CN111996614A - Antibacterial nanofiber material and application thereof - Google Patents

Antibacterial nanofiber material and application thereof Download PDF

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CN111996614A
CN111996614A CN202010675225.2A CN202010675225A CN111996614A CN 111996614 A CN111996614 A CN 111996614A CN 202010675225 A CN202010675225 A CN 202010675225A CN 111996614 A CN111996614 A CN 111996614A
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titanium dioxide
antibacterial
nanofiber material
modified titanium
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不公告发明人
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Jiaxing Juetuo Technology Co ltd
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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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • 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
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent

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  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Artificial Filaments (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention discloses an antibacterial nanofiber material and application thereof, belonging to the technical field of nanofiber materials, and the antibacterial nanofiber material is prepared by carrying out electrostatic spinning on a spinning solution containing modified titanium dioxide nanoparticles, wherein the preparation method of the modified titanium dioxide nanoparticles comprises the following steps: uniformly mixing polydatin and titanium dioxide nanoparticle dispersion liquid, adding water while stirring, performing suction filtration, washing, performing ball milling by using a ball mill, and calcining to obtain modified titanium dioxide nanoparticles. The antibacterial nanofiber material prepared from the modified titanium dioxide nanoparticles, PET and PA6 has the antibacterial performance at least up to 90%, and the antibacterial rate is reduced by less than 1% after washing for 50 times.

Description

Antibacterial nanofiber material and application thereof
Technical Field
The invention belongs to the technical field of nanofiber materials, and particularly relates to a nanofiber material with antibacterial property and application thereof.
Background
The antibacterial fiber is a novel functional fiber with the function of killing or inhibiting microorganisms, and is widely used for household textiles (including underwear, sport suits, old pregnant infant clothes and the like) and medical textiles (surgical gowns, hospital gowns, bedsheets, curtains, bandages and the like). The fabric made of the antibacterial fiber can resist the adhesion of bacteria on the fabric, reduce the bacteria number on the fabric, ensure the safety between people and fabric and environment and keep people away from the invasion of germs. The earliest concept of using antibacterial materials by human beings dates back to the age of rock novelties over ten thousand years ago, and then people begin to use salt to pickle foods for long-term storage, and the salt becomes the earliest antiseptic and antibacterial material used by human beings. Currently, the most popular is to finish the fibers with antimicrobial agents.
The antibacterial agent can be classified into inorganic type, organic type and natural type. The inorganic antibacterial agent is widely applied due to the advantages of broad-spectrum antibacterial property, durability, washing resistance, heat resistance, acid and alkali resistance, difficult generation of drug resistance by bacteria, no toxicity or harm to human health and the like. Inorganic antimicrobial agents generally refer to metal ions having antimicrobial function, such as Ag+、Cu2+、Zn2+、Ti4+And the like, which have strong killing effect on most pathogenic bacteria, can be sterilized by only adding 6 to 10 percent (mass fraction). In recent years, inorganic antibacterial agents typified by titanium dioxide fine aggregate particles have been widely studied and used. The titanium dioxide nano particles have the characteristics of simple application process and low cost, can decompose bacteria and pollutants under natural light, have good chemical stability, thermal stability, no irritation, no secondary pollution, safety, no toxicity and the like, become one of green and environment-friendly nano antibacterial materials with the development prospect, and have great practical application significance and profound development significance.
In the process of adding titanium dioxide nanoparticles into spinning solution for electrostatic spinning to obtain the antibacterial fiber, the titanium dioxide nanoparticles are easy to form aggregates and block a needle head, so that the antibacterial effect is poor, the durability of the fiber loaded with the titanium dioxide nanoparticles is poor, the titanium dioxide nanoparticles are easy to fall off in the processes of washing and rubbing to influence the antibacterial effect, and when the titanium dioxide nanoparticles are added into the spinning solution for spinning to prepare the antibacterial fiber, nodes are formed in the fiber, and the mechanical property of the fiber is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of modified titanium dioxide with small particle size and antibacterial effect.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a method for producing a modified titanium dioxide, comprising: uniformly mixing polydatin and titanium dioxide nanoparticle dispersion liquid, adding water while stirring, performing suction filtration, washing, performing ball milling by using a ball mill, and calcining to obtain modified titanium dioxide nanoparticles. After titanium dioxide nanoparticles are modified by polydatin, titanium oxide-carbon bonds are generated on the surfaces of the nanoparticles, non-bonding parts of the polydatin are coated on the surfaces to form a protective film, a barrier is established between the protective film and surrounding media, the dispersibility of the titanium dioxide nanoparticles is improved, the number of nodes in spinning fibers is reduced, and the polydatin forms interaction force with main fiber molecules under the action of a chain structure due to hydroxyl and phenyl groups of the polydatin, so that the fibers and titanium dioxide are combined more tightly, and the titanium dioxide nanoparticles can be prevented from being separated from the fibers by mechanical operations such as washing and the like; the modified titanium dioxide nano particles improve the dispersibility, the obtained small-particle-size nano particles are more stable and are not easy to agglomerate and block a spinning needle, and the titanium dioxide nano particles are uniformly loaded on the fiber when the fiber is spun, so that the antibacterial active sites are increased, and the antibacterial effect is improved.
Preferably, the titanium dioxide nanoparticles are modified: ultrasonically dispersing titanium dioxide nanoparticles in absolute ethyl alcohol to obtain titanium dioxide nanoparticle dispersion liquid, adding polydatin, stirring and dispersing for 0.5-3h to obtain polydatin/titanium dioxide mixed liquid; adding water into the mixed solution under stirring, performing suction filtration, dispersing the filter cake in water again, stirring for 0.5-3h, and repeating the suction filtration and washing for 2-3 times; drying at the temperature of 20-50 ℃, and ball-milling for 3-12h by using a ball mill to obtain titanium dioxide pretreatment powder; placing the titanium dioxide pretreatment powder in a crucible, calcining in a muffle furnace at 100-180 ℃ for 2-6h, and preparing to obtain modified titanium dioxide; the mass fraction of the titanium dioxide nano particle dispersion liquid is 0.5-5 wt%, the addition amount of polydatin is 500 wt% of the titanium dioxide nano particles, and the addition amount of water in the mixed solution is 80-400 wt% of absolute ethyl alcohol.
More preferably, the stirring speed is 100-500r/min during the modification of the titanium dioxide nano particles.
More preferably, the rate of addition of water to the mixture is 1-5 mL/min.
More preferably, the ball milling strength is 200-.
The invention also aims to provide a preparation method of the antibacterial nanofiber material with good antibacterial effect, good washing resistance effect and good mechanical property.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of an antibacterial nanofiber material comprises the following steps: dissolving PET slices, PA6 particles and the modified titanium dioxide of claim 4 in a solvent, uniformly stirring, and then carrying out electrostatic spinning to obtain an antibacterial nanofiber material; the solvent is a mixed solution of dichloromethane and trifluoroacetic acid.
Preferably, the antibacterial nanofiber material is prepared by: dissolving PET slices, PA6 particles and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 5-9 wt% of the solvent, the adding amount of the PA6 particles is 1-5 wt% of the solvent, the adding amount of the modified titanium dioxide nanoparticles is 2-10 wt% of the PET chips, the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 20-90 wt%, and the mass fraction of the trifluoroacetic acid is 10-80 wt%.
