CN103834050A - Method for preparing gelatin/nano-silver/chitosan derivative composite film - Google Patents
Method for preparing gelatin/nano-silver/chitosan derivative composite film Download PDFInfo
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- CN103834050A CN103834050A CN201410107258.1A CN201410107258A CN103834050A CN 103834050 A CN103834050 A CN 103834050A CN 201410107258 A CN201410107258 A CN 201410107258A CN 103834050 A CN103834050 A CN 103834050A
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Abstract
The invention provides a method for preparing a gelatin/nano-silver/chitosan derivative composite film. The composite film is prepared by the following steps: by taking gelatin as a main raw material, heating to raise the temperature for dissolving gelatin particles, preparing gelatin/nano-silver sol through an in-situ reduction method, and preparing a gelatin/nano-silver film by adopting a self-assembling method in the solution; assembling a chitosan derivative macromolecule on the surface of the gelatin/nano-silver film by further adopting an electrostatic self-assembling method, and thus preparing the gelatin/nano-silver/chitosan derivative antibacterial composite film. The composite film has high biocompatibility and high antibacterial and bactericidal performance and is environment-friendly. Moreover, because the main raw material is gelatin, the composite film is rich in source, low in price, and good in film-forming property and has wide application prospects in aspects such as human skin, medical antibiosis and hemostatic materials. Meanwhile, the composite film is simple in preparation process and low in equipment requirement.
Description
Technical field
The invention belongs to biomaterial, polymer chemistry and biochemical interdisciplinary field, disclose a kind of preparation method of gelatin/nano-silver antibacterial composite film of chitosan derivatives modification.
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, hemostasis and promotes the performances such as organization healing.The gelatin resources reserve of China is enriched, wide material sources, cheap, and due to performances such as the good reactive behavior of gelatin, film-forming properties, solidifiability, biocompatibility, degradability, green environmental protection and recyclabilities, make it become in recent years the study hotspot of biological macromolecule material scientific domain.At present, gelatin is mainly limited to surperficial coating, weighting agent or linking agent etc. in the application in biological macromolecule material field, and taking gelatin as main raw material(s), in-situ reducing is prepared nanometer silver and the research that is applied to self-assembled film field is applied to rarely seen report.
Nanometer silver has good sterilization and anti-microbial effect, is just used for accelerating wound healing, treatment infection, purified water source etc. by people since ancient times.Nanometer silver, compared with common silver, has larger specific surface area, surface energy and reactive behavior.Modern study result shows, nanometer silver is better than traditional silver ion disinfectant far away to the killing action of fatal bacillus, coccus, silk bacterium; And nano silver particles has overcome the characteristic that ionic state silver can not be stable in solution, and therefore nanometer silver has the incomparable advantage of sterilant such as conventional silver ion and large size argent in sterilization, antibacterial field.
Chitosan is also a kind of natural macromolecular material, has good biological activity, biocompatibility, biological degradability, film-forming properties and antibiotic and sterilizing, can promote preferably wound healing and tissue repair.Up to now, chitosan has application comparatively at biological macromolecule material, biochemical reaction and biomedical sector.Chitosan contains free amino group, can be with coordinations such as the structural carboxyl of gelatin molecule, hydroxyl, sulfydryls and be cross-linked.At present, the compound preparation of chitosan and gelatin mainly adopts the mode of heating blend, and the modes such as less employing electrostatic self-assembled and heat cross-linking.
Therefore this patent is in conjunction with the advantage of gelatin, nanometer silver and chitosan, adopt gelatin in-situ reducing to prepare the method such as nanometer silver and self-assembly chitosan derivative and prepare gelatin/nanometer silver/chitosan derivatives laminated film, to utilizing gelatin and chitosan and derivative good biocompatibility, degradability, the bactericidal properties that nanometer silver and chitosan derivatives are good is applied in the fields such as Medical sterilization dressing, hemostatic material and human body skin material.
Summary of the invention
The present invention is intended at least solve one of above-mentioned technological deficiency.
