CN106867005A - Sodium alginate with antibacterial and promotion wound healing function carries silver-colored graphene composite film and its application - Google Patents

Sodium alginate with antibacterial and promotion wound healing function carries silver-colored graphene composite film and its application Download PDF

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CN106867005A
CN106867005A CN201710104161.9A CN201710104161A CN106867005A CN 106867005 A CN106867005 A CN 106867005A CN 201710104161 A CN201710104161 A CN 201710104161A CN 106867005 A CN106867005 A CN 106867005A
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sodium alginate
composite film
silver
graphene
graphene composite
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CN106867005B (en
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陆杨
闫旭
薛敬哲
胡康棣
徐维平
潘晓锋
李飞
宋永红
吴亚东
苏杨
何涛
刘建楠
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Hefei University of Technology
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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
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • 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
    • A61L15/28Polysaccharides or their derivatives
    • 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
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • 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
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104Silver, e.g. silver sulfadiazine
    • 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
    • A61L2300/40Biologically 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
    • CCHEMISTRY; METALLURGY
    • 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
    • C08J2305/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
    • C08J2305/04Alginic acid; Derivatives thereof
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08K3/00Use of inorganic substances as compounding ingredients
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    • C08K2003/0806Silver
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/16Applications used for films

Abstract

Silver-colored graphene composite film and its application are carried the invention discloses the sodium alginate with antibacterial and promotion wound healing function, it is characterised in that:It is that will carry after silver-colored graphene solution be well mixed with sodium alginate soln, preparation film forming is assembled by spraying.Composite membrane provided by the present invention, preparation method is simple, and has antibacterial simultaneously and promote the function of wound healing, for as wound surgical dressing, there is obvious effect, with larger clinical practice potentiality.

Description

Sodium alginate with antibacterial and promotion wound healing function-load silver Graphene is combined Film and its application
Technical field
The present invention relates to sodium alginate composite simultaneously, and in particular to a kind of that there is promotion wound healing function and antibacterial The sodium alginate of function-load silver graphene composite film and preparation method thereof.
Background technology
Sodium alginate is a kind of natural polymer, the brown alga in main source Yu Haiyang.Sodium alginate be by β- A kind of block copolymerization that two kinds of cellular constructions of D-MANNOSE aldehydic acid and α-L- guluronic acid residues are made up of α -1-4 glycosidic bonds Thing.As a kind of natural materials of polysaccharide, sodium alginate macromolecular material have good biocompatibility, water imbibition, thoroughly The good characteristics such as oxygen, nontoxicity and film forming.Based on this, alginate films and answering that other macromolecules are mixed with The concern that film causes researcher in the application of antibacterial and wound class wound dressing is closed, and some alginates wound auxiliary materials are Obtain commercialized application, such as Comfeel PlusTM (health and happiness guarantor), SorbsanTM (UDL laboratories) and TegagenTM (3m Medical treatment) etc..Not only antibacterial effect is not good enough but also mechanical property is poor for single alginate films, meets the hygroscopic expansion of water, melts Change.Application in terms of these shortcomings make single sodium alginate film in antibacterial and promote wound healing is restricted.Therefore, one Plant not only to have and promote wound healing and antibacterial functions but also with excellent mechanical performances, the sodium alginate composite urgency of convenient use Need exploitation.
The U.S.《Cell transplantation》(Cell Transplant, volume 19, the 399-408 pages in 2010), it was recently reported that pass through By be crosslinked alginic acid combined with CXCL12 be made can promote wound healing and reduce wound scar formed Sodium alginate combine dressing.Although the sodium alginate for preparing by this method/CXCL12 compound can To promote the healing of wound, but do not possess good antibacterial functions, it is impossible to effectively reduce or prevent wound in agglutination The middle risk for infecting.
Britain《Materials chemistry magazine》(Journal of Materials Chemistry, volume 2011,21, the 4593rd- Page 4597), it was recently reported that by silver nitrate and reduced graphene-polystyrene sulphuric acid sodium compound being mixed with antibacterial The silver/graphene antimicrobial composite material of effect.Although effect of the silver/graphite alkene compound with antibacterial prepared by this method, But simultaneously without the function that can promote wound healing.In addition, silver/graphite alkene compound is liquid compound, do not made For into film-form, the convenience for storing and using is not good enough.
In sum, existing some antibacterials or the material of promotion wound healing, otherwise the only function with antibacterial, it is impossible to Accelerate the healing rate of wound, cause wound healing slow;Only there is the function of promoting wound healing, it is impossible to effective anti- Bacterium, causes wound to occur infected risk during healing, is unfavorable for the healing and recovery of wound, is unsuitable for promoting and answers With.
The content of the invention
Weak point of the present invention existing for the above-mentioned prior art of solution, there is provided with antibacterial and promotion wound healing The sodium alginate of function-load silver graphene composite film and preparation method thereof, and use it for as wound surgical dressing, it is intended to solve Certainly existing wound surgical dressing effect is single, can not simultaneously take into account the shortcoming of antibacterial and promotion wound healing function.
The present invention is adopted the following technical scheme that to solve technical problem:
The preparation method of the sodium alginate with antibacterial and promotion wound healing function-load silver graphene composite film, it is special Point is to carry out as follows:
A, take 100~300mg graphene oxide sheets and be added in 150~300mL distilled water, after ultrasonic disperse, add 2g Polystyrene sulphuric acid sodium, stirring and dissolving adds 150~400 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, gained Product through suction filtration, it is lyophilized after, that is, obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound;
B, the reduced form graphene oxide-polystyrene sulphuric acid sodium compound that step a is obtained is added to 50~ In 100mL water, it is well mixed, is put into single neck bottle, be heated to 60 DEG C, is then the nitre of 0.02mol/L by 5~10mL concentration Sour silver solution is added in single neck bottle with the speed of 0.5mL/h, and constant temperature stirring 10h is continued after adding, and is centrifuged and removes supernatant, is obtained Silver-colored graphene solution must be carried;
C, carry described silver-colored graphene solution and mix with the sodium alginate soln that 5~25mL concentration is 15~35mg/mL, shake Swing, ultrasound, the silver-colored Graphene mixed solution of sodium alginate-loads is obtained after being well mixed;
D, the sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, that is, obtain marine alga Sour sodium-load silver graphene composite film.
Sodium alginate of the invention-load silver graphene composite film, can as needed make arbitrary shape or size, each original Material consumption also can equal proportion amplify, for example according to above-mentioned condition can obtain thickness be 10~40 μm, size be 1~100cm2's Composite membrane.
Sodium alginate of the invention-load silver graphene composite film has imitative concba lamellar structure, and this structure can be effective Improve its mechanical property.
Compared with the prior art, the present invention has the beneficial effect that:
1st, sodium alginate provided by the present invention-load silver graphene composite film, preparation method is simple, and has antibacterial simultaneously (such as anti-candida albicanses and anti-Escherichia coli) and the function of promotion wound healing, for as wound surgical dressing, having substantially Effect, with larger clinical practice potentiality.
2nd, sodium alginate provided by the present invention-load silver graphene composite film, with low toxicity, pollution-free, biocompatibility The good and low advantage of cytotoxicity, is a kind of security material very high;
3rd, sodium alginate provided by the present invention-load silver graphene composite film, the equal controllable of its size, thickness, practicality By force, with clinical and market application potential higher;
4th, sodium alginate provided by the present invention-load silver graphene composite film is layer structure, and good mechanical properties have Pliability very high, flexible folding, for it provides good mechanics as the film with antibacterial and promotion wound healing Basis.
Brief description of the drawings
(a) cross-sectional scans electron microscope of the sodium alginate-load silver graphene composite film prepared by Fig. 1 embodiment of the present invention 1 (SEM, Zeiss Supra 40, Germany), (b) transmission electron microscope figure (TEM, Hitachi HT7700), (c) Mapping power spectrums and (d) ESEM power spectrum (EDS, X-Max, Oxford).
(a) cross-sectional scans electron microscope and thickness of several thickness composite membranes of the Fig. 2 prepared by the embodiment of the present invention 1- The relation curve (b) of density.
Fig. 3 is (a) XRD and (b) ultraviolet absorpting spectrum of several different films prepared by the embodiment of the present invention 1.
Fig. 4 is the cross-sectional scans electron microscope of several different films prepared by the embodiment of the present invention 1.
Fig. 5 is the mechanical property figure of several different films prepared by the embodiment of the present invention 1.
Fig. 6 is anti-Escherichia coli and the antifungal design sketch of several different films prepared by the embodiment of the present invention 1.
Fig. 7 is the effect that sodium alginate prepared by the embodiment of the present invention 1-load silver graphene composite film promotes wound healing Figure.
