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 PDF

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Publication number
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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silver
nano
solution
gel
concentration
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CN105036109B (en
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何丹农
冉伟
张春明
王艳丽
徐少洪
陈超
金彩虹
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Yufengnanuo Technology (Shanghai) Co., Ltd
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Shanghai Na Xu Industrial Co Ltd
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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

A kind of preparation method of multi-stage porous carbon material load nanometer silver composite functional material
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.
CN201510360816.XA 2015-06-26 2015-06-26 Preparation method of hierarchical pore carbon material and loaded nano-silver composite functional material Active CN105036109B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

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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

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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)

* Cited by examiner, † Cited by third party
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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Patentee before: SHANGHAI NAXU INDUSTRIAL Co.,Ltd.