CN105036109A - Preparation method of hierarchical pore carbon material and loaded nano-silver composite functional material - Google Patents
Preparation method of hierarchical pore carbon material and loaded nano-silver composite functional material Download PDFInfo
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- CN105036109A CN105036109A CN201510360816.XA CN201510360816A CN105036109A CN 105036109 A CN105036109 A CN 105036109A CN 201510360816 A CN201510360816 A CN 201510360816A CN 105036109 A CN105036109 A CN 105036109A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 19
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002149 hierarchical pore Substances 0.000 title abstract 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- -1 polyoxyethylene Polymers 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
- 238000005057 refrigeration Methods 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004159 Potassium persulphate Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 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 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 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 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 230000002829 reductive effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 238000003837 high-temperature calcination Methods 0.000 abstract description 3
- 229920000620 organic polymer Polymers 0.000 abstract description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract 3
- 229920002125 Sokalan® Polymers 0.000 abstract 3
- 229960001631 carbomer Drugs 0.000 abstract 3
- 239000002243 precursor Substances 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000588832 Bordetella pertussis Species 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000186216 Corynebacterium Species 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 241000991587 Enterovirus C Species 0.000 description 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 1
- 241000701085 Human alphaherpesvirus 3 Species 0.000 description 1
- 241000711386 Mumps virus Species 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 241000588769 Proteus <enterobacteria> Species 0.000 description 1
- 241000191940 Staphylococcus Species 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- RRKGBEPNZRCDAP-UHFFFAOYSA-N [C].[Ag] Chemical compound [C].[Ag] RRKGBEPNZRCDAP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 206010013023 diphtheria Diseases 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 241000712461 unidentified influenza virus Species 0.000 description 1
- 241001515965 unidentified phage Species 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a preparation method of a hierarchical pore carbon material and loaded nano-silver composite functional material. The preparation method comprises the steps of firstly adding a KOH solution to adjust a nano-silver solution to be alkaline, adding a carbomer solution, stirring, standing to obtain a nano-silver gel, freeze drying the gel to obtain a frothy silver carrying precursor, roasting, cleaning up by using dilute hydrochloric acid, distilled water and ethanol to finally obtain the hierarchical pore carbon material and loaded nano-silver composite functional material. Organic polymer carbomer is adopted as a carbon source, the nano-silver gel is prepared, so that nano-silver is evenly dispersed in a molecular network of the carbomer, the network structure of the gel is kept by a freeze-drying method to obtain the precursor, and KOH added when the gel is prepared can activate a carbon material during high-temperature calcination to enable the carbon material to produce a great amount of micropores and mesoporous. The synthetic composite material can be widely applied to fields of supercapacitors, antibacterial nano products and the like.
Description
Technical field
The invention belongs to technical field of composite preparation, be specifically related to a kind of preparation method of porous carbon materials loaded with nano silver composite material.
Background technology
Nano material silver is as a kind of remarkably antibacterial in recent years, and conduction energy and material, obtains great concern.Multistage pore canal carbon material is that one has satisfactory electrical conductivity, extra specific surface area, material.Silver carbon can be widely used in indoor air purification field, and decontamination effect improving is better than ordinary granular, powdery, gac.The pollutent that silver carbon composite is removed in various degree has: the acidic and alkaline gas such as formaldehyde, nitrogen oxide, tetracol phenixin, chlorine, benzene, dicarbaldehyde, acetone, ethanol, ether, methyl alcohol, acetic acid, ethyl ester, vinylbenzene, phosgene, foul gas.The bacteriophage that the silver ions of silver contained by carbon is killed has: staphylococcus, intestinal bacteria, suis, pneumococcus, diphtheria corynebacterium, Bacillus proteus, bordetella pertussis, meningococcus, hemophilus influenza, poliovirus, mumps virus, varicella zoster virus, various influenza virus.In addition, silver-colored carbon composite also can be used for field of energy source materials, such as electrode material for super capacitor.The present invention adopts organic polymer Carmomer as carbon source, the Argent grain that self-control particle diameter is less than 5nm is loaded article, by preparing nano silver gel, that nanometer silver is disperseed in Carmomer molecular network is homogeneous, and keep the network structure of gel to obtain presoma by freeze-drying method, the KOH added when preparing gel, can activated carbon material when high-temperature calcination, carbon material is made to produce a large amount of micropore and mesoporous, the matrix material of synthesis can be widely used in ultracapacitor, the fields such as antimicrobial nano product.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of preparation method of porous carbon materials loaded with nano silver composite material.
A preparation method for multi-stage porous carbon material load nanometer silver composite functional material, is characterized in that, comprise the following steps:
(1) getting silver nitrate powder adds in deionized water, add Potassium Persulphate again and stir 12h, form colourless transparent solution, then add stablizer, polyoxyethylene glycol and PVP, add reductive agent glucose and sodium borohydride after stirring, stir and obtain flaxen Nano silver solution.Wherein in colourless transparent solution, silver nitrate concentration is 1g/L, Potassium Persulphate concentration is 5g/L, and the concentration of stablizer sodium borohydride, polyoxyethylene glycol and PVP is 0.01g/L.Concentration is regulated to be 10 ~ 1000ppm solution deionized water again;
(2) adding potassium hydroxide solution, is that 10 ~ 1000ppm polymeric PTC materials nanometer silver monomer solution regulates PH=6 ~ 9 by the concentration that step 1 is obtained;
(3) add the Carmomer aqueous solution of 1%, stir 15 ~ 30min and obtain nano silver gel;
(4) this gel refrigeration drying is obtained spumescence and carry silver-colored presoma;
(5) then by the roasting 3 ~ 10 hours under 500 ~ 1200 DEG C of ar gas environments of this presoma, wash away residual potassium hydroxide with dilute hydrochloric acid, then use distilled water, ethanol purge totally obtains final porous carbon loaded with nano silver composite material.
The advantage adopting method of the present invention to prepare multi-stage porous carbon material load nanometer silver composite functional material is:
(1) synthetic method is simply novel, repeatable strong, through the carrying effect of porous carbon, nano silver material can be made to disperse at porous carbon materials surface uniform.
(2) adopt organic polymer Carmomer as carbon source, the Argent grain that self-control particle diameter is less than 5nm is loaded article, by preparing nano silver gel, that nanometer silver is disperseed in Carmomer molecular network is homogeneous, and keep the network structure of gel to obtain presoma by freeze-drying method, the KOH added when preparing gel, can activated carbon material when high-temperature calcination, make carbon material produce a large amount of micropore and mesoporous.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the matrix material of preparation in embodiment four.
Embodiment
Further illustrate the present invention below by embodiment, instead of limit the scope of the invention.
Embodiment one:
Adding KOH solution is that the homemade polymeric PTC materials Nano silver solution of 10ppm regulates PH=6 by 100mL concentration, adds 1g Carmomer solution, stirs 15min and obtain nano silver gel.This gel refrigeration drying is obtained spumescence and carries silver-colored presoma.Then by this presoma roasting 3h under 500 DEG C of ar gas environments, with dilute hydrochloric acid, distilled water, ethanol purge totally obtains final porous carbon loaded with nano silver composite material.
Embodiment two:
Adding KOH solution is that the homemade polymeric PTC materials Nano silver solution of 200ppm regulates PH=7 by 100mL concentration, adds the Carmomer solution of 1g, stirs 20min and obtain nano silver gel.This gel refrigeration drying is obtained spumescence and carries silver-colored presoma.Then by this presoma roasting 3 ~ 10h under 800 DEG C of ar gas environments, with dilute hydrochloric acid, distilled water, ethanol purge totally obtains final porous carbon loaded with nano silver composite material.
Embodiment three:
Adding KOH solution is that the homemade polymeric PTC materials Nano silver solution of 500ppm regulates PH=8 by 100mL concentration, adds the Carmomer solution of 1g, stirs 25min and obtain nano silver gel.This gel refrigeration drying is obtained spumescence and carries silver-colored presoma.Then by this presoma roasting 7h under 1000 DEG C of ar gas environments, with dilute hydrochloric acid, distilled water, ethanol purge totally obtains final porous carbon loaded with nano silver composite material.
Embodiment four:
Adding KOH solution is that the homemade polymeric PTC materials Nano silver solution of 1000ppm regulates PH=9 by 100mL concentration, adds the Carmomer solution of 1g, stirs 30min and obtain nano silver gel.This gel refrigeration drying is obtained spumescence and carries silver-colored presoma.Then by this presoma roasting 10h under 1200 DEG C of ar gas environments, with dilute hydrochloric acid, distilled water, ethanol purge totally obtains final porous carbon loaded with nano silver composite material.Fig. 1 is the transmission electron microscope picture of the matrix material of preparation in embodiment four.