Preferably, the antibacterial nanofiber material can also be prepared as follows: dissolving PET slices, PA6 particles, lanosterol, isomagnoflorine and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 5-9 wt% of the solvent, the adding amount of the PA6 particles is 1-5 wt% of the solvent, the adding amount of the lanosterol is 1-8 wt% of the PET chips, the adding amount of the isomagnoflorine is 1-10 wt% of the PET chips, the adding amount of the modified titanium dioxide nanoparticles is 2-10 wt% of the PET chips, the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 20-90 wt%, and the mass fraction of the trifluoroacetic acid is 10-80 wt%. Lanosterol has a multi-element annular structure, and molecules of lanosterol contain chain structures, so that the lanosterol and polydatin of the modified titanium dioxide nanoparticles can form an entangled form in spinning, and a rigid structure is formed due to the annular structure and entanglement in the molecules, so that the mechanical strength of spinning fibers is improved; the isomagnoflorine molecules contain benzene rings and ether bond structures, the molecules can rotate freely, and the isomagnoflorine contains hydroxyl groups, ether groups, carbonyl groups and other groups, so that hydrogen bonds can be formed among the isomagnoflorine, the modified titanium dioxide nano particles, PA6 and PET, and the mechanical property of the spinning fiber is improved; when the lanosterol and the isomagnoflorine are added together, hydrogen bonds and intermolecular entanglement are formed between the lanosterol and the polydatin in the modified nanoparticles, and a tighter effect is formed between the lanosterol and the polydatin and between the lanosterol and PET and PA6, so that stronger mechanical properties are provided for spinning fibers.
The antibacterial nanofiber material is prepared from the modified titanium dioxide nanoparticles, the lanosterol and the isomagnoflorine, so that the antibacterial nanofiber material has the following beneficial effects: the antibacterial rate is high and reaches at least 90 percent; after 50 times of washing, the antibacterial property is reduced, and the antibacterial rate is reduced by less than 1%; the mechanical property is improved, and the tensile strength is improved by at least 6 percent. Therefore, the invention is a preparation method of the antibacterial nanofiber material with good antibacterial effect, good washing resistance effect and good mechanical property. The antibacterial fiber obtained by the invention can be used for household textiles and medical textiles.
Drawings
FIG. 1 is an infrared image of titanium dioxide nanoparticles before and after modification;
FIG. 2 is a graph of antimicrobial rate of antimicrobial nanofiber material before and after washing;
FIG. 3 is a drawing mechanics diagram of the antibacterial nanofiber material;
fig. 4 is a graph of the elongation at break of the antimicrobial nanofiber material;
fig. 5 is a graph of young's modulus of the antibacterial nanofiber material.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
example 1:
a method for preparing antibacterial nano-fiber,
modification of titanium dioxide nanoparticles: ultrasonically dispersing titanium dioxide nanoparticles in absolute ethyl alcohol to obtain titanium dioxide nanoparticle dispersion liquid, adding polydatin, stirring and dispersing for 1h to obtain polydatin/titanium dioxide mixed liquid; adding water into the mixed solution under stirring, performing suction filtration, dispersing the filter cake in water again, stirring for 1h, and repeating the suction filtration and washing for 2 times; drying at the temperature of 25 ℃, and ball-milling for 12 hours by using a ball mill to obtain titanium dioxide pretreatment powder; placing the titanium dioxide pretreatment powder in a crucible, calcining for 4 hours in a muffle furnace at 150 ℃ to prepare modified titanium dioxide; the mass fraction of the titanium dioxide nanoparticle dispersion liquid is 4 wt%, the addition amount of polydatin is 160 wt% of the titanium dioxide nanoparticles, the addition amount of water in the mixed solution is 200 wt% of absolute ethyl alcohol, the stirring speed is 200r/min in the modification process of the titanium dioxide nanoparticles, the speed of adding water in the mixed solution is 5mL/min, and the ball milling strength is 300 r/min.
Preparing an antibacterial nanofiber material: dissolving PET slices, PA6 particles and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 6 wt% of the solvent, the adding amount of the PA6 particles is 4 wt% of the solvent, the adding amount of the modified titanium dioxide nanoparticles is 8 wt% of the PET chips, and the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 60 wt%, and the mass fraction of the trifluoroacetic acid is 40 wt%.
