WO2017185714A1 - 一种纳米纤维抗菌非织造材料及制备方法 - Google Patents

一种纳米纤维抗菌非织造材料及制备方法 Download PDF

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Publication number
WO2017185714A1
WO2017185714A1 PCT/CN2016/105638 CN2016105638W WO2017185714A1 WO 2017185714 A1 WO2017185714 A1 WO 2017185714A1 CN 2016105638 W CN2016105638 W CN 2016105638W WO 2017185714 A1 WO2017185714 A1 WO 2017185714A1
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Prior art keywords
antibacterial
nanofiber
particles
nano
zinc oxide
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PCT/CN2016/105638
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English (en)
French (fr)
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邱邦胜
葛杨
黄肖瑶
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江苏盛纺纳米材料科技股份有限公司
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Publication of WO2017185714A1 publication Critical patent/WO2017185714A1/zh

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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/14—Layered products comprising a layer of metal next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • 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
    • 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
    • D04H1/4374—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 using different kinds of webs, e.g. by layering webs
    • 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
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/728—Hydrophilic

Definitions

  • the invention belongs to the field of non-woven materials, and in particular relates to a nanofiber antibacterial nonwoven material and a preparation method thereof.
  • Nonwoven materials are also known as nonwovens, nonwovens, nonwovens, nonwovens or nonwovens.
  • Nonwoven technology is a material processing technology that originates from textiles but transcends textiles. It combines four flexible materials processing technologies of textile, paper, leather and plastic, and fully combines and applies many modern high technologies, such as computer control, information technology, high pressure jet, plasma, infrared, laser technology. No matter in aerospace technology, environmental protection, agricultural technology, medical care or people's daily life, non-woven new materials have become an increasingly important and important product. With the development of science and technology and the improvement of people's living standards, people's health awareness is continuously enhanced. Antibacterial and antibacterial processing or treatment of non-woven materials can effectively reduce or avoid the impact of bacteria on health.
  • non-woven products having antibacterial and antibacterial properties is generally carried out by adding an antibacterial agent bacteriostatic agent or a finishing method to the spinning solution.
  • an antibacterial agent bacteriostatic agent or a finishing method to the spinning solution.
  • the addition of the antibacterial agent in the spinning solution is easy to mix unevenly with the polymer, and it is easy to block the spinneret, and the continuous production cannot be ensured.
  • the process of the finishing method is complicated, the cost is high, and the antibacterial property of the prepared non-woven material is obtained. Room for improvement.
  • one of the objects of the present invention is to provide a nanofiber antibacterial nonwoven material which is excellent in antibacterial properties.
  • a nanofiber antibacterial nonwoven material comprising at least two layers of nanofiber antibacterial layer, two adjacent layers
  • a nanofiber hydrophilic layer is disposed between the nanofiber antibacterial layers, and the nanofibers of the nanofiber antibacterial layer are arranged in a three-dimensional space to form pores having nanometer particles and nanofiber clusters, and nanometers are distributed in the pores.
  • Silver antibacterial particles and nano zinc oxide antibacterial particles are distributed in the pores.
  • Nano-zinc oxide has strong antibacterial and bactericidal effects and its broad-spectrum antibacterial property. Due to its quantum effect, small size effect and large specific surface area, it has the antibacterial effect unmatched by traditional inorganic antibacterial agents. A new generation of antimicrobial materials for the future.
  • Zinc oxide is a wide bandgap II, group VI compound semiconductor material with a regular hexagonal wurtzite structure. It is white in color, has good stability, does not discolor at high temperature, does not decompose, is inexpensive, and is rich in resources.
  • the nano-ZnO antibacterial particles in the antibacterial layer of nanofibers will decompose and freely move negatively charged electrons and positively charged holes after being irradiated by ultraviolet rays. This process is very easy to occur.
  • Positively charged holes oxidize water in the nonwoven to produce hydroxyl radicals, while electrons reduce oxygen in the air to active oxygen atoms. Both hydroxyl radicals and reactive oxygen atoms can interact with organic or unsaturated bonds in the bacteria. A reaction occurs that decomposes the components of the microorganisms and acts as an antibacterial agent. At the same time, the nano zinc oxide antibacterial particles slowly release zinc ions in an aqueous medium, bind to the bacterial microbial proteins, and destroy the enzymes of the bacterial electron transport and the -SH groups to achieve a double sterilization effect. The nano zinc oxide antibacterial particles also have certain anti-radiation, anti-wrinkle and anti-static effects.
  • One-dimensional zinc oxide nanomaterials refer to ZnO nanomaterials with nanometer size below 100 nm and two-dimensional nanoscale in space, including nanorods, nanowires, nanotubes, and nanoparticles.
  • one-dimensional semiconductor materials such as nanowires, nanorods, and nanorings have received extensive attention due to their unique physical, chemical, and biological properties.
  • the invention applies the antibacterial property and the small particle size of the one-dimensional zinc oxide nano material.
  • Metallic silver itself has a strong antibacterial activity, and it is prepared into nano silver particles by means of nanotechnology, which has higher practical value and good antibacterial effect.
  • the silver ions in the nano-silver particles combine with the bacterial membrane cells to destroy the membrane structure under the strong oxidation, and the substances in the bacterial membrane are leaked out, leading to the formation of the cell membrane shell. Glycans can not be synthesized normally, so that the bacteria's DNA is exposed and reacts with silver ions, which blocks the normal reproductive pathway of bacteria and thus plays a sterilization role.
