CN108018620B - Antibacterial zirconium sodium silver phosphate alginate fiber and preparation method thereof - Google Patents
Antibacterial zirconium sodium silver phosphate alginate fiber and preparation method thereof Download PDFInfo
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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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- 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
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic 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
- 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
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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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
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
- A61L2300/104—Silver, e.g. silver sulfadiazine
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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
Abstract
The invention relates to the technical field of medical material preparation, in particular to antibacterial zirconium sodium silver phosphate alginate fibers and a preparation method of the antibacterial zirconium sodium silver phosphate alginate fibers. The preparation method of the antibacterial zirconium sodium silver alginate fiber comprises the following steps: (1) grinding zirconium sodium silver powder; (2) preparing zirconium sodium silver phosphate dispersion liquid; (3) preparing a sodium alginate solution with the mass percentage of 2-5%; (4) mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3); (5) filtering and defoaming the spinning solution, and metering the spinning solution by a metering pump and spraying the spinning solution from a spinneret plate into a coagulating bath; (6) washing in a washing bath; (7) the antibacterial zirconium sodium silver phosphate alginate fiber is prepared through the working procedures of drafting, drying and winding. The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the invention can slowly release silver ions, and the silver ions are uniformly distributed and have good antibacterial effect.
Description
Technical Field
The invention relates to the technical field of medical material preparation, in particular to antibacterial zirconium sodium silver phosphate alginate fibers and a preparation method of the antibacterial zirconium sodium silver phosphate alginate fibers.
Background
Alginic acid (Alginic acid) is a polysaccharide extracted from natural seaweed and linearly polymerized from mono-uronic acid, the Alginic acid monomers are β -1, 4-D-mannuronic acid (M) and α -1, 4-L-guluronic acid (G), Alginic acid is generally used in the form of alginate, such as sodium alginate, calcium alginate, etc. sodium alginate is favored for its specific functions of promoting wound healing, absorbing moisture, preserving moisture, biocompatibility, and being absorbable by the human body.
However, the single alginic acid fiber has poor antibacterial effect and poor mechanical property, and is easy to absorb water to swell and melt when meeting water. These disadvantages have limited the use of the single sodium alginate fibre for antibacterial and wound healing applications. The silver ions have the characteristics of outstanding antibacterial capability, high safety and the like, so the silver ions are the first choice of the ionic antibacterial material. However, the silver-plated fibers of the prior art have the following problems: (1) non-uniformity of the antimicrobial; (2) the antibacterial agent is only present in the surface layer of the fiber, and is easy to fall off, and once the antibacterial agent falls off, the antibacterial agent cannot be supplemented, so that the antibacterial agent is not resistant to washing and the durability of the antibacterial effect is not ideal.
Disclosure of Invention
One of the objectives of the present invention is to provide a method for preparing an antibacterial zirconium sodium silver phosphate alginate fiber, in order to overcome the above-mentioned disadvantages of the prior art, the prepared antibacterial zirconium sodium silver phosphate alginate fiber has a uniform distribution of silver ions, can slowly release silver ions, and has a good antibacterial effect.
In order to solve the technical problems, the invention adopts the following technical scheme that the preparation method of the antibacterial zirconium sodium silver phosphate alginate fiber comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 5-10 mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 2-3 hours, adding a dispersing agent, wherein the adding amount of the dispersing agent is 0.5-1 time of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain sodium alginate solution with mass percent of 2-5%;
(4) mixing the homogeneous solution obtained in the step (2) and the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, placing the mixture into a water bath shaking pot, shaking the mixture for 2 hours at a constant temperature of 50-60 ℃ and 50-200r/min, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 15-20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump and spraying the solution from a spinneret plate into a coagulating bath;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 80-85:20: 1;
(7) and (3) drawing, drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
In the invention, after the zirconium sodium silver phosphate and the sodium alginate are mixed, the zirconium sodium silver phosphate has small particles and can be mutually fused with the sodium alginate in forms of permeation, ion exchange and the like, silver ions can be complexed with hydroxyl and carboxyl on a macromolecular chain of alginate fiber, and the silver particles are not easy to agglomerate and are distributed more uniformly due to the dispersion effect of a dispersing agent, so that the silver particles are distributed on the surface of the alginate fiber and are distributed in the alginate fiber; in addition, due to the wrapping effect of alginate fiber macromolecules and the bonding effect of xanthan gum, silver particles are not easy to fall off.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the invention has uniform silver ion distribution and can slowly release silver ions, the release time of the silver ions lasts over 78 hours, the release ratio of the silver ions exceeds 84%, and the antibacterial effect is good.
The antibacterial zirconium sodium silver alginate fiber prepared by the invention has the liquid absorption amount of 15-18g/g fiber to distilled water, so that the antibacterial zirconium sodium silver alginate fiber can better absorb wound penetrating fluid and maintain the moist environment of a wound surface.
The antibacterial zirconium sodium silver alginate fiber prepared by the invention has good antibacterial effect, and especially has better antibacterial and bacteriostatic effects when being used after being slightly heated, and can generate obvious antibacterial effect on escherichia coli, staphylococcus aureus and the like.
Further, the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, then adding the distilled water, and uniformly stirring to obtain the xanthan gum. The washing bath has the advantages that silver can be adhered to the fiber more uniformly, the silver attached to the fiber can not be washed off while calcium salt in the coagulation bath remained on the surface of the fiber is washed off, and the prepared alginate fiber is more soft and is not easy to harden.
Further, the dispersing agent is polyacrylamide or sodium dodecyl sulfate.
Further, the spinning solution in the step (4) also comprises an antibacterial agent, and the specific operation steps of the step (4) are as follows: according to the following steps: weighing honeysuckle and folium artemisiae argyi according to the mass ratio of 1, uniformly mixing, grinding and crushing, adding an ethanol solution with the same mass as the mixture into the crushed mixture, wherein the mass fraction of the ethanol solution is 35-40%, soaking for 30-40 minutes, then adding clear water with the weight being 25 times of the weight of the mixture, uniformly mixing, heating to boil, decocting with slow fire until the residual liquid amount is 1/3-1/2 of the initial liquid amount, and filtering to obtain a decoction; mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, adding decoction with a volume of 1-3% of the volume of the mixed solution into the mixed solution, stirring for 15-20 minutes by using a magnetic stirrer, then placing into a water bath shaking pot, shaking for 2 hours at a constant temperature of 50-60 ℃ under the condition of 50-200r/min, and then placing into an ultrasonic mixer for ultrasonic mixing for 15-20 minutes to prepare a uniform spinning solution. Its advantage is high antibacterial effect.
Further, the specific operation of step (5) is: pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.3-0.4%, the coagulating temperature of the first coagulating bath is 30-40 ℃, and the coagulating time is 2-3 minutes; then introducing into a second coagulating bath, wherein the second coagulating bath is 3-5% calcium chloride water solution by mass, the temperature of the second coagulating bath is 40-45 ℃, and the coagulating time is 2-3 minutes. According to the invention, the sodium citrate solution is used as the first coagulation bath, so that silver can be effectively prevented from being oxidized, and the sodium alginate fiber is prevented from being blackened in the processing process.
Further, the drying temperature of the step (7) is 45-50 ℃.
Further, the drying method of the step (7) is vacuum freeze drying.
The invention also discloses the antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
The invention also discloses an application of the antibacterial zirconium sodium silver phosphate alginate fiber in preparation of medical sanitary dressings. When the antibacterial zirconium sodium silver phosphate alginate fiber is used, silver ions are more favorably released after the antibacterial zirconium sodium silver phosphate alginate fiber is slightly heated (30-45 ℃), so the use effect is better.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the invention, after the zirconium sodium silver phosphate and the sodium alginate are mixed, the zirconium sodium silver phosphate has small particles and can be mutually fused with the sodium alginate in forms of permeation, ion exchange and the like, silver ions can be complexed with hydroxyl and carboxyl on a macromolecular chain of alginate fiber, and the silver particles are not easy to agglomerate and are distributed more uniformly due to the dispersion effect of a dispersing agent, so that the silver particles are distributed on the surface of the alginate fiber and are distributed in the alginate fiber; in addition, due to the wrapping effect of alginate fiber macromolecules and the bonding effect of xanthan gum, silver particles are not easy to fall off.
(2) The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the invention has uniform silver ion distribution and can slowly release silver ions, the release time of the silver ions lasts over 78 hours, the release ratio of the silver ions exceeds 84%, and the antibacterial effect is good.
(3) The antibacterial zirconium sodium silver alginate fiber prepared by the invention has the liquid absorption amount of 15-18g/g fiber to distilled water, so that the antibacterial zirconium sodium silver alginate fiber can better absorb wound penetrating fluid and maintain the moist environment of a wound surface.
(4) The antibacterial zirconium sodium silver alginate fiber prepared by the invention has good antibacterial effect, and especially has better antibacterial and bacteriostatic effects when being used after being slightly heated, and can generate obvious antibacterial effect on escherichia coli, staphylococcus aureus and the like.
Detailed Description
The following examples are provided to facilitate a better understanding of the present invention and are not intended to limit the same. The experimental procedures in the following examples are conventional unless otherwise specified.
Example 1
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 5mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 2 hours, adding polyacrylamide, wherein the adding amount of the polyacrylamide is 0.8 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with the mass percentage of 3%;
(4) mixing the homogeneous solution obtained in the step (2) and the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, placing the mixture into a water bath shaking pot, shaking the mixture at a constant temperature of 60 ℃ and 50r/min for 2 hours, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.3%, the coagulating temperature of the first coagulating bath is 30 ℃, and the coagulating time is 3 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 4%, the temperature of the second coagulation bath is 40-45 ℃, and the coagulation time is 3 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 80:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, drying at 45 ℃ and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 2
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 8mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 2 hours, adding polyacrylamide, wherein the adding amount of the polyacrylamide is 0.7 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with the mass percent of 2%;
(4) mixing the homogeneous solution obtained in the step (2) and the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, placing the mixture into a water bath shaking pot, shaking the mixture at a constant temperature of 50 ℃ and 200r/min for 2 hours, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.4%, the coagulating temperature of the first coagulating bath is 35 ℃, and the coagulating time is 2 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 3%, the temperature of the second coagulation bath is 40 ℃, and the coagulation time is 2 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 82:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, drying at 50 ℃ and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 3
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 10mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 3 hours, adding polyacrylamide, wherein the adding amount of the polyacrylamide is 1 time of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with the mass percentage of 3%;
(4) mixing the homogeneous solution obtained in the step (2) and the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, placing the mixture into a water bath shaking pot, shaking the mixture at a constant temperature of 55 ℃ and 200r/min for 2 hours, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 15 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering the spinning solution by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.4%, the coagulating temperature of the first coagulating bath is 40 ℃, and the coagulating time is 3 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 3%, the temperature of the second coagulation bath is 40 ℃, and the coagulation time is 3 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 80:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, vacuum freeze drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 4
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 6mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 2 hours, adding sodium dodecyl sulfate, wherein the adding amount of the sodium dodecyl sulfate amine is 0.5 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with a mass percentage of 4%;
(4) mixing the homogeneous solution obtained in the step (2) and the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, placing the mixture into a water bath shaking pot, shaking the mixture at a constant temperature of 55 ℃ and 150r/min for 2 hours, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 15 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.3%, the coagulating temperature of the first coagulating bath is 35 ℃, and the coagulating time is 2 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 5%, the temperature of the second coagulation bath is 45 ℃, and the coagulation time is 2 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 80:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, vacuum freeze drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 5
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 9mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 3 hours, adding sodium dodecyl sulfate, wherein the adding amount of the sodium dodecyl sulfate is 0.5 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with the mass percent of 5%;
(4) according to the following steps: weighing honeysuckle and folium artemisiae argyi according to the mass ratio of 1, uniformly mixing, grinding and crushing, adding an ethanol solution with the same mass as the mixture into the crushed mixture, wherein the mass fraction of the ethanol solution is 35%, soaking for 40 minutes, then adding clear water with the weight being 25 times of the weight of the mixture, uniformly mixing, heating to boil, decocting with slow fire until the residual liquid amount is 1/3-1/2 of the initial liquid amount, and filtering to obtain a decoction; mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, adding a decoction liquid with the volume being 3% of the volume of the mixed solution into the mixed solution, stirring the mixture for 20 minutes by using a magnetic stirrer, then placing the mixture into a water bath shaking pot, shaking the mixture for 2 hours at a constant temperature of 50 ℃ and 150r/min, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering the spinning solution by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.4%, the coagulating temperature of the first coagulating bath is 30 ℃, and the coagulating time is 3 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 5%, the temperature of the second coagulation bath is 45 ℃, and the coagulation time is 3 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to the weight ratio of 85:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, vacuum freeze drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 6
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 8mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 3 hours, adding sodium dodecyl sulfate, wherein the adding amount of the sodium dodecyl sulfate is 0.6 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with the mass percentage of 3%;
(4) according to the following steps: weighing honeysuckle and folium artemisiae argyi according to the mass ratio of 1, uniformly mixing, grinding and crushing, adding an ethanol solution with the same mass as the mixture into the crushed mixture, wherein the mass fraction of the ethanol solution is 40%, soaking for 30 minutes, then adding clear water with the weight being 25 times of the weight of the mixture, uniformly mixing, heating to boil, decocting with slow fire until the residual liquid amount is 1/3-1/2 of the initial liquid amount, and filtering to obtain a decoction; mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, adding a decoction liquid with the volume being 1% of the volume of the mixed solution into the mixed solution, stirring for 15 minutes by using a magnetic stirrer, then placing the mixed solution into a water bath shaking pot, shaking for 2 hours at a constant temperature of 55 ℃ under the condition of 100r/min, and then placing the mixed solution into an ultrasonic mixer for ultrasonic mixing for 15 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.3%, the coagulating temperature of the first coagulating bath is 40 ℃, and the coagulating time is 3 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 4%, the temperature of the second coagulation bath is 42 ℃, and the coagulation time is 2 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 80:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, vacuum freeze drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 7
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 7mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 3 hours, adding polyacrylamide, wherein the adding amount of the polyacrylamide is 0.8 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with a mass percentage of 4%;
(4) according to the following steps: weighing honeysuckle and folium artemisiae argyi according to the mass ratio of 1, uniformly mixing, grinding and crushing, adding an ethanol solution with the same mass as the mixture into the crushed mixture, wherein the mass fraction of the ethanol solution is 40%, soaking for 35 minutes, then adding clear water with the weight being 25 times of the weight of the mixture, uniformly mixing, heating to boil, decocting with slow fire until the residual liquid amount is 1/3-1/2 of the initial liquid amount, and filtering to obtain a decoction; mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, adding a decoction liquid with the volume being 3% of the volume of the mixed solution into the mixed solution, stirring the mixture for 20 minutes by using a magnetic stirrer, then placing the mixture into a water bath shaking pot, shaking the mixture for 2 hours at a constant temperature of 60 ℃ and 100r/min, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering the spinning solution by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.4%, the coagulating temperature of the first coagulating bath is 30 ℃, and the coagulating time is 2 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 4%, the temperature of the second coagulation bath is \45 ℃, and the coagulation time is 3 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to the weight ratio of 85:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, vacuum freeze drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Example 8
A preparation method of antibacterial zirconium sodium silver alginate fibers comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 7mg of zirconium sodium silver phosphate into each 100ml of deionized water, stirring for 2 hours, adding sodium dodecyl sulfate, wherein the adding amount of the sodium dodecyl sulfate is 0.9 times of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution;
(3) dissolving sodium alginate in deionized water, and stirring to obtain a sodium alginate solution with a mass percentage of 4%;
(4) according to the following steps: weighing honeysuckle and folium artemisiae argyi according to the mass ratio of 1, uniformly mixing, grinding and crushing, adding an ethanol solution with the same mass as the mixture into the crushed mixture, wherein the mass fraction of the ethanol solution is 40%, soaking for 35 minutes, then adding clear water with the weight being 25 times of the weight of the mixture, uniformly mixing, heating to boil, decocting with slow fire until the residual liquid amount is 1/3-1/2 of the initial liquid amount, and filtering to obtain a decoction; mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, adding a decoction liquid with a volume of 2% of the volume of the mixed solution into the mixed solution, stirring the mixture for 18 minutes by using a magnetic stirrer, then placing the mixture into a water bath shaking pot, shaking the mixture for 2 hours at a constant temperature of 55 ℃ and 150r/min, and placing the mixture into an ultrasonic mixer for ultrasonic mixing for 20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.3%, the coagulating temperature of the first coagulating bath is 35 ℃, and the coagulating time is 3 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 5%, the temperature of the second coagulation bath is 40 ℃, and the coagulation time is 3 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to the weight ratio of 85:20: 1; the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, adding the distilled water, and uniformly stirring to obtain the xanthan gum;
(7) and (3) drawing, vacuum freeze drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
The antibacterial zirconium sodium silver phosphate alginate fiber prepared by the preparation method.
An application of the antibacterial zirconium phosphate sodium silver alginate fiber in the preparation of medical sanitary dressing.
Results of the experiment
The antibacterial silver sodium zirconium phosphate alginate fibers obtained in examples 1 to 7 were subjected to performance measurement.
1. Measurement of liquid absorption amount: weighing 0.1g of blended fiber sample, and soaking in 50mL of distilled water for 30 min; centrifuging and dehydrating the fiber after water absorption for 15min, wherein the rotating speed of a centrifuge is 2000r/min, weighing, and recording the mass as M1; the fiber was then placed in an oven at 105 ℃ to a constant weight, weighed, and the mass recorded as M2. The liquid absorption amount of the fiber was (M1-M2)/M2. The results show that the antibacterial silver sodium zirconium phosphate alginate fibers obtained in examples 1 to 8 have a distilled water absorption of 15 to 18g/g fiber. Therefore, the wound dressing has high liquid absorption amount, can well absorb wound penetrating fluid, and can maintain the moist environment of the wound surface.
2. Antibacterial property: activating Escherichia coli and Staphylococcus aureus, inoculating strain to the slant, culturing at 37 deg.C for 12 hr, washing the bacterial solution on the slant with sterile water, measuring OD value, to ensure that the strains inoculated each time are equal in quantity, bacterial liquid with the equal strains is taken and coated on a culture medium plate, a filter paper sheet with the diameter of 0.6cm is placed in the plate by tweezers, the antibacterial zirconium sodium silver alginate fibers prepared in the embodiments 1 to 8 of the invention are respectively cut into round pieces with the diameter of 0.6cm, the antibacterial zirconium sodium silver alginate fiber round pieces prepared in the embodiments 1 to 8 of the invention are respectively placed on the filter paper pieces of the experiments 1 to 8, each experiment group is provided with 3 parallel pieces, the pieces are cultured in a constant temperature incubator at 37 ℃ for 12h, sterile common gauze with the diameter of 0.6cm is placed on the filter paper pieces of a blank control group, and the diameters of the inhibition zones of the experiment group and the control group are measured. The results are shown in Table 1
TABLE 1 antimicrobial Properties of different treatment groups
As can be seen from Table 1, the antibacterial zirconium sodium silver phosphate alginate fiber prepared by the invention has good antibacterial effect and obvious antibacterial effect on escherichia coli, staphylococcus aureus and the like.
3. And (3) measuring the slow release effect of silver ions: a certain amount of the antibacterial zirconium sodium silver phosphate alginate fibers prepared in the embodiments 1-8 of the invention are weighed and filled into a dialysis bag (the molecular weight cut-off is 2000), then the dialysis bag is put into deionized water, and the amount of silver ions in the deionized water at different times is measured to judge the slow release capacity of the gel. The result shows that the antibacterial zirconium sodium silver phosphate alginate fiber prepared by the invention can slowly release silver ions, the release time of the silver ions lasts over 78 hours, the release ratio of the silver ions exceeds 84%, and the antibacterial effect is good.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (7)
1. A preparation method of antibacterial zirconium sodium silver alginate fibers is characterized by comprising the following steps: the method comprises the following steps:
(1) grinding the zirconium sodium silver phosphate powder by using a ball mill to prepare 200-300nm zirconium sodium silver phosphate;
(2) adding 200-300nm zirconium sodium silver phosphate into deionized water, adding 5-10 mg of zirconium sodium silver phosphate into every 100ml of deionized water, stirring for 2-3 hours, adding a dispersing agent, wherein the adding amount of the dispersing agent is 0.5-1 time of the mass of the zirconium sodium silver phosphate, and performing ultrasonic dispersion to form a homogeneous solution; the dispersant is polyacrylamide or lauryl sodium sulfate;
(3) dissolving sodium alginate in deionized water, and stirring to obtain sodium alginate solution with mass percent of 2-5%;
(4) mixing the homogeneous solution obtained in the step (2) and the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, placing the mixture into a water bath shaking pot, shaking the mixture for 2 hours at a constant temperature of 50-60 ℃ and 50-200r/min, and then placing the mixture into an ultrasonic mixer for ultrasonic mixing for 15-20 minutes to prepare a uniform spinning solution;
(5) pouring the mixed spinning solution into a dissolving kettle for filtering and defoaming, and then metering by a metering pump to spray the spinning solution from a spinneret plate into a first coagulating bath, wherein the first coagulating bath is a citric acid solution with the mass fraction of 0.3-0.4%, the coagulating temperature of the first coagulating bath is 30-40 ℃, and the coagulating time is 2-3 minutes; then introducing the mixture into a second coagulation bath, wherein the second coagulation bath is a calcium chloride aqueous solution with the mass fraction of 3-5%, the temperature of the second coagulation bath is 40-45 ℃, and the coagulation time is 2-3 minutes;
(6) after passing through a coagulating bath, the fibers enter a washing bath for washing, wherein the washing bath is formed by mixing ethanol, distilled water and xanthan gum according to a weight ratio of 80-85:20: 1;
(7) and (3) drawing, drying and winding the fiber washed by the washing bath to obtain the antibacterial zirconium sodium silver alginate fiber.
2. The method for preparing the antibacterial silver sodium zirconium phosphate alginate fiber according to claim 1, wherein the method comprises the following steps: the preparation method of the washing bath comprises the following steps: firstly, weighing ethanol, distilled water and xanthan gum according to a ratio, then dissolving the xanthan gum in the ethanol, then adding the distilled water, and uniformly stirring to obtain the xanthan gum.
3. The method for preparing the antibacterial silver sodium zirconium phosphate alginate fiber according to claim 1, wherein the method comprises the following steps: the spinning solution in the step (4) also comprises an antibacterial agent, and the specific operation steps in the step (4) are as follows: according to the following steps: weighing honeysuckle and folium artemisiae argyi according to the mass ratio of 1, uniformly mixing, grinding and crushing, adding an ethanol solution with the same mass as the mixture into the crushed mixture, wherein the mass fraction of the ethanol solution is 35-40%, soaking for 30-40 minutes, then adding clear water with the weight being 25 times of the weight of the mixture, uniformly mixing, heating to boil, decocting with slow fire until the residual liquid amount is 1/3-1/2 of the initial liquid amount, and filtering to obtain a decoction; mixing the homogeneous solution obtained in the step (2) with the sodium alginate solution obtained in the step (3) according to a volume ratio of 1:4, adding decoction with a volume of 1-3% of the volume of the mixed solution into the mixed solution, stirring for 15-20 minutes by using a magnetic stirrer, then placing into a water bath shaking pot, shaking for 2 hours at a constant temperature of 50-60 ℃ under the condition of 50-200r/min, and then placing into an ultrasonic mixer for ultrasonic mixing for 15-20 minutes to prepare a uniform spinning solution.
4. The method for preparing the antibacterial silver sodium zirconium phosphate alginate fiber according to claim 1, wherein the method comprises the following steps: the drying temperature of the step (7) is 45-50 ℃.
5. The method for preparing the antibacterial silver sodium zirconium phosphate alginate fiber according to claim 1, wherein the method comprises the following steps: the drying method of the step (7) is vacuum freeze drying.
6. The antibacterial zirconium sodium silver alginate fiber prepared by the preparation method of the antibacterial zirconium sodium silver alginate fiber of any one of claims 1 to 5.
7. The use of the antibacterial zirconium sodium silver phosphate alginate fiber of claim 6 in the manufacture of medical sanitary dressings.
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