Electrostatic spinning parameters: the spinning speed is 0.002mm/s, the voltage is 14.5kV, and the receiving distance is 15 cm.
Example 2:
a method for preparing antibacterial nano-fiber,
modification of titanium dioxide nanoparticles: ultrasonically dispersing titanium dioxide nanoparticles in absolute ethyl alcohol to obtain titanium dioxide nanoparticle dispersion liquid, adding polydatin, stirring and dispersing for 1h to obtain polydatin/titanium dioxide mixed liquid; adding water into the mixed solution under stirring, performing suction filtration, dispersing the filter cake in water again, stirring for 1h, and repeating the suction filtration and washing for 2 times; drying at the temperature of 25 ℃, and ball-milling for 12 hours by using a ball mill to obtain titanium dioxide pretreatment powder; placing the titanium dioxide pretreatment powder in a crucible, calcining for 4 hours in a muffle furnace at 150 ℃ to prepare modified titanium dioxide; the mass fraction of the titanium dioxide nanoparticle dispersion liquid is 4 wt%, the addition amount of polydatin is 300 wt% of the titanium dioxide nanoparticles, the addition amount of water in the mixed solution is 200 wt% of absolute ethyl alcohol, the stirring speed is 200r/min in the modification process of the titanium dioxide nanoparticles, the speed of adding water in the mixed solution is 5mL/min, and the ball milling strength is 300 r/min.
Preparing an antibacterial nanofiber material: dissolving PET slices, PA6 particles and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 6 wt% of the solvent, the adding amount of the PA6 particles is 4 wt% of the solvent, the adding amount of the modified titanium dioxide nanoparticles is 8 wt% of the PET chips, and the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 60 wt%, and the mass fraction of the trifluoroacetic acid is 40 wt%.
Electrostatic spinning parameters: the spinning speed is 0.002mm/s, the voltage is 14.5kV, and the receiving distance is 15 cm.
Example 3:
a method for preparing antibacterial nano-fiber,
modification of titanium dioxide nanoparticles: ultrasonically dispersing titanium dioxide nanoparticles in absolute ethyl alcohol to obtain titanium dioxide nanoparticle dispersion liquid, adding polydatin, stirring and dispersing for 1h to obtain polydatin/titanium dioxide mixed liquid; adding water into the mixed solution under stirring, performing suction filtration, dispersing the filter cake in water again, stirring for 1h, and repeating the suction filtration and washing for 2 times; drying at the temperature of 25 ℃, and ball-milling for 12 hours by using a ball mill to obtain titanium dioxide pretreatment powder; placing the titanium dioxide pretreatment powder in a crucible, calcining for 4 hours in a muffle furnace at 150 ℃ to prepare modified titanium dioxide; the mass fraction of the titanium dioxide nanoparticle dispersion liquid is 4 wt%, the addition amount of polydatin is 300 wt% of the titanium dioxide nanoparticles, the addition amount of water in the mixed solution is 200 wt% of absolute ethyl alcohol, the stirring speed is 200r/min in the modification process of the titanium dioxide nanoparticles, the speed of adding water in the mixed solution is 5mL/min, and the ball milling strength is 300 r/min.
Preparing an antibacterial nanofiber material: dissolving PET slices, PA6 particles and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 6 wt% of the solvent, the adding amount of the PA6 particles is 4 wt% of the solvent, the adding amount of the modified titanium dioxide nanoparticles is 4 wt% of the PET chips, the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 60 wt%, and the mass fraction of the trifluoroacetic acid is 40 wt%.
Electrostatic spinning parameters: the spinning speed is 0.002mm/s, the voltage is 14.5kV, and the receiving distance is 15 cm.