Specific embodiment
Graphene oxide sheet used by following embodiments is prepared as follows:
By the H that 50mL concentration is 98%2SO4, 10g K2S2O8, 10g P2O5Mixed solution be heated to 70 DEG C, add 30g graphite powders obtain mixture A after stirring;After mixture A is cooled into room temperature, with distilled water filtering and washing to its pH value It is neutrality, after the product after washing is dried in atmosphere, obtains pre-oxidizing graphite powder;15g pre-oxidation graphite powders are taken to be added to 500mL, the 98% of 0 DEG C dense H2SO4In obtain mixed solution B;Under stirring, water bath condition, slowly add in mixed solution B Enter the KMnO of 60g4, add KMnO4During keep system temperature at 15 DEG C, obtain mixed solution C;Mixed solution C is heated up To 40 DEG C, 3h is stirred, add 950mL distilled water, the 30% of 3L distilled water and 50mL H was then added in 15 minutes2O2, obtain To yellow product D;By the HCl filtration washings that 5L volumetric concentrations are 10% of the metal ion in yellow product D, dry, obtain final product To graphene oxide sheet.
Embodiment 1
The present embodiment carries out the preparation of sodium alginate-load silver graphene composite film as follows:
A, take 200mg graphene oxide sheets and be added in 200mL distilled water, after ultrasonic disperse, add 2g polystyrene sulphur Sour sodium, stirring and dissolving adds 200 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, and products therefrom is through suction filtration, lyophilized Afterwards, reduced form graphene oxide-polystyrene sulphuric acid sodium compound is obtained;
B, by step a obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound add into 50mL water, mix Close uniform, be put into single neck bottle of 100mL, be heated to 60 DEG C, be then the silver nitrate solution of 0.02mol/L by 5mL concentration It is slowly added into single neck bottle by double injection pump with the speed of 0.5mL/h, constant temperature stirring 10h is continued after adding, is centrifuged and removes Supernatant (in order to remove the silver nitrate not grown on graphene film), obtains and carries silver-colored graphene solution;
C, silver-colored graphene solution will be carried with 5mL concentration for the sodium alginate soln of 20mg/mL mix, it is concussion, ultrasonic, mix Sodium alginate-load silver Graphene mixed solution is obtained after uniform;
D, with sheet glass as substrate, sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, Obtain sodium alginate-load silver graphene composite film.
Sodium alginate prepared by Fig. 1 the present embodiment-load silver graphene composite film (a) cross-sectional scans electron microscope (SEM, Zeiss Supra 40, Germany), (b) transmission electron microscope figure (TEM, Hitachi HT7700), (c) Mapping energy Spectrum and (d) ESEM power spectrum (EDS, X-Max, Oxford).It can be seen that sodium alginate-load silver graphene composite film is stratiform Structure, comprising carbon, sodium, silver-colored three kinds of characteristic elements, and the Argent grain in the original solution of sodium alginate-load silver graphene composite film It is evenly distributed, Argent grain size is in 10nm or so.
By the simple regulation and control to spraying construction from part, sodium alginate-load silver Graphene mixed solution can be prepared into not The composite membrane of stack pile, Fig. 2 (a) be the present embodiment prepared by several thickness composite membranes cross-sectional scans electron microscope (SEM, Zeiss Supra 40, Germany), it can be seen that the Modulatory character of composite film thickness.By analysis, the composite membrane for being obtained The unit plane of the silver-colored Graphene of sodium alginate-loads in thickness and the sodium alginate being sprayed in substrate-load silver Graphene mixed solution Product quality is linear, such as shown in Fig. 2 (b).
To contrast the performance of different films, the present embodiment is produced as follows several films as follows:
The preparation method of sodium alginate film:The sodium alginate of 2g is added in the deionized water of 100mL, then stir, Ultrasound, until sodium alginate is thoroughly dissolved in deionized water (concentration of sodium alginate soln is 20mg/mL).With sheet glass as base Bottom, film forming is prepared by spraying construction from part by sodium alginate soln, that is, obtain sodium alginate film.
The preparation method of sodium alginate-graphene composite film:The sodium alginate soln for preparing is mixed with graphene solution (sodium alginate is 4 with the mass ratio of Graphene afterwards:1), concussion, ultrasound, until graphene solution mixes with sodium alginate soln Uniformly.Then the mixture of the two is prepared into sodium alginate-graphene composite film by spraying the method for assembling.
The preparation method of sodium alginate-silver composite membrane:The sodium alginate soln of preparation is mixed with the nano-Ag particles aqueous solution (sodium alginate is 12.5 with the mass ratio of nano-Ag particles for conjunction:1) afterwards concussion, ultrasound, until nano-Ag particles solution and marine alga Acid sodium solution is well mixed.Then the mixture of the two is prepared into sodium alginate-silver composite membrane by spraying the method for assembling.
Fig. 3 (a) is four kinds of XRDs of film, it can be seen that:Only sodium alginate-load silver graphene composite film be The characteristic peak of silver is occurred in that at 2theta=38.2 ° and 2theta=44.3 °, and Graphene is occurred in that at 2theta=20 ° Characteristic peak.Demonstrate the composition that sodium alginate manufactured in the present embodiment-load silver graphene composite film contains silver and Graphene.
As shown in Fig. 3 (b), using ultraviolet-uisible spectrophotometer to sodium alginate-load silver graphene composite film and marine alga Sour sodium-graphene composite film is analyzed, it can be seen that sodium alginate-load silver graphene composite film is at wavelength is equal to 446nm There is the absworption peak of obvious silver, and as the sodium alginate-graphene composite film of control then without this peak.Further demonstrate sea Mosanom-load silver graphene composite film contains the composition of silver.
Fig. 4 is that ((a) is sodium alginate film to four kinds of SEM figures of film, and (b) is sodium alginate-silver composite membrane, and (c) is marine alga Sour sodium-graphene composite film, (d) is sodium alginate-load silver graphene composite film), it can be seen that:In four kinds of films, sodium alginate Film and sodium alginate-silverskin are not incorporated into Graphene, so its section does not have layer structure;And sodium alginate-graphene film and Sodium alginate-load silver graphene film makes section form layer structure because graphene-doped.The incorporation of nanoscale graphite alkene piece and The ordered lamellar structure of formation enhances the mechanical property of film.
As shown in figure 5, the 4 kinds of films for preparing to be carried out the test of mechanical property, it can be seen that containing Graphene composition two The tensile stress of kind of film (the silver-colored graphene composite film of sodium alginate-loads and sodium alginate-graphene composite film) is respectively 161.2 ± 4.6Mpa and 146 ± 6.0MPa;Without graphene-containing composition two kinds of tensile stresses of film (sodium alginate film and sodium alginate- Silver composite membrane) there was only 57.0 ± 5.0MPa and 65.0 ± 4.9MPa respectively.Illustrate that the addition of Graphene composition improves film Tensile stress.The elongation strain numerical value of sodium alginate film is 6.5%, sodium alginate-load silver graphene composite film, sodium alginate- Graphene composite film, the elongation strain numerical value of sodium alginate-silver composite membrane are respectively 5.2%, 5.7%, 6.3%, illustrate stone The addition of black alkene composition does not cause significant reduction to the elongation strain of film.
Be 4 kinds of anti-microbial properties of film of test, four kinds of films are cut into diameter is about 1 centimeter of circle of size, and respectively with it is dense Spend is 1 × 106Escherichia coli and candida albicans temperature be 37 DEG C of culture mediums in co-culture 24 hours, then observe and clap According to as shown in Figure 6.It can be seen that:By the co-cultivation of 24 hours, sodium alginate-load silver graphene composite film was to Escherichia coli There is antibacterial effect with candida albicans.Sodium alginate-graphene composite film and sodium alginate film are then substantially to two kinds of lifes of bacterium Unrestraint effect long.Although growth of the sodium alginate-silver composite membrane to two kinds of bacterium has inhibition, the mechanical property of film It is poor compared with sodium alginate-load silver graphene composite film, there occurs the phenomenon of water absorption and swelling.
It is the promotion wound healing function of 4 sodium alginates of test-load silver graphene composite film, by adult male SD rats fiber crops Back hair is rejected after liquor-saturated, is cut using aseptic operation and is each side cut the circular wound of diameter about 1.2cm at back, its In, left dorsal wound makees any treatment as a control group, not.Right Wound sticks the alginic acid essentially identical with wound size Sodium-load silver graphene composite film was observed simultaneously as test group respectively at first day, the 3rd day, the 5th day and the 7th day Taking Pictures recording, as shown in Figure 7.As can be seen that the skin wounds of experimental group occurred in that obvious healing sign at the 7th day, and By contrast, the skin wounds of control group do not heal significantly sign after 7 days.This illustrates sodium alginate-load silver graphite Alkene composite membrane has the function of promoting Wound healing.
Therefore, sodium alginate of the invention-load silver graphene composite film, is provided simultaneously with antibacterial and promotes wound healing function Function, with very big clinical application potentiality.
Embodiment 2
The present embodiment prepares sodium alginate-load silver graphene composite film as follows:
A, take 300mg graphene oxide sheets and be added in 200mL distilled water, after ultrasonic disperse, add 2g polystyrene sulphur Sour sodium, stirring and dissolving adds 200 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, and products therefrom is through suction filtration, lyophilized Afterwards, that is, reduced form graphene oxide-polystyrene sulphuric acid sodium compound is obtained;
B, by step a obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound add into 100mL water, It is well mixed, it is put into single neck bottle of 250mL, 60 DEG C are heated to, then by 10mL concentration for the silver nitrate of 0.02mol/L is molten Liquid is slowly added into single neck bottle with the speed of 0.5mL/h by double injection pump, and constant temperature stirring 10h is continued after adding, and is centrifuged and is gone Except supernatant, obtain and carry silver-colored graphene solution;
C, silver-colored graphene solution will be carried with 10mL concentration for the sodium alginate soln of 25mg/mL mix, it is concussion, ultrasonic, it is mixed Close uniform rear acquisition sodium alginate-load silver Graphene mixed solution;
D, with sheet glass as substrate, sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, Obtain sodium alginate-load silver graphene composite film.
Through X-ray diffraction (Philips X'Pert PRO SUPER X-ray diffractometer) and ESEM Power spectrum (EDS, X-Max, Oxford) proves, the sodium alginate prepared by the present embodiment-load silver graphene composite film contain carbon, Sodium, silver-colored three kinds of characteristic elements.Show the marine alga prepared by the present embodiment by antibacterial experiment and rat skin Wound Healing Experiments Sour sodium-load silver graphene composite film has good antibacterial functions and the good function of promoting rat skin wound healing.
Embodiment 3
The present embodiment prepares sodium alginate-load silver graphene composite film as follows:
A, take 200mg graphene oxide sheets and be added in 300mL distilled water, after ultrasonic disperse, add 2g polystyrene sulphur Sour sodium, stirring and dissolving adds 400 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, and products therefrom is through suction filtration, lyophilized Afterwards, that is, reduced form graphene oxide-polystyrene sulphuric acid sodium compound is obtained;
B, by step a obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound add into 100mL water, It is well mixed, it is put into single neck bottle of 250mL, 60 DEG C are heated to, then by 10mL concentration for the silver nitrate of 0.02mol/L is molten Liquid is slowly added into single neck bottle with the speed of 0.5mL/h by double injection pump, and constant temperature stirring 10h is continued after adding, and is centrifuged and is gone Except supernatant, obtain and carry silver-colored graphene solution;
C, silver-colored graphene solution will be carried with 15mL concentration for the sodium alginate soln of 30mg/mL mix, it is concussion, ultrasonic, it is mixed Close uniform rear acquisition sodium alginate-load silver Graphene mixed solution;
D, with sheet glass as substrate, sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, Obtain sodium alginate-load silver graphene composite film.
Through X-ray diffraction (Philips X'Pert PRO SUPER X-ray diffractometer) and ESEM Power spectrum (EDS, X-Max, Oxford) proves, the sodium alginate prepared by the present embodiment-load silver graphene composite film contain carbon, Sodium, silver-colored three kinds of characteristic elements.Show the marine alga prepared by the present embodiment by antibacterial experiment and rat skin Wound Healing Experiments Sour sodium-load silver graphene composite film has good antibacterial functions and the good function of promoting rat skin wound healing.
