CN116043533B - Tear-resistant antibacterial nonwoven fabric and preparation method thereof - Google Patents
Tear-resistant antibacterial nonwoven fabric and preparation method thereof Download PDFInfo
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- CN116043533B CN116043533B CN202310014061.2A CN202310014061A CN116043533B CN 116043533 B CN116043533 B CN 116043533B CN 202310014061 A CN202310014061 A CN 202310014061A CN 116043533 B CN116043533 B CN 116043533B
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- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 86
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 49
- 108010022355 Fibroins Proteins 0.000 claims abstract description 49
- 229910052802 copper Inorganic materials 0.000 claims abstract description 49
- 239000010949 copper Substances 0.000 claims abstract description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 36
- -1 polypropylene Polymers 0.000 claims abstract description 30
- 239000000741 silica gel Substances 0.000 claims abstract description 23
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 23
- 239000004743 Polypropylene Substances 0.000 claims abstract description 18
- 229920001155 polypropylene Polymers 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims description 76
- 239000008367 deionised water Substances 0.000 claims description 46
- 229910021641 deionized water Inorganic materials 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 239000002131 composite material Substances 0.000 claims description 38
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 27
- 229910052700 potassium Inorganic materials 0.000 claims description 27
- 239000011591 potassium Substances 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 25
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 18
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 18
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 17
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 11
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 11
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 11
- 239000001263 FEMA 3042 Substances 0.000 claims description 11
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 11
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 11
- 229940033123 tannic acid Drugs 0.000 claims description 11
- 235000015523 tannic acid Nutrition 0.000 claims description 11
- 229920002258 tannic acid Polymers 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 150000003376 silicon Chemical class 0.000 description 25
- 238000002791 soaking Methods 0.000 description 16
- 238000007664 blowing Methods 0.000 description 15
- 230000001105 regulatory effect Effects 0.000 description 12
- 238000005096 rolling process Methods 0.000 description 10
- 238000009987 spinning Methods 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 239000004744 fabric Substances 0.000 description 8
- 238000009210 therapy by ultrasound Methods 0.000 description 8
- 238000007605 air drying Methods 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 238000009630 liquid culture Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- D06M11/77—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 silicon or compounds thereof
- D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- 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
-
- 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
- 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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- 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
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
-
- 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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Engineering & Computer Science (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明涉及无纺布制造技术领域，具体为一种抗撕裂抗菌型无纺布及其制备方法。本发明使用聚丙烯、琥珀酰聚糖制备了一种聚丙烯无纺布，并将无纺布上浸泡在抗菌整理液中，轧压，制得了一种抗撕裂抗菌型无纺布。本发明在抗菌整理液中添加了二氧化硅凝胶，添加了聚六亚甲基胍、丝素蛋白对二氧化硅进行进一步改性，增强了无纺布的抗撕裂性能以及抗菌性能。同时在抗菌整理液中添加具有抗菌效果的纳米铜粒子，进一步加强无纺布的抗菌效果。The present invention relates to the technical field of non-woven fabric manufacturing, and specifically to a tear-resistant antibacterial non-woven fabric and a preparation method thereof. The present invention uses polypropylene and succinoglycan to prepare a polypropylene non-woven fabric, and soaks the non-woven fabric in an antibacterial finishing liquid, and rolls and presses to obtain a tear-resistant antibacterial non-woven fabric. The present invention adds silica gel to the antibacterial finishing liquid, and adds polyhexamethylene guanidine and silk fibroin to further modify the silica, thereby enhancing the tear resistance and antibacterial properties of the non-woven fabric. At the same time, nano copper particles with antibacterial effect are added to the antibacterial finishing liquid to further enhance the antibacterial effect of the non-woven fabric.
Description
Technical Field
The invention relates to the technical field of non-woven fabric manufacturing, in particular to a tearing-resistant antibacterial non-woven fabric and a preparation method thereof.
Background
The non-woven fabric is also called as non-woven fabric, is not interwoven and knitted together by one yarn, breaks through the traditional spinning principle, and has the advantages of short process flow, high production rate, low cost, high yield and wide application. The non-woven fabric is breathable, has excellent filtering performance, does not generate fiber scraps, has high filtering efficiency and durability, is similar to cotton handfeel, is easier to form than cotton fabrics, and has lower manufacturing cost. The non-woven fabric has bright color, light weight and environment protection, can be recycled, and is widely applied to medical treatment, clothing, industry and agriculture, and has a very wide application range. However, the existing non-woven fabrics are easy to prepare, and still have the problems of poor antibacterial property and poor tear resistance.