Example 4:
a method for preparing antibacterial nano-fiber,
modification of titanium dioxide nanoparticles: ultrasonically dispersing titanium dioxide nanoparticles in absolute ethyl alcohol to obtain titanium dioxide nanoparticle dispersion liquid, adding polydatin, stirring and dispersing for 1h to obtain polydatin/titanium dioxide mixed liquid; adding water into the mixed solution under stirring, performing suction filtration, dispersing the filter cake in water again, stirring for 1h, and repeating the suction filtration and washing for 2 times; drying at the temperature of 25 ℃, and ball-milling for 12 hours by using a ball mill to obtain titanium dioxide pretreatment powder; placing the titanium dioxide pretreatment powder in a crucible, calcining for 4 hours in a muffle furnace at 150 ℃ to prepare modified titanium dioxide; the mass fraction of the titanium dioxide nanoparticle dispersion liquid is 4 wt%, the addition amount of polydatin is 300 wt% of the titanium dioxide nanoparticles, the addition amount of water in the mixed solution is 200 wt% of absolute ethyl alcohol, the stirring speed is 200r/min in the modification process of the titanium dioxide nanoparticles, the speed of adding water in the mixed solution is 5mL/min, and the ball milling strength is 300 r/min.
Preparing an antibacterial nanofiber material: dissolving PET slices, PA6 particles, lanosterol, isomagnoflorine and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 6 wt% of the solvent, the adding amount of the PA6 particles is 4 wt% of the solvent, the adding amount of the lanosterol is 2 wt% of the PET chips, the adding amount of the isomagnoflorine is 2 wt% of the PET chips, the adding amount of the modified titanium dioxide nanoparticles is 8 wt% of the PET chips, and the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 60 wt%, and the mass fraction of the trifluoroacetic acid is 40 wt%.
Electrostatic spinning parameters: the spinning speed is 0.002mm/s, the voltage is 14.5kV, and the receiving distance is 15 cm.
Example 5:
a method for preparing antibacterial nano-fiber,
modification of titanium dioxide nanoparticles: ultrasonically dispersing titanium dioxide nanoparticles in absolute ethyl alcohol to obtain titanium dioxide nanoparticle dispersion liquid, adding polydatin, stirring and dispersing for 1h to obtain polydatin/titanium dioxide mixed liquid; adding water into the mixed solution under stirring, performing suction filtration, dispersing the filter cake in water again, stirring for 1h, and repeating the suction filtration and washing for 2 times; drying at the temperature of 25 ℃, and ball-milling for 12 hours by using a ball mill to obtain titanium dioxide pretreatment powder; placing the titanium dioxide pretreatment powder in a crucible, calcining for 4 hours in a muffle furnace at 150 ℃ to prepare modified titanium dioxide; the mass fraction of the titanium dioxide nanoparticle dispersion liquid is 4 wt%, the addition amount of polydatin is 300 wt% of the titanium dioxide nanoparticles, the addition amount of water in the mixed solution is 200 wt% of absolute ethyl alcohol, the stirring speed is 200r/min in the modification process of the titanium dioxide nanoparticles, the speed of adding water in the mixed solution is 5mL/min, and the ball milling strength is 300 r/min.
Preparing an antibacterial nanofiber material: dissolving PET slices, PA6 particles, lanosterol, isomagnoflorine and modified titanium dioxide nano particle powder in a solvent to obtain a spinning solution, and statically spinning to obtain an antibacterial nanofiber material; the adding amount of the PET chips is 6 wt% of the solvent, the adding amount of the PA6 particles is 4 wt% of the solvent, the adding amount of the lanosterol is 6 wt% of the PET chips, the adding amount of the isomagnoflorine is 8 wt% of the PET chips, the adding amount of the modified titanium dioxide nanoparticles is 8 wt% of the PET chips, and the solvent is a mixed solution of dichloromethane and trifluoroacetic acid, wherein the mass fraction of the dichloromethane is 60 wt%, and the mass fraction of the trifluoroacetic acid is 40 wt%.
Electrostatic spinning parameters: the spinning speed is 0.002mm/s, the voltage is 14.5kV, and the receiving distance is 15 cm.