For this reason, first object of the present invention is to propose a kind of preparation method with good biocompatibility, simple to operate, environmental protection, cheap gelatin/nanometer silver/chitosan derivative antibacterial laminated film, and the method comprises the steps:
(1) preparation of aqueous gelatin solution:
Gelatin is joined to deionized water, stir and be warming up to 60 ° of C-80 ° of C insulation reaction 1-3 hour, prepare aqueous gelatin solution;
(2) preparation of gelatin/nano silver colloidal sol:
In the prepared aqueous gelatin solution of step (1), add Silver Nitrate, be warming up to preset 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 the mixing solutions that the vitriol oil and hydrogen peroxide volume ratio are 7:3, and 3-6 hour, takes out and uses deionized water rinsing; Immersed again the scheduled time in the prepared gelatin/nano silver colloidal sol of step (2), taken out and blot the unnecessary gelatin/nano silver colloidal sol in surface, at room temperature cooling standing 10 minutes-30 minutes, obtained gelatin/nano silver film;
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film:
Gelatin/nano silver film that step (3) is obtained is dipped in 5-20 minute in the chitosan derivative solution of mass concentration 1-3%, take out and use deionized water rinsing, under predetermined Heating temperature, heat the scheduled time, make the antibacterial laminated film of gelatin/nanometer silver/chitosan.
Preferably, in step (1), the mass concentration scope of the described aqueous gelatin solution of preparation is 6.25%-20%.
Preferably, in the Silver Nitrate adding in step (2) and aqueous gelatin solution, the quality of gelatin is 1:40-7:40 than scope.
Preferably, be warming up to preset temperature described in step (2) and in the insulated and stirred reaction scheduled time, described predetermined temperature range is 90 ° of C-95 ° of C, the described scheduled time is 1-2 hour.
Preferably, film substrate described in step (3) is any in quartz plate, sheet glass, titanium dioxide silicon chip, the gauze of fibrous substrate or the bandage of fibrous substrate.
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 remains on 60 ° of C-65 ° of C.
Preferably, predetermined Heating temperature scope 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 in chitosan, cm-chitosan, CMC, chitosan hydrochloride, chitosan quaternary ammonium salt, hydroxypropyl chitosan, N-trimethyl chitin, 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.
Compared with prior art, tool has the following advantages and beneficial effect in the present invention: employing gelatin is main raw material(s), has improved the utilization ratio of gelatin resource, reduced 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; The nanometer silver shape that adopts in-situ reducing method to prepare is regular, dimensional stabilizing, be evenly distributed, contact with gelatin molecule closely; Adopt chitosan or derivatives thereof, by self-assembly mode, gelatin/nano silver film is carried out to finishing, the film high-sequential of preparing is arranged, defect is few, bonding force is strong, there is good biocompatibility and bactericidal properties, and the waste after this film is used can comparatively fast be degraded voluntarily, is conducive to protection of the environment; This preparation method is simple, to plant and instrument require low, be convenient to method and promote the use of.
Embodiment
The present invention, taking gelatin as main raw material, first makes gelatin/nano silver colloidal sol liquid by in-situ reducing Silver Nitrate, prepares gelatin/nano silver film in the mode of self-assembly; Taking chitosan derivatives as coating materials, 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: get 4g gelatin particle in beaker, add the deionized water of 30mL in beaker, stir and be warming up to 70 DEG C and insulation reaction 1 hour, the aqueous gelatin solution that preparation quality concentration is 11.8%.
(2) preparation of gelatin/nano silver colloidal sol: aqueous gelatin solution 30mL prepared by step (1) pours in the there-necked flask of 50mL, adds 0.5g Silver Nitrate powder in there-necked flask, is warming up to 95 DEG C and insulated and stirred reaction 1 hour.
(3) preparation of gelatin/nano silver film: quartz plate is immersed in the mixing solutions that the vitriol oil and hydrogen peroxide volume ratio are 7:3, after 3 hours, take out and use deionized water rinsing; Immersed again afterwards the middle gelatin/nano silver colloidal sol of 65 DEG C of preparing of step (2) 1 hour, taken out and blot the unnecessary gelatin/nano silver colloidal sol in surface, at room temperature cooling standing 10 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: it is in 1.5% chitosan derivative solution 10 minutes that gelatin/nano silver film is dipped in to mass concentration, take out and use deionized water rinsing, be placed on the warm table of 45 DEG C and heat 40 minutes, make gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
embodiment 2
(1) preparation of aqueous gelatin solution: get 8g gelatin particle in beaker, add the deionized water of 32mL in beaker, stir and be warming up to 80 DEG C and insulation reaction 1 hour, the aqueous gelatin solution that preparation quality concentration is 20%.
