLE 3 mechanical Property test results of the nonwoven fabrics prepared in each example and each comparative example
Remarking: the specification of the test sample is 30g/m 2 (ii) a "standard": test method for nonwoven fabrics GB/T-24218.3-2010.
And (4) analyzing results: the observation of experimental result data shows that the anti-fracture capability of the prepared anthocyanin-nanogold antibacterial non-woven fabric is that the anti-fracture capability is shown in example 9> example 7> example 6> example 3> example 4 ≈ comparative example 2> example 5> example 2> example 8> comparative example 6> comparative example 1> comparative example 5, the anti-fracture capability of the non-woven fabric prepared by the polypropylene fiber without polylactic acid and antibacterial agent is obviously lower than that of the non-woven fabrics prepared by the polypropylene fibers with polylactic acid and the non-woven fabrics prepared by the polypropylene fibers with polylactic acid, and the anti-fracture capability of the non-woven fabric prepared by the anthocyanin-nanogold antibacterial non-woven fabrics is obviously lower than that of the non-woven fabrics prepared by the polypropylene fibers with polylactic acid and the antibacterial agent, namely the non-woven fabrics prepared by the polypropylene fibers with polylactic acid, namely the non-woven fabrics prepared by the anthocyanin-woven fabrics prepared by the polylactic acid and the nano-woven fabrics prepared by the polypropylene fibers with the polylactic acid is obviously lower than that of the non-woven fabrics prepared by the polypropylene fibers with the polylactic acid and the polylactic acid, namely the non-woven fabrics prepared by the polypropylene fibers with the non-woven fabrics with the polylactic acid, and the comparative examples 2 and the comparative example 1. Secondly, with the increase of the adding proportion of the polylactic acid, the fracture resistance of the finally prepared non-woven fabric is stronger, for example, the fracture resistance of example 9 is obviously better than that of example 7, and the fracture resistance of example 7 is obviously better than that of examples 2-6. Furthermore, the fracture resistance of the original non-woven fabric is reduced with the increase of the addition ratio of the inorganic antibacterial agent, as in examples 3-6, when the addition ratio of the polylactic acid is the same, the fracture resistance of the prepared non-woven fabric is reduced with the increase of the addition amount of the antibacterial powder, as in example 6 < example 3 < example 4 < example 5, and the fracture resistance is example 6> example 3> example 4 ≈ comparative example 2> example 5. Comparative example 5 although the fracture resistance was significantly enhanced by adding an excessive amount of polylactic acid, the original mechanical properties were significantly deteriorated due to the addition of a large amount of the antibiotic powder additive. Therefore, the formula proportion among polylactic acid, polypropylene and anthocyanin-nanogold antibacterial powder is critical to prepare the antibacterial non-woven fabric with good anti-fracture capability and continuous and effective antibacterial performance.
In conclusion, the invention provides the anthocyanin-nanogold antibacterial non-woven fabric with strong antibacterial property. The anthocyanin-nanogold antibacterial colloidal solution with high safety is prepared into anthocyanin-nanogold antibacterial powder with uniform size and controllable particle size through a special ball milling process, then the anthocyanin-nanogold antibacterial powder is uniformly mixed with polypropylene fibers and polylactic acid in a certain proportion, and an antibacterial non-woven fabric is prepared through an injection molding machine and a melt-blown injection molding machine. The anthocyanin-nanogold antibacterial material with strong antibacterial property is independently developed, no toxic reagent is involved in the preparation process, the main antibacterial mechanism realizes the antibacterial (bacteriostasis) action of multiple mechanisms on bacteria through the large specific surface area of nanogold particles, and thus the drug resistance is not easy to generate. The first problem in processing the anthocyanin-nanogold antibacterial colloidal solution into powder is how to ensure that nanogold is not agglomerated, so that anthocyanin-nanogold particles are loaded on materials with porous structures, such as nano hydroxyapatite or montmorillonite, so that the anthocyanin-nanogold particles have good release degree. Therefore, the finally prepared anthocyanin-nanogold antibacterial non-woven fabric has good antibacterial property and degradability, and simultaneously has good antibacterial stability and biological safety, and can be widely applied to the fields of protective clothing, masks, mattresses, baby diapers and the like which need antibacterial non-woven fabric raw materials.
The technical features of the embodiments and examples described above can be combined in any suitable manner, and for the sake of brevity, all possible combinations of the technical features of the embodiments and examples described above are not described, but should be considered within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, so as to understand the technical solutions of the present invention specifically and in detail, but not to be understood as the limitation of the protection scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Furthermore, it should be understood that after reading the above teachings of the present invention, various changes or modifications may be made to the invention by those skilled in the art, and equivalents may be obtained and still fall within the scope of the present application. It should also be understood that the technical solutions provided by the present invention, which are obtained by logical analysis, reasoning or limited experiments, are within the scope of the present invention as set forth in the appended claims. Therefore, the protection scope of the present patent shall be subject to the content of the appended claims, and the description and drawings can be used to explain the content of the claims.
