CN102108127A - Method for preparing chitosan nano composite material membrane - Google Patents
Method for preparing chitosan nano composite material membrane Download PDFInfo
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- CN102108127A CN102108127A CN2009102006548A CN200910200654A CN102108127A CN 102108127 A CN102108127 A CN 102108127A CN 2009102006548 A CN2009102006548 A CN 2009102006548A CN 200910200654 A CN200910200654 A CN 200910200654A CN 102108127 A CN102108127 A CN 102108127A
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Abstract
The invention relates to a method for preparing a chitosan nano composite material membrane, which is to prepare the nano composite material membrane by blending and casting chitosan and graphite oxide by a solution intercalation blending process. Compared with the prior art, the chitosan nano composite material membrane is formed conveniently and controllable in thickness and has biodegradability, bacterial resistance, conductivity, environmental friendliness, high mechanical performance and high thermal resistance and can be widely used in biosensor, food preservation and packaging material industries and other industries.
Description
Technical field
The present invention relates to a kind of preparation method of chitosan nano composite material film, relate in particular to a kind of nano-composite material membrane of antibacterial, biodegradable, the conduction that is applicable to that bio-sensing, food fresh keeping, wrapping material use.
Background technology
Chitosan film has good adsorption, germ resistance, biocompatibility and biological degradability, therefore uses very extensive.Though chitosan film has above-mentioned plurality of advantages because its use temperature is low, the undesirable and mechanical property of thermotolerance not high drawbacks limit its range of application.Therefore, chitosan film is carried out modification, improving its thermotolerance, mechanical property and making it have functional conductive is very significant work.
Graphite is the natural inorganic material, and sheet interlayer spacing increases after oxidation, adsorbs polar polymer easily and forms intercal type and exfoliated nano-composite.Oxidized graphite flake layer has iris action, can significantly reduce the rate of heat release of polymkeric substance, promote the formation of carbon-coating, thereby prepared bill of material reveals good thermal stability.Simultaneously, the dispersive oxidized graphite flake layer has huge radius-thickness ratio in matrix material, easily forms conductive network, so this matrix material has low percolation threshold and high conductivity.And graphite oxide is as nanometer lamella filler, and energy is the mechanical property of strongthener significantly.
Summary of the invention
Purpose of the present invention is exactly for a kind of preparation method with chitosan nano composite material film of biocidal property, electroconductibility, biodegradable, environmentally safe is provided.
Purpose of the present invention can be achieved through the following technical solutions: a kind of preparation method of chitosan nano composite material film is characterized in that this composite material film is to be made by curtain coating after chitosan and the blend of graphite oxide intercalation, specifically may further comprise the steps:
(1) 0.1～10 weight part graphite oxide is dispersed in the solvent of 10～100 times of weight, ultrasonic dispersing is 3～10 hours under stirring, and obtains graphite oxide colloid suspension liquid;
(2) 100 weight part chitosans are dissolved in the solvent, the graphite oxide suspension liquid that adds step (1) gained, ultra-sonic dispersion, stirring 0.5～2 hour, mixing, is 6.0～7.0 with sodium hydroxide or the potassium hydroxide solution adjust pH of 0.1M, and curtain coating is filmed, be lower than 100 ℃ of following solvent flashing film forming at vacuum drying oven, soaked 5～10 hours with sodium hydroxide or potassium hydroxide solution with 0.1M then, distilled water is washed till neutrality, obtains the chitosan nano composite material film.
Described graphite oxide is that the Hummers method is prepared.
Described chitosan is the technical grade chitosan.
The described solvent of step (1) is N,N-dimethylacetamide or N, dinethylformamide.
The described solvent of step (2) is acetic acid solution or the 1v/v% sulphuric acid soln of 1v/v%.
The content of described graphite oxide is 0.1～10% of chitosan mass
Compared with prior art, the present invention combines the electroconductibility of graphite itself, good filming, biocidal property and the biological degradability of chitosan, utilizes the solution intercalation blending method that chitosan and graphite oxide blend curtain coating have been prepared the chitosan nano composite material film.Preparation method of the present invention is simple to operate, and chitosan and graphite are natural matter and effective, aboundresources, and environmentally safe, this film forming is convenient, controllable thickness.Nano-composite material membrane has biological degradability, biocidal property, electroconductibility, environmentally safe, and mechanical property and good heat resistance can be widely used in industries such as bio-sensing, food fresh keeping, wrapping material, have enlarged the Application Areas of chitosan greatly.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
The mechanical property of above-mentioned chitosan nano composite material film and the testing standard of conductivity see Table 1.
Table 1
| Performance index | Testing standard |
| Tensile strength (MPa) | GB1040-92 |
| Elongation at break (%) | GB1040-92 |
| Volume conductance (S/cm) (r.t.) | Standard four electrode method (sample 7 * 3 * 0.5mm 3) |
Embodiment 1
Graphite oxide is dispersed in the N,N-dimethylacetamide solvent of 50 times of weight, ultra-sonic dispersion 10 hours is uniformly dispersed.Chitosan is dissolved in the 1v/v% acetic acid solution.Above-mentioned chitosan solution and graphite oxide solution are mixed, stirred 2 hours, transferring pH value with the sodium hydroxide solution of 0.1M is 6.0～7.0, pour in the ready-formed mould, in 80 ℃ of following solvent flashing film forming of vacuum drying oven, the sodium hydroxide solution with 0.1M soaked 10 hours then, and distilled water is washed till neutrality.The content of graphite oxide is respectively the 2wt% of chitosan mass, 5wt%, 8wt%, 10wt%.The performance of made chitosan nano composite material film sees attached list 2.
Embodiment 2
With embodiment 1, the solvent that only changes graphite oxide is N, dinethylformamide.The performance of made chitosan nano composite material film sees attached list 2.
Embodiment 3
With embodiment 1, the solvent that only changes chitosan is a sulfuric acid.The performance of made chitosan nano composite material film sees attached list 2.
Embodiment 4
With embodiment 2, the solvent that only changes chitosan is a sulfuric acid.The performance of made chitosan nano composite material film sees attached list 2.
For the mechanical property of the chitosan nano composite material film of investigating the present invention preparation and the effect of conductivity, the prepared matrix material of the foregoing description is carried out mechanical property and conducting performance test.For details see attached table 2.
Subordinate list 2
Embodiment 5
A kind of preparation method with chitosan nano composite material film of biocidal property, electroconductibility, biodegradable, environmentally safe, this matrix material is prepared by chitosan and the blend of graphite oxide intercalation and gets, its mechanical property and thermotolerance significantly improve than chitosan film, had the unexistent electroconductibility of chitosan film itself, concrete preparation method carries out by the following step:
(1) the prepared graphite oxide of 0.1 weight part Hummers method is dispersed in the solvent N,N-dimethylacetamide of 10 times of weight, ultrasonic dispersing is 3 hours under stirring, and obtains graphite oxide colloid suspension liquid;
(2) 100 weight part chitosans are dissolved in the 1v/v% sulphuric acid soln, the graphite oxide suspension liquid that adds step (1) gained, ultra-sonic dispersion, stirring 0.5 hour, mixing, is 6.0 with the potassium hydroxide solution adjust pH of 0.1M, and curtain coating is filmed, in 80 ℃ of following solvent flashing film forming of vacuum drying oven, potassium hydroxide solution with 0.1M soaked 5 hours then, and distilled water is washed till neutrality, obtains the chitosan nano composite material film.
Embodiment 6
A kind of preparation method with chitosan nano composite material film of biocidal property, electroconductibility, biodegradable, environmentally safe, this matrix material is prepared by chitosan and the blend of graphite oxide intercalation and gets, its mechanical property and thermotolerance significantly improve than chitosan film, had the unexistent electroconductibility of chitosan film itself, concrete preparation method carries out by the following step:
(1) the prepared graphite oxide of 10 weight part Hummers methods is dispersed in the solvent N of 100 times of weight, in the dinethylformamide, stirred down ultrasonic dispersing 10 hours, obtain graphite oxide colloid suspension liquid;
(2) 100 weight part technical grade chitosans are dissolved in the acetic acid solution of 1v/v%, the graphite oxide suspension liquid that adds step (1) gained, ultra-sonic dispersion, stirring 2 hours, mixing, is 7.0 with the sodium hydroxide solution adjust pH of 0.1M, and curtain coating is filmed, be lower than 100 ℃ of following solvent flashing film forming at vacuum drying oven, potassium hydroxide solution with 0.1M soaked 10 hours then, and distilled water is washed till neutrality, obtains the chitosan nano composite material film.
Claims (6)
1. the preparation method of a chitosan nano composite material film is characterized in that, this composite material film is to be made by curtain coating after chitosan and the blend of graphite oxide intercalation, specifically may further comprise the steps:
(1) 0.1～10 weight part graphite oxide is dispersed in the solvent of 10～100 times of weight, ultrasonic dispersing is 3～10 hours under stirring, and obtains graphite oxide colloid suspension liquid;
(2) 100 weight part chitosans are dissolved in the solvent, the graphite oxide suspension liquid that adds step (1) gained, ultra-sonic dispersion, stirring 0.5～2 hour, mixing, is 6.0～7.0 with sodium hydroxide or the potassium hydroxide solution adjust pH of 0.1M, and curtain coating is filmed, be lower than 100 ℃ of following solvent flashing film forming at vacuum drying oven, soaked 5～10 hours with sodium hydroxide or potassium hydroxide solution with 0.1M then, distilled water is washed till neutrality, obtains the chitosan nano composite material film.
2. the preparation method of a kind of chitosan nano composite material film according to claim 1 is characterized in that, described graphite oxide is that the Hummers method is prepared.
3. the preparation method of a kind of chitosan nano composite material film according to claim 1 is characterized in that, described chitosan is the technical grade chitosan.
4. the preparation method of a kind of chitosan nano composite material film according to claim 1 is characterized in that, the described solvent of step (1) is N,N-dimethylacetamide or N, dinethylformamide.
5. the preparation method of a kind of chitosan nano composite material film according to claim 1 is characterized in that, the described solvent of step (2) is acetic acid solution or the 1v/v% sulphuric acid soln of 1v/v%.
6. the preparation method of a kind of chitosan nano composite material film according to claim 1 is characterized in that, the content of described graphite oxide is 0.1～10% of chitosan mass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200910200654 CN102108127B (en) | 2009-12-24 | 2009-12-24 | Method for preparing chitosan nano composite material membrane |
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| CN 200910200654 CN102108127B (en) | 2009-12-24 | 2009-12-24 | Method for preparing chitosan nano composite material membrane |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380349A (en) * | 2011-10-24 | 2012-03-21 | 武汉大学 | Graphite oxide/magnetic chitosan composite adsorbent and preparation method thereof |
| CN103757917A (en) * | 2014-01-26 | 2014-04-30 | 江汉大学 | Method for preparing chitosan-based composite material with electroactivity |
| CN104629097A (en) * | 2013-11-13 | 2015-05-20 | 中国科学院海洋研究所 | Carboxymethyl chitosan-hydrotalcite nanocomposite hydrogel film and preparation method thereof |
| CN104642534A (en) * | 2015-02-06 | 2015-05-27 | 玉林师范学院 | Graphene oxide-chitosan composite nano preservative and preparation method thereof |
| CN106543471A (en) * | 2016-10-21 | 2017-03-29 | 华东理工大学 | The preparation method of graphene nanometer sheet and Chitosan Composites |
| CN106892401A (en) * | 2017-01-17 | 2017-06-27 | 天津理工大学 | A kind of sandwich construction nano generator and preparation method thereof |
| CN107402247A (en) * | 2017-07-21 | 2017-11-28 | 张娟 | A kind of preparation method of electrochemical sensor nano-graphene/chitosan complex film modified electrode |
| CN107522996A (en) * | 2017-10-09 | 2017-12-29 | 浙江卫星新材料科技有限公司 | A kind of preparation method of Graphene antibiosis composition and antibacterial super absorbent resin |
| CN111705357A (en) * | 2020-06-18 | 2020-09-25 | 浙江正道环保科技有限公司 | ABS plastic surface coating deplating process |
-
2009
- 2009-12-24 CN CN 200910200654 patent/CN102108127B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 司有苗: ""壳聚糖/无机有序多孔材料的制备及对Cu2+、Pb2+的吸附性能研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑（月刊）》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380349A (en) * | 2011-10-24 | 2012-03-21 | 武汉大学 | Graphite oxide/magnetic chitosan composite adsorbent and preparation method thereof |
| CN104629097A (en) * | 2013-11-13 | 2015-05-20 | 中国科学院海洋研究所 | Carboxymethyl chitosan-hydrotalcite nanocomposite hydrogel film and preparation method thereof |
| CN104629097B (en) * | 2013-11-13 | 2017-02-08 | 中国科学院海洋研究所 | Carboxymethyl chitosan-hydrotalcite nanocomposite hydrogel film and preparation method thereof |
| CN103757917A (en) * | 2014-01-26 | 2014-04-30 | 江汉大学 | Method for preparing chitosan-based composite material with electroactivity |
| CN103757917B (en) * | 2014-01-26 | 2016-02-17 | 江汉大学 | The preparation method of the electroactive chitosan-based composite of a kind of tool |
| CN104642534A (en) * | 2015-02-06 | 2015-05-27 | 玉林师范学院 | Graphene oxide-chitosan composite nano preservative and preparation method thereof |
| CN106543471A (en) * | 2016-10-21 | 2017-03-29 | 华东理工大学 | The preparation method of graphene nanometer sheet and Chitosan Composites |
| CN106543471B (en) * | 2016-10-21 | 2018-08-07 | 华东理工大学 | The preparation method of graphene nanometer sheet and Chitosan Composites |
| CN106892401A (en) * | 2017-01-17 | 2017-06-27 | 天津理工大学 | A kind of sandwich construction nano generator and preparation method thereof |
| CN107402247A (en) * | 2017-07-21 | 2017-11-28 | 张娟 | A kind of preparation method of electrochemical sensor nano-graphene/chitosan complex film modified electrode |
| CN107522996A (en) * | 2017-10-09 | 2017-12-29 | 浙江卫星新材料科技有限公司 | A kind of preparation method of Graphene antibiosis composition and antibacterial super absorbent resin |
| CN107522996B (en) * | 2017-10-09 | 2019-12-20 | 浙江卫星新材料科技有限公司 | Preparation method of graphene composition for enhancing absorption performance of super absorbent resin |
| CN111705357A (en) * | 2020-06-18 | 2020-09-25 | 浙江正道环保科技有限公司 | ABS plastic surface coating deplating process |
| CN111705357B (en) * | 2020-06-18 | 2021-11-16 | 浙江元力再生资源有限公司 | ABS plastic surface coating deplating process |
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| CN102108127B (en) | 2013-06-12 |
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Denomination of invention: Method for preparing chitosan nano composite material membrane Effective date of registration: 20191202 Granted publication date: 20130612 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |