CN113209354A - Preparation method of antibacterial dressing - Google Patents
Preparation method of antibacterial dressing Download PDFInfo
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- CN113209354A CN113209354A CN202110354307.1A CN202110354307A CN113209354A CN 113209354 A CN113209354 A CN 113209354A CN 202110354307 A CN202110354307 A CN 202110354307A CN 113209354 A CN113209354 A CN 113209354A
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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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- 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
- A61L15/26—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
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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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- 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
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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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
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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
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Abstract
The invention discloses a preparation method of an antibacterial dressing, which comprises the following steps: weighing the following raw materials in parts by weight: 25-35 parts of 15% silver nitrate solution by mass, 10-20 parts of plant fiber, 1-5 parts of polyvinylpyrrolidone, 3-8 parts of antibacterial precursor and 50-80 parts of deionized water; heating the silver nitrate solution and the plant fiber to the temperature of 120-; preparing the composite fiber into carbonized fiber; adding polyvinylpyrrolidone into deionized water, magnetically stirring at the rotating speed of 100-150r/min for 30min to prepare a polymer aqueous solution, adding an antibacterial precursor and carbonized fibers, drying for 4 to prepare a primary material, and washing for three times to prepare the antibacterial dressing; the dressing has an antibacterial effect through silver ions and the antibacterial precursor, the components are environment-friendly, and residues cannot pollute the environment.
Description
Technical Field
The invention belongs to the technical field of medical supplies, and particularly relates to a preparation method of an antibacterial dressing.
Background
Conventional wound dressings include gauze, absorbent cotton, bandages and the like. However, from the medical point of view, these conventional wound dressings have no properties such as wound healing and repair, and also have no antibacterial activity, and thus the clinical application range is limited. Therefore, the novel medical dressing which can promote wound healing, has high-efficiency antibacterial property and is more convenient to use is gradually developed. Of decisive importance in these wound dressings are the various antimicrobial agents contained therein, which have an antimicrobial effect. Different components in the antibacterial agent play a key role in the healing effect of the wound, and the technical problem to be solved by the invention is how to provide the antibacterial dressing which has high antibacterial property and is beneficial to wound recovery.
Chinese invention patent CN201410592615.8 discloses a medical biological antibacterial dressing for nasal cavity and oral cavity and a preparation method thereof, the medical biological antibacterial dressing is composed of modified chitosan, camellia oil, peppermint oil, alum, olive oil, almond oil, garlic extract, fructus momordicae extract, liquorice extract and aniseed oil, the invention contains a plurality of raw materials with the efficacies of clearing away heat and toxic material, relieving swelling and pain, cooling blood, stopping bleeding, sterilizing, removing diseases, resisting anaphylaxis source, moistening skin and promoting tissue regeneration, the raw materials supplement each other, can effectively inhibit and kill germs, relieve swelling, relieve pain, stop bleeding, moisten skin and promote tissue regeneration, improve the ventilation function of nasal cavity and nasal sinus, and form a hidden protective film on the surface of mucosa, can effectively cure allergic rhinitis and chronic nasosinusitis, prevent and treat oral diseases, particularly oral ulcer, gingivitis and the like, has low cost and quick curative effect, the disease is not easy to relapse, but the application performs antibiosis through the traditional Chinese medicine extract, so that the antibacterial effect is low.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a preparation method of an antibacterial dressing.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of the antibacterial dressing comprises the following steps:
step S1, weighing the following raw materials in parts by weight: 25-35 parts of 15% silver nitrate solution by mass, 10-20 parts of plant fiber, 1-5 parts of polyvinylpyrrolidone, 3-8 parts of antibacterial precursor and 50-80 parts of deionized water.
S2, placing a silver nitrate solution with the mass fraction of 15% and plant fibers into a steam pressure container, heating to 120-130 ℃, preserving heat and reacting for 30min, cooling, washing with deionized water for three times, drying to obtain composite fibers, and cooling to room temperature;
s3, placing the composite fiber in a carbonization furnace, introducing nitrogen to discharge air, heating to 450-500 ℃ at a heating rate of 5-10 ℃/min, and carbonizing for 30min at the temperature to obtain carbonized fiber;
step S4, adding polyvinylpyrrolidone into deionized water, magnetically stirring for 30min at the rotating speed of 100-; freezing and drying with liquid nitrogen at-80 deg.C for 48-72 hr to obtain primary material, washing with acetone for three times, and oven drying to obtain antibacterial dressing.
