CN103834050B - The preparation method of gelatin/nanometer silver/chitosan derivatives laminated film - Google Patents
The preparation method of gelatin/nanometer silver/chitosan derivatives laminated film Download PDFInfo
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- CN103834050B CN103834050B CN201410107258.1A CN201410107258A CN103834050B CN 103834050 B CN103834050 B CN 103834050B CN 201410107258 A CN201410107258 A CN 201410107258A CN 103834050 B CN103834050 B CN 103834050B
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Abstract
The present invention proposes the preparation method of a kind of gelatin/nanometer silver/chitosan derivatives laminated film.This laminated film, with gelatin as primary raw material, dissolves the method such as gelatin particle and in-situ reducing by heat temperature raising, prepares gelatin/nano silver colloidal sol, use the mode of self assembly in the solution to prepare gelatin/nano silver film；Use electrostatic self-assembled method further, chitosan derivatives macromole is assembled in the surface of gelatin/nano silver film, prepares gelatin/nanometer silver/chitosan derivative antibacterial laminated film.This laminated film has good biocompatibility and antibacterial, bactericidal property, and environmentally friendly；It is gelatin because of its main raw material(s) again, abundance, cheap, good film-forming property, it is with a wide range of applications at aspects such as human body skin, medical antibacterial and hemostatic materials；The preparation technology of this kind of laminated film is simple simultaneously, low for equipment requirements.
Description
Technical field
The invention belongs to biomaterial, polymer chemistry and biochemical interdisciplinary field, disclose the preparation method of gelatin/nano-silver antibacterial composite film that a kind of chitosan derivatives is modified.
Background technology
Gelatin, as the extract of animal collagen tissue, is a kind of natural polymer and biological macromolecule material, and it has good biocompatibility, no antigen, stops blooding and promote the performances such as organization healing.The gelatin resources reserve of China is abundant, wide material sources, cheap, and due to performances such as good reactivity, film property, coagulability, biocompatibility, degradability, green environmental protection and the recyclabilities of gelatin so that it is become the study hotspot of biological macromolecule material scientific domain in recent years.At present, the gelatin application in biological macromolecule material field is limited primarily to surface capping agents, filler or cross-linking agent etc., and with gelatin as main raw material(s), in-situ reducing is prepared nanometer silver and the research application being applied to self-assembled film field is rarely reported.
Nanometer silver has good sterilization and antibacterial action, is the most just commonly used by people for accelerating wound healing, treatment infection, purifies water source etc..Nanometer silver, compared with common silver, has bigger specific surface area, surface energy and reactivity.Modern study result shows, nanometer silver is better than far away traditional silver ion disinfectant to fatal bacillus, coccus, the killing action of silk bacterium；And nano silver particles overcomes the characteristic that ionic state silver in the solution can not be stable, therefore nanometer silver has, in sterilization, antibacterial field, the advantage that the antibacterial such as conventional silver ion and large scale argent is incomparable.
Chitosan is also a kind of natural macromolecular material, has good biological activity, biocompatibility, biological degradability, film property and antibiotic and sterilizing, can preferably promote wound healing and tissue repair.Up to now, chitosan has application more at biological macromolecule material, biochemical reaction and biomedical sector.Chitosan contains free amino group, can be coordinated with the carboxyl in gelatin molecule structure, hydroxyl, sulfydryl etc. and cross-link.At present, the compound preparation of chitosan and gelatin mainly uses the mode that heating is blended, and the mode such as less employing electrostatic self-assembled and heat cross-linking.
Therefore this patent combines the advantage of gelatin, nanometer silver and chitosan, use gelatin in-situ reducing to prepare the method such as nanometer silver and self-assembly chitosan derivant and prepare gelatin/nanometer silver/chitosan derivatives laminated film, to utilizing gelatin and chitosan and the good bactericidal properties of derivative good biocompatibility, degradability, nanometer silver and chitosan derivatives to be applied in the fields such as Medical sterilization dressing, hemostatic material and human body skin material.
Summary of the invention
It is contemplated that at least solve one of above-mentioned technological deficiency.
To this end, the first of the present invention purpose is to propose a kind of have good biocompatibility, simple to operate, environmental protection, the preparation method of cheap gelatin/nanometer silver/chitosan derivative antibacterial laminated film, the method comprises the steps:
(1) preparation of aqueous gelatin solution:
Gelatin joins deionized water, and stirring is warming up to 60 ° of C-80 ° of C insulation reaction 1-3 hour, prepares aqueous gelatin solution；
(2) preparation of gelatin/nano silver colloidal sol:
In the aqueous gelatin solution prepared by step (1), add silver nitrate, be warming up to predetermined temperature the insulated and stirred reaction scheduled time, obtain gelatin/nano silver colloidal sol；
(3) preparation of gelatin/nano silver film:
Film substrate is dipped in concentrated sulphuric acid and mixed solution that hydrogen peroxide volume ratio is 7:3,3-6 hour, takes out and use deionized water rinsing；Being dipped in the scheduled time in the gelatin/nano silver colloidal sol prepared by step (2) again, take out and blot the gelatin/nano silver colloidal sol of excess surface, at room temperature cooling stands 10 minutes-30 minutes, obtains gelatin/nano silver film；
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film:
Gelatin/nano silver film that step (3) obtains is dipped in the chitosan derivative solution of mass concentration 1-3% 5-20 minute, take out and use deionized water rinsing, heat the scheduled time under predetermined heating-up temperature, prepare gelatin/antibacterial laminated film of nanometer silver/chitosan.
Preferably, in step (1), the mass concentration scope of institute's gelatin water solution of preparation is 6.25%-20%.
Preferably, the silver nitrate added in step (2) is 1:40-7:40 with the quality of gelatin in aqueous gelatin solution than scope.
Preferably, being warming up to predetermined temperature and in the insulated and stirred reaction scheduled time described in step (2), described predetermined temperature range is 90 ° of C-95 ° of C, and the described scheduled time is 1-2 hour.
Preferably, any one during film substrate is the binder of piezoid, sheet glass, titanium dioxide silicon chip, the gauze of fibrous substrate or fibrous substrate described in step (3).
Preferably, the described scheduled time scope that in step (3), film substrate immerses in gelatin/nano silver colloidal sol is 1-3 hour.
Preferably, when in step (3), film substrate immerses in gelatin/nano silver colloidal sol, described gelatin/nano silver colloidal sol temperature is maintained at 60 ° of C-65 ° of C.
Preferably, heating temperature range predetermined described in step (4) is 40 ° of C-45 ° of C, and described scheduled time scope is 40 minutes-60 minutes.
Preferably, described laminated film is mainly used in the fields such as artificial skin, medical antibacterial dressing and hemostatic material.
Preferably; described chitosan derivatives is any one in chitosan, carboxymethyl chitosan, CMC, chitosan hydrochlorate, chitosan quaternary ammonium salt, hydroxypropyl chitosan, N-N-trimethyl chitosan TMC, N-Nmaleoyl chitosan, beta cyclodextrin grafted chitosan, Allan sodium phosphate chitosan.
Above-mentioned gelatin/nanometer silver/chitosan derivative antibacterial laminated film prepared by the present invention, is mainly used in the fields such as artificial skin, bio-medical disinfectant dressing and hemostatic material.
The present invention compared with prior art, has the advantage that and beneficial effect: employing gelatin is main raw material(s), improves the utilization rate of gelatin resource, reduce simultaneously existing bio-medical thin-film material to fossil feedstock according to patience；Gelatin has many good characteristics such as wide material sources, cheap, environmental protection, good biocompatibility and recoverable；Use that the nanometer silver shape prepared of in-situ reducing method is regular, dimensionally stable, being evenly distributed contacts closely with gelatin molecule；Use chitosan or derivatives thereof, by self assembly mode, gelatin/nano silver film is carried out surface modification; the thin film high-sequential prepared arranges, defect is few, adhesion is strong; there is good biocompatibility and bactericidal properties; and this thin film with after garbage can degrade the most voluntarily, be conducive to protecting environment；This preparation method is simple, it is low to require instrument and equipment, be easy to method promotes the use of.
Detailed description of the invention
The present invention, with gelatin as primary raw material, first passes through in-situ reducing silver nitrate and prepares gelatin/nano silver colloidal sol liquid, prepare gelatin/nano silver film in the way of self assembly；With chitosan derivatives as coating material, prepare gelatin/nanometer silver/chitosan derivative antibacterial laminated film by electrostatic self-assembled mode.
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment
1
(1) preparation of aqueous gelatin solution: take 4g gelatin particle in beaker, adds the deionized water of 30mL in beaker, and stirring is warming up to 70 DEG C and insulation reaction 1 hours, and preparation mass concentration is the aqueous gelatin solution of 11.8%.
(2) preparation of gelatin/nano silver colloidal sol: poured into aqueous gelatin solution 30mL prepared by step (1) in the there-necked flask of 50mL, addition 0.5g silver nitrate powder, in there-necked flask, is warming up to 95 DEG C and insulated and stirred is reacted 1 hours.
(3) preparation of gelatin/nano silver film: piezoid is immersed in concentrated sulphuric acid and mixed solution that hydrogen peroxide volume ratio is 7:3, after 3 hours, take out and use deionized water rinsing；Being dipped in the gelatin/nano silver colloidal sol of 65 DEG C of preparation 1 hour in step (2) the most again, take out and blot the gelatin/nano silver colloidal sol of excess surface, at room temperature cooling stands 10 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: gelatin/nano silver film is dipped in the chitosan derivative solution that mass concentration is 1.5% 10 minutes, take out and use deionized water rinsing, it is placed on the warm table of 45 DEG C heating 40 minutes, prepares gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
Embodiment
2
(1) preparation of aqueous gelatin solution: take 8g gelatin particle in beaker, adds the deionized water of 32mL in beaker, and stirring is warming up to 80 DEG C and insulation reaction 1 hours, and preparation mass concentration is the aqueous gelatin solution of 20%.
(2) preparation of gelatin/nano silver colloidal sol: poured into aqueous gelatin solution 30mL prepared by step (1) in the there-necked flask of 50mL, addition 0.6g silver nitrate powder, in there-necked flask, is warming up to 95 DEG C and insulated and stirred is reacted 1 hours.
(3) preparation of gelatin/nano silver film: piezoid is immersed in concentrated sulphuric acid and mixed solution that hydrogen peroxide volume ratio is 7:3, after 3 hours, take out and use deionized water rinsing；Being dipped in the gelatin/nano silver colloidal sol of 60 DEG C of preparation 2 hours in step (2) the most again, take out and blot the gelatin/nano silver colloidal sol of excess surface, at room temperature cooling stands 20 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: gelatin/nano silver film is dipped in the chitosan derivative solution that mass concentration is 2% 10 minutes, take out and use deionized water rinsing, it is placed on the warm table of 40 DEG C heating 60 minutes, prepares gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
Embodiment
3
(1) preparation of aqueous gelatin solution: take 4g gelatin particle in beaker, adds the deionized water of 60mL in beaker, and stirring is warming up to 65 DEG C and insulation reaction 2 hours, and preparation mass concentration is the aqueous gelatin solution of 6.25%.
(2) preparation of gelatin/nano silver colloidal sol: poured into aqueous gelatin solution 30mL prepared by step (1) in the there-necked flask of 50mL, addition 0.1g silver nitrate powder, in there-necked flask, is warming up to 90 DEG C and insulated and stirred is reacted 1 hours.
(3) preparation of gelatin/nano silver film: piezoid is immersed in concentrated sulphuric acid and mixed solution that hydrogen peroxide volume ratio is 7:3, after 3 hours, take out and use deionized water rinsing；Being dipped in the gelatin/nano silver colloidal sol of 60 DEG C of preparation 3 hours in step (2) the most again, take out and blot the gelatin/nano silver colloidal sol of excess surface, at room temperature cooling stands 15 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: gelatin/nano silver film is dipped in the chitosan derivative solution that mass concentration is 1% 10 minutes, take out and use deionized water rinsing, it is placed on the warm table of 45 DEG C heating 50 minutes, prepares gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
Embodiment
4
(1) preparation of aqueous gelatin solution: take 4g gelatin particle in beaker, adds the deionized water of 30mL in beaker, and stirring is warming up to 75 DEG C and insulation reaction 1.5 hours, and preparation mass concentration is the aqueous gelatin solution of 11.8%.
(2) preparation of gelatin/nano silver colloidal sol: poured into aqueous gelatin solution 30mL prepared by step (1) in the there-necked flask of 50mL, addition 0.6g silver nitrate powder, in there-necked flask, is warming up to 95 DEG C and insulated and stirred is reacted 1 hours.
(3) preparation of gelatin/nano silver film: piezoid is immersed in concentrated sulphuric acid and mixed solution that hydrogen peroxide volume ratio is 7:3, after 3 hours, take out and use deionized water rinsing；Being dipped in the gelatin/nano silver colloidal sol of 65 DEG C of preparation 3 hours in step (2) the most again, take out and blot the gelatin/nano silver colloidal sol of excess surface, at room temperature cooling stands 20 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: gelatin/nano silver film is dipped in the chitosan derivative solution that mass concentration is 3% 10 minutes, take out and use deionized water rinsing, it is placed on the warm table of 45 DEG C heating 60 minutes, prepares gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
Alternatively, in above-described embodiment, film substrate piezoid as gelatin/nano silver film is possible with sheet glass, titanium dioxide silicon chip, the gauze of fibrous substrate or binder etc. any one replaces, and the preparation method that uses above-mentioned film substrate to carry out time prepared by gelatin/nano silver film is similar with embodiment 1-4 with preparation condition, is not repeated at this.
In addition; the chitosan derivatives used in above-described embodiment can be any one in chitosan itself, carboxymethyl chitosan, CMC, chitosan hydrochlorate, chitosan quaternary ammonium salt, hydroxypropyl chitosan, N-N-trimethyl chitosan TMC, N-Nmaleoyl chitosan, beta cyclodextrin grafted chitosan, Allan sodium phosphate chitosan.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, being appreciated that and these embodiments can carry out multiple change without departing from the principles and spirit of the present invention, revise, replace and modification, the scope of the present invention is limited by claims and equivalent thereof.
Claims (10)
1. the preparation method of gelatin/nanometer silver/chitosan derivative antibacterial laminated film, it is characterised in that institute
State preparation method to comprise the steps:
(1) preparation of aqueous gelatin solution:
Gelatin joins deionized water, and stirring is warming up to 60 DEG C-80 DEG C and insulation reaction 1-3 hour, system
For going out aqueous gelatin solution；
(2) preparation of gelatin/nano silver colloidal sol:
In the aqueous gelatin solution prepared by step (1), add silver nitrate, be warming up to predetermined temperature and insulated and stirred is anti-
Answer the scheduled time, obtain gelatin/nano silver colloidal sol；
(3) preparation of gelatin/nano silver film:
Film substrate is dipped in concentrated sulphuric acid and mixed solution that hydrogen peroxide volume ratio is 7:3,3-6 hour, takes out
And use deionized water rinsing；It is dipped in the scheduled time in the gelatin/nano silver colloidal sol prepared by step (2) again, takes
Going out and blot the gelatin/nano silver colloidal sol of excess surface, at room temperature cooling stands 10 minutes-30 minutes, obtains
Gelatin/nano silver film；
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film:
Gelatin/nano silver film that step (3) obtains is dipped in the chitosan derivative solution of mass concentration 1-3%
5-20 minute, take out and with deionized water rinsing, heat the scheduled time under predetermined heating-up temperature, preparing gelatin
The antibacterial laminated film of/nanometer silver/chitosan.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: in step (1), the mass concentration scope of institute's gelatin water solution of preparation is 6.25%-20%.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: the silver nitrate added in step (2) with the quality of gelatin in aqueous gelatin solution than scope is
1:40-7:40。
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: it is warming up to predetermined temperature described in step (2) and in the insulated and stirred reaction scheduled time, described
Predetermined temperature range is 90 DEG C-95 DEG C, and the described scheduled time is 1-2 hour.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: film substrate described in step (3) is piezoid, sheet glass, titanium dioxide silicon chip, fibre
Gauze at the bottom of Wiki or any one in the binder of fibrous substrate.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: the described scheduled time that in step (3), film substrate immerses in gelatin/nano silver colloidal sol
Scope is 1-3 hour.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: when in step (3), film substrate immerses in gelatin/nano silver colloidal sol, described gelatin/
Nano silver colloidal sol temperature is maintained at 60 DEG C-65 DEG C.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: heating temperature range predetermined described in step (4) is 40 DEG C-45 DEG C, described predetermined
Time range is 40 minutes-60 minutes.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: described laminated film is mainly used in artificial skin, medical antibacterial dressing and hemostatic material field.
The preparation side of gelatin/nanometer silver/chitosan derivative antibacterial laminated film the most according to claim 1
Method, it is characterised in that: described chitosan derivatives be chitosan, carboxymethyl chitosan, CMC,
Chitosan hydrochlorate, chitosan quaternary ammonium salt, hydroxypropyl chitosan, N-N-trimethyl chitosan TMC, N-maleylation shell are poly-
Any one in sugar, beta cyclodextrin grafted chitosan, Allan sodium phosphate chitosan.
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| CN104233436B (en) * | 2014-09-15 | 2016-09-14 | 武汉理工大学 | A kind of chitosan/gelatin/nano-silver conductive antibacterial biological material and preparation method thereof |
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| CN106963982A (en) * | 2017-04-24 | 2017-07-21 | 广东医科大学附属医院 | A kind of repair materials adhered to anti-bacteria wet keeping appropriate tissue and its preparation method and application |
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| CN110522945B (en) * | 2019-10-11 | 2020-07-03 | 山东速康医疗科技有限公司 | Medical biogel hemostatic dressing and preparation method thereof |
| CN110755678B (en) * | 2019-11-13 | 2021-08-17 | 中国矿业大学 | 3D printing antibacterial hydrogel wound dressing based on green in-situ reduction |
| CN112717194B (en) * | 2020-12-30 | 2022-02-18 | 河南亚都实业有限公司 | Degradable chitosan-based composite hemostatic film |
| CN113185729A (en) * | 2021-03-26 | 2021-07-30 | 南京航空航天大学 | Flexible silver nanowire transparent electromagnetic shielding film and preparation method thereof |
| CN115636885B (en) * | 2022-10-26 | 2023-08-11 | 湖北中医药大学 | Quaternary ammonium cyclodextrin and preparation method and application thereof, silver nanoparticle cyclodextrin compound and preparation method and application thereof |
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| CN101073830A (en) * | 2007-06-15 | 2007-11-21 | 东华大学 | Gelatin-silver nano-material, its production and use |
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| 含纳米银的明胶/壳聚糖纳米纤维的制备及其抗菌性能研究;徐雄立;《化工新型材料》;20100228;第38卷(第2期);第23-25页 * |
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