CN113018499A - Preparation method of ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture - Google Patents

Preparation method of ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture Download PDF

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CN113018499A
CN113018499A CN202110250789.6A CN202110250789A CN113018499A CN 113018499 A CN113018499 A CN 113018499A CN 202110250789 A CN202110250789 A CN 202110250789A CN 113018499 A CN113018499 A CN 113018499A
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polyvinyl alcohol
preparation
ozone oil
hydrogel
composite
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李莉
张育宁
李忠平
秦瑶
郭书萍
崔红宙
帅慧荣
刘宏业
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First Hospital of Shanxi Medical University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/18Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
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    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
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    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/44Medicaments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/46Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
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    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404Biocides, antimicrobial agents, antiseptic agents
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
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    • C08J2329/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K3/02Elements
    • C08K3/04Carbon
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Abstract

The invention particularly relates to a preparation method of an ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption, which solves the problems that the healing speed is slow and pain and secondary injury are generated during dressing change when a dry dressing is adopted for treating skin wounds at present. A preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture comprises the following steps: a. adding polyvinyl alcohol into deionized water to obtain a polyvinyl alcohol solution; b. adding a graphene oxide solution into a polyvinyl alcohol solution to prepare a reaction solution; c. repeatedly and circularly freezing and thawing the reaction solution to obtain composite hydrogel; d. spraying silicic acid gel on the back layer of the composite hydrogel, and dripping ozone oil on the inner layer to finish the preparation of the ozone oil hydrogel composite application for sterilization, virus resistance and moisture absorption. The composite patch formed by the invention has the effects of moisture absorption, sterilization, antivirus and antifungal, and has high air permeability and waterproofness.

Description

Preparation method of ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture
Technical Field
The invention relates to the technical field of medicines, in particular to a preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting viruses and absorbing moisture.
Background
The skin is the largest organ of the human body, which constitutes the first barrier for the interaction between the human body and the external environment, and once burns, wounds, skin diseases and the like occur, the care of the healing process is extremely important.
The key to healing of various wounds in the skin treatment process lies in cleaning and infection resistance, so how to perform special care on the wounds is always an important subject and field of research. The self-repair of the skin is limited and may be accompanied by the occurrence of various infections. The use of wound dressings is thus an effective adjunct to promoting skin tissue repair or healing.
Currently, the most important care modalities for clinical skin wound treatment are via topical administration (antibiotics) and gauze fixation. Traditional dry dressings such as gauze and the like can maintain the wound area dry and absorb wound exudate, but cannot create a moist environment for the repair and reconstruction of skin tissues, and the antibacterial action of the used antibiotics is limited, the effects on viruses and fungi are not obvious, so that the generation of drug-resistant bacteria is easily caused, the healing speed is influenced, and pain and secondary injury are caused during dressing change.
Disclosure of Invention
The invention provides a preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture, and aims to solve the problems that the healing speed is low and pain and secondary injury are caused during dressing change when a dry dressing is used for treating the existing skin wound.
The invention is realized by adopting the following technical scheme: a preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture comprises the following steps:
a. adding 8-12g of polyvinyl alcohol into per hundred milliliters of deionized water, stirring for 2-5 hours, and cooling to room temperature to obtain a polyvinyl alcohol solution, wherein the temperature of the deionized water is 92-96 ℃;
b. adding a graphene oxide solution with a mass-to-volume ratio of 4mg/ml into a polyvinyl alcohol solution, stirring at room temperature for 12-24h to prepare a reaction solution, wherein the volume ratio of the polyvinyl alcohol solution to the graphene oxide solution is 1: 0.5-2;
c. transferring the reaction solution into a glass container, sealing, freezing at the temperature of minus 15-20 ℃, then thawing at room temperature, and repeatedly freezing and thawing circularly to obtain the composite hydrogel;
d. spraying silicic acid gel on the back layer of the composite hydrogel, and dehydrating and aging at 60-70 deg.C for 3-5 h;
e. and (3) dripping ozone into the inner layer of the composite hydrogel, carrying out negative pressure treatment on the back layer of the composite hydrogel, sealing and standing, wherein the volume ratio of the ozone oil to the polyvinyl alcohol solution is 1:3-6, and thus, the preparation of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption is completed.
A hydrogel is a hydrophilic polymer that swells and retains a large amount of water and maintains a three-dimensional (3D) network structure, and can be processed into various shapes as compared to conventional therapies, thereby being more effectively contacted with a wound; when the hydrogel dressing is applied to a wound, the hydrogel dressing can not adhere to the wound and destroy the new tissue, can provide a good moist healing environment for the wound, and can embed medicaments to kill various bacteria, improve the microenvironment of the wound surface and avoid wound infection.
Graphene oxide is a novel typical two-dimensional material, is also a biological material with excellent biocompatibility, can promote the growth of human and mammalian cells, and the excellent biocompatibility enables the graphene oxide material to be widely applied to tissue engineering, tissue implantation, wound treatment, drug release and the like, while the characteristic of easy functionalization enables the graphene oxide-based material to become an ideal candidate material for synthesizing various functional materials. Two-dimensional graphene oxide is introduced into a polymer network of the hydrogel, so that the whole hydrogel structure tends to be more stable, and the mechanical property is stronger.
Ozone is also called as triatomic oxygen and is a natural oxidant, and the ozone is a broad-spectrum, high-efficiency, quick, safe and secondary-pollution-free sterilizing gas which is known at present and can kill various pathogens such as bacterial spores, viruses, fungi and the like. The ozone oil is a pure natural mixture generated by reacting pure ozone gas with edible vegetable oil-camellia oil by using an ozone curing technology, has the characteristics of broad-spectrum sterilization, strong penetrability, high safety, no drug resistance and the like, and is widely applied to the aspects of antibiosis, antiphlogosis, itching relieving, detoxification and the like of skin and mucous membrane in clinic.
The reaction solution is frozen for 20 hours and unfrozen for 4 hours in a glass container, and is repeatedly frozen and unfrozen for three times in a freezing and crosslinking mode.
The negative pressure treatment time of the composite hydrogel back layer is 5s, and the sealing and standing time is 3 h.
The invention has the following beneficial effects:
1. the ozone oil and the hydrogel are compounded for the first time, and the formed compound application has the dual functions of moisture absorption, sterilization and antivirus, has small irritation to skin mucosa, is convenient to use, good in sterilization effect, good in stability, easy to store, free of side effect, residue and drug resistance;
2. the hydrogel selects graphene oxide and polyvinyl alcohol as main components, and the graphene oxide and the polyvinyl alcohol are interpenetrated and crosslinked to form a stable network structure, so that the hydrogel has better toughness and mechanical strength;
3. ozone oil is loaded in hydrogel formed by graphene oxide and polyvinyl alcohol through adsorption reaction, and the antibacterial and disinfecting effects of the hydrogel composite application are further improved under the synergistic effect of the ozone, the graphene oxide and the polyvinyl alcohol hydrogel;
4. the method adopts a simple physical method for compounding, effectively ensures the safety and the feasibility, and has high air permeability and waterproofness.
Detailed Description
Example 1
A preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture comprises the following steps:
a. adding 8 polyvinyl alcohol into per hundred milliliters of deionized water, stirring for 2 hours, and cooling to room temperature to obtain a polyvinyl alcohol solution, wherein the temperature of the deionized water is 92 ℃;
b. adding a graphene oxide solution with a mass-to-volume ratio of 4mg/ml into a polyvinyl alcohol solution, stirring at room temperature for 12 hours to prepare a reaction solution, wherein the volume ratio of the polyvinyl alcohol solution to the graphene oxide solution is 1: 0.5;
c. transferring the reaction solution into a glass container, sealing, freezing at-15 ℃, then thawing at room temperature, and repeatedly freezing and thawing circularly to obtain the composite hydrogel;
d. spraying silicic acid gel on the back layer of the composite hydrogel, and dehydrating and aging at 60 ℃ for 3 h;
e. and (3) dripping ozone into the inner layer of the composite hydrogel, carrying out negative pressure treatment on the back layer of the composite hydrogel, sealing and standing, wherein the volume ratio of the ozone oil to the polyvinyl alcohol solution is 1:3, and thus, the preparation of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption is completed.
The reaction solution is frozen for 20 hours and unfrozen for 4 hours in a glass container, and is repeatedly frozen and unfrozen for three times in a freezing and crosslinking mode.
The negative pressure treatment time of the composite hydrogel back layer is 5s, and the sealing and standing time is 3 h.
Example 2
A preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture comprises the following steps:
a. adding 12g of polyvinyl alcohol into per hundred milliliters of deionized water, stirring for 5 hours, and cooling to room temperature to obtain a polyvinyl alcohol solution, wherein the temperature of the deionized water is 96 ℃;
b. adding a graphene oxide solution with a mass-to-volume ratio of 4mg/ml into a polyvinyl alcohol solution, and stirring at room temperature for 24 hours to prepare a reaction solution, wherein the volume ratio of the polyvinyl alcohol solution to the graphene oxide solution is 1: 2;
c. transferring the reaction solution into a glass container, sealing, freezing at-20 ℃, then thawing at room temperature, and repeatedly freezing and thawing circularly to obtain the composite hydrogel;
d. spraying silicic acid gel on the back layer of the composite hydrogel, and dehydrating and aging at 70 ℃ for 5 h;
e. and (3) dropping ozone oil into the inner layer of the composite hydrogel, sealing and standing the composite hydrogel after the back layer is subjected to negative pressure treatment, wherein the volume ratio of the ozone oil to the polyvinyl alcohol solution is 1:6, and thus the preparation of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption is completed.
The reaction solution is frozen for 20 hours and unfrozen for 4 hours in a glass container, and is repeatedly frozen and unfrozen for three times in a freezing and crosslinking mode.
The negative pressure treatment time of the composite hydrogel back layer is 5s, and the sealing and standing time is 3 h.
Example 3
A preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture comprises the following steps:
a. adding 9g of polyvinyl alcohol into per hundred milliliters of deionized water, stirring for 4 hours, and cooling to room temperature to obtain a polyvinyl alcohol solution, wherein the temperature of the deionized water is 95 ℃;
b. adding a graphene oxide solution with a mass-to-volume ratio of 4mg/ml into a polyvinyl alcohol solution, stirring at room temperature for 19 hours to prepare a reaction solution, wherein the volume ratio of the polyvinyl alcohol solution to the graphene oxide solution is 1: 0.9;
c. transferring the reaction solution into a glass container, sealing, freezing at-18 ℃, then thawing at room temperature, and repeatedly freezing and thawing circularly to obtain the composite hydrogel;
d. spraying silicic acid gel on the back layer of the composite hydrogel, and dehydrating and aging at 68 ℃ for 4 h;
e. and (3) dropping ozone oil into the inner layer of the composite hydrogel, sealing and standing the composite hydrogel after the back layer is subjected to negative pressure treatment, wherein the volume ratio of the ozone oil to the polyvinyl alcohol solution is 1:4, and thus the preparation of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption is completed.
The reaction solution is frozen for 20 hours and unfrozen for 4 hours in a glass container, and is repeatedly frozen and unfrozen for three times in a freezing and crosslinking mode.
The negative pressure treatment time of the composite hydrogel back layer is 5s, and the sealing and standing time is 3 h.
In the specific implementation process, the ozone oil is selected from sea gift presented to a senior at one's first visit as a mark of esteem ozone bacteriostatic oil produced by lake south sea gift presented to a senior at one's first visit as a mark of esteem medical science and technology limited.
Common pathogenic bacteria are bacterial infections of staphylococcus aureus, hemolytic streptococcus, coagulase negative staphylococcus + methicillin resistant staphylococcus, pseudomonas aeruginosa + enterobacter cloacae, staphylococcus viridis + coagulase negative staphylococcus, candida albicans, enterococcus faecalis, escherichia coli and the like in sequence.
Returning the wound surface bacterial culture result, wherein 51 cases of the ozone oil-water gel composite application and 54 cases of the other group of hydrogel application are positive, the two groups are treated by intravenous drip of antibiotics for 5 days according to the drug sensitivity result, the wound surface bacterial culture is rechecked after 5 days, and 45 cases of the hydrogel-loaded ozone oil composite application are converted into negative results; only 20 of the hydrogel patch groups turned negative (see table 1), and the patients with positive bacterial culture still need antibiotic treatment; after 2 weeks of treatment, the healing status of the wound surfaces of the two groups are compared (see table 2); pain scores before and after the two applications were compared (see table 3).
TABLE 1 Positive test rate (%)
Figure BDA0002965978730000061
Note: the difference before treatment has no statistical significance, and P is more than 0.05; the differences of 3d, 5d, 7d and 10d after treatment have statistical significance, and P is less than 0.05.
TABLE 2 comparison of wound healing rates of two groups
Figure BDA0002965978730000062
TABLE 3 comparison of pain scores before and after two applications of treatment: (
Figure BDA0002965978730000063
Minute)
Figure BDA0002965978730000064
Figure BDA0002965978730000071
Through t test of independent samples at different time points, the hydrogel application and the ozone oil-water gel composite application before treatment are not statistically different, and are statistically different 3 days, 7 days and 2 weeks after treatment, and the pain score of the hydrogel application is higher than that of the ozone oil-water gel composite application.
Figure BDA0002965978730000072
Through analysis of variance of repeated measurements, there were statistical differences in pain scores at different times, in pain scores of different groups, and in interaction with different groups at different times.