Comparative example 1:
compared with example 2, the comparative example is different only in that the modified titanium dioxide nanoparticle powder is replaced by the titanium dioxide nanoparticle powder in the preparation of the antibacterial nanofiber material.
Comparative example 2:
compared with example 2, the comparative example is different only in that the modified titanium dioxide nanoparticle powder is not added in the preparation of the antibacterial nanofiber material.
Comparative example 3:
compared with example 5, the difference of the comparative example is that no isomagnoflorine is added in the preparation of the antibacterial nanofiber material.
Comparative example 4:
the comparative example is different from example 5 only in that lanosterol is not added in the preparation of the antibacterial nanofiber material.
Test example 1:
1. infrared spectroscopy detection
Drying the titanium dioxide nanoparticle samples before and after modification obtained in the embodiment 2 in a vacuum drying oven at 50 ℃ for 24h, tabletting by KBr, and performing a spectrum range of 500-4000cm-1。
The infrared test is shown in fig. 1, wherein a is the infrared spectrum of the titanium dioxide nano particles, and b is the spectrum of the modified titanium dioxide nano particles; compared with the titanium dioxide nano-particle, the infrared spectrum of the modified titanium dioxide nano-particle is 3000-3600cm-1A stronger hydroxyl absorption peak appears between the two, and the peak is 2930cm-1The absorption peak of alkyl appears at 1320cm-1The absorption peak of titanium, carbon and oxygen appears, which indicates that the polydatin and the titanium dioxide nano particles generate titanium, carbon and oxygen chemical bonds through dehydration reaction under the calcination condition, and indicates that the polydatin is successfully grafted to the titanium dioxide nano particles.
2. Particle size measurement
The titanium dioxide nanoparticles before, after and after modification obtained in example 2 were prepared into a solution having a concentration of 0.1g/L, 1mL of the solution was added to a sample cell (1 cm. times.1 cm. times.4 cm), and the aggregate particle diameter in the solution was measured by a nanometer laser particle size analyzer.
TABLE 1 titanium dioxide nanoparticle size
Figure BDA0002583808120000071
Particle size test as shown in table 1, the particle size of the modified titanium dioxide nanoparticles obtained in example 2 is smaller, and the particle size after ball milling is also better than that of example 1, which indicates that the titanium dioxide nanoparticles with smaller particle size can be obtained when the addition amount of polydatin is higher.
Test example 2:
1. antibacterial testing
1.1 Pre-Wash antibacterial test
Bacterial culture
(1) Preparation of nutrient agar culture medium: weighing 60g of agar powder, dissolving the agar powder in 1000mL of sterilized distilled water, heating and dissolving, after complete dissolution, performing steam sterilization at 120 ℃ for 20min, taking out a sterilized agar culture medium, pouring the agar culture medium into sterilized culture dishes in a super clean bench, subpackaging each culture dish by about 15mL on average, after the agar is cooled and solidified, collecting the agar culture medium and packaging with a sealing film;
(2) preparation of nutrient broth culture solution: weighing 5g of beef extract, 10g of peptone and 5g of sodium chloride, adding the beef extract, the peptone and the sodium chloride into sterilized distilled water for dissolving, after complete dissolution, performing steam sterilization at 120 ℃ for 20min, taking out sterilized broth culture medium, subpackaging the broth culture medium into sterilized test tubes with plugs in a super clean bench, subpackaging 10mL of each test tube on average, and performing steam sterilization at 120 ℃ for 20min on the test tubes filled with nutrient broth culture solution;
(3) the E.coli strain (100. mu.L) was added to the test tube of the nutrient broth described in step (2) by a pipette in a sterile operation, and the test tube was placed in a biochemical incubator and cultured at 37 ℃ for 24 hours.
