CN113186649B - Colorful antibacterial nanofiber membrane and preparation method and application thereof - Google Patents
Colorful antibacterial nanofiber membrane and preparation method and application thereof Download PDFInfo
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- CN113186649B CN113186649B CN202110482203.9A CN202110482203A CN113186649B CN 113186649 B CN113186649 B CN 113186649B CN 202110482203 A CN202110482203 A CN 202110482203A CN 113186649 B CN113186649 B CN 113186649B
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- 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
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/44—Medicaments
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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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
- D01F1/06—Dyes
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/402—Anaestetics, analgesics, e.g. lidocaine
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
Abstract
The invention relates to the technical field of preparation of nano medical fiber materials, and particularly discloses a colorful antibacterial nanofiber membrane and a preparation method and application thereof. The multicolor antibacterial nanofiber membrane comprises an aminated chitosan carrier and a natural dye doped in the aminated carrier; wherein the amino content of the aminated chitosan is 40% -45%, and the natural dyes are baicalin, gardenia yellow, gardenia blue and carthamin. The multicolor antibacterial nanofiber membrane is prepared by an electrostatic spinning technology. The nanofiber membrane prepared by the invention has the advantages of being colorful, strong in adsorption performance and good in antibacterial effect, can remarkably improve the healing effect of a wound surface, and has wide application prospects in the field of medical dressings.
Description
Technical Field
The invention relates to the technical field of preparation of nano medical fiber materials, in particular to a colorful antibacterial nanofiber membrane and a preparation method and application thereof.
Background
The skin is the largest organ of the human body, has the function of maintaining the stability of body fluid, electrolytes and nutrient components in the human body, and is also an important component of the immune system of the body. When human skin is damaged, medical dressings are needed to protect wounds. Medical dressing is a skin substitute for temporarily covering wounds caused by mechanical, heat source, chemicals or other skin diseases, etc., and has the main functions of cleaning and covering the wounds, controlling and absorbing wound exudates, and protecting the wounds from harmful bacterial infection.
In modern society, children pursue colorfulness, teenagers pursue independent activities, and the old pursue practicability, so that the wound dressing has the tendency of diversification, high-grade and functionalization. Therefore, there is a need to develop a wound dressing with excellent performance and capable of presenting multiple colors. The electrostatic spinning technology has the advantages of simple operation, low cost, capability of preparing the nanofiber with high porosity and large specific surface area, maximally simulating extracellular matrix and the like, and is widely applied to the field of preparation of wound repair materials. However, since nanofibers have small diameters and large surface areas, have a low dye concentration per unit area, and reflect light more, it is difficult to deeply dye nanofibers. In order to realize deep dyeing of the nanofibers, a heavy metal mordant is generally required to be used, but the heavy metal mordant is not beneficial to wound healing. Therefore, the existing nanofiber wound dressing is difficult to meet the diversified requirements of people, and practical application of the nanofiber dressing is limited. Therefore, there is a need to develop a medical nanofiber membrane which is colorful and helps to accelerate wound healing.
Disclosure of Invention
Aiming at the problems that the currently commonly used medical nanofiber membrane in the prior art is single in color, cannot realize deep dyeing and is poor in functionality, the invention provides a colorful antibacterial nanofiber membrane and a preparation method and application thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a colorful antibacterial nanofiber membrane comprises an aminated chitosan carrier and a natural dye doped in the aminated carrier; wherein, the amino content in the aminated chitosan is 40% -45%, and the natural dyes are baicalin, gardenia yellow, gardenia blue and carthamin.
The baicalin, the gardenia yellow, the gardenia blue pigment and the safflower pigment can be products sold in the market at present, and can also be obtained by adopting a conventional extraction method in the field. The safflower pigment can be safflower yellow and safflower red.
Compared with the prior art, the colorful antibacterial nanofiber membrane provided by the invention has the advantages that the aminated chitosan with the amino content of 40% -45% is used as a carrier, the baicalin, gardenia yellow, gardenia blue and safflower pigment are used as natural dyes, and the abundant amino and hydroxyl groups on the molecular chain of the chitosan are combined with the natural dyes through hydrogen bonds, so that the chitosan and the specific natural dyes are chelated with each other, the rate of the natural dyes on the nanofibers is improved, the coloring depth and the fastness of the natural dyes are greatly improved, the defect that heavy metal mordant is required to be used for dyeing the natural dyes is avoided, the selected specific dyes also have the effects of bacteriostasis, analgesia, hemostasis and the like, multiple effects of the nanometer fiber membrane such as colorfulness, bacteriostasis, accelerated healing and the like are realized, and the colorful antibacterial nanometer fiber membrane has higher popularization and application values.
Preferably, the aminated chitosan is obtained by modifying chitosan by triethylenetetramine and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide.