(2) preparation of gelatin/nano silver colloidal sol: aqueous gelatin solution 30mL prepared by step (1) pours in the there-necked flask of 50mL, adds 0.6g Silver Nitrate powder in there-necked flask, is warming up to 95 DEG C and insulated and stirred reaction 1 hour.
(3) preparation of gelatin/nano silver film: quartz plate is immersed in the mixing solutions that the vitriol oil and hydrogen peroxide volume ratio are 7:3, after 3 hours, take out and use deionized water rinsing; Immersed again afterwards the middle gelatin/nano silver colloidal sol of 60 DEG C of preparing of step (2) 2 hours, taken out and blot the unnecessary gelatin/nano silver colloidal sol in surface, at room temperature cooling standing 20 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: it is in 2% chitosan derivative solution 10 minutes that gelatin/nano silver film is dipped in to mass concentration, take out and use deionized water rinsing, be placed on the warm table of 40 DEG C and heat 60 minutes, make gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
embodiment 3
(1) preparation of aqueous gelatin solution: get 4g gelatin particle in beaker, add the deionized water of 60mL in beaker, stir and be warming up to 65 DEG C and insulation reaction 2 hours, the aqueous gelatin solution that preparation quality concentration is 6.25%.
(2) preparation of gelatin/nano silver colloidal sol: aqueous gelatin solution 30mL prepared by step (1) pours in the there-necked flask of 50mL, adds 0.1g Silver Nitrate powder in there-necked flask, is warming up to 90 DEG C and insulated and stirred reaction 1 hour.
(3) preparation of gelatin/nano silver film: quartz plate is immersed in the mixing solutions that the vitriol oil and hydrogen peroxide volume ratio are 7:3, after 3 hours, take out and use deionized water rinsing; Immersed again afterwards the middle gelatin/nano silver colloidal sol of 60 DEG C of preparing of step (2) 3 hours, taken out and blot the unnecessary gelatin/nano silver colloidal sol in surface, at room temperature cooling standing 15 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: it is in 1% chitosan derivative solution 10 minutes that gelatin/nano silver film is dipped in to mass concentration, take out and use deionized water rinsing, be placed on the warm table of 45 DEG C and heat 50 minutes, make gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
embodiment 4
(1) preparation of aqueous gelatin solution: get 4g gelatin particle in beaker, add the deionized water of 30mL in beaker, stir and be warming up to 75 DEG C and insulation reaction 1.5 hours, the aqueous gelatin solution that preparation quality concentration is 11.8%.
(2) preparation of gelatin/nano silver colloidal sol: aqueous gelatin solution 30mL prepared by step (1) pours in the there-necked flask of 50mL, adds 0.6g Silver Nitrate powder in there-necked flask, is warming up to 95 DEG C and insulated and stirred reaction 1 hour.
(3) preparation of gelatin/nano silver film: quartz plate is immersed in the mixing solutions that the vitriol oil and hydrogen peroxide volume ratio are 7:3, after 3 hours, take out and use deionized water rinsing; Immersed again afterwards the middle gelatin/nano silver colloidal sol of 65 DEG C of preparing of step (2) 3 hours, taken out and blot the unnecessary gelatin/nano silver colloidal sol in surface, at room temperature cooling standing 20 minutes.
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film: it is in 3% chitosan derivative solution 10 minutes that gelatin/nano silver film is dipped in to mass concentration, take out and use deionized water rinsing, be placed on the warm table of 45 DEG C and heat 60 minutes, make gelatin/nanometer silver/chitosan derivative antibacterial laminated film.