  • the nano silver particles are added to the non-woven material, which has remarkable antibacterial, antiseptic and anti-inflammatory effects, and is very suitable for medical use.
  • the method of adding nano silver particles to the non-woven material is mostly soaking or coating. After repeated washing, the content of nano silver particles is less and less, which affects the antibacterial effect of the nano silver fiber. Repeated soaking or coating increases the amount of nano-silver particles and also increases the chance of oxidation of the nano-silver particles, making the appearance of the nonwoven yellow.
  • the binding force between the nano silver particles and the nano fibers is strong, and the bacteriostasis rate of 98% or more can be maintained after repeated washing, so that the nanofiber antibacterial layer has a long-lasting antibacterial property.
  • the nanofibers of the nanofiber antibacterial layer are arranged in a three-dimensional space to form a joint, and the nano silver antibacterial particles and the nano zinc oxide antibacterial particles are distributed around the joint. After spinning, the nanofibers are cross-aligned, and a plurality of joints are formed at each intersection. Nano-silver antibacterial particles with nanometer-scale particle size and nano-zinc oxide antibacterial particles are attached to the joint to exert a long-lasting antibacterial effect, forming a joint. The more the nano silver antibacterial particles and the nano zinc oxide antibacterial particles are distributed, the better the antibacterial function.
  • the nanofibers of the nanofiber antibacterial layer have an average diameter of 0.1 to 500 nm, for example, 0.1 nm, 0.5 nm, 10 nm, 20 nm, 30 nm, 40 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, 100 nm, 150 nm, 200 nm, 250 nm, 300 nm, 350 nm, 400 nm, 450 nm, 500 nm;
  • the nanofiber antibacterial layer has a thickness of 10 to 100 ⁇ m, for example, 10 ⁇ m, 20 ⁇ m, 30 ⁇ m, 40 ⁇ m, 50 ⁇ m, 60 ⁇ m, 70 ⁇ m, 80 ⁇ m, 90 ⁇ m, 100 ⁇ m; the nanofiber hydrophilic layer has a thickness of 10 to 50 ⁇ m.
  • the nano silver antibacterial particles have an average particle diameter of 20 to 30 nm, for example, 21 nm, 22 nm, 23 nm, 24 nm, 25 nm, 26 nm, 27 nm, 28 nm, 29 nm, 30 nm;
  • the nano zinc oxide antibacterial particles have an average particle diameter of 10 to 150 nm, for example, 10 nm, 15 nm, 20 nm, 25 nm, 30 nm, 35 nm, 40 nm, 45 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, 100 nm, 110 nm, 120 nm, 130 nm, 140 nm, 150 nm; the nano zinc oxide antibacterial particles are one-dimensional nano zinc oxide antibacterial particles;
  • the mass ratio of the nano silver antibacterial particles to the nano zinc oxide antibacterial particles is 1: (2 to 10), for example, 1:2, 1:3, 1:4, 1:5, 1:6 , 1:7, 1:8, 1:9, 1:10.
  • the nanofiber antibacterial layer is prepared by electrospinning a spinning solution to which the nano silver antibacterial particles and the nano zinc oxide antibacterial particles are added.
  • the polymer is polypropylene.
  • the mass ratio of the total amount of the nano silver antibacterial particles and the nano zinc oxide antibacterial particles to the polymer is 1: (15 to 30), for example, 1:15, 1:20, 1:25, 1: 30.
  • a second object of the present invention is to provide a method for preparing a nanofiber antibacterial nonwoven material, comprising the following steps:
  • nanofiber antibacterial material prepared in step 1) and the nanofiber hydrophilic material prepared in step 2) are cross-laid, and after hot rolling, a nanofiber antibacterial non-woven material having a nanofiber antibacterial layer and a nanofiber hydrophilic layer is prepared. .
  • step 1) is: adding nano silver antibacterial particles and nano zinc oxide antibacterial particles to the polymer, and melting to form a spinning solution, applying high voltage positive electricity on the spinning liquid nozzle, and spinning the solution Electrospinning to prepare nanofiber antibacterial materials;
  • the specific process of step 2) is: melting the polymer to form a spinning solution, applying high-voltage positive electricity on the spinning liquid nozzle, electrospinning the spinning solution, and obtaining a nanofiber material after spinning.
  • the nanofiber material is prepared by hydrophilic treatment to obtain a nanofiber hydrophilic material.
  • step 1) and step 2) the polymer is polypropylene
  • the spinning solution has an extrusion rate of 0.5 to 2 ml/h, the spinning voltage is 30 to 60 kV, and the receiving distance is 15 to 40 cm;
  • the mass ratio of the nano silver antibacterial particles to the nano zinc oxide antibacterial particles is 1: (2 to 10); the total amount of the nano silver antibacterial particles and the nano zinc oxide antibacterial particles
  • the mass ratio to the polymer is 1: (15 ⁇ 30);
  • the hydrophilic treatment is: preparing a hydrophilic solvent by diluting the hydrophilic agent with high-purity water, applying a hydrophilic solvent to the nanofiber material, and drying to prepare a nanofiber hydrophilic material.