Embodiment 4
The present embodiment prepares sodium alginate-load silver graphene composite film as follows:
A, take 100mg graphene oxide sheets and be added in 150mL distilled water, after ultrasonic disperse, add 2g polystyrene sulphur Sour sodium, stirring and dissolving adds 150 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, and products therefrom is through suction filtration, lyophilized Afterwards, that is, reduced form graphene oxide-polystyrene sulphuric acid sodium compound is obtained;
B, by step a obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound add into 100mL water, It is well mixed, it is put into single neck bottle of 150mL, 60 DEG C are heated to, then by 10mL concentration for the silver nitrate of 0.02mol/L is molten Liquid is slowly added into single neck bottle with the speed of 0.5mL/h by double injection pump, and constant temperature stirring 10h is continued after adding, and is centrifuged and is gone Except supernatant, obtain and carry silver-colored graphene solution;
C, silver-colored graphene solution will be carried with 15mL concentration for the sodium alginate soln of 30mg/mL mix, it is concussion, ultrasonic, it is mixed Close uniform rear acquisition sodium alginate-load silver Graphene mixed solution;
D, with sheet glass as substrate, sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, Obtain sodium alginate-load silver graphene composite film.
Through X-ray diffraction (Philips X'Pert PRO SUPER X-ray diffractometer) and ESEM Power spectrum (EDS, X-Max, Oxford) proves, the sodium alginate prepared by the present embodiment-load silver graphene composite film contain carbon, Sodium, silver-colored three kinds of characteristic elements.Show the marine alga prepared by the present embodiment by antibacterial experiment and rat skin Wound Healing Experiments Sour sodium-load silver graphene composite film has good antibacterial functions and the good function of promoting rat skin wound healing.
Embodiment 5
The present embodiment prepares sodium alginate-load silver graphene composite film as follows:
A, take 100mg graphene oxide sheets and be added in 200mL distilled water, after ultrasonic disperse, add 2g polystyrene sulphur Sour sodium, stirring and dissolving adds 400 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, and products therefrom is through suction filtration, lyophilized Afterwards, that is, reduced form graphene oxide-polystyrene sulphuric acid sodium compound is obtained;
B, by step a obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound add into 100mL water, It is well mixed, it is put into single neck bottle of 250mL, 60 DEG C are heated to, then by 10mL concentration for the silver nitrate of 0.02mol/L is molten Liquid is slowly added into single neck bottle with the speed of 0.5mL/h by double injection pump, and constant temperature stirring 10h is continued after adding, and is centrifuged and is gone Except supernatant, obtain and carry silver-colored graphene solution;
C, silver-colored graphene solution will be carried with 5mL concentration for the sodium alginate soln of 15mg/mL mix, it is concussion, ultrasonic, mix Sodium alginate-load silver Graphene mixed solution is obtained after uniform;
D, with sheet glass as substrate, sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, Obtain sodium alginate-load silver graphene composite film.
Through X-ray diffraction (Philips X'Pert PRO SUPER X-ray diffractometer) and ESEM Power spectrum (EDS, X-Max, Oxford) proves, the sodium alginate prepared by the present embodiment-load silver graphene composite film contain carbon, Sodium, silver-colored three kinds of characteristic elements.Show the marine alga prepared by the present embodiment by antibacterial experiment and rat skin Wound Healing Experiments Sour sodium-load silver graphene composite film has good antibacterial functions and the good function of promoting rat skin wound healing.
Exemplary embodiment of the invention is the foregoing is only, is not intended to limit the invention, it is all of the invention Any modification, equivalent and improvement made within spirit and principle etc., should be included within the scope of the present invention.

Claims (5)

1. there is antibacterial and promote the preparation method of the sodium alginate-load silver graphene composite film of wound healing function, its feature It is to carry out as follows:
A, take 100~300mg graphene oxide sheets and be added in 150~300mL distilled water, after ultrasonic disperse, add 2g polyphenyl Oxyethylene sulfate, stirring and dissolving adds 150~400 μ L hydrazine hydrates, is heated to 100 DEG C of back flow reactions 24 hours, products therefrom Through suction filtration, it is lyophilized after, obtain reduced form graphene oxide-polystyrene sulphuric acid sodium compound;
B, by step a obtain the reduced form graphene oxide-polystyrene sulphuric acid sodium compound add to 50~100mL water In, it is well mixed, it is put into single neck bottle, 60 DEG C are heated to, then by 5~10mL concentration for the silver nitrate of 0.02mol/L is molten Liquid is added in single neck bottle with the speed of 0.5mL/h, and constant temperature stirring 10h is continued after adding, and is centrifuged and removes supernatant, is obtained and is carried silver Graphene solution;
C, carry described silver-colored graphene solution and mix with the sodium alginate soln that 5~25mL concentration is 15~35mg/mL, shake, Ultrasound, obtains sodium alginate-load silver Graphene mixed solution after being well mixed;
D, the sodium alginate-load silver Graphene mixed solution is prepared into film forming by spraying construction from part, that is, obtain sodium alginate- Carry silver-colored graphene composite film.
