CN101880037A - Preparation method of porous carbon material - Google Patents
Preparation method of porous carbon material Download PDFInfo
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- CN101880037A CN101880037A CN2009101365882A CN200910136588A CN101880037A CN 101880037 A CN101880037 A CN 101880037A CN 2009101365882 A CN2009101365882 A CN 2009101365882A CN 200910136588 A CN200910136588 A CN 200910136588A CN 101880037 A CN101880037 A CN 101880037A
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Abstract
The invention relates to a preparation method of a porous carbon material, which belongs to the field of materials and in particular to a porous carbon material prepared by using gelatin as the precursor of carbon and calcium carbonate as a template. The preparation process thereof comprises the following steps: uniformly mixing gelatin aqueous solution with certain concentration with nano calcium carbonate in a certain mass ratio, and preparing the porous carbon material with uniform hole distribution and good connectivity by utilizing the high dispersibility of the gelatin and the characteristic that the calcium carbonate can be decomposed to generate gas after being heated. The technical process of the invention has strong controllability, environmental protection, low cost and good product electric conductivity and can be applied to the fields of electrode materials, adsorbing materials and the like.
Description
Technical field:
The invention belongs to the material technology field, be specifically related to a kind of preparation method of porous carbon materials.
Background technology:
Porous carbon materials has highly developed specific surface and porosity, as absorption, electrode materials and support of the catalyst, is widely used in the fractionation by adsorption and the fields such as purification, double layer capacitor and catalysis of gas.At its purposes difference to its structure require differently, the porous carbon materials of the research pore size and the controlled accent that distributes just is significant.
Aspect control carbon material pore texture, people have proposed several different methods such as catalytic activation method, template carborization, mixed with polymers and have prepared porous carbon materials.The porous carbon materials even aperture distribution of template preparation method preparation, pore size is controlled.Patent (CN 101012057) discloses a kind of method of template one-step synthesis meso-porous carbon material.The mixture of silicon-dioxide/template that this method direct roasting vitriolization is crossed or itself and sucrose mixture are removed silicon-dioxide then and are obtained mesoporous carbon.
Existing inorganic mould material mainly comprises SiO
2Colloidal sol (gel) (Shan, KimM, HyeonT.Carbon, 2003,41 (8): 1525-1532; HanS, KimS, LimH, etal.Microporous andMaeroporous Materials, 2003,58 (2): 131-135), zeolite (Ma Z X, Kyotani T, TomitaA.Carbon, 2002,40:2367-2374.), Al
2O
3(Kim M J, Choi J H, Park J B.etal.ThimSolid Films, 2003,435:312-317) etc.Wherein, with SiO
2More for the research of template report, it can synthesize aperture homogeneous, porous carbon materials that specific surface area is big, has broad application prospects.But this method also exists deficiency, SiO
2Template is removed difficulty, must use hydrofluoric acid, and is difficult to remove difficulty fully, experimental results show that this is a kind of promptly expensive method of waste again, and environment is had pollution.
With the macro-molecular protein gelatin is the presoma of carbon, and nano-calcium carbonate is that the advantage that template prepares the method for porous carbon materials is: (1) template is cheap and easy to get, and can water or dilute hydrochloric acid can remove template; (2) carbon matrix precursor gelatin carbon content is higher than 50%, has the characteristic and the surfactivity of sol-gel, can help template and disperse, and makes the even pore distribution of the porous carbon of preparation; (3) preparation process is environment friendly and pollution-free; (4) electric conductivity is higher than general graphitized carbon black at present.
Summary of the invention:
The object of the present invention is to provide a kind of method for preparing porous carbon materials, the advantage of this method is to utilize the good dispersiveness of gelatin to make the even pore distribution of the carbon material of preparation; The utilization nano-calcium carbonate is that template can realize interior activation, makes the connective good of hole.This preparation process is environment friendly and pollution-free, the controllability of product and good reproducibility, and good product electric conductivity.
The present invention is the presoma of carbon with the gelatin, and nano-calcium carbonate is the preparation method of template porous carbon materials, may further comprise the steps:
1) be mixed with certain density aqueous gelatin solution with gelatin is water-soluble, wherein the mass concentration of gelatin is at 1-50wt%;
2) gelatin solution and nano-calcium carbonate are mixed with certain mass ratio, be cooled to that room temperature is congealed and dry, wherein the mass ratio of gelatin and nano-calcium carbonate is greater than 0.5;
3) with the solid of above-mentioned gelatin and nano-calcium carbonate calcium compounds in 500-1200 ℃, roasting under the nitrogen protection;
4) carbon material that obtains of roasting is soaked in the 0.5mol/L dilute hydrochloric acid solution and sloughs template, and makes system be neutral, drying with distilled water flush away residual hydrochloric acid.
Preparation technology of the present invention is simple, and cost is low, the process environmental protection.Adopt this method by processing condition such as control nano-calcium carbonate particle diameter, raw material ratio, prepare the porous carbon materials in different apertures, guarantee that carbon material has high-specific surface area, large pore volume and uniform pore size.It is multi-field that these characteristics have determined that porous carbon materials can be widely applied to, the aspects such as electrode, support of the catalyst, stratographic analysis and nano electron device manufacturing that comprise fractionation by adsorption, ultracapacitor and fuel cell are also for the condition that provides further is provided.
The used gelatin of the present invention is for being the gelatin of feedstock production with animal skin, bone, muscle or phosphorus.
Description of drawings:
The mass ratio of Fig. 1 gelatin and lime carbonate is the SEM figure of 9: 3 preparation porous carbon materials
The mass ratio of Fig. 2 gelatin and lime carbonate is the SEM figure of 9: 1 preparation porous carbon materials
Embodiment:
Embodiment 1
Weighing 9g gelatin is in 81g distilled water, and at room temperature swelling is heated to 60 ℃ of dissolvings then and makes aqueous gelatin solution, adds the 18g nano-calcium carbonate again and stirs, and is cooled to room temperature and congeals, and it is taken out from beaker, and drying is cut into small pieces.500 ℃ of roastings are 1 hour under nitrogen protection, and stove takes out after reducing to room temperature, sloughs template with 0.5mol/L dilute hydrochloric acid, and distilled water wash is to neutral, and drying can obtain porous carbon materials.
Embodiment 2
Weighing 9g gelatin is in 36g distilled water, and at room temperature swelling is heated to 60 ℃ of dissolvings then and makes aqueous gelatin solution, adