CN103757917B - The preparation method of the electroactive chitosan-based composite of a kind of tool - Google Patents
The preparation method of the electroactive chitosan-based composite of a kind of tool Download PDFInfo
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- CN103757917B CN103757917B CN201410037627.4A CN201410037627A CN103757917B CN 103757917 B CN103757917 B CN 103757917B CN 201410037627 A CN201410037627 A CN 201410037627A CN 103757917 B CN103757917 B CN 103757917B
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 76
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 42
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000835 fiber Substances 0.000 claims abstract description 32
- 229920000128 polypyrrole Polymers 0.000 claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 25
- 229920002101 Chitin Polymers 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 14
- 229920000767 polyaniline Polymers 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000007711 solidification Methods 0.000 claims abstract description 11
- 230000008023 solidification Effects 0.000 claims abstract description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 239000011324 bead Substances 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- 239000008188 pellet Substances 0.000 claims description 10
- 239000012528 membrane Substances 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000002166 wet spinning Methods 0.000 claims description 3
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 229920001940 conductive polymer Polymers 0.000 abstract description 7
- 239000002322 conducting polymer Substances 0.000 abstract description 6
- 239000012620 biological material Substances 0.000 abstract description 2
- 150000003233 pyrroles Chemical class 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- CYGKLLHTPPFPHH-UHFFFAOYSA-N aniline;hydrate Chemical compound O.NC1=CC=CC=C1 CYGKLLHTPPFPHH-UHFFFAOYSA-N 0.000 description 2
- 230000023402 cell communication Effects 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 238000007766 curtain coating Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011263 electroactive material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004643 material aging Methods 0.000 description 1
- 230000014511 neuron projection development Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses the preparation method of the electroactive chitosan-based composite of a kind of tool, belong to conducting polymer and technical field of biological material.This comprises the following steps: dissolve shitosan with the aqueous acetic acid that mass percent is 1 ~ 10%, obtain the chitosan solution that mass percent is 0.1 ~ 7%; Chitosan solution is entered into the solidification liquid that mass percent is 3 ~ 20%, after washing, drying, obtain chitosan material; Chitin fiber is immersed in concentration be 0.1 ~ 20% pyrrole monomer or the aniline monomer aqueous solution in obtain shitosan pyrrole monomer or aniline monomer composite; It is in the oxidant of 0.1 ~ 20% that shitosan pyrrole monomer or aniline monomer composite are immersed in concentration, and after taking out, washing, drying obtain the electroactive shitosan polypyrrole of tool or polyaniline composite material.The chitosan-based composite utilizing the method to prepare has electroactive and biocompatibility.
Description
Technical field
The invention belongs to conducting polymer and technical field of biological material, particularly the preparation method of the electroactive chitosan-based composite of a kind of tool.
Background technology
Shitosan is the alkaline polysaccharide of nature rich content, has good adsorptivity, antibacterial activity, and medical accessory, anti-biotic material and packaging material for food are used widely.Chitosan material has the feature of fully biodegradable and good biocompatibility.Prepare chitin fiber by wet spinning, prepare chitosan-based bead by methods such as orifice balling-up, spraying dry, by casting film-forming, the methods such as rotary spraying prepare chitosan film material.
The electrical conductive activities such as polypyrrole and polyaniline polymer has characteristic of semiconductor, has good antistatic behaviour, lower electrical conductivity, has broad application prospects in the field of electromagnetic shielding.The electroactive materials such as the polypyrrole of difference in functionality and polyaniline can be prepared by controlling polymerization process, as utilized oxidation and the reduction reaction of polypyrrole, polypyrrole being combined with lithium ion, the ultracapacitor of unique properties can be designed.In addition, polypyrrole has good biocompatibility, can obtain a series of there is biologically active by control design case, can with the new material of protein bound, for growth and the control of cell, as containing the PC12 cells cultivated in polypyrrole culture medium, neurite outgrowth and the propagation of cell significantly can be strengthened under the induction of electro photoluminescence.
Shitosan-the conductive polymer composite of current bibliographical information often using shitosan as dispersant, for stable dispersed electro-conductive macromolecule, if shitosan is as the dispersant of polypyrrole-Yin microballoon.Shitosan-polypyrrole plural gel is directly added in the acetum of shitosan by pyrrole monomer, then by potassium persulfate oxidation agent, oxidizable pyrrole is become polypyrrole, is put in deionized water solution by above-mentioned composite solution and is frozen into gel.There is oxidant and formed crosslinked with shitosan while oxidation pyrrole monomer in the method, affects the degree of polymerization and the electric conductivity thereof of polypyrrole.
Summary of the invention
The object of the invention is for solving the problem and provide a kind of preparation method with the chitosan-based composite of electroactive and biocompatibility.
The technical solution adopted in the present invention is:
A preparation method for the electroactive chitosan-based composite of tool, comprises the following steps:
(1) dissolve shitosan with the aqueous acetic acid that mass percent is 1 ~ 10%, obtain the chitosan solution that mass percent is 0.1 ~ 7%;
(2) chitosan solution that above-mentioned steps obtains is entered into the solidification liquid that mass percent is 3 ~ 20%, after washing, drying, obtain chitosan material;
(3) chitosan material that above-mentioned steps obtains is immersed in concentration be 0.1 ~ 20% pyrrole monomer or the aniline monomer aqueous solution in obtain shitosan pyrrole monomer or aniline monomer composite;
(4) it is in the oxidant of 0.1 ~ 20% that shitosan pyrrole monomer above-mentioned steps obtained or aniline monomer composite are immersed in concentration, and after taking out, washing, drying obtain the electroactive shitosan polypyrrole of tool or polyaniline composite material.
Preferably, the solidification liquid in described step (2) is sodium hydrate aqueous solution.
Preferably, the oxidant in described step (4) is ferric trichloride, potassium peroxydisulfate and ammonium persulfate.
Further, the chitosan material that described step (2) obtains can be chitin fiber, Chitosan Beads and chitosan film.
Preferably, described chitin fiber adopts wet spinning to prepare, and the diameter of chitin fiber is 0.06 ~ 0.5mm.
Preferably, the method that described Chitosan Beads drips balling-up by spraying, orifice balling-up or syringe prepares, and the diameter of Chitosan Beads is 0.5 ~ 3.0mm.
Preferably, described chitosan film adopts casting film-forming, spin coating process prepares, and the thickness of chitosan film is 0.1 ~ 3mm.
Further, when the chitosan material that described step (2) obtains is chitin fiber, what described step (3) obtained is shitosan pyrrole monomer or aniline monomer composite fibre, and what described step (4) obtained is the electroactive shitosan polypyrrole of tool or polyaniline composite fibre.
Further, when the chitosan material that described step (2) obtains is Chitosan Beads, what described step (3) obtained is shitosan pyrrole monomer or aniline monomer composite pellets, and what described step (4) obtained is the electroactive shitosan polypyrrole of tool or polyaniline composite pellets.
Further, when the chitosan material that described step (2) obtains is chitosan film, what described step (3) obtained is shitosan pyrrole monomer or aniline monomer composite membrane, and what described step (4) obtained is the electroactive shitosan polypyrrole of tool or polyaniline composite film.
The present invention has the following advantages:
The present invention is by chitin fiber, bead or membrane material absorption pyrroles or aniline monomer, pyrroles or aniline monomer are uniformly distributed in chitosan material, and oxidized dose is oxidized to the conducting polymers such as polypyrrole, the reunion of polypyrrole and the affected problem of the degree of polymerization thereof can be avoided, conducting polymer is made to can be uniformly dispersed in chitosan-based material, and forming strong bonded with shitosan, the degree of polymerization of the polypyrrole of composite is high.Preparation method of the present invention is simple, and be easy to operation, production cost is low, and material has electroactive and feature that is biocompatibility, will at radiation-proof fabric, and the fields such as cell communications, Co ntrolled release device and chemical sensor are applied.
Detailed description of the invention
Embodiment 1
Dissolve shitosan with the acetum that mass percent is 1% and obtain the chitosan solution that mass percent is 1%, chitosan solution is expressed in solidification liquid and prepares chitin fiber, solidification liquid to be mass percent be 3% sodium hydrate aqueous solution, chitin fiber is washed, drying obtains the chitin fiber that diameter is 0.06mm.Chitin fiber being immersed in percentage is obtain shitosan pyrrole monomer composite fibre in pyrroles's aqueous solution of 1%, composite fibre being immersed in mass percent is in the potassium persulfate solution of 1% again, and after fiber takes out, washing drying obtains tool electroactive shitosan-polypyrrole composite fibre.
Embodiment 2
Preparing mass percent with the acetum that mass percent is 10% is the chitosan solution of 7%, chitosan solution is prepared chitin fiber by injector to inject to the method for solidification liquid, solidification liquid to be mass percent be 20% sodium hydrate aqueous solution, chitin fiber is washed, drying obtains the chitin fiber that diameter is 0.5mm.Chitin fiber being immersed in mass percent is obtain shitosan-pyrrole monomer composite fibre in pyrroles's aqueous solution of 10%, composite fibre being immersed in mass percent is in the liquor ferri trichloridi of 10%, and after fiber takes out, washing drying obtains tool electroactive shitosan-polypyrrole composite fibre.
Embodiment 3
Preparing mass percent with the acetum that mass percent is 1% is the chitosan solution of 0.1%, and mass fraction is that the sodium hydrate aqueous solution of 3% is as coagulating bath.Chitosan solution is added drop-wise in solidification liquid by syringe and obtains bead, obtain dry for bead washing the Chitosan Beads that diameter is 0.5mm.Bead being immersed in mass fraction is obtain shitosan-aniline monomer composite pellets in the aniline-water solution of 0.1%, then composite pellets being immersed in mass percent is in the potassium persulfate solution of 0.1%, and after being taken out by bead, washing drying obtains tool electroactive shitosan polyaniline composite pellets.
Embodiment 4
Preparing mass fraction with the acetum that volume fraction is 10% is the chitosan solution of 7%, and mass fraction is that the sodium hydrate aqueous solution of 20% is as coagulating bath.Chitosan solution is added drop-wise in solidification liquid by syringe and obtains bead, obtain dry for bead washing the Chitosan Beads that diameter is 3mm.Chitosan Beads being immersed in mass fraction is obtain shitosan-pyrrole monomer composite pellets in pyrroles's aqueous solution of 20%, then composite pellets being immersed in mass percent is in the ammonium persulfate solution of 20%, and after being taken out by bead, washing drying obtains tool electroactive shitosan polypyrrole composite pellets.
Embodiment 5
Preparing mass percent with the acetum that mass percent is 1% is the chitosan solution of 5%, by chitosan solution curtain coating on glass plate, glass plate being dipped into mass fraction is obtain chitosan film in the sodium hydrate aqueous solution of 10%, obtains the chitosan film that thickness is 3mm after film being washed drying.Chitosan film being immersed in mass fraction is obtain shitosan-aniline monomer composite membrane in the aniline-water solution of 10%, composite membrane being immersed in mass percent is in the ferric chloride aqueous solutions of 10%, and after being taken out by film, washing drying obtains the electroactive shitosan composite polypyrrole film of tool.
Embodiment 6
Preparing mass percent with the acetum that mass percent is 10% is the chitosan solution of 1%, by chitosan solution curtain coating on glass plate, glass plate being dipped into mass fraction is obtain chitosan film in the sodium hydrate aqueous solution of 3%, obtains the chitosan film that thickness is 0.1mm after film being washed drying.Chitosan film being immersed in mass fraction is obtain shitosan-pyrrole monomer composite membrane in pyrroles's aqueous solution of 10%, composite membrane being immersed in mass percent is in the ferric chloride aqueous solutions of 0.1%, and after being taken out by film ball, washing drying obtains the electroactive shitosan composite polypyrrole film of tool.
The chitosan-based composite that above embodiment prepares is by chitin fiber, bead or membrane material absorption pyrroles or aniline monomer, pyrroles or aniline monomer are uniformly distributed in chitosan material, and oxidized dose is oxidized to the conducting polymers such as polypyrrole, the reunion of polypyrrole and the affected problem of the degree of polymerization thereof can be avoided, conducting polymer is made to can be uniformly dispersed in chitosan-based material, and forming strong bonded with shitosan, the degree of polymerization of the polypyrrole of composite is high.Preparation method of the present invention is simple, and be easy to operation, production cost is low, and material has electroactive and feature that is biocompatibility, will at radiation-proof fabric, and the fields such as cell communications, Co ntrolled release device and chemical sensor are applied.
It should be noted last that, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (5)
1. a preparation method for the electroactive chitosan-based composite of tool, is characterized in that, comprise the following steps:
(1) dissolve shitosan with the aqueous acetic acid that mass percent is 1 ~ 10%, obtain the chitosan solution that mass percent is 0.1 ~ 7%;
(2) chitosan solution that above-mentioned steps obtains is entered into the solidification liquid that mass percent is 3 ~ 20%, after washing, drying, obtain chitosan material;
(3) chitosan material that above-mentioned steps obtains is immersed in mass percent be 0.1 ~ 20% pyrrole monomer or the aniline monomer aqueous solution in obtain shitosan pyrrole monomer or aniline monomer composite;
(4) it is in the oxidant of 0.1 ~ 20% that shitosan pyrrole monomer above-mentioned steps obtained or aniline monomer composite are immersed in mass percent, and after taking out, washing, drying obtain the electroactive shitosan polypyrrole of tool or polyaniline composite material;
The chitosan material that described step (2) obtains is chitin fiber, Chitosan Beads or chitosan film;
Described chitin fiber adopts wet spinning to prepare, and the diameter of chitin fiber is 0.06 ~ 0.5mm;
When the chitosan material that described step (2) obtains is chitin fiber, what described step (3) obtained is shitosan pyrrole monomer or aniline monomer composite fibre, and what described step (4) obtained is the electroactive shitosan polypyrrole of tool or polyaniline composite fibre;
When the chitosan material that described step (2) obtains is Chitosan Beads, what described step (3) obtained is shitosan pyrrole monomer or aniline monomer composite pellets, and what described step (4) obtained is the electroactive shitosan polypyrrole of tool or polyaniline composite pellets;
When the chitosan material that described step (2) obtains is chitosan film, what described step (3) obtained is shitosan pyrrole monomer or aniline monomer composite membrane, and what described step (4) obtained is the electroactive shitosan polypyrrole of tool or polyaniline composite film.
2. the preparation method of the electroactive chitosan-based composite of tool according to claim 1, is characterized in that, the solidification liquid in described step (2) is sodium hydrate aqueous solution.
3. the preparation method of the electroactive chitosan-based composite of tool according to claim 1, is characterized in that, the oxidant in described step (4) is ferric trichloride, potassium peroxydisulfate or ammonium persulfate.
4. the preparation method of the electroactive chitosan-based composite of tool according to claim 1, it is characterized in that, the method that described Chitosan Beads drips balling-up by spraying, orifice balling-up or syringe prepares, and the diameter of Chitosan Beads is 0.5 ~ 3.0mm.
5. the preparation method of the electroactive chitosan-based composite of tool according to claim 1, is characterized in that, described chitosan film adopts casting film-forming, spin coating process prepares, and the thickness of chitosan film is 0.1 ~ 3mm.
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| CN104151630A (en) * | 2014-08-08 | 2014-11-19 | 江汉大学 | Preparation method of chitosan-based composite material having electroactivity |
| WO2017214741A1 (en) * | 2016-06-14 | 2017-12-21 | 杨磊 | Process for preparing chitosan/polyvinyl alcohol composite electrically-conductive nanofibre |
| CN107083057A (en) * | 2017-04-29 | 2017-08-22 | 成都博美实润科技有限公司 | A kind of preparation method for having electroactive carboxyl chitosan based composites |
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| CN112190549B (en) * | 2020-10-13 | 2022-10-14 | 上海交通大学医学院附属新华医院 | Ultrafast charge reversible chitosan-based nanogel and preparation method and application thereof |
| CN112779784B (en) * | 2021-01-27 | 2023-01-03 | 南京信息工程大学 | Chitosan-polypyrrole conductive fiber with core-shell structure and preparation method thereof |
| CN113930245B (en) * | 2021-11-16 | 2023-03-31 | 天津科技大学 | Environment-friendly Cr (VI) polluted soil remediation agent and preparation method thereof |
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