Further, the plant fiber is any one of sisal fiber, bamboo fiber and flax fiber.
Further, the antibacterial precursor is prepared by the following steps:
step S1, adding tetraethoxysilane and methyltrimethoxysilane into absolute ethyl alcohol, and uniformly stirring at a rotating speed of 100r/min for 10min to prepare a solution a; uniformly mixing absolute ethyl alcohol and deionized water according to the weight ratio of 1: 10 to prepare a solution b; putting the solution a into a 50-65 ℃ water bath kettle, preserving heat, adding the solution b into the solution a, controlling the dropping time to be 10min, completely adding the solution a, uniformly mixing the solution a and the solution b, adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 3.6, preserving heat to react for 2h, adding ammonia water with the mass fraction of 10% to adjust the pH until the pH is 7.5, adding silicon nitride particles, continuously stirring for 30min to prepare sol, concentrating until the viscosity is 6-7cp, and drying at normal pressure to prepare gel.
And S2, pouring the sodium alcohol ether sulphate into a beaker filled with absolute ethyl alcohol, adding methyl methacrylate, magnetically stirring for 10min, uniformly mixing, adding deionized water to prepare a microemulsion, adding the gel prepared in the step S1 into the microemulsion, and heating in a water bath at 60 ℃ for 5h to prepare the antibacterial precursor.
In the step S1, tetraethoxysilane and methyltrimethoxysilane are used as raw materials, 10% diluted hydrochloric acid is added to adjust the pH and serve as a catalyst in the hydrolysis process, silicic acid and hemisilicic acid monomers can be generated after the solution a and the solution b are mixed, 10% ammonia water is added to adjust the pH on one hand and serve as a catalyst in the polycondensation process on the other hand, the hydrolyzed monomers are subjected to polycondensation to form smaller cross-linked bodies, then the cross-linked bodies are stacked to form sol, silicon nitride particles are added, and then drying is carried out at normal pressure to prepare gel; in the step S2, a microemulsion is prepared from sodium fatty alcohol polyoxyethylene ether sulfate and methyl methacrylate, and then mixed with gel to prepare an antibacterial precursor, wherein in the reaction process, part of carboxyl groups in the microemulsion react with hydroxyl groups on the surface of the nano titanium dioxide, and esterification condensation forms strong chemical bonds, so that the gel can be easily dispersed in an organic system, the dispersibility of the gel is improved, and the uniformity of the precursor is ensured.
Further, in step S1, the weight ratio of ethyl orthosilicate, methyltrimethoxysilane and absolute ethyl alcohol is controlled to be 2: 1: 10, the volume ratio of solution a to solution b is 1.5: 1, and the amount of silicon nitride particles is one half of the weight of ethyl orthosilicate.
Further, in step S2, the weight ratio of the sodium fatty alcohol-polyoxyethylene ether sulfate, the methyl methacrylate, the absolute ethyl alcohol and the deionized water is controlled to be 1: 2: 3, and the weight ratio of the microemulsion to the gel is controlled to be 5: 1.
The invention has the beneficial effects that:
according to the antibacterial dressing, silver ions are loaded on plant fibers in the preparation process, then the plant fibers are carbonized to form silver ion loaded carbon fibers, the carbon fibers are provided with high specific surface area and numerous micropores, the micropores have strong adsorption capacity, and further can stably load the silver ions, then an antibacterial precursor and the carbonized fibers are added into a polymer aqueous solution, a uniform system is formed by high-speed stirring, and the mixture is frozen and dried to prepare the antibacterial dressing;
in the preparation process, in the step S1, tetraethoxysilane and methyltrimethoxysilane are used as raw materials, 10% of diluted hydrochloric acid is added to adjust the pH and serve as a catalyst in the hydrolysis process, silicic acid and hemisilicic acid monomers can be generated after the solution a and the solution b are mixed, 10% of ammonia water is added to adjust the pH on one hand and serve as a catalyst in the polycondensation process on the other hand, the hydrolyzed monomers are subjected to polycondensation to form a smaller cross-linked body, then the cross-linked body is stacked to form sol, silicon nitride particles are added, and then drying is carried out at normal pressure to prepare gel; in the step S2, a microemulsion is prepared from sodium fatty alcohol polyoxyethylene ether sulfate and methyl methacrylate, and then mixed with gel to prepare an antibacterial precursor, wherein in the reaction process, part of carboxyl groups in the microemulsion react with hydroxyl groups on the surface of the nano titanium dioxide, and esterification condensation forms strong chemical bonds, so that the gel can be easily dispersed in an organic system, the dispersibility of the gel is improved, and the uniformity of the precursor is ensured.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of the antibacterial dressing comprises the following steps:
step S1, weighing the following raw materials in parts by weight: 25 parts of 15% silver nitrate solution by mass, 10 parts of bamboo fiber, 1 part of polyvinylpyrrolidone, 3 parts of antibacterial precursor and 50 parts of deionized water.
Step S2, placing a silver nitrate solution with the mass fraction of 15% and bamboo fibers into a steam pressure container, heating to 120 ℃, preserving heat, reacting for 30min, cooling, washing with deionized water for three times, drying to obtain composite fibers, and cooling to room temperature;
step S3, placing the composite fiber in a carbonization furnace, introducing nitrogen to discharge air, heating to 500 ℃ at a heating rate of 10 ℃/min, and carbonizing for 30min at the temperature to obtain carbonized fiber;
step S4, adding polyvinylpyrrolidone into deionized water, magnetically stirring for 30min at a rotating speed of 100r/min to prepare a polymer aqueous solution, adding an antibacterial precursor, increasing the rotating speed to 500r/min, adding carbonized fibers after stirring for 30min at a constant speed, stirring for 10h at a constant speed, ultrasonically standing, and removing bubbles in the solution; freezing and drying with liquid nitrogen at-80 deg.C for 48h to obtain primary material, washing with acetone for three times, and oven drying to obtain antibacterial dressing.
The antibacterial precursor is prepared by the following steps:
step S1, adding tetraethoxysilane and methyltrimethoxysilane into absolute ethyl alcohol, and uniformly stirring at a rotating speed of 100r/min for 10min to prepare a solution a; uniformly mixing absolute ethyl alcohol and deionized water according to the weight ratio of 1: 10 to prepare a solution b; putting the solution a into a 65 ℃ water bath kettle, preserving heat, adding the solution b into the solution a, controlling the dropping time to be 10min, completely adding the solution a, uniformly mixing the solution a and the solution b, adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 3.6, preserving heat to react for 2h, adding ammonia water with the mass fraction of 10% to adjust the pH until the pH is 7.5, adding silicon nitride particles, continuously stirring the mixture for 30min to prepare sol, concentrating the sol until the viscosity is 6cp, drying the sol at normal pressure to prepare gel, and controlling the weight ratio of ethyl orthosilicate, methyltrimethoxysilane and absolute ethyl alcohol to be 2: 1: 10, the volume ratio of the solution a to the solution b to be 1.5: 1, and the dosage of the silicon nitride particles to be one half of the weight of the ethyl orthosilicate.
Step S2, pouring the fatty alcohol-polyoxyethylene ether sodium sulfate into a beaker filled with absolute ethyl alcohol, then adding methyl methacrylate, magnetically stirring for 10min, uniformly mixing, adding deionized water to prepare a microemulsion, adding the gel prepared in the step S1 into the microemulsion, heating in a water bath at 60 ℃ for 5h to prepare an antibacterial precursor, controlling the weight ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the methyl methacrylate to the absolute ethyl alcohol to the deionized water to be 1: 2: 3, and controlling the weight ratio of the microemulsion to the gel to be 5: 1.
Example 2
A preparation method of the antibacterial dressing comprises the following steps:
step S1, weighing the following raw materials in parts by weight: the antibacterial bamboo fiber fabric comprises, by mass, 28 parts of 15% silver nitrate solution, 14 parts of bamboo fiber, 3 parts of polyvinylpyrrolidone, 5 parts of an antibacterial precursor and 55 parts of deionized water.
Step S2, placing a silver nitrate solution with the mass fraction of 15% and bamboo fibers into a steam pressure container, heating to 120 ℃, preserving heat, reacting for 30min, cooling, washing with deionized water for three times, drying to obtain composite fibers, and cooling to room temperature;
step S3, placing the composite fiber in a carbonization furnace, introducing nitrogen to discharge air, heating to 500 ℃ at a heating rate of 10 ℃/min, and carbonizing for 30min at the temperature to obtain carbonized fiber;
step S4, adding polyvinylpyrrolidone into deionized water, magnetically stirring for 30min at a rotating speed of 100r/min to prepare a polymer aqueous solution, adding an antibacterial precursor, increasing the rotating speed to 500r/min, adding carbonized fibers after stirring for 30min at a constant speed, stirring for 10h at a constant speed, ultrasonically standing, and removing bubbles in the solution; freezing and drying with liquid nitrogen at-80 deg.C for 48h to obtain primary material, washing with acetone for three times, and oven drying to obtain antibacterial dressing.
The antibacterial precursor is prepared by the following steps:
step S1, adding tetraethoxysilane and methyltrimethoxysilane into absolute ethyl alcohol, and uniformly stirring at a rotating speed of 100r/min for 10min to prepare a solution a; uniformly mixing absolute ethyl alcohol and deionized water according to the weight ratio of 1: 10 to prepare a solution b; putting the solution a into a 65 ℃ water bath kettle, preserving heat, adding the solution b into the solution a, controlling the dropping time to be 10min, completely adding the solution a, uniformly mixing the solution a and the solution b, adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 3.6, preserving heat to react for 2h, adding ammonia water with the mass fraction of 10% to adjust the pH until the pH is 7.5, adding silicon nitride particles, continuously stirring the mixture for 30min to prepare sol, concentrating the sol until the viscosity is 6cp, drying the sol at normal pressure to prepare gel, and controlling the weight ratio of ethyl orthosilicate, methyltrimethoxysilane and absolute ethyl alcohol to be 2: 1: 10, the volume ratio of the solution a to the solution b to be 1.5: 1, and the dosage of the silicon nitride particles to be one half of the weight of the ethyl orthosilicate.
Step S2, pouring the fatty alcohol-polyoxyethylene ether sodium sulfate into a beaker filled with absolute ethyl alcohol, then adding methyl methacrylate, magnetically stirring for 10min, uniformly mixing, adding deionized water to prepare a microemulsion, adding the gel prepared in the step S1 into the microemulsion, heating in a water bath at 60 ℃ for 5h to prepare an antibacterial precursor, controlling the weight ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the methyl methacrylate to the absolute ethyl alcohol to the deionized water to be 1: 2: 3, and controlling the weight ratio of the microemulsion to the gel to be 5: 1.
Example 3
A preparation method of the antibacterial dressing comprises the following steps:
step S1, weighing the following raw materials in parts by weight: 30 parts of 15% silver nitrate solution by mass, 18 parts of bamboo fiber, 4 parts of polyvinylpyrrolidone, 6 parts of antibacterial precursor and 70 parts of deionized water.
S2, placing a silver nitrate solution with the mass fraction of 15% and bamboo fibers into a steam pressure container, heating to 120-130 ℃, preserving heat and reacting for 30min, cooling, washing with deionized water for three times, drying to obtain composite fibers, and cooling to room temperature;
step S3, placing the composite fiber in a carbonization furnace, introducing nitrogen to discharge air, heating to 500 ℃ at a heating rate of 10 ℃/min, and carbonizing for 30min at the temperature to obtain carbonized fiber;
step S4, adding polyvinylpyrrolidone into deionized water, magnetically stirring for 30min at a rotating speed of 100r/min to prepare a polymer aqueous solution, adding an antibacterial precursor, increasing the rotating speed to 500r/min, adding carbonized fibers after stirring for 30min at a constant speed, stirring for 10h at a constant speed, ultrasonically standing, and removing bubbles in the solution; freezing and drying with liquid nitrogen at-80 deg.C for 48h to obtain primary material, washing with acetone for three times, and oven drying to obtain antibacterial dressing.
The antibacterial precursor is prepared by the following steps:
step S1, adding tetraethoxysilane and methyltrimethoxysilane into absolute ethyl alcohol, and uniformly stirring at a rotating speed of 100r/min for 10min to prepare a solution a; uniformly mixing absolute ethyl alcohol and deionized water according to the weight ratio of 1: 10 to prepare a solution b; putting the solution a into a 65 ℃ water bath kettle, preserving heat, adding the solution b into the solution a, controlling the dropping time to be 10min, completely adding the solution a, uniformly mixing the solution a and the solution b, adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 3.6, preserving heat to react for 2h, adding ammonia water with the mass fraction of 10% to adjust the pH until the pH is 7.5, adding silicon nitride particles, continuously stirring the mixture for 30min to prepare sol, concentrating the sol until the viscosity is 6cp, drying the sol at normal pressure to prepare gel, and controlling the weight ratio of ethyl orthosilicate, methyltrimethoxysilane and absolute ethyl alcohol to be 2: 1: 10, the volume ratio of the solution a to the solution b to be 1.5: 1, and the dosage of the silicon nitride particles to be one half of the weight of the ethyl orthosilicate.
Step S2, pouring the fatty alcohol-polyoxyethylene ether sodium sulfate into a beaker filled with absolute ethyl alcohol, then adding methyl methacrylate, magnetically stirring for 10min, uniformly mixing, adding deionized water to prepare a microemulsion, adding the gel prepared in the step S1 into the microemulsion, heating in a water bath at 60 ℃ for 5h to prepare an antibacterial precursor, controlling the weight ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the methyl methacrylate to the absolute ethyl alcohol to the deionized water to be 1: 2: 3, and controlling the weight ratio of the microemulsion to the gel to be 5: 1.
Example 4
A preparation method of the antibacterial dressing comprises the following steps:
step S1, weighing the following raw materials in parts by weight: 35 parts of 15% silver nitrate solution by mass, 20 parts of bamboo fiber, 5 parts of polyvinylpyrrolidone, 8 parts of antibacterial precursor and 80 parts of deionized water.
Step S2, placing a silver nitrate solution with the mass fraction of 15% and bamboo fibers into a steam pressure container, heating to 120 ℃, preserving heat, reacting for 30min, cooling, washing with deionized water for three times, drying to obtain composite fibers, and cooling to room temperature;
step S3, placing the composite fiber in a carbonization furnace, introducing nitrogen to discharge air, heating to 500 ℃ at a heating rate of 10 ℃/min, and carbonizing for 30min at the temperature to obtain carbonized fiber;
step S4, adding polyvinylpyrrolidone into deionized water, magnetically stirring for 30min at a rotating speed of 100r/min to prepare a polymer aqueous solution, adding an antibacterial precursor, increasing the rotating speed to 500r/min, adding carbonized fibers after stirring for 30min at a constant speed, stirring for 10h at a constant speed, ultrasonically standing, and removing bubbles in the solution; freezing and drying with liquid nitrogen at-80 deg.C for 48h to obtain primary material, washing with acetone for three times, and oven drying to obtain antibacterial dressing.
The antibacterial precursor is prepared by the following steps:
step S1, adding tetraethoxysilane and methyltrimethoxysilane into absolute ethyl alcohol, and uniformly stirring at a rotating speed of 100r/min for 10min to prepare a solution a; uniformly mixing absolute ethyl alcohol and deionized water according to the weight ratio of 1: 10 to prepare a solution b; putting the solution a into a 65 ℃ water bath kettle, preserving heat, adding the solution b into the solution a, controlling the dropping time to be 10min, completely adding the solution a, uniformly mixing the solution a and the solution b, adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 3.6, preserving heat to react for 2h, adding ammonia water with the mass fraction of 10% to adjust the pH until the pH is 7.5, adding silicon nitride particles, continuously stirring the mixture for 30min to prepare sol, concentrating the sol until the viscosity is 6cp, drying the sol at normal pressure to prepare gel, and controlling the weight ratio of ethyl orthosilicate, methyltrimethoxysilane and absolute ethyl alcohol to be 2: 1: 10, the volume ratio of the solution a to the solution b to be 1.5: 1, and the dosage of the silicon nitride particles to be one half of the weight of the ethyl orthosilicate.
Step S2, pouring the fatty alcohol-polyoxyethylene ether sodium sulfate into a beaker filled with absolute ethyl alcohol, then adding methyl methacrylate, magnetically stirring for 10min, uniformly mixing, adding deionized water to prepare a microemulsion, adding the gel prepared in the step S1 into the microemulsion, heating in a water bath at 60 ℃ for 5h to prepare an antibacterial precursor, controlling the weight ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the methyl methacrylate to the absolute ethyl alcohol to the deionized water to be 1: 2: 3, and controlling the weight ratio of the microemulsion to the gel to be 5: 1.
Comparative example 1
In this comparative example, no antimicrobial precursor was added as compared to example 1.
Comparative example 2
This comparative example is a medical dressing in the market.
The antibacterial properties of examples 1 to 4 and comparative examples 1 to 2 were measured, and the results are shown in the following table;
as can be seen from the above table, the bacteriostatic ratio of the examples 1-4 to Escherichia coli is 38.8-39.2%, the bacteriostatic ratio to Staphylococcus aureus is 41.0-41.5%, and the bacteriostatic ratio to Candida albicans is 39.6-40.2%; the comparative examples 1-2 have 11.2-28.5% of escherichia coli inhibition rate, 12.1-32.8% of staphylococcus aureus inhibition rate and 11.8-31.5% of candida albicans inhibition rate.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (5)
1. The preparation method of the antibacterial dressing is characterized by comprising the following steps:
step S1, weighing the following raw materials in parts by weight: 25-35 parts of 15% silver nitrate solution by mass, 10-20 parts of plant fiber, 1-5 parts of polyvinylpyrrolidone, 3-8 parts of antibacterial precursor and 50-80 parts of deionized water;
s2, placing a silver nitrate solution with the mass fraction of 15% and plant fibers into a steam pressure container, heating to 120-130 ℃, preserving heat and reacting for 30min, cooling, washing with deionized water for three times, drying to obtain composite fibers, and cooling to room temperature;
s3, placing the composite fiber in a carbonization furnace, introducing nitrogen to discharge air, heating to 450-500 ℃ at a heating rate of 5-10 ℃/min, and carbonizing for 30min at the temperature to obtain carbonized fiber;
step S4, adding polyvinylpyrrolidone into deionized water, magnetically stirring for 30min at the rotating speed of 100-; freezing and drying with liquid nitrogen at-80 deg.C for 48-72 hr to obtain primary material, washing with acetone for three times, and oven drying to obtain antibacterial dressing.
2. The method for preparing an antibacterial dressing according to claim 1, wherein the plant fiber is any one of sisal fiber, bamboo fiber and flax fiber.
3. The method for preparing the antibacterial dressing according to claim 1, wherein the antibacterial precursor is prepared by the following steps:
step S1, adding tetraethoxysilane and methyltrimethoxysilane into absolute ethyl alcohol, and uniformly stirring at a rotating speed of 100r/min for 10min to prepare a solution a; uniformly mixing absolute ethyl alcohol and deionized water according to the weight ratio of 1: 10 to prepare a solution b; placing the solution a in a water bath kettle at 50-65 ℃, preserving heat, adding the solution b into the solution a, controlling the dripping time to be 10min, completely adding the solution a, uniformly mixing the solution a and the solution b, adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 3.6, preserving heat to react for 2h, adding ammonia water with the mass fraction of 10% to adjust the pH until the pH is 7.5, adding silicon nitride particles, continuously stirring for 30min to prepare sol, concentrating until the viscosity is 6-7cp, and drying at normal pressure to prepare gel;
and S2, pouring the sodium alcohol ether sulphate into a beaker filled with absolute ethyl alcohol, adding methyl methacrylate, magnetically stirring for 10min, uniformly mixing, adding deionized water to prepare a microemulsion, adding the gel prepared in the step S1 into the microemulsion, and heating in a water bath at 60 ℃ for 5h to prepare the antibacterial precursor.
4. The method for preparing an antibacterial dressing according to claim 3, wherein the weight ratio of the ethyl orthosilicate, the methyltrimethoxysilane and the anhydrous ethanol in step S1 is controlled to be 2: 1: 10, the volume ratio of the solution a to the solution b is 1.5: 1, and the amount of the silicon nitride particles is one half of the weight of the ethyl orthosilicate.
5. The method for preparing an antibacterial dressing according to claim 3, wherein in step S2, the weight ratio of the sodium alcohol ether sulfate, the methyl methacrylate, the absolute ethyl alcohol and the deionized water is controlled to be 1: 2: 3, and the weight ratio of the microemulsion to the gel is controlled to be 5: 1.
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| CN114921873A (en) * | 2022-05-27 | 2022-08-19 | 苏州工业园区安泽汶环保技术有限公司 | Preparation method of bactericidal and antiviral carbon fiber cloth composite material for air purification |
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