Claims (3)

1. A preparation method of an ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture is characterized by comprising the following steps: the method comprises the following steps:
a. adding 8-12g of polyvinyl alcohol into per hundred milliliters of deionized water, stirring for 2-5 hours, and cooling to room temperature to obtain a polyvinyl alcohol solution, wherein the temperature of the deionized water is 92-96 ℃;
b. adding a graphene oxide solution with a mass-to-volume ratio of 4mg/ml into a polyvinyl alcohol solution, stirring at room temperature for 12-24h to prepare a reaction solution, wherein the volume ratio of the polyvinyl alcohol solution to the graphene oxide solution is 1: 0.5-2;
c. transferring the reaction solution into a glass container, sealing, freezing at the temperature of minus 15-20 ℃, then thawing at room temperature, and repeatedly freezing and thawing circularly to obtain the composite hydrogel;
d. spraying silicic acid gel on the back layer of the composite hydrogel, and dehydrating and aging at 60-70 deg.C for 3-5 h;
e. and (3) dripping ozone into the inner layer of the composite hydrogel, carrying out negative pressure treatment on the back layer of the composite hydrogel, sealing and standing, wherein the volume ratio of the ozone oil to the polyvinyl alcohol solution is 1:3-6, and thus, the preparation of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption is completed.
2. The preparation method of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption according to claim 1 is characterized in that: the reaction solution is frozen for 20 hours and unfrozen for 4 hours in a glass container, and is repeatedly frozen and unfrozen for three times in a freezing and crosslinking mode.
3. The preparation method of the ozone oil-water gel composite application for sterilization, virus resistance and moisture absorption according to claim 1 or 2, which is characterized in that: the negative pressure treatment time of the composite hydrogel back layer is 5s, and the sealing and standing time is 3 h.
CN202110250789.6A 2021-03-08 2021-03-08 Preparation method of ozone oil-water gel composite application capable of sterilizing, resisting virus and absorbing moisture Pending CN113018499A (en)

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CN113637183A (en) * 2021-08-17 2021-11-12 安徽大学 Modified graphene-loaded nano-silver/polyvinyl alcohol antibacterial hydrogel and preparation method thereof

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