Triethylene tetramine and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide are selected to modify the chitosan, so that the amino content in the modified chitosan can be obviously improved, and the amino content can reach 40-45%, thereby being beneficial to improving the coloring depth and the fastness of the natural dye.
Preferably, the content of the natural dye in the aminated chitosan carrier is 4% -25%.
The content of the preferable natural dye can ensure that the nanofiber membrane has higher dyeing depth and fastness, and is beneficial to improving the antibacterial performance of the nanofiber membrane.
The invention also provides a preparation method of the multicolor antibacterial nanofiber membrane, which comprises the following steps:
step one, uniformly mixing chitosan and organic amine, heating and refluxing for reaction, filtering, washing and drying to obtain aminated chitosan; the organic amine is a mixture of triethylene tetramine and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide;
step two, adding the aminated chitosan, the natural dye and the egg white into a dilute acid solution, and uniformly mixing to obtain a spinning solution;
and step three, injecting the spinning solution into an electrostatic spinning device for electrostatic spinning, and drying the obtained electrospun fibers to obtain the multicolor antibacterial nanofiber membrane.
The preparation method of the colorful antibacterial nanofiber membrane provided by the invention is simple to operate, the colorful antibacterial nanofiber membrane can be constructed by a one-step method, the prepared nanofiber membrane has the advantages of large specific surface area, strong adsorption performance and high speed, the healing promotion capability of the nanofiber membrane can be obviously improved, and the preparation method has high practical value.
Preferably, in the first step, the preparation method of chitosan comprises the following steps: adding shrimp shells into a dilute hydrochloric acid solution, soaking for 2-3h, filtering, washing to be neutral, then adding into a sodium hydroxide solution, hydrolyzing at 80-100 ℃ for 3-4h, filtering, and washing to be neutral to obtain the chitosan.
Preferably, in the first step, the concentration of the dilute hydrochloric acid is 5-8wt%. The concentration of the sodium hydroxide solution is 45-50wt%.
The preparation method of chitosan provided by the invention can improve the amino content in the chitosan by controlling the concentration of hydrochloric acid and the hydrolysis temperature and time, and has the advantages of wide raw material source, low cost and simple operation.
Preferably, in the first step, the mass-to-volume ratio of the chitosan to the organic amine is 0.08 to 0.12, wherein the unit of mass is gram and the unit of volume is milliliter.
Preferably, the volume ratio of the triethylenetetramine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide in the organic amine is 4-6.
Preferably, in the first step, the heating reflux reaction time is 2-4h.
The proportion of each substance and the reaction time in the first step are preferably selected, so that the modified chitosan with high amino content can be obtained.
Preferably, in the second step, the addition amount of the aminated chitosan is 2-5wt% of the mass of the dilute acid solution.
Preferably, in the second step, the addition amount of the natural dye is 0.2-0.5wt% of the mass of the dilute acid solution.
Preferably, in the second step, the adding amount of the egg white is 0.5-0.6wt% of the mass of the diluted acid solution.
Preferably, the concentration of the dilute acid solution is 0.1-0.5mol/L.
Optionally, the dilute acid solution is a hydrochloric acid solution, an acetic acid solution or a lactic acid solution.
Preferably, in the third step, the parameters of the electrostatic spinning are as follows: the distance between the nozzle and the aluminum foil is 10-15cm, the spinning voltage is 20-30kV, the spinning flow rate is 0.5-2mL/h, and the humidity is 25% -35%.
The optimized electrostatic spinning parameters are favorable for obtaining and forming a continuous nanofiber membrane, so that the prepared nanofiber has a porous structure, gas exchange is facilitated, bacterial invasion is prevented, wound exudate is effectively absorbed, a moist wound healing environment is maintained, and the wound healing is accelerated.
The invention also provides application of the colorful antibacterial nanofiber membrane in medical dressings.
The nanofiber membrane provided by the invention has the advantages of being colorful, strong in adsorption performance, high in antibacterial property and the like, can obviously improve the healing effect of a wound surface, and has a wide application prospect in the field of medical dressings.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to better illustrate the invention, the following examples are given by way of further illustration.
Example 1
The embodiment of the invention provides a preparation method of a colorful antibacterial nanofiber membrane, which comprises the following steps:
step one, adding cleaned and dried shrimp shells into a 5wt% hydrochloric acid solution, soaking for 3 hours at room temperature, filtering, washing with water to be neutral, then adding into a 45wt% sodium hydroxide solution, hydrolyzing for 3 hours at 100 ℃, filtering, washing with water to be neutral, and drying to obtain chitosan;
weighing 10g of chitosan, dissolving in 100mL of a mixed solution of triethylenetetramine and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide, wherein the volume ratio of triethylenetetramine to 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide is 6;
adding 50mL of 0.4mol/L acetic acid solution into the obtained aminated chitosan, uniformly mixing, adding baicalin and egg white, and uniformly mixing to obtain a spinning solution; wherein the adding amount of the aminated chitosan is 3wt% of the mass of the acetic acid solution, the adding amount of the baicalin is 0.2wt% of the mass of the acetic acid solution, and the adding amount of the egg white is 0.6wt% of the mass of the acetic acid solution;
and step four, injecting the spinning solution into an electrostatic spinning device, controlling the distance between a spray head and the aluminum foil to be 12cm, the spinning voltage to be 20kV, the spinning flow rate to be 1mL/h and the humidity to be 30% for electrospinning, and drying the prepared electrospun fiber membrane in vacuum for 24h to obtain the colorful antibacterial nanofiber membrane.
And (3) determining the amino content of the aminated chitosan prepared in the second step by using an Element Analyzer (EA), wherein the amino content is determined to be 45%.
And (4) performance testing:
and calculating the bacteriostatic rate according to a method of the bacteriostatic rate of the standard GB/T20944.3-2008 'evaluation of textile antibacterial performance'.
Measurement of K/S value of fiber Membrane: and (3) testing by adopting a color measuring and matching instrument, folding 4 layers of dyed samples (without light), measuring the K/S value of the fabric, measuring different positions of the sample 3, and averaging.
And (3) testing the color fastness to rubbing of the fiber film: and measuring for 3 times according to GB/T3920-2008 ' color fastness to rubbing ' of textile color fastness test ', and taking an average value.
The K/S value of the nanofiber membrane prepared in the embodiment reaches 12.7, the dry rubbing fastness is 4-5, the wet rubbing fastness is 3 grade, and the bacteriostasis rate is 98.9%.
Example 2
The embodiment of the invention provides a preparation method of a colorful antibacterial nanofiber membrane, which comprises the following steps:
step one, adding cleaned and dried shrimp shells into 6wt% hydrochloric acid solution, soaking for 2.5 hours at room temperature, filtering, washing with water to be neutral, then adding into 50wt% sodium hydroxide solution, hydrolyzing for 3.5 hours at 90 ℃, filtering, washing with water to be neutral, and drying to obtain chitosan;
weighing 10g of chitosan, dissolving in 100mL of a mixed solution of triethylenetetramine and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide, wherein the volume ratio of triethylenetetramine to 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide is 4;
adding 50mL of 0.1mol/L acetic acid solution into the obtained aminated chitosan, uniformly mixing, adding baicalin and egg white, and uniformly mixing to obtain a spinning solution; wherein the addition amount of the aminated chitosan is 5wt% of the mass of the acetic acid solution, the addition amount of the baicalin is 0.4wt% of the mass of the acetic acid solution, and the addition amount of the egg white is 0.5wt% of the mass of the acetic acid solution;
and step four, injecting the spinning solution into an electrostatic spinning device, controlling the distance between a spray head and the aluminum foil to be 15cm, controlling the spinning voltage to be 30kV, controlling the spinning flow rate to be 2mL/h and controlling the humidity to be 35%, carrying out electrospinning, and carrying out vacuum drying on the prepared electrospun fiber membrane for 24h to obtain the colorful antibacterial nanofiber membrane.
And (3) determining the amino content of the aminated chitosan prepared in the second step by using an Element Analyzer (EA), wherein the amino content is determined to be 42%.
The nanofiber membrane prepared in the embodiment is subjected to performance test according to the test method in the embodiment 1, and the nanofiber membrane prepared in the embodiment has a K/S value of 12.9, dry rubbing fastness of 4-5, wet rubbing fastness of grade 3 and a bacteriostasis rate of 99.2%.
Example 3
The embodiment of the invention provides a preparation method of a colorful antibacterial nanofiber membrane, which comprises the following steps:
step one, adding cleaned and dried shrimp shells into 8wt% hydrochloric acid solution, soaking for 2h at room temperature, filtering, washing with water to be neutral, then adding into 48wt% sodium hydroxide solution, hydrolyzing for 4h at 80 ℃, filtering, washing with water to be neutral, and drying to obtain chitosan;
step two, weighing 10g of chitosan, dissolving the chitosan into 100mL of a mixed solution of triethylene tetramine and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide, wherein the volume ratio of the triethylene tetramine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide is 5;
adding 50mL of 0.5mol/L acetic acid solution into the obtained aminated chitosan, uniformly mixing, adding baicalin and egg white, and uniformly mixing to obtain a spinning solution; wherein the adding amount of the aminated chitosan is 2wt% of the mass of the acetic acid solution, the adding amount of the baicalin is 0.5wt% of the mass of the acetic acid solution, and the adding amount of the egg white is 0.5wt% of the mass of the acetic acid solution;
and step four, injecting the spinning solution into an electrostatic spinning device, controlling the distance between a spray head and the aluminum foil to be 10cm, the spinning voltage to be 25kV, the spinning flow rate to be 0.5mL/h and the humidity to be 25%, carrying out electrospinning, and carrying out vacuum drying on the obtained electrospun fiber film for 24h to obtain the colorful antibacterial nanofiber film.
And (3) determining the amino content of the aminated chitosan prepared in the second step by adopting an Element Analyzer (EA), wherein the amino content is determined to be 43%.
The nanofiber membrane prepared in the embodiment is subjected to performance test according to the test method in the embodiment 1, and the nanofiber membrane prepared in the embodiment has a K/S value of 11.9, dry rubbing fastness of 4-5, wet rubbing fastness of grade 3 and a bacteriostasis rate of 99.3%.
The acetic acid solution in the third step of the embodiment 1 to 3 can be replaced by hydrochloric acid solution or lactic acid solution, and the baicalin can be replaced by other natural dyes, such as gardenia yellow, gardenia blue or safflower pigment, and the like, and the technical effects basically equivalent to those of the embodiment 1 to 3 can be achieved.
Comparative example 1
This comparative example provides a stretchable nanofiber membrane prepared exactly as in example 1, except that triethylenetetramine and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide were replaced with equal amounts of ethylenediamine and carbodiimide in step one.
The performance test of the prepared nanofiber membrane is carried out according to the test method of example 1, and the nanofiber membrane prepared in the comparative example has the K/S value of 10.5, the dry rubbing fastness of 4, the wet rubbing fastness of 3 grades and the bacteriostasis rate of 95.7 percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A colorful antibacterial nanofiber membrane is characterized by comprising an aminated chitosan carrier and a natural dye doped in the aminated carrier; wherein, the amino content in the aminated chitosan is 40% -45%, and the natural dyes are baicalin, gardenia yellow, gardenia blue and carthamin;
the aminated chitosan is obtained by modifying chitosan with triethylene tetramine and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide.
2. The multi-colored antimicrobial nanofiber membrane according to claim 1, wherein the natural dye is present in an amount of 4% to 25% in the aminated chitosan carrier.
3. The method for preparing a multicolor antibacterial nanofiber film as claimed in any one of claims 1 to 2, characterized by comprising the steps of:
step one, uniformly mixing chitosan and organic amine, heating and refluxing for reaction, filtering, washing and drying to obtain aminated chitosan; the organic amine is a mixture of triethylene tetramine and 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide;
step two, adding the aminated chitosan, the natural dye and the egg white into a dilute acid solution, and uniformly mixing to obtain a spinning solution;
and step three, injecting the spinning solution into an electrostatic spinning device for electrostatic spinning, and drying the obtained electrospun fibers to obtain the multicolor antibacterial nanofiber membrane.
4. A method for preparing a multicolor antibacterial nanofiber membrane as claimed in claim 3, wherein in step one, the method for preparing chitosan comprises the following steps: adding shrimp shells into a dilute hydrochloric acid solution, soaking for 2-3h, filtering, washing to be neutral, then adding into a sodium hydroxide solution, hydrolyzing at 80-100 ℃ for 3-4h, filtering, and washing to be neutral to obtain the chitosan.
5. The method for preparing a multicolor antibacterial nanofiber film according to claim 3, wherein in the first step, the mass-to-volume ratio of chitosan to organic amine is 0.08-0.12.
6. The method for preparing a multicolor antibacterial nanofiber film according to claim 5, wherein in the first step, the volume ratio of triethylenetetramine to 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide in the organic amine is 4-6; and/or
In the first step, the heating reflux reaction time is 2-4h.
7. The method for preparing a multicolor antibacterial nanofiber membrane as claimed in claim 3, wherein in the second step, the addition amount of the aminated chitosan is 2-5wt% of the mass of the dilute acid solution; and/or
In the second step, the adding amount of the natural dye is 0.2 to 0.5 weight percent of the mass of the dilute acid solution; and/or
In the second step, the adding amount of the egg white is 0.5 to 0.6 weight percent of the mass of the dilute acid solution.
8. A method for preparing a colorful antibacterial nanofiber membrane as claimed in claim 3, wherein in step three, the parameters of electrostatic spinning are as follows: the distance between the nozzle and the aluminum foil is 10-15cm, the spinning voltage is 20-30kV, the spinning flow rate is 0.5-2mL/h, and the humidity is 25% -35%.
9. Use of a multicolored antimicrobial nanofibrous film according to any of claims 1 to 2 in a medical dressing.
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