  • the beneficial effects of the present invention are: the nanofiber antibacterial nonwoven material of the present invention, comprising at least two layers of nanofiber antibacterial layer, and the adjacent two layers of the nanofiber antibacterial layer are provided with nanofiber pro
  • the nanofibers of the nanofiber antibacterial layer are arranged in a three-dimensional space to form pores having nano-particles and nano-fiber clusters, wherein the nano-silver antibacterial particles and nano-zinc oxide antibacterial particles are distributed in the holes;
  • the nano silver particles in the layer and the nano zinc oxide antibacterial particles are distributed in the nanofibers of the nanofiber antibacterial layer, and the nanofibers and the nanofiber clusters are arranged in a three-dimensional space, and the antibacterial particles are not easily peeled off, and the nanometer level is
  • the combination of nano silver particles and nano zinc oxide makes the nanofiber antibacterial nonwoven material have long-lasting antibacterial properties, and together enhances the antibacterial properties of the nanofiber antibacterial nonwoven material.
  • the nanofiber hydrophilic layer is
  • the method for preparing the nanofiber antibacterial nonwoven material of the invention adopts the method of electrospinning, the method is simple, the nanometer-level antibacterial particles are uniformly distributed in the nanofiber, and the combination is firm. The continuous production is ensured, and the antibacterial property of the product is improved.
  • the prepared nanofiber antibacterial non-woven material can be widely used in the fields of daily necessities, medical care, infants and adult hygiene products.
  • FIG. 1 is a schematic structural view of a nanofiber antibacterial nonwoven material of the present invention
  • FIG. 3 is a schematic view showing the structure of a nanofiber antibacterial layer of the nanofiber antibacterial nonwoven material of the present invention.
  • 1-nanofiber antibacterial layer 2-nanofiber hydrophilic layer; 31-nano silver antibacterial particle; 32-nano zinc oxide antibacterial particle; 4-nano fiber.
  • the nanofiber antibacterial nonwoven material of the present invention comprises at least two nanofiber antibacterial layers 1 , and a nanofiber hydrophilic layer 2 and a nanofiber antibacterial layer are disposed between two adjacent nanofiber antibacterial layers 1 .
  • the nanofibers 4 of 1 are arranged in a three-dimensional space to form pores having nano-particles and nano-fiber clusters, and nano-silver antibacterial particles 31 and nano-zinc oxide antibacterial particles 32 are distributed in the holes;
  • FIG. 1 shows only one embodiment of the present invention.
  • the nanofiber hydrophilic layer 2 is disposed as a basic constituent unit between the adjacent two layers of the nanofiber antibacterial layer 1, and the nanofiber antibacterial nonwoven material may include two, three, four or more.
  • a number of basic components specifically the number of components of the basic component can be adjusted according to the needs of the actual product.
  • the nanofibers 4 are arranged in a three-dimensional space to form pores having nano-particles and nano-fiber clusters; or, the nano-fibers 4 are arranged in a three-dimensional space to form a plurality of joints, and the spun nanofibers are formed. 4
  • the average diameter is about small and the number is larger, and the more joints are formed.
  • nano silver antibacterial particles 31 and nano zinc oxide antibacterial particles 32 are distributed around the joint, and the more the joints, the nano silver antibacterial particles 31 and the nano zinc oxide antibacterial particles 32. The more distribution, the better the antibacterial function.
  • nanofiber antibacterial nonwoven material prepared by the present invention The properties of the nanofiber antibacterial nonwoven material prepared by the present invention are illustrated below by way of specific examples. Unless otherwise specified, the various starting materials of the present invention are commercially available or can be prepared according to conventional methods in the art.
  • Adding 0.2g of nano silver antibacterial particles and 0.5g of nano zinc oxide antibacterial particles to 20g polypropylene to make a spinning solution applying high voltage positive electricity on the spinning liquid nozzle, electrospinning the spinning solution, and spinning
  • the extrusion rate of the liquid is 1-2 ml/h
  • the spinning voltage is 60KV
  • the receiving distance is 40cm
  • the nanofiber antibacterial material is prepared; 20g of polypropylene is melted to prepare a spinning solution, and a high pressure is applied on the spinning liquid nozzle.
  • Electrolytic, electrospinning the spinning solution, the spinning solution is extruded at a rate of 1 to 2 ml/h, the spinning voltage is 60 kV, and the receiving distance is 40 cm.
  • the nanofiber material is prepared, and the hydrophilic agent is prepared by diluting with high purity water. Forming a hydrophilic solvent, applying a hydrophilic solvent to the nanofiber material, and drying to prepare a nanofiber hydrophilic material; and preparing the nano silver nanofiber antibacterial material and the nanofiber hydrophilic material to be cross-laid and heated After rolling, a nanofiber antibacterial nonwoven material having a nanofiber antibacterial layer and a nanofiber hydrophilic layer is prepared. The antibacterial properties of the prepared nanofiber antibacterial non-woven materials were tested.
  • the results showed that the inhibition rate against the representative bacteria such as Staphylococcus aureus, Escherichia coli and Candida albicans was greater than 99.9%, and the inhibition rate was greater than 98% in 2 hours;
  • the hydrophilic property of the nanofiber antibacterial nonwoven material has a drip penetration time of 0.8 s and a hydrophilic ratio of 500% or more.