2. the sodium alginate prepared by preparation method described in a kind of claim 1-load silver graphene composite film.
3. sodium alginate according to claim 2-load silver graphene composite film, it is characterised in that:Sodium alginate-the load Silver-colored graphene composite film has imitative concba lamellar structure.
4. sodium alginate according to claim 2-load silver graphene composite film, it is characterised in that:Sodium alginate-the load Silver-colored graphene composite film has antibacterial and promotes wound healing function simultaneously.
5. a kind of application of the sodium alginate in claim 2~4 described in any one-load silver graphene composite film, its feature It is:For as wound surgical dressing.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109207984A (en) * 2018-08-20 2019-01-15 中国科学院金属研究所 The preparation method of corrosion resistant antibiotic anti-biofouling multifunctional metal-base protective coating
CN109481727A (en) * 2018-09-30 2019-03-19 佛山市华健科创科技有限公司 A kind of photocatalysis antibacterial aerogel dressing and preparation method thereof
CN109568648A (en) * 2018-11-27 2019-04-05 合肥工业大学 A kind of preparation method and applications with antibacterial and the irreversible composite hydrogel of thermal induction for promoting wound healing function
CN113100253A (en) * 2021-04-14 2021-07-13 深圳清华大学研究院 Preparation method of carbon oxide nanohorn/sodium alginate-silver composite antibacterial agent, antibacterial coating and antibacterial film
CN113694244A (en) * 2021-09-01 2021-11-26 东华大学 Cotton gauze reinforced hydrogel conductive dressing with photo-thermal antibacterial and healing promoting effects and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1709108A1 (en) * 2004-01-28 2006-10-11 Qinetiq Nanomaterials Limited Method of manufacture of polymer composites
CN102125056A (en) * 2011-01-10 2011-07-20 中国科学技术大学 Method for preparing silver/graphene antimicrobial composite material
CN103446621A (en) * 2013-05-07 2013-12-18 哈尔滨工程大学 Nano-silver-containing sodium alginate based antibacterial medical dressing and preparation method thereof
CN106192074A (en) * 2016-07-15 2016-12-07 东华大学 A kind of preparation method of the graphene oxide/Sargassum composite fibre being loaded with nano silver particles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1709108A1 (en) * 2004-01-28 2006-10-11 Qinetiq Nanomaterials Limited Method of manufacture of polymer composites
CN102125056A (en) * 2011-01-10 2011-07-20 中国科学技术大学 Method for preparing silver/graphene antimicrobial composite material
CN103446621A (en) * 2013-05-07 2013-12-18 哈尔滨工程大学 Nano-silver-containing sodium alginate based antibacterial medical dressing and preparation method thereof
CN106192074A (en) * 2016-07-15 2016-12-07 东华大学 A kind of preparation method of the graphene oxide/Sargassum composite fibre being loaded with nano silver particles

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109207984A (en) * 2018-08-20 2019-01-15 中国科学院金属研究所 The preparation method of corrosion resistant antibiotic anti-biofouling multifunctional metal-base protective coating
CN109481727A (en) * 2018-09-30 2019-03-19 佛山市华健科创科技有限公司 A kind of photocatalysis antibacterial aerogel dressing and preparation method thereof
CN109568648A (en) * 2018-11-27 2019-04-05 合肥工业大学 A kind of preparation method and applications with antibacterial and the irreversible composite hydrogel of thermal induction for promoting wound healing function
CN109568648B (en) * 2018-11-27 2021-01-29 合肥工业大学 Preparation method and application of heat-induced irreversible composite hydrogel with antibacterial and wound healing promoting functions
CN113100253A (en) * 2021-04-14 2021-07-13 深圳清华大学研究院 Preparation method of carbon oxide nanohorn/sodium alginate-silver composite antibacterial agent, antibacterial coating and antibacterial film
CN113100253B (en) * 2021-04-14 2022-08-05 深圳清华大学研究院 Preparation method of carbon oxide nanohorn/sodium alginate-silver composite antibacterial agent, antibacterial coating and antibacterial film
CN113694244A (en) * 2021-09-01 2021-11-26 东华大学 Cotton gauze reinforced hydrogel conductive dressing with photo-thermal antibacterial and healing promoting effects and preparation method thereof

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