In order to solve the problems, the invention provides a tearing-resistant antibacterial non-woven fabric and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a tearing-resistant antibacterial non-woven fabric and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
A preparation method of a tearing-resistant antibacterial non-woven fabric is characterized by comprising the following steps:
Step one, taking a modified silicon dioxide-silk fibroin composite solution, a modified nano copper sol and deionized water, and uniformly mixing to obtain an antibacterial finishing liquid;
step two, uniformly mixing polypropylene and succinoglycan, drying, melt-blowing, spinning and rolling to obtain non-woven fabrics;
Soaking the non-woven fabric in deionized water for 30-40min, cleaning, airing, soaking the non-woven fabric in the antibacterial finishing liquid for 20-25min at 25-35 ℃, rolling, and drying at 70-75 ℃ to obtain the tearing-resistant antibacterial non-woven fabric.
More optimally, in the first step, the preparation method of the modified silica-silk fibroin composite solution comprises the steps of taking silica gel, heating to 45-50 ℃, adding polyhexamethylene guanidine, continuously stirring for 3-5h, adding silk fibroin and ethylenediamine tetraacetic acid, stirring for 70-80min at 25-30 ℃, carrying out ultrasonic treatment for 70-80min, and drying to obtain the modified silica-silk fibroin composite solution.
More optimally, the preparation method of the silica gel comprises the steps of taking absolute ethyl alcohol and tetraethoxysilane, stirring for 18-20min at 25-28 ℃, adding ammonia water, stirring for 2-3h, adjusting the pH value of a solution to 5-5.5 by hydrochloric acid, adding tannic acid, continuously stirring for 2-3h, adding concentrated ammonia water, adjusting the pH value to 8-8.5, and aging for 11-12h to obtain the silica gel.
More optimally, in the first step, the preparation method of the modified nano copper sol comprises the steps of taking potassium borohydride and deionized water, uniformly stirring to obtain a potassium borohydride solution, taking copper sulfate, adding deionized water to obtain a copper sulfate solution, adding sodium dodecyl sulfate, polyvinylpyrrolidone and ethylenediamine, stirring for 1-2h, heating to 42-45 ℃, continuously stirring, adding the potassium borohydride solution, and continuously stirring for 3-5min to obtain the modified nano copper sol.
More optimally, in the first step, the mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is 25 (2-3) to 10-12.
More preferably, the non-woven fabric comprises, by weight, 60-70 parts of polypropylene and 8-12 parts of succinoglycan.
More optimally, in the second step, polypropylene and succinoglycan are uniformly mixed, dried for 1-2 hours at 75-80 ℃, melt-blown and spun at 240-260 ℃, and rolled, wherein the rolling speed is set to be (5-10) m/min, and the non-woven fabric is prepared.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention prepares a polypropylene non-woven fabric by using polypropylene and succinoglycan, and the non-woven fabric is soaked in the antibacterial finishing liquid and rolled to prepare the tearing-resistant antibacterial non-woven fabric.
According to the invention, the silica gel is added into the antibacterial finishing liquid, and the tannic acid is used for preparing the silica gel, so that the specific surface area of the silica is increased, the active sites of the silica are greatly increased, more polyhexamethylene guanidine with antibacterial performance is grafted on the surface of the silica, and the antibacterial effect of the finishing liquid is enhanced. And then silk fibroin is added to further modify the silicon dioxide, so that the tear resistance of the non-woven fabric is enhanced.
According to the invention, ethylenediamine is used for modifying the nano copper particles, amino groups are grafted on the nano copper, the amino groups can react with silicon hydroxyl groups on silicon dioxide, the dispersibility of the nano copper in finishing liquid is enhanced, and the antibacterial effect of the non-woven fabric is improved. Meanwhile, the nano copper can be chelated with ethylenediamine tetraacetic acid in the modified silicon dioxide-silk fibroin composite solution, so that the stability of the nano copper is enhanced, and the antibacterial effect of the non-woven fabric is enhanced.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution to the modified nano copper sol to the deionized water is 25 (2-3) to 10-12, so that the antibacterial effect of the non-woven fabric reaches the optimal state.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The chemicals used in the present invention were purchased from the following routes:
polypropylene, Z30S, purchased from singapore petrochemical company, china petrochemical;
Ethyl orthosilicate was purchased from the company of the sciences of the ridge.