  • Adding 0.1g of nano silver antibacterial particles and 0.5g of nano zinc oxide antibacterial particles to 10g polypropylene to make a spinning solution applying high voltage positive electricity on the spinning liquid nozzle, electrospinning the spinning solution, and spinning
  • the extrusion rate of the liquid is 1-2 ml/h
  • the spinning voltage is 40KV
  • the receiving distance is 20cm
  • the nanofiber antibacterial material is prepared; 10g of polypropylene is melted to form a spinning solution, and a high pressure is applied on the spinning liquid nozzle.
  • Electricity The spinning solution is electrospun, the spinning solution is extruded at a rate of 1 to 2 ml/h, the spinning voltage is 40 KV, and the receiving distance is 20 cm.
  • the nanofiber material is prepared, and the hydrophilic agent is diluted with high-purity water to prepare a pro-parent.
  • An aqueous solvent after applying a hydrophilic solvent to the nanofiber material, drying the nanofiber hydrophilic material; and preparing the nano silver nanofiber antibacterial material and the nanofiber hydrophilic material, and after hot rolling
  • a nanofiber antibacterial nonwoven material having a nanofiber antibacterial layer and a nanofiber hydrophilic layer is prepared. The antibacterial properties of the prepared nanofiber antibacterial non-woven materials were tested.
  • the results showed that the inhibition rate against the representative bacteria such as Staphylococcus aureus, Escherichia coli and Candida albicans was greater than 99.9%, and the inhibition rate was greater than 98% in 2 hours;
  • the hydrophilic property of the nanofiber antibacterial nonwoven material has a drip penetration time of 0.8 s and a hydrophilic ratio of 500% or more.
  • Adding 0.15g of nano silver antibacterial particles and 0.75g of nano zinc oxide antibacterial particles to 15g polypropylene to make a spinning solution applying high voltage positive electricity on the spinning liquid nozzle, electrospinning the spinning solution, and spinning
  • the extrusion rate of the liquid is 0.5-1 ml/h
  • the spinning voltage is 35KV
  • the receiving distance is 25cm
  • the nanofiber antibacterial material is prepared; 15g polypropylene is melted to form a spinning solution, and a high pressure is applied on the spinning liquid nozzle.
  • Positive electrolysis, electrospinning the spinning solution, the spinning solution is extruded at a rate of 0.5 to 1 ml/h, the spinning voltage is 35 kV, and the receiving distance is 25 cm.
  • the nanofiber material is prepared, and the hydrophilic agent is diluted with high purity water.
  • the results showed that the inhibition rate against the representative bacteria such as Staphylococcus aureus, Escherichia coli and Candida albicans was greater than 99.9%, and the inhibition rate was greater than 98% in 2 hours;
  • the hydrophilic property of the nanofiber antibacterial nonwoven material has a drip penetration time of 0.8 s and a hydrophilic ratio of 500% or more.
  • the nanofiber material is prepared, and the hydrophilic agent is diluted with high purity water. After preparing a hydrophilic solvent, the hydrophilic solvent is applied to the nanofiber material, and the nanofiber hydrophilic material is prepared by drying; the prepared nano silver nanofiber antibacterial material and the nanofiber hydrophilic material are cross-laid, After hot rolling, a nanofiber antibacterial nonwoven material having a nanofiber antibacterial layer and a nanofiber hydrophilic layer is prepared. The antibacterial properties of the prepared nanofiber antibacterial non-woven materials were tested.
  • the results showed that the inhibition rate against the representative bacteria such as Staphylococcus aureus, Escherichia coli and Candida albicans was greater than 99.9%, and the inhibition rate was greater than 98% in 2 hours;
  • the hydrophilic property of the nanofiber antibacterial nonwoven material has a drip penetration time of 0.9 s and a hydrophilic ratio of 500% or more.
  • the nanofiber antibacterial non-woven material of the invention has good antibacterial property, strong antibacterial effect, and excellent hydrophilic property, and the hydrophilic ratio is more than 500%, and the preparation method of the invention is simple in process, and the nanometer antibacterial particles are in the nanometer.
  • the fibers are evenly distributed and firmly combined to ensure continuous production and improve the antibacterial properties of the products.
  • the prepared nanofiber antibacterial nonwoven materials can be widely used in the fields of daily necessities, medical care, infants and adult hygiene products.

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  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

一种纳米纤维抗菌非织造材料及制备方法，其中非织造材料包括至少两层纳米纤维抗菌层（1），相邻两层纳米纤维抗菌层（1）之间设置有纳米纤维亲水层（2），纳米纤维抗菌层（1）的纳米纤维（4）在三维空间交叉排列，形成具有纳米微粒、纳米纤维团簇的孔洞，孔洞内分布有纳米银抗菌颗粒（31）和纳米氧化锌抗菌颗粒（32）；纳米银颗粒（31）和纳米氧化锌抗菌颗粒（32）分布于具有纳米微粒、纳米纤维团簇的孔洞中，并且抗菌颗粒不易脱落，共同作用使纳米纤维抗菌非织造材料有持久的抗菌性。另外，纳米纤维亲水层（2）提供了纳米纤维抗菌非织造材料良好的亲水性能。本发明制备方法制得的纳米纤维抗菌非织造材料可广泛应用于日用品、医疗保健、婴幼儿及成人卫生用品等领域。

Description

一种纳米纤维抗菌非织造材料及制备方法 技术领域
本发明属于非织造材料领域，具体涉及一种纳米纤维抗菌非织造材料及制备方法。
背景技术
非织造材料又称非织造布、非织布、非织造织物、无纺织物或无纺布。非织造技术是一门源于纺织，但又超越纺织的材料加工技术。它结合了纺织、造纸、皮革和塑料四大柔性材料加工技术，并充分结合和运用了诸多现代高新技术，如计算机控制、信息技术、高压射流、等离子体、红外、激光技术等。无论在航天技术、环保治理、农业技术、医用保健或是人们的日常生活等许多领域，非织造新材料已成为一种愈来愈广泛的重要产品。随着科学技术的发展和人们生活水平的提高，人们的健康意识不断增强，对非织造材料进行抗菌、抑菌性加工或处理，可以有效地降低或避免细菌对身体健康的影响。生产具有抗菌、抑菌性的非织造材料产品，一般是通过在纺丝液中添加抗菌剂抑菌剂或后整理的方法进行的。但是，在纺丝液中添加抗菌剂容易与聚合物混合不均匀，容易堵塞喷丝板，无法保证连续生产，后整理方法的工艺复杂，成本较高，并且制备成的非织造材料的抗菌性能有待提高。
发明内容
针对现有技术的不足，本发明的目的之一在于提供一种纳米纤维抗菌非织造材料，抗菌性能优良。
为达此目的，本发明采用以下技术方案：
一种纳米纤维抗菌非织造材料，包括至少两层纳米纤维抗菌层，相邻两层 所述纳米纤维抗菌层之间设置有纳米纤维亲水层，所述纳米纤维抗菌层的纳米纤维在三维空间交叉排列，形成具有纳米微粒、纳米纤维团簇的孔洞，所述孔洞内分布有纳米银抗菌颗粒以及纳米氧化锌抗菌颗粒。
纳米氧化锌具有较强抑菌、杀菌作用及其广谱的抗菌性，且由于量子效应、小尺寸效应和具有较大比表面积，因而具有传统无机抗菌剂无法比拟的抗菌效果，成为很有发展前景的新一代抗菌材料。氧化锌是一种宽禁带II，VI族化合物半导体材料，具有规整的六角形纤锌矿结构，本身为白色，稳定性好，高温下不变色、不分解、价格低廉、资源丰富。纳米纤维抗菌层中的纳米氧化锌抗菌颗粒经紫外线照射后会自行分解出自由移动带负电荷的电子和带正电荷的空穴，这个过程极易发生。带正电荷的空穴会氧化非织造材料中的水产生羟自由基，同时电子使空气中的氧还原成活性氧原子，羟自由基和活性氧原子均能与细菌体内的有机物或不饱和键发生反应，分解微生物的组成成分，起到抗菌作用。同时，纳米氧化锌抗菌颗粒在含水介质中缓慢释放锌离子，与细菌微生物蛋白质结合，并破坏细菌电子传递的酶与-SH基团反应，达到双重杀菌的效果。纳米氧化锌抗菌颗粒还具有一定的防辐射、抗皱、抗静电作用。一维氧化锌纳米材料是指纳米尺寸低于100nm并且空间有两维为纳米尺度的ZnO纳米材料，包括纳米棒，纳米线，纳米管，纳米颗粒等。近年来随着纳米技术的发展，一维半导体材料如纳米线、纳米棒、纳米环等由于其独特的物理、化学和生物特性而受到广泛的关注。本发明应用了一维氧化锌纳米材料的抗菌性能以及粒径小的特点。
金属银本身就有很强的抑菌活性，借助纳米技术将其制备成纳米银颗粒，实用价值更高，抗菌效果很好。纳米银颗粒中的银离子与细菌膜细胞结合，在超强的氧化作用下破坏膜结构，细菌膜内物质随之外泄，导致细胞膜生成物壳 聚糖不能正常合成，使细菌的DNA裸露，并和银离子反应，阻断了细菌的正常繁殖途径，从而起到灭菌的作用。将纳米银颗粒加在非织造材料上，具有显著的抗菌、防腐、消炎效果，很适合于医疗上使用。目前，将纳米银颗粒加在非织造材料上的方法大多是浸泡或涂布，经过多次水洗后，纳米银颗粒含量越来越少，影响纳米银纤维的抗菌效果。反复浸泡或涂布，增加了纳米银颗粒用量，也增加了纳米银颗粒氧化的机会，使非织造材料的外观变黄。纳米银颗粒与纳米纤维之间的结合力强，经多次洗涤后仍可以保持98％以上的抑菌率，使纳米纤维抗菌层具有持久的抗菌性。
其中，所述纳米纤维抗菌层的纳米纤维在三维空间交叉排列形成接点，所述接点周围分布有所述纳米银抗菌颗粒以及所述纳米氧化锌抗菌颗粒。经过纺丝后，纳米纤维之间交叉排列，各交叉点形成若干接点，粒径为纳米级别的纳米银抗菌颗粒以及纳米氧化锌抗菌颗粒附于接点上，起到持久的抗菌作用，形成的接点越多，纳米银抗菌颗粒以及纳米氧化锌抗菌颗粒的分布越多，抗菌功能越好。