Alternatively, in above-described embodiment as the film substrate of gelatin/nano silver film---quartz plate also can utilize sheet glass, titanium dioxide silicon chip, fibrous substrate gauze or bandage etc. any replace, and it is similar to adopt above-mentioned film substrate to carry out the preparation method of gelatin/nano silver film while preparing and preparation condition and embodiment 1-4, is not repeated at this.
In addition; the chitosan derivatives adopting in above-described embodiment can be any in chitosan itself, cm-chitosan, CMC, chitosan hydrochloride, chitosan quaternary ammonium salt, hydroxypropyl chitosan, N-trimethyl chitin, N-Nmaleoyl chitosan, beta-cyclodextrin grafted chitosan, Allan sodium phosphate chitosan.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is by claims and be equal to and limit.
Claims (10)
1. a preparation method for gelatin/nanometer silver/chitosan derivative antibacterial laminated film, is characterized in that described preparation method comprises the steps:
(1) preparation of aqueous gelatin solution:
Gelatin is joined to deionized water, stir and be warming up to 60 ° of C-80 ° of C insulation reaction 1-3 hour, prepare aqueous gelatin solution;
(2) preparation of gelatin/nano silver colloidal sol:
In the prepared aqueous gelatin solution of step (1), add Silver Nitrate, be warming up to preset 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 the mixing solutions that the vitriol oil and hydrogen peroxide volume ratio are 7:3, and 3-6 hour, takes out and uses deionized water rinsing; Immersed again the scheduled time in the prepared gelatin/nano silver colloidal sol of step (2), taken out and blot the unnecessary gelatin/nano silver colloidal sol in surface, at room temperature cooling standing 10 minutes-30 minutes, obtained gelatin/nano silver film;
(4) preparation of gelatin/nanometer silver/chitosan derivative antibacterial laminated film:
Gelatin/nano silver film that step (3) is obtained is dipped in 5-20 minute in the chitosan derivative solution of mass concentration 1-3%, take out and use deionized water rinsing, under predetermined Heating temperature, heat the scheduled time, make the antibacterial laminated film of gelatin/nanometer silver/chitosan.
2. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, is characterized in that: in step (1), the mass concentration scope of the described aqueous gelatin solution of preparation is 6.25%-20%.
3. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, is characterized in that: in the Silver Nitrate adding in step (2) and aqueous gelatin solution, the quality of gelatin is 1:40-7:40 than scope.
4. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, it is characterized in that: described in step (2), be warming up to preset temperature insulated and stirred and react in the scheduled time, described predetermined temperature range is 90 ° of C-95 ° of C, and the described scheduled time is 1-2 hour.
5. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, is characterized in that: film substrate described in step (3) is any in quartz plate, sheet glass, titanium dioxide silicon chip, the gauze of fibrous substrate or the bandage of fibrous substrate.
6. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, is characterized in that: the described scheduled time scope that in step (3), film substrate immerses in gelatin/nano silver colloidal sol is 1-3 hour.
7. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, it is characterized in that: when in step (3), film substrate immerses in gelatin/nano silver colloidal sol, described gelatin/nano silver colloidal sol temperature remains on 60 ° of C-65 ° of C.
8. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, it is characterized in that: predetermined Heating temperature scope described in step (4) is 40 ° of C-45 ° of C, described scheduled time scope is 40 minutes-60 minutes.
9. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film, is characterized in that: described laminated film is mainly used in the fields such as artificial skin, medical antibacterial dressing and hemostatic material.
10. the preparation method of gelatin/nanometer silver according to claim 1/chitosan derivative antibacterial laminated film; it is characterized in that: described chitosan derivatives is any in chitosan, cm-chitosan, CMC, chitosan hydrochloride, chitosan quaternary ammonium salt, hydroxypropyl chitosan, N-trimethyl chitin, N-Nmaleoyl chitosan, beta-cyclodextrin grafted chitosan, Allan sodium phosphate chitosan.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104233436A (en) * | 2014-09-15 | 2014-12-24 | 武汉理工大学 | Chitosan/gelatin/nano-silver conductive antibacterial material and preparation method thereof |
| CN106751920A (en) * | 2016-12-01 | 2017-05-31 | 西南大学 | Preparation method of the enhanced laminated film anti-biotic material of polyvinyl alcohol silk gum Nano Silver and products thereof and application |
| CN106727923A (en) * | 2017-01-17 | 2017-05-31 | 普宁康特生物科技有限公司 | A kind of anti-bacteriostatic solution of Quaternary Ammonium Salt of Chitosan silver particles and preparation method thereof |
| 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 |
| CN107137766A (en) * | 2017-05-03 | 2017-09-08 | 中国矿业大学 | The preparation method at antimicrobial artificial arthrodesis interface |
| CN107955198A (en) * | 2016-10-14 | 2018-04-24 | 中国科学院大连化学物理研究所 | A kind of preparation method of nano-silver thread-chitosan self assembly conductive film coating |
| CN110089794A (en) * | 2019-05-07 | 2019-08-06 | 王玉萍 | A kind of wig service life of extending washes maintaining method |
| CN110450487A (en) * | 2019-08-12 | 2019-11-15 | 广东美士达药包材料股份有限公司 | A kind of degradable drug packing material and preparation method thereof |
| CN110522945A (en) * | 2019-10-11 | 2019-12-03 | 杨鑫 | A kind of medical bio gel bleeding-stopping dressing and preparation method thereof |
| CN110755678A (en) * | 2019-11-13 | 2020-02-07 | 中国矿业大学 | 3D printing antibacterial hydrogel wound dressing based on green in-situ reduction |
| CN112717194A (en) * | 2020-12-30 | 2021-04-30 | 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 |
| CN115636885A (en) * | 2022-10-26 | 2023-01-24 | 湖北中医药大学 | Quaternary ammonium cyclodextrin, preparation method and application thereof, silver nanoparticle cyclodextrin compound, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104233436A (en) * | 2014-09-15 | 2014-12-24 | 武汉理工大学 | Chitosan/gelatin/nano-silver conductive antibacterial material and preparation method thereof |
| CN107955198A (en) * | 2016-10-14 | 2018-04-24 | 中国科学院大连化学物理研究所 | A kind of preparation method of nano-silver thread-chitosan self assembly conductive film coating |
| CN106751920A (en) * | 2016-12-01 | 2017-05-31 | 西南大学 | Preparation method of the enhanced laminated film anti-biotic material of polyvinyl alcohol silk gum Nano Silver and products thereof and application |
| CN106751920B (en) * | 2016-12-01 | 2019-07-09 | 西南大学 | Preparation method of the enhanced laminated film anti-biotic material of polyvinyl alcohol-silk gum-nano silver and products thereof and application |
| CN106727923A (en) * | 2017-01-17 | 2017-05-31 | 普宁康特生物科技有限公司 | A kind of anti-bacteriostatic solution of Quaternary Ammonium Salt of Chitosan silver particles and preparation method thereof |
| 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 |
| CN107137766A (en) * | 2017-05-03 | 2017-09-08 | 中国矿业大学 | The preparation method at antimicrobial artificial arthrodesis interface |
| CN110089794A (en) * | 2019-05-07 | 2019-08-06 | 王玉萍 | A kind of wig service life of extending washes maintaining method |
| CN110450487A (en) * | 2019-08-12 | 2019-11-15 | 广东美士达药包材料股份有限公司 | A kind of degradable drug packing material and preparation method thereof |
| CN110522945A (en) * | 2019-10-11 | 2019-12-03 | 杨鑫 | A kind of medical bio gel bleeding-stopping dressing and preparation method thereof |
| CN111790002A (en) * | 2019-10-11 | 2020-10-20 | 杨鑫 | Preparation method of medical biogel hemostatic dressing |
| CN110755678A (en) * | 2019-11-13 | 2020-02-07 | 中国矿业大学 | 3D printing antibacterial hydrogel wound dressing based on green in-situ reduction |
| CN112717194A (en) * | 2020-12-30 | 2021-04-30 | 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 |
| CN115636885A (en) * | 2022-10-26 | 2023-01-24 | 湖北中医药大学 | Quaternary ammonium cyclodextrin, preparation method and application thereof, silver nanoparticle cyclodextrin compound, and preparation method and application 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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