Example 1
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
Taking 100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane, stirring for 19min at 27 ℃, adding 36mL of ammonia water, stirring for 2.5h, regulating the pH value of the solution to 5.5 by 0.1mol/L of hydrochloric acid, adding 1g of tannic acid, continuously stirring for 2.5h, adding 28% of concentrated ammonia water by mass fraction, regulating the pH value to 8, and aging for 11.5h to obtain silica gel;
8g of silica gel is taken, the temperature is raised to 47 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 4 hours, 6g of silk fibroin and 2g of ethylenediamine tetraacetic acid are added, stirring is carried out for 75 minutes at 28 ℃, ultrasonic treatment is carried out for 75 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Preparing modified nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate, 2.5g of polyvinylpyrrolidone and 2mL of ethylenediamine, stirring for 1.5h, heating to 43 ℃, continuously stirring, adding the potassium borohydride solution, converting the solution from light blue to reddish brown, and continuously stirring for 4min to obtain the modified nano copper sol.
And step three, preparing an antibacterial finishing liquid:
and (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 5g of modified nano copper sol and 22g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is 25:2.5:11.
Step four, preparing non-woven fabrics:
Uniformly mixing 65 parts of polypropylene and 10 parts of succinoglycan, drying at 77 ℃ for 1.5 hours, and carrying out melt-blowing spinning at 250 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
Soaking non-woven fabric in deionized water for 35min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 30deg.C for 23min, rolling on vertical padder, and drying at 72deg.C to obtain anti-tear antibacterial non-woven fabric.
Example 2
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
Taking 100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane, stirring for 18min at 25 ℃, adding 36mL of ammonia water, stirring for 2h, regulating the pH value of the solution to 5 by 0.1mol/L of hydrochloric acid, adding 1g of tannic acid, continuously stirring for 2h, adding 28% of concentrated ammonia water by mass fraction, regulating the pH value to 8, and aging for 11h to obtain silica gel;
8g of silica gel is taken, the temperature is raised to 45 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 3 hours, 6g of silk fibroin and 2g of ethylenediamine tetraacetic acid are added, stirring is carried out for 70 minutes at 25 ℃, ultrasonic treatment is carried out for 70 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Preparing modified nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate, 2.5g of polyvinylpyrrolidone and 2mL of ethylenediamine, stirring for 1h, heating to 42 ℃, continuously stirring, adding the potassium borohydride solution, converting the solution from light blue to reddish brown, and continuously stirring for 3min to obtain the modified nano copper sol.
And step three, preparing an antibacterial finishing liquid:
And (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 4g of modified nano copper sol and 20g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is 25:2:10.
Step four, preparing non-woven fabrics:
Uniformly mixing 60 parts of polypropylene and 8 parts of succinoglycan, drying for 1h at 75 ℃, and carrying out melt-blowing spinning at 240 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
soaking non-woven fabric in deionized water for 30min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 25deg.C for 20min, rolling on vertical padder, and drying at 70deg.C to obtain anti-tear antibacterial non-woven fabric.
Example 3
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
Taking 100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane, stirring for 20min at 28 ℃, adding 36mL of ammonia water, stirring for 3h, regulating the pH value of the solution to 5.5 by 0.1mol/L of hydrochloric acid, adding 1g of tannic acid, continuously stirring for 3h, adding 28% of concentrated ammonia water by mass fraction, regulating the pH value to 8.5, and aging for 12h to obtain silica gel;
8g of silica gel is taken, the temperature is raised to 50 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 5 hours, 6g of silk fibroin and 2g of ethylenediamine tetraacetic acid are added, stirring is carried out for 80 minutes at 30 ℃, ultrasonic treatment is carried out for 80 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Preparing modified nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate, 2.5g of polyvinylpyrrolidone and 2mL of ethylenediamine, stirring for 2 hours, heating to 45 ℃, continuously stirring, adding the potassium borohydride solution, converting the solution from light blue to reddish brown, and continuously stirring for 5 minutes to obtain the modified nano copper sol.
And step three, preparing an antibacterial finishing liquid:
and (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 6g of modified nano copper sol and 24g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is 25:3:12.
Step four, preparing non-woven fabrics:
Uniformly mixing 70 parts of polypropylene and 12 parts of succinoglycan, drying for 2 hours at 80 ℃, and carrying out melt-blowing spinning at 260 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
Soaking non-woven fabric in deionized water for 40min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 35deg.C for 25min, rolling on vertical padder, and drying at 75deg.C to obtain anti-tear antibacterial non-woven fabric.