Claims (1)
1. a preparation method for multi-stage porous carbon material load nanometer silver composite functional material, is characterized in that, comprise the following steps:
(1) getting silver nitrate powder adds in deionized water, add Potassium Persulphate again and stir 12h, form colourless transparent solution, then add stablizer, polyoxyethylene glycol and PVP, add reductive agent glucose and sodium borohydride after stirring, stir and obtain flaxen Nano silver solution;
Wherein in colourless transparent solution, silver nitrate concentration is 1g/L, Potassium Persulphate concentration is 5g/L, and the concentration of stablizer sodium borohydride, polyoxyethylene glycol and PVP is 0.01g/L;
Concentration is regulated to be 10 ~ 1000ppm solution deionized water again;
(2) adding potassium hydroxide solution, is that 10 ~ 1000ppm polymeric PTC materials nanometer silver monomer solution regulates PH=6 ~ 9 by the concentration that step 1 is obtained;
(3) add the Carmomer aqueous solution of 1%, stir 15 ~ 30min and obtain nano silver gel;
(4) this gel refrigeration drying is obtained spumescence and carry silver-colored presoma;
(5) then by the roasting 3 ~ 10 hours under 500 ~ 1200 DEG C of ar gas environments of this presoma, wash away residual potassium hydroxide with dilute hydrochloric acid, then use distilled water, ethanol purge totally obtains final porous carbon loaded with nano silver composite material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510360816.XA CN105036109B (en) | 2015-06-26 | 2015-06-26 | Preparation method of hierarchical pore carbon material and loaded nano-silver composite functional material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692686A (en) * | 2016-04-28 | 2016-06-22 | 北京化工大学常州先进材料研究院 | Preparation method of nanometer zinc oxide powder |
| CN106290186A (en) * | 2016-07-25 | 2017-01-04 | 肇庆学院 | A kind of doping porous carbon Nano silver grain visualizing rapid mercury detection ion |
| CN106374010A (en) * | 2016-10-09 | 2017-02-01 | 天津市职业大学 | Preparation method of nano-silver composite stannic oxide transparent conducting thin film |
| CN107398562A (en) * | 2017-07-14 | 2017-11-28 | 山西农业大学 | The preparation method of fulvic acid nano silver gel |
| CN108249437A (en) * | 2018-02-12 | 2018-07-06 | 西安工程大学 | A kind of preparation method of active carbon loading silver |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
-
2015
- 2015-06-26 CN CN201510360816.XA patent/CN105036109B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103567431A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Nanometer silver colloid solution and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 杨立群等: "含纳米银的抗菌水凝胶研究", 《中山大学学报( 自然科学版)》 * |
| 杨维佳等: "多孔碳微球负载纳米银的制备及抗菌性能", 《太原理工大学学报》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692686A (en) * | 2016-04-28 | 2016-06-22 | 北京化工大学常州先进材料研究院 | Preparation method of nanometer zinc oxide powder |
| CN105692686B (en) * | 2016-04-28 | 2017-11-17 | 北京化工大学常州先进材料研究院 | A kind of preparation method of nanometer Zinc oxide powder |
| CN106290186A (en) * | 2016-07-25 | 2017-01-04 | 肇庆学院 | A kind of doping porous carbon Nano silver grain visualizing rapid mercury detection ion |
| CN106290186B (en) * | 2016-07-25 | 2019-03-29 | 肇庆学院 | A kind of doping porous carbon Nano silver grain visualizing rapid mercury detection ion |
| CN106374010A (en) * | 2016-10-09 | 2017-02-01 | 天津市职业大学 | Preparation method of nano-silver composite stannic oxide transparent conducting thin film |
| CN107398562A (en) * | 2017-07-14 | 2017-11-28 | 山西农业大学 | The preparation method of fulvic acid nano silver gel |
| CN107398562B (en) * | 2017-07-14 | 2019-06-04 | 山西农业大学 | The preparation method of fulvic acid nano silver gel |
| CN108249437A (en) * | 2018-02-12 | 2018-07-06 | 西安工程大学 | A kind of preparation method of active carbon loading silver |
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