Determination of bacterial concentration
(1) Marking the bacterial liquid cultured in the bacterial culture step (3) as a bacterial stock solution, taking 1mL of the bacterial stock solution by a pipette for aseptic operation, filling the bacterial stock solution into 10mL of nutrient broth culture solution test tubes subpackaged in the step (2), and shaking up;
(2) transferring 1mL of the bacterial liquid according to the operation (1), adding the bacterial liquid into a 10mL nutrient broth culture liquid test tube which is subpackaged in the bacterial culture step (2), and shaking up to obtain bacterial liquid;
(3) taking 100 mu L of the bacterial liquid out, uniformly coating the bacterial liquid on a nutrient agar culture substrate prepared in the bacterial culture step (1), placing the nutrient agar culture substrate in a biochemical incubator, and culturing for 24 hours at 37 ℃;
(4) after the culture is completed, the number of bacteria in the culture dish is counted, and the concentration of the initially cultured bacteria is 6.9X 107CFU/mL。
The antibacterial nanofiber materials obtained in the examples and the comparative examples are placed in a culture dish filled with bacterial liquid with known concentration, the culture dish is placed under a 15W ultraviolet lamp for 8cm, and after 8min, the concentration of the bacterial liquid in one experiment is measured by using a plate coating method.
1.2 post-Wash antibacterial testing
10g of the antibacterial nanofiber material obtained in each example and comparative example was put into an SW-12A type colorfastness to washing tester (a tin-free textile apparatus factory), water and 6g of a neutral detergent were added, washing was carried out at 40 ℃ for 25min, water was drained, washing was carried out with water for 2min, dewatering was carried out for 1min, washing was carried out again for 2min, dewatering was carried out for 1min, which was one cycle, 1 washing was counted, and this cycle was repeated until 50 washes were reached. And finally, drying the antibacterial nanofiber material for antibacterial performance test.
The antibacterial test result is shown in fig. 2, wherein in the antibacterial test result before washing, the antibacterial effect of example 2 is the best, reaching 99.3%, and the antibacterial effect of comparative example 2 is the worst, only 33.5%; compared with the example 1, the example 2 shows that when the titanium dioxide nano particles are modified, the higher the addition amount of the polydatin is, the better the dispersibility of the corresponding titanium dioxide nano particles is, and the better the antibacterial performance is; compared with example 3, the example 2 shows that the higher the addition amount of the modified titanium dioxide nano particles is, the better the antibacterial performance is; compared with the comparative example 1, the example 2 shows that the antibacterial performance of the modified titanium dioxide nano particles is better than that of the unmodified titanium dioxide nano particles; compared with the comparative example 2, the antibacterial performance of the fiber obtained by adding the modified dioxide nano particles is better than that of the fiber without the modified dioxide nano particles;
in the antibacterial test result after washing, the antibacterial performance of the same example 2 is the best, the antibacterial rate is reduced by 0.4%, the antibacterial performance of the performance comparative example 2 is the worst, and the antibacterial rate is reduced by 2.9%; compared with the example 1, the antibacterial rate of the example 1 is reduced by 0.8%, which shows that when the titanium dioxide nanoparticles are modified, the higher the addition amount of the polydatin is, the better the binding property of the corresponding titanium dioxide nanoparticles in the spinning fiber is, and the smaller the rise and fall of the antibacterial performance after washing is; compared with example 3, the antibacterial rate of example 3 is reduced by 0.6%, which shows that the higher the addition amount of the modified titanium dioxide nanoparticles is, the less the antibacterial performance is reduced after washing; compared with the comparative example 1, the example 2 shows that the antibacterial performance of the titanium dioxide nano particles after being modified and washed is superior to that of the unmodified titanium dioxide nano particles; example 2 compared to comparative example 2, shows that the antibacterial performance of the fiber obtained after adding the modified dioxide nanoparticles is better than that of the fiber without adding.
2. Mechanical Property test
And (4) adopting a universal tester to test the tensile mechanical property.
The antibacterial nanofiber materials obtained in each example and comparative example were prepared into a rectangular sample of 4 × 150mm, and the tensile test was performed at a loading rate of 15 mm/min. On average, 6 tests were performed per sample.
