CN104289727B - A kind of method preparing Nano Silver for reducing agent with modification of chitosan - Google Patents
A kind of method preparing Nano Silver for reducing agent with modification of chitosan Download PDFInfo
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- CN104289727B CN104289727B CN201410565387.5A CN201410565387A CN104289727B CN 104289727 B CN104289727 B CN 104289727B CN 201410565387 A CN201410565387 A CN 201410565387A CN 104289727 B CN104289727 B CN 104289727B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 23
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 17
- 230000004048 modification Effects 0.000 title claims abstract description 17
- 238000012986 modification Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 16
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims abstract description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 15
- 150000004676 glycans Chemical class 0.000 description 8
- 229920001282 polysaccharide Polymers 0.000 description 8
- 239000005017 polysaccharide Substances 0.000 description 8
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 108010054033 Chitin deacetylase Proteins 0.000 description 1
- 241000238424 Crustacea Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 108010022355 Fibroins Proteins 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-N hydroperoxyl Chemical compound O[O] OUUQCZGPVNCOIJ-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The present invention relates to a kind of method preparing Nano Silver for reducing agent with modification of chitosan, dissolving the chitosan in the acetic acid solution of 3%; bath raio 1:50; ultrasonic 1-12h; be subsequently added the sodium metaperiodate of 2-10g/L, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly by deionized water; centrifugal, dry for standby；Then according to the volume ratio of 10:1-1:1, chitosan solution modified for 0.01-100g/L sodium metaperiodate is mixed with the silver ammino solution of 0.01-100g/L, ultrasonic 1-10h under the temperature conditions of 20 DEG C-80 DEG C, obtain nano-class silver colloidal solution, repeatedly clean by ethanol and deionized water, centrifugal, it is dried after processing and obtains Nano Silver.The present invention uses the modified shitosan of sodium metaperiodate as reducing agent and stabilizer, possesses the advantages such as technique simple, reaction gentleness, environmental protection.
Description
Technical field
The invention belongs to field of nanometer material technology, particularly to a kind of method preparing Nano Silver for reducing agent with modification of chitosan.
Background technology
Nano Silver has excellent conductivity of heat, electric conductivity, surface-active and catalytic performance, has huge using value in optics, catalysis, microelectronics, bio-sensing, the field such as antibacterial.The preparation of traditional Nano Silver is divided into Physical and chemical method.Instrument and equipment is required higher by Physical, and producing cost is expensive.Chemical method many employings hydrazine hydrate, formaldehyde, polyalcohol, organic amine etc. make reducing agent, although these reducing agents have high activity, but to bad environmental, and easily there is agglomeration in the Nano Silver prepared.
In recent years, green, environmental protection, efficient and cheap method is used to prepare Nano Silver and be increasingly becoming the focus of research.The green reducing agent used at present specifically includes that vitamin, sodium citrate, pyro acid, hydroquinones, Tea Polyphenols, glucose, fructose, sucrose, plant and pericarp extract, microorganism etc..
Chitin is a kind of natural organic high-molecular polysaccharide, in the cell membrane of the crust, fungi and the plant that are distributed widely in nature Crustaceans (shrimp, crab, insect).Reserves natural organic high-molecular material on earth accounts for second, is only second to cellulose.Shitosan is the product after chitin deacetylase base, is a kind of linear macromolecule.Chinese invention patent CN201310555491.1 uses nano wire fibroin, chitosan in situ reduction silver nitrate to prepare Nano Silver.Chinese invention patent CN201310434034.7 uses shitosan (Mr=60000-120000) to make reducing agent, a small amount of sodium citrate used as stabilizers, prepares particle diameter at below 5nm, and monodispersity is good, and the nano silver colloidal sol of environmental protection.Chinese invention patent CN201410049491.9 provides a kind of method preparing stable Nano Silver, wherein uses the micella of amphipathic chitosan graft polycaprolactone or derivatives thereof copolymer as stabilizer.Above-mentioned document is used mostly shitosan and as stabilizer or uses modified shitosan as reducing agent.
Selective oxidation refers to suppress the oxidation of other position hydroxyl while certain ad-hoc location hydroxyl of oxidation of polysaccharides, and can effectively suppress the degraded of polysaccharide in oxidation reaction process.After sodium metaperiodate selective oxidation polysaccharide, can be by C2、C3Hydroxyl oxygen chemical conversion aldehyde radical on position, the functional modification for polysaccharide provides reactivity point, and available activity aldehyde radical carries out functional modification to polysaccharide, can generate numerous functional polysaccharide derivative, significantly expand the range of application of polysaccharide.Have no with sodium metaperiodate selective oxidation shitosan as reducing agent at present and the report of Nano Silver prepared by stabilizer.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, it is desirable to provide a kind of method preparing Nano Silver for reducing agent with modification of chitosan.
The technical scheme is that:
Dissolving the chitosan in the acetic acid solution of 3%, bath raio 1:50, ultrasonic 1-12h, be subsequently added the sodium metaperiodate of 2-10g/L, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly by deionized water, centrifugal, dry for standby；Then according to the volume ratio of 10:1-1:1, chitosan solution modified for 0.01-100g/L sodium metaperiodate is mixed with the silver ammino solution of 0.01-100g/L, ultrasonic 1-10h under the temperature conditions of 20 DEG C-80 DEG C, obtain nano-class silver colloidal solution, repeatedly clean by ethanol and deionized water, centrifugal, it is dried after processing and obtains Nano Silver.
Preferably, described silver ammino solution is the complex compound that nitrate or silver sulfate are formed with ammoniacal liquor.
Preferably, described centrifugal be to be centrifuged 5-20min with the rotating speed of 8000-12000r/min.
Preferably, described dry process refers to drying box temperature is set in 40 DEG C, is dried 1-24h in the environment of vacuum.
There is advantages that
Use sodium metaperiodate by the saccharide residue C of shitosan2And C3Position is oxidized to the aldehyde radical with reproducibility, can be Nano Silver by silver ion reduction, hydroxyl present in shitosan simultaneously, similar cancellated cage molecule can be formed by means of hydrogen bond or ionic bond, thus be coordinated with silver ion, prevent Nano Silver from reuniting, and then obtain stable Nano silver solution.The present invention uses the modified shitosan of sodium metaperiodate as reducing agent and stabilizer, possesses the advantages such as technique simple, reaction gentleness, environmental protection.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.
Embodiment 1:
2g shitosan being dissolved in 3% acetic acid solution of 100ml, ultrasonic 1h, is subsequently added the sodium metaperiodate of 2g/L, at 80 DEG C, lucifuge reaction 60min, cleans repeatedly by deionized water, centrifugal, dry for standby；
1g modification of chitosan is dissolved in 100ml deionized water, obtain the modification of chitosan aqueous solution of concentration 10g/L, mix with the silver ammino solution of 10ml concentration 10g/L, ultrasonic 1h under the temperature conditions of 80 DEG C, obtain nano-class silver colloidal solution, repeatedly cleaning by ethanol and deionized water, the rotating speed of 9000r/min is centrifuged 10min, is dried 20h and obtains Nano Silver under 40 DEG C of vacuum environments.
Embodiment 2:
2g shitosan being dissolved in 3% acetic acid solution of 100ml, ultrasonic 5h, is subsequently added the sodium metaperiodate of 5g/L, at 60 DEG C, lucifuge reaction 30min, cleans repeatedly by deionized water, centrifugal, dry for standby；
1g modification of chitosan is dissolved in 50ml deionized water, obtain the modification of chitosan aqueous solution of concentration 20g/L, mix with the silver ammino solution of 10ml concentration 5g/L, ultrasonic 10h under the temperature conditions of 20 DEG C, obtain nano-class silver colloidal solution, repeatedly cleaning by ethanol and deionized water, the rotating speed of 8000r/min is centrifuged 10min, is dried 24h and obtains Nano Silver under 40 DEG C of vacuum environments.
Embodiment 3:
2g shitosan being dissolved in 3% acetic acid solution of 100ml, ultrasonic 10h, is subsequently added the sodium metaperiodate of 10g/L, at 40 DEG C, lucifuge reaction 10min, cleans repeatedly by deionized water, centrifugal, dry for standby；
1g modification of chitosan is dissolved in 20ml deionized water, obtain the modification of chitosan aqueous solution of concentration 50g/L, mix with the silver ammino solution of 10ml concentration 50g/L, ultrasonic 4h under the temperature conditions of 40 DEG C, obtain nano-class silver colloidal solution, the rotating speed of 10000r/min is centrifuged 15min, is dried 4h and obtains Nano Silver under 40 DEG C of vacuum environments.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot all of embodiment be given exhaustive.Every belong to obvious change that technical scheme amplified out or the variation row still in protection scope of the present invention.
Claims (4)
1. the method preparing Nano Silver for reducing agent with modification of chitosan, it is characterised in that:
(1) dissolving the chitosan in the acetic acid solution of 3%, bath raio 1:50, ultrasonic 1-12h, be subsequently added the sodium metaperiodate of 2-10g/L, at 40-80 DEG C, lucifuge reaction 10-60min, cleans repeatedly by deionized water, centrifugal, dry for standby；
(2) according to the volume ratio of 10:1-1:1, by chitosan solution modified for the sodium metaperiodate of 0.01-100g/L, mix with the silver ammino solution of 0.01-100g/L, ultrasonic 1-10h under the temperature conditions of 20 DEG C-80 DEG C, obtain nano-class silver colloidal solution, repeatedly clean by ethanol and deionized water, centrifugal, it is dried after processing and obtains Nano Silver.
A kind of method preparing Nano Silver for reducing agent with modification of chitosan the most according to claim 1, it is characterised in that the silver ammino solution described in step 2 is the complex compound that silver nitrate or silver sulfate are formed with ammoniacal liquor.
A kind of method preparing Nano Silver for reducing agent with modification of chitosan the most according to claim 1, it is characterised in that centrifugal described in step 2 is to be centrifuged 5-20min with the rotating speed of 8000-12000r/min.
A kind of method preparing Nano Silver for reducing agent with modification of chitosan the most according to claim 1, it is characterised in that the dry process described in step 2 refers to drying box temperature is set in 40 DEG C, is dried 1-24h in the environment of vacuum.
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| CN104815990B (en) * | 2015-04-20 | 2017-05-03 | 西安理工大学 | Method for preparing nanometer sliver colloid with liquid phase reduction method |
| CN105040418A (en) * | 2015-08-22 | 2015-11-11 | 苏州正业昌智能科技有限公司 | Manufacture method of nano-gold antibacterial blended fabric |
| CN105040419A (en) * | 2015-08-22 | 2015-11-11 | 苏州正业昌智能科技有限公司 | Antibacterial cotton/cashmere/spun silk fabric |
| CN105040436A (en) * | 2015-08-22 | 2015-11-11 | 苏州正业昌智能科技有限公司 | Finishing method of antibacterial cotton fabric |
| CN105131349A (en) * | 2015-08-22 | 2015-12-09 | 苏州正业昌智能科技有限公司 | Preparation method of graphene oxide-chitosan composite material |
| CN105478792B (en) * | 2015-12-05 | 2017-08-04 | 浙江大学 | A kind of environment-friendly preparation method thereof of modification of chitosan nano silver colloidal sol |
| CN105442307B (en) * | 2015-12-16 | 2017-07-04 | 厦门大学 | A kind of preparation method of loading nano silvery anti-bacterial fibre |
| CN106215222B (en) * | 2016-07-07 | 2019-07-23 | 四川大学 | A method of oxidation chitosan oligosaccharide crosslinked with collagen and in-situ preparation nano silver preparation antibacterial Collagen Type VI |
| CN106513703B (en) * | 2016-11-22 | 2018-05-15 | 宁波工程学院 | A kind of preparation method of chitosan Ag nano composite membranes |
| CN109317692A (en) * | 2018-11-17 | 2019-02-12 | 璧典附 | One kind is using modified sugar as reducing agent and protectant nano silver and preparation method thereof |
| CN112371991A (en) * | 2020-09-09 | 2021-02-19 | 华南理工大学 | Succinylated chitosan coated monodisperse nano-silver particle and preparation method thereof |
| CN114086405B (en) * | 2021-12-22 | 2024-02-13 | 中纺院（浙江）技术研究院有限公司 | Biological reducing agent and method for applying biological reducing agent to plant indigo dyed yarns |
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| KR101525099B1 (en) * | 2008-06-30 | 2015-06-02 | 도와 일렉트로닉스 가부시키가이샤 | Metal microparticle containing composition and process for production of the same |
| CN102327284B (en) * | 2009-08-11 | 2012-09-19 | 聊城大学 | Liquid Phase Synthesis of Silver, Chitosan and/or Derivative Nanocomposites |
| CN102371358A (en) * | 2011-11-18 | 2012-03-14 | 复旦大学 | Aqueous-phase preparation method for re-dispersible nano-copper particles |
| CN103285819A (en) * | 2013-03-28 | 2013-09-11 | 苏州正业昌智能科技有限公司 | An electrostatically spun chitosan nano-fiber film for adsorption of heavy metal ions and a preparation method thereof |
| CN103467620A (en) * | 2013-09-12 | 2013-12-25 | 深圳先进技术研究院 | Activity modification method for chitosan materials |
| CN103642070A (en) * | 2013-11-11 | 2014-03-19 | 青岛文创科技有限公司 | Antibiotic composite membrane of nano-silk fibroin-chitosan-nano-silver |
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