Example 4 silica was modified without adding ethylenediamine tetraacetic acid, and the other steps were the same as in example 1.
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
Taking 100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane, stirring for 19min at 27 ℃, adding 36mL of ammonia water, stirring for 2.5h, regulating the pH value of the solution to 5.5 by 0.1mol/L of hydrochloric acid, adding 1g of tannic acid, continuously stirring for 2.5h, adding 28% of concentrated ammonia water by mass fraction, regulating the pH value to 8, and aging for 11.5h to obtain silica gel;
8g of silica gel is taken, the temperature is raised to 47 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 4 hours, 6g of silk fibroin is added, stirring is carried out for 75 minutes at 28 ℃, ultrasonic treatment is carried out for 75 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Preparing modified nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate, 2.5g of polyvinylpyrrolidone and 2mL of ethylenediamine, stirring for 1.5h, heating to 43 ℃, continuously stirring, adding the potassium borohydride solution, converting the solution from light blue to reddish brown, and continuously stirring for 4min to obtain the modified nano copper sol.
And step three, preparing an antibacterial finishing liquid:
and (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 5g of modified nano copper sol and 22g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is 25:2.5:11.
Step four, preparing non-woven fabrics:
Uniformly mixing 65 parts of polypropylene and 10 parts of succinoglycan, drying at 77 ℃ for 1.5 hours, and carrying out melt-blowing spinning at 250 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
Soaking non-woven fabric in deionized water for 35min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 30deg.C for 23min, rolling on vertical padder, and drying at 72deg.C to obtain anti-tear antibacterial non-woven fabric.
Example 5 silica was modified without addition of tannic acid, and the remainder was the same as in example 1.
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane are taken and stirred for 19min at 27 ℃, 36mL of ammonia water is added, and the mixture is stirred for 3h and kept stand for 24h, thus obtaining the silica gel.
8G of silica gel is taken, the temperature is raised to 47 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 4 hours, 6g of silk fibroin and 2g of ethylenediamine tetraacetic acid are added, stirring is carried out for 75 minutes at 28 ℃, ultrasonic treatment is carried out for 75 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Preparing modified nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate, 2.5g of polyvinylpyrrolidone and 2mL of ethylenediamine, stirring for 1.5h, heating to 43 ℃, continuously stirring, adding the potassium borohydride solution, converting the solution from light blue to reddish brown, and continuously stirring for 4min to obtain the modified nano copper sol.
And step three, preparing an antibacterial finishing liquid:
and (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 5g of modified nano copper sol and 22g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is 25:2.5:11.
Step four, preparing non-woven fabrics:
Uniformly mixing 65 parts of polypropylene and 10 parts of succinoglycan, drying at 77 ℃ for 1.5 hours, and carrying out melt-blowing spinning at 250 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
Soaking non-woven fabric in deionized water for 35min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 30deg.C for 23min, rolling on vertical padder, and drying at 72deg.C to obtain anti-tear antibacterial non-woven fabric.
EXAMPLE 6 modification of a nano copper sol without ethylenediamine, the rest was the same as in example 1.
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
Taking 100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane, stirring for 19min at 27 ℃, adding 36mL of ammonia water, stirring for 2.5h, regulating the pH value of the solution to 5.5 by 0.1mol/L of hydrochloric acid, adding 1g of tannic acid, continuously stirring for 2.5h, adding 28% of concentrated ammonia water by mass fraction, regulating the pH value to 8, and aging for 11.5h to obtain silica gel;
8g of silica gel is taken, the temperature is raised to 47 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 4 hours, 6g of silk fibroin and 2g of ethylenediamine tetraacetic acid are added, stirring is carried out for 75 minutes at 28 ℃, ultrasonic treatment is carried out for 75 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Step two, preparing nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate and 2.5g of polyvinylpyrrolidone, stirring for 1.5h, heating to 43 ℃, continuously stirring, adding the potassium borohydride solution, changing the solution from light blue to reddish brown, and continuously stirring for 4min to obtain the nano copper sol.
And step three, preparing an antibacterial finishing liquid:
and (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 5g of nano copper sol and 22g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the nano copper sol and the deionized water is 25:2.5:11.