Among the mechanical property test results, the tensile strength test result is shown in fig. 3, the elongation at break test result is shown in fig. 4, and the young's modulus test result is shown in fig. 5.
In the tensile strength test results, the tensile strength of example 5 is the best, and the tensile strength of example 2 is the worst; compared with example 2, the example 5 shows that the addition of lanosterol and isomagnoflorine improves the mechanical strength of the antibacterial nanofiber material; compared with example 4, the example 5 shows that the mechanical strength of the antibacterial nanofiber material can be further improved by increasing the addition amount of lanosterol and isomagnoflorine; example 5 compared to comparative example 3, shows that the use of lanosterol in combination with isomagnoflorine is superior to the use of lanosterol alone; example 5 compared to comparative example 4, shows that the use of lanosterol together with isomagnoflorine is superior to the use of isomagnoflorine alone; compared with example 2, the comparison example 3 shows that the mechanical strength of the antibacterial nanofiber material can be improved by adding the lanosterol alone; compared with the example 2, the comparative example 4 shows that the mechanical strength of the antibacterial nanofiber material can be improved by adding isomagnoflorine alone; and also proves that the effect of the common use of the lanosterol and the isomagnoflorine is better than that of the single use of either substance.
The variation trend of the measurement result of the elongation at break is consistent with the variation trend of the Young modulus test result and the variation trend of the tensile strength, and the effects of lanosterol and isomagnoflorine can be proved.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.

Claims (10)

1. A method for producing a modified titanium dioxide, comprising: uniformly mixing polydatin and titanium dioxide nanoparticle dispersion liquid, adding water while stirring, performing suction filtration, washing, performing ball milling by using a ball mill, and calcining to obtain modified titanium dioxide nanoparticles.
2. The process for producing a modified titanium dioxide as claimed in claim 1, wherein: the mass fraction of the titanium dioxide nano particle dispersion liquid is 0.5-5 wt%.
3. The process for producing a modified titanium dioxide as claimed in claim 1, wherein: the addition amount of the polydatin is 500 wt% of the titanium dioxide nano-particles.
4. A modified titanium dioxide produced by the process according to any one of claims 1 to 3.
5. Use of the modified titanium dioxide as claimed in claim 4 in an antibacterial material.
6. A preparation method of an antibacterial nanofiber material comprises the following steps: dissolving PET slices, PA6 particles and the modified titanium dioxide of claim 4 in a solvent, uniformly stirring, and then carrying out electrostatic spinning to obtain an antibacterial nanofiber material; the solvent is a mixed solution of dichloromethane and trifluoroacetic acid.
7. The method for preparing an antibacterial nanofiber material as claimed in claim 6, which is characterized in that: in the solvent, the mass fraction of the dichloromethane is 20-90 wt%, and the mass fraction of the trifluoroacetic acid is 10-80 wt%.
8. The method for preparing an antibacterial nanofiber material as claimed in claim 6, which is characterized in that: the adding amount of the PET slices is 5-9 wt% of the solvent.
9. The method for preparing an antibacterial nanofiber material as claimed in claim 6, which is characterized in that: the addition amount of the modified titanium dioxide nano particles is 2-10 wt% of the PET chips.
10. The antibacterial nanofiber material prepared by the method of any one of claims 6 to 9.
CN202010675225.2A 2020-07-14 2020-07-14 Antibacterial nanofiber material and application thereof Withdrawn CN111996614A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112552258A (en) * 2020-12-22 2021-03-26 许昌学院 Thiazole amide isomagnoline derivative and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112552258A (en) * 2020-12-22 2021-03-26 许昌学院 Thiazole amide isomagnoline derivative and preparation method and application thereof
CN112552258B (en) * 2020-12-22 2023-02-28 许昌学院 Thiazole amide isomagnanide derivative and preparation method and application thereof

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