Claims (13)
1. A preparation method of degradable antibacterial non-woven fabric is characterized by comprising the following steps:
mixing antibacterial colloid and a filler, stirring, infiltrating the filler with the antibacterial colloid, and performing ball milling and drying on the obtained mixture to prepare antibacterial powder;
mixing the antibacterial powder, the polypropylene master batch and the polylactic acid master batch, stirring and granulating to prepare antibacterial master batch;
mixing the antibacterial master batches and polypropylene cellulose, and melt-blowing to prepare degradable antibacterial non-woven fabric;
wherein the content of the first and second substances,
the antibacterial colloid comprises anthocyanin-modified nano-gold particles, the average particle size of the nano-gold particles is 3-5 nm, the polydispersity index is 0.01-0.2, and the particle size of particles in a product obtained by ball milling is 50-300 nm;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (10-50): (0.001-0.35);
the mass ratio of the antibacterial master batch to the polypropylene cellulose is 1: (45-55);
the granulation conditions include: the temperature is 135-255 ℃, and the pressure is 2.5kg/cm 2 -7.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 145-235 ℃, and the pressure is 3.5kg/cm 2 -8kg/cm 2 。
2. The method for preparing a degradable antimicrobial nonwoven according to claim 1, characterized in that it has one or more of the following technical features:
(1) The filler is selected from one or more of nano hydroxyapatite, montmorillonite and starch;
(2) One or more of zirconia balls and agate balls are adopted for ball milling;
(3) The viscosity average molecular weight of the polypropylene master batch is 9-14 ten thousand daltons;
(4) The viscosity average molecular weight of the polylactic acid master batch is 14-18 ten thousand daltons; and the combination of (a) and (b),
(5) The viscosity average molecular weight of the polypropylene cellulose is 10-30 ten thousand daltons.
3. The method for preparing degradable antibacterial non-woven fabric according to claim 1 or 2,
the filler is montmorillonite and starch;
the ball milling conditions include: zirconium oxide balls are adopted;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (28-50): (0.001-0.3);
the granulation conditions include: the temperature is 140-240 ℃, and the pressure is 3kg/cm 2 -7kg/cm 2 ；
Conditions for melt blowing include: the temperature is 150-225 ℃, and the pressure is 4.5kg/cm 2 -7.5kg/cm 2 。
4. The method for preparing degradable antibacterial non-woven fabric according to claim 3,
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-50): (0.005-0.15);
the granulation conditions include: the temperature is 210-220 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 210-220 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 。
5. The method for preparing a degradable antimicrobial nonwoven according to claim 3, characterized in that it has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (1-23): (1-20);
(2) In the step of preparing the antibacterial powder, the stirring conditions comprise: 15rpm-1200rpm,21 ℃ -85 ℃;
(3) The soaking time is 2-11 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.2-11); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 100rpm-850rpm, and the ball milling time is 0.3h-6.5h.
6. The method for preparing a degradable antimicrobial nonwoven fabric according to claim 5, characterized in that the method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (2.5-22): (1.5-15);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 150rpm-950rpm,26 ℃ -75 ℃;
(3) The soaking time is 3-10 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.3-9.5); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 120rpm-750rpm, and the ball milling time is 0.5h-5h.
7. The method for preparing a degradable antimicrobial nonwoven according to any of claims 4 to 6, characterized in that it has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the montmorillonite to the starch is 1: (2.5-6): (1.5-4);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 200rpm-400rpm,27 ℃ -30 ℃;
(3) The soaking time is 4-6 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.5-5.5); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 250rpm-650rpm, and the ball milling time is 1h-4h.
8. The method for preparing degradable antibacterial non-woven fabric according to claim 1 or 2,
the filler is nano hydroxyapatite and starch;
the ball milling conditions include: agate balls are adopted;
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-45): (0.001-0.25);
the granulation conditions include: the temperature is 140-220 ℃, and the pressure is 3kg/cm 2 -6kg/cm 2 ；
Conditions for melt blowing include: the temperature is 150-210 ℃, and the pressure is 4.5kg/cm 2 -6.5kg/cm 2 。
9. The method for preparing degradable antibacterial nonwoven fabric according to claim 8,
the mass ratio of the polypropylene master batch to the polylactic acid master batch to the antibacterial powder is 100: (30-45): (0.008-0.25);
the granulation conditions include: the temperature is 205-210 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 ；
Conditions for melt blowing include: the temperature is 205-210 ℃, and the pressure is 4.5kg/cm 2 -5.5kg/cm 2 。
10. The method for preparing degradable antibacterial non-woven fabric according to claim 8, wherein the method has one or more of the following technical characteristics:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1-23): (1-20);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 15rpm-1200rpm,21 ℃ -85 ℃;
(3) The soaking time is 2-11 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.2-11); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 100rpm-850rpm, and the ball milling time is 0.3h-6.5h.
11. The method for preparing degradable antibacterial non-woven fabric according to claim 10, wherein the preparation method has one or more of the following technical characteristics:
(1) The mass ratio of the antibacterial colloid, the nano hydroxyapatite and the starch is 1: (1-20): (1-15);
(2) In the step of preparing the antibacterial powder, the stirring conditions include: 150rpm-800rpm,26 ℃ -70 ℃;
(3) The soaking time is 4-9 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (0.35-9); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 200rpm-650rpm, and the ball milling time is 1h-6h.
12. The method for preparing a degradable antimicrobial nonwoven according to any of claims 9 to 11, characterized in that the method has one or more of the following technical features:
(1) The mass ratio of the antibacterial colloid to the nano hydroxyapatite to the starch is 1: (1.75-3.5): (1.2-2.5);
(2) In the step of preparing the antibacterial powder, the stirring conditions comprise: 200rpm-450rpm,30 ℃ -35 ℃;
(3) The soaking time is 5-8 h;
(4) The mass ratio of the mixture to the zirconia balls is 1: (2-4); and the combination of (a) and (b),
(5) The rotation speed of the ball milling is 200rpm-350rpm, and the ball milling time is 2h-4h.
13. A degradable antibacterial nonwoven fabric, which is prepared by the preparation method of any one of claims 1 to 12.
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