Step four, preparing non-woven fabrics:
Uniformly mixing 65 parts of polypropylene and 10 parts of succinoglycan, drying at 77 ℃ for 1.5 hours, and carrying out melt-blowing spinning at 250 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
Soaking non-woven fabric in deionized water for 35min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 30deg.C for 23min, rolling on vertical padder, and drying at 72deg.C to obtain anti-tear antibacterial non-woven fabric.
Example 7 the amount of modified nano copper sol added was reduced, and the remainder was the same as in example 1.
Step one, preparing a modified silicon dioxide-silk fibroin composite solution:
Taking 100mL of absolute ethyl alcohol and 34mL of tetraethoxysilane, stirring for 19min at 27 ℃, adding 36mL of ammonia water, stirring for 2.5h, regulating the pH value of the solution to 5.5 by 0.1mol/L of hydrochloric acid, adding 1g of tannic acid, continuously stirring for 2.5h, adding 28% of concentrated ammonia water by mass fraction, regulating the pH value to 8, and aging for 11.5h to obtain silica gel;
8g of silica gel is taken, the temperature is raised to 47 ℃, 0.7g of polyhexamethylene guanidine is added, stirring is continued for 4 hours, 6g of silk fibroin and 2g of ethylenediamine tetraacetic acid are added, stirring is carried out for 75 minutes at 28 ℃, ultrasonic treatment is carried out for 75 minutes, and drying is carried out, thus obtaining the modified silica-silk fibroin composite solution.
Preparing modified nano copper sol:
Taking 0.16g of potassium borohydride and 20mL of deionized water, uniformly stirring to obtain a potassium borohydride solution, taking 0.6g of copper sulfate, adding 50mL of deionized water to obtain a copper sulfate solution, adding 1.5g of sodium dodecyl sulfate, 2.5g of polyvinylpyrrolidone and 2mL of ethylenediamine, stirring for 1.5h, heating to 43 ℃, continuously stirring, adding the potassium borohydride solution, converting the solution from light blue to reddish brown, and continuously stirring for 4min to obtain the modified nano copper sol.
And step three, preparing an antibacterial finishing liquid:
and (3) uniformly mixing 50g of modified silicon dioxide-silk fibroin composite solution, 2g of modified nano copper sol and 22g of deionized water to obtain the antibacterial finishing liquid.
The mass ratio of the modified silicon dioxide-silk fibroin composite solution, the modified nano copper sol and the deionized water is controlled to be 25:1:11.
Step four, preparing non-woven fabrics:
Uniformly mixing 65 parts of polypropylene and 10 parts of succinoglycan, drying at 77 ℃ for 1.5 hours, and carrying out melt-blowing spinning at 250 ℃ at a winding speed of 5m/min and a melt-blowing fabric receiving distance of 300mm to prepare a non-woven fabric;
Soaking non-woven fabric in deionized water for 35min, cleaning, air drying, soaking non-woven fabric in antibacterial finishing liquid at 30deg.C for 23min, rolling on vertical padder, and drying at 72deg.C to obtain anti-tear antibacterial non-woven fabric.
Experiment
The tear-resistant antibacterial nonwoven fabrics prepared in examples 1 to 7 were subjected to performance test, and the tear strength of the nonwoven fabrics was tested according to FZ-60006-91 measurement of nonwoven fabric tear strength. Cutting non-woven fabrics into square sheets with the length of 6cm multiplied by 6cm, sterilizing at 120 ℃ for 30min, then placing into a conical flask, adding 80mL of liquid culture medium, adding 5mL of bacteria liquid to be tested, oscillating for 18h at the constant temperature of 25 ℃, taking out the bacteria liquid, diluting, taking out 1mL of diluted bacteria liquid by a pipette, adding the bacteria liquid onto a flat plate, culturing at 37 for 48h, and testing the bacteriostasis rate.
The data obtained are shown in the following table:
It is concluded from the above data that example 4 does not add ethylenediamine tetraacetic acid, the stability of nano copper is poor, and the antibacterial effect of the nonwoven fabric is poor. In example 5, tannic acid is not added to modify silicon dioxide, the active site of the silicon dioxide is reduced, the grafting rate of polyhexamethylene guanidine is reduced, and the antibacterial effect is weakened. In example 6, the nano copper sol was modified without adding ethylenediamine, so that the dispersibility of nano copper in the finishing liquid was deteriorated, and the antibacterial effect of the nonwoven fabric was deteriorated. Example 7 the antibacterial effect of the nonwoven fabric was deteriorated by reducing the addition amount of the modified nano copper sol.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto, but may be modified or substituted for some of the technical features thereof by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
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