其中，所述纳米纤维抗菌层的纳米纤维的平均直径为0.1～500nm，例如0.1nm、0.5nm、10nm、20nm、30nm、40nm、50nm、60nm、70nm、80nm、90nm、100nm、150nm、200nm、250nm、300nm、350nm、400nm、450nm、500nm；
优选地，所述纳米纤维抗菌层的厚度为10～100μm，例如10μm、20μm、30μm、40μm、50μm、60μm、70μm、80μm、90μm、100μm；所述纳米纤维亲水层的厚度为10～50μm，例如10μm、15μm、20μm、25μm、30μm、35μm、40μm、45μm、50μm。
其中，所述纳米银抗菌颗粒的平均粒径为20～30nm，例如21nm、22nm、 23nm、24nm、25nm、26nm、27nm、28nm、29nm、30nm；
优选地，所述纳米氧化锌抗菌颗粒的平均粒径为10～150nm，例如10nm、15nm、20nm、25nm、30nm、35nm、40nm、45nm、50nm、60nm、70nm、80nm、90nm、100nm、110nm、120nm、130nm、140nm、150nm；所述纳米氧化锌抗菌颗粒为一维纳米氧化锌抗菌颗粒；
更优选地，所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒的质量比为1∶(2～10)，例如1∶2、1∶3、1∶4、1∶5、1∶6、1∶7、1∶8、1∶9、1∶10。
其中，所述纳米纤维抗菌层由添加了所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒的纺丝液经静电纺丝制备而成。
其中，所述聚合物为聚丙烯。
其中，所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒总量与所述聚合物的质量比为1∶(15～30)，例如1∶15、1∶20、1∶25、1∶30。
本发明的目的之二在于提供一种纳米纤维抗菌非织造材料的制备方法，包括如下步骤：
1)采用包含有纳米银抗菌颗粒和纳米氧化锌抗菌颗粒的纺丝液制备纳米纤维抗菌材料；
2)制备纳米纤维亲水材料；
3)将步骤1)制备的纳米纤维抗菌材料和步骤2)制备的纳米纤维亲水材料交叉铺设，经热轧后制备成具有纳米纤维抗菌层和纳米纤维亲水层的纳米纤维抗菌非织造材料。
其中，步骤1)的具体过程为：在聚合物中添加纳米银抗菌颗粒和纳米氧化锌抗菌颗粒，经熔融后制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，制备纳米纤维抗菌材料；
优选地，步骤2)的具体过程为：将聚合物熔融后制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝后得到纳米纤维材料，将所述纳米纤维材料经亲水处理后制备得到纳米纤维亲水材料。
其中，步骤1)和步骤2)中，所述聚合物为聚丙烯；
所述静电纺丝的具体工艺参数为：纺丝液的挤出速率为0.5～2ml/h，纺丝电压为30～60KV，接收距离为15～40cm；
优选地，步骤1)中，所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒的质量比为1∶(2～10)；所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒总量与所述聚合物的质量比为1∶(15～30)；
步骤2)中，所述亲水处理为：将亲水剂用高纯水稀释后制备成亲水溶剂，将亲水溶剂涂覆于所述纳米纤维材料后，经烘干制备纳米纤维亲水材料。
与现有技术相比，本发明的有益效果为：本发明的纳米纤维抗菌非织造材料，包括至少两层纳米纤维抗菌层，相邻两层所述纳米纤维抗菌层之间设置有纳米纤维亲水层，所述纳米纤维抗菌层的纳米纤维在三维空间交叉排列，形成具有纳米微粒、纳米纤维团簇的孔洞，所述孔洞内分布有纳米银抗菌颗粒以及纳米氧化锌抗菌颗粒；纳米纤维抗菌层中的纳米银颗粒以及纳米氧化锌抗菌颗粒，分布于纳米纤维抗菌层的纳米纤维在三维空间交叉排列形成的具有纳米微粒、纳米纤维团簇的孔洞中，并且抗菌颗粒不易脱落，纳米级别的纳米银颗粒和纳米氧化锌共同作用，使纳米纤维抗菌非织造材料有持久的抗菌性，共同增强了纳米纤维抗菌非织造材料的抗菌性能。另外，纳米纤维亲水层的设计使得纳米纤维抗菌非织造材料具有良好的亲水性能，亲水倍率达500％以上。
另外，本发明的纳米纤维抗菌非织造材料的制备方法，采用静电纺丝的方法，该方法工艺简单，纳米级别的抗菌颗粒在纳米纤维中分布均匀，结合牢固， 保证了连续生产，并且提高了产品的抗菌性能，制备得到的纳米纤维抗菌非织造材料可以广泛应用于日用品、医疗保健、婴幼儿及成人卫生用品等领域。
附图说明
图1为本发明的纳米纤维抗菌非织造材料的结构示意图；
图2为本发明的纳米纤维抗菌非织造材料的电镜图；
图3为本发明的纳米纤维抗菌非织造材料的纳米纤维抗菌层的结构示意图。
附图标记如下：
1-纳米纤维抗菌层；2-纳米纤维亲水层；31-纳米银抗菌颗粒；32-纳米氧化锌抗菌颗粒；4-纳米纤维。
具体实施方式
下面结合附图1、图2和图3并通过实施例来进一步说明本发明的技术方案。
如图1所示，本发明的纳米纤维抗菌非织造材料，包括至少两层纳米纤维抗菌层1，相邻两层纳米纤维抗菌层1之间设置有纳米纤维亲水层2，纳米纤维抗菌层1的纳米纤维4在三维空间交叉排列，形成具有纳米微粒、纳米纤维团簇的孔洞，孔洞内分布有纳米银抗菌颗粒31以及纳米氧化锌抗菌颗粒32；图1仅显示了本发明的一个实施例，不限于此，以相邻两层纳米纤维抗菌层1之间设置有纳米纤维亲水层2为一个基本组成单位，纳米纤维抗菌非织造材料可以包括两个、三个、四个或更多个基本组成单位，具体可根据实际产品的需要来调节基本组成单位的组成个数。如图2所示，纳米纤维4在三维空间交叉排列，形成具有纳米微粒、纳米纤维团簇的孔洞；或者说，纳米纤维4在三维空间交叉排列形成若干个接点，经纺丝后的纳米纤维4平均直径约小、数量越多，形成的接点越多。如图3所示，接点周围分布有纳米银抗菌颗粒31以及纳米氧化锌抗菌颗粒32，并且接点越多，纳米银抗菌颗粒31和纳米氧化锌抗菌颗粒32 的分布越多，抗菌功能越好。
下面通过具体实施例来说明本发明制备的纳米纤维抗菌非织造材料的性能。如无具体说明，本发明的各种原料均可市售购得，或根据本领域的常规方法制备得到。
实施例1
在20g聚丙烯中添加0.2g的纳米银抗菌颗粒和0.5g的纳米氧化锌抗菌颗粒制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为1～2ml/h，纺丝电压为60KV，接收距离为40cm，制备纳米纤维抗菌材料；将20g聚丙烯熔融后制备成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为1～2ml/h，纺丝电压为60KV，接收距离为40cm，制备纳米纤维材料，将亲水剂用高纯水稀释后制备成亲水溶剂，将亲水溶剂涂覆于所述纳米纤维材料后，经烘干制备纳米纤维亲水材料；将制备的纳米银的纳米纤维抗菌材料与纳米纤维亲水材料交叉铺设，经热轧后制备成具有纳米纤维抗菌层和纳米纤维亲水层的纳米纤维抗菌非织造材料。测试制备的纳米纤维抗菌非织造材料的抗菌性能，结果表明对金黄色葡萄球菌、大肠杆菌、白色念球菌等代表菌的抑菌率大于99.9％，2小时抑菌率大于98％；测试制备的纳米纤维抗菌非织造材料的亲水性能，滴水穿透时间为0.8s，亲水倍率为500％以上。
实施例2
在10g聚丙烯中添加0.1g的纳米银抗菌颗粒和0.5g的纳米氧化锌抗菌颗粒制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为1～2ml/h，纺丝电压为40KV，接收距离为20cm，制备纳米纤维抗菌材料；将10g聚丙烯熔融后制成纺丝液，在纺丝液喷头上施加高压正电， 对纺丝液进行静电纺丝，纺丝液的挤出速率为1～2ml/h，纺丝电压为40KV，接收距离为20cm，制备纳米纤维材料，将亲水剂用高纯水稀释后制备成亲水溶剂，将亲水溶剂涂覆于所述纳米纤维材料后，经烘干制备纳米纤维亲水材料；将制备的纳米银的纳米纤维抗菌材料与纳米纤维亲水材料交叉铺设，经热轧后制备成具有纳米纤维抗菌层和纳米纤维亲水层的纳米纤维抗菌非织造材料。测试制备的纳米纤维抗菌非织造材料的抗菌性能，结果表明对金黄色葡萄球菌、大肠杆菌、白色念球菌等代表菌的抑菌率大于99.9％，2小时抑菌率大于98％；测试制备的纳米纤维抗菌非织造材料的亲水性能，滴水穿透时间为0.8s，亲水倍率为500％以上。
实施例3
在15g聚丙烯中添加0.15g的纳米银抗菌颗粒和0.75g的纳米氧化锌抗菌颗粒制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为0.5～1ml/h，纺丝电压为35KV，接收距离为25cm，制备纳米纤维抗菌材料；将15g聚丙烯经熔融后制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为0.5～1ml/h，纺丝电压为35KV，接收距离为25cm，制备纳米纤维材料，将亲水剂用高纯水稀释后制备成亲水溶剂，将亲水溶剂涂覆于所述纳米纤维材料后，经烘干制备纳米纤维亲水材料；将制备的纳米银的纳米纤维抗菌材料与纳米纤维亲水材料交叉铺设，经热轧后制备成具有纳米纤维抗菌层和纳米纤维亲水层的纳米纤维抗菌非织造材料。测试制备的纳米纤维抗菌非织造材料的抗菌性能，结果表明对金黄色葡萄球菌、大肠杆菌、白色念球菌等代表菌的抑菌率大于99.9％，2小时抑菌率大于98％；测试制备的纳米纤维抗菌非织造材料的亲水性能，滴水穿透时间为0.8s，亲水倍率为500％以上。
实施例4
在12g聚丙烯中添加0.12g的纳米银抗菌颗粒和0.8g的纳米氧化锌抗菌颗粒制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为1～1.5ml/h，纺丝电压为30KV，接收距离为15cm，制备纳米纤维抗菌材料；将12g聚丙烯熔融后制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝液的挤出速率为1～1.5ml/h，纺丝电压为30KV，接收距离为15cm，制备纳米纤维材料，将亲水剂用高纯水稀释后制备成亲水溶剂，将亲水溶剂涂覆于所述纳米纤维材料后，经烘干制备纳米纤维亲水材料；将制备的纳米银的纳米纤维抗菌材料与纳米纤维亲水材料交叉铺设，经热轧后制备成具有纳米纤维抗菌层和纳米纤维亲水层的纳米纤维抗菌非织造材料。测试制备的纳米纤维抗菌非织造材料的抗菌性能，结果表明对金黄色葡萄球菌、大肠杆菌、白色念球菌等代表菌的抑菌率大于99.9％，2小时抑菌率大于98％；测试制备的纳米纤维抗菌非织造材料的亲水性能，滴水穿透时间为0.9s，亲水倍率为500％以上。
本发明的纳米纤维抗菌非织造材料，抗菌性能好，抗菌效果持久性强，并且亲水性能优良，亲水倍率达500％以上，并且本发明的制备方法工艺简单，纳米级别的抗菌颗粒在纳米纤维中分布均匀，结合牢固，保证了连续生产，并且提高了产品的抗菌性能，制备得到的纳米纤维抗菌非织造材料可以广泛应用于日用品、医疗保健、婴幼儿及成人卫生用品等领域。
尽管本发明中所涉及的数值范围(尺寸、工艺参数)在上述实施例中未列举出具体数值，但本领域的技术人员完全可以想象到只要落入上述该数值范围内的任何数值均可实施本发明，当然也包括若干项数值范围内具体值的任意组 合。此处，出于篇幅的考虑，省略了给出某一项或多项数值范围内具体值的实施例，此不应当视为本发明的技术方案的公开不充分。
申请人声明，本发明通过上述实施例来说明本发明的技术原理。这些描述只是为了解释本发明的原理，而不能以任何方式解释为对本发明保护范围的限制。所属技术领域的技术人员应该明了，对本发明的任何改进，对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等，均落在本发明的保护范围和公开范围之内。

Claims (10)

  1. 一种纳米纤维抗菌非织造材料，其特征在于，包括至少两层纳米纤维抗菌层，相邻两层所述纳米纤维抗菌层之间设置有纳米纤维亲水层，所述纳米纤维抗菌层的纳米纤维在三维空间交叉排列，形成具有纳米微粒、纳米纤维团簇的孔洞，所述孔洞内分布有纳米银抗菌颗粒以及纳米氧化锌抗菌颗粒。
  2. 根据权利要求1所述的纳米纤维抗菌非织造材料，其特征在于，所述纳米纤维抗菌层的纳米纤维在三维空间交叉排列形成接点，所述接点周围分布有所述纳米银抗菌颗粒以及所述纳米氧化锌抗菌颗粒。
  3. 根据权利要求1所述的纳米纤维抗菌非织造材料，其特征在于，所述纳米纤维抗菌层的纳米纤维的平均直径为0.1～500nm。
  4. 根据权利要求1所述的纳米纤维抗菌非织造材料，其特征在于，所述纳米纤维抗菌层的厚度为10～100μm；
    优选地，所述纳米纤维亲水层的厚度为10～50μm；
    优选地，所述纳米银抗菌颗粒的平均粒径为20～30nm；
    优选地，所述纳米氧化锌抗菌颗粒的平均粒径为10～150nm，所述纳米氧化锌抗菌颗粒为一维纳米氧化锌抗菌颗粒；
    更优选地，所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒的质量比为1∶(2～10)。
  5. 根据权利要求1所述的纳米纤维抗菌非织造材料，其特征在于，所述纳米纤维抗菌层由添加了所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒的纺丝液经静电纺丝制备而成，所述纺丝液包括聚合物。
  6. 根据权利要求5所述的纳米纤维抗菌非织造材料，其特征在于，所述聚合物为聚丙烯。
  7. 根据权利要求5所述的纳米纤维抗菌非织造材料，其特征在于，所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒总量与所述聚合物的质量比为1∶(15～30)。
  8. 一种如权利要求1所述的纳米纤维抗菌非织造材料的制备方法，其特征在于，包括如下步骤：
    1)采用包含有纳米银抗菌颗粒和纳米氧化锌抗菌颗粒的纺丝液制备纳米纤维抗菌材料；
    2)制备纳米纤维亲水材料；
    3)将步骤1)制备的纳米纤维抗菌材料和步骤2)制备的纳米纤维亲水材料交叉铺设，经热轧后制备成具有纳米纤维抗菌层和纳米纤维亲水层的纳米纤维抗菌非织造材料。
  9. 根据权利要求8所述的制备方法，其特征在于，
    步骤1)的具体过程为：在聚合物中添加纳米银抗菌颗粒和纳米氧化锌抗菌颗粒，熔融后制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，制备纳米纤维抗菌材料；
    优选地，步骤2)的具体过程为：将聚合物熔融后制成纺丝液，在纺丝液喷头上施加高压正电，对纺丝液进行静电纺丝，纺丝后得到纳米纤维材料，将所述纳米纤维材料经亲水处理后制备得到纳米纤维亲水材料。
  10. 根据权利要求9所述的制备方法，其特征在于，步骤1)和步骤2)中，所述聚合物为聚丙烯；
    所述静电纺丝的具体工艺参数为：纺丝液的挤出速率为0.5～2ml/h，纺丝电压为30～60KV，接收距离为15～40cm；
    优选地，步骤1)中，所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒的 质量比为1∶(2～10)；所述纳米银抗菌颗粒和所述纳米氧化锌抗菌颗粒总量与所述聚合物的质量比为1∶(15～30)；
    步骤2)中，所述亲水处理为：将亲水剂用高纯水稀释后制备成亲水溶剂，将亲水溶剂涂覆于所述纳米纤维材料后，经烘干制备纳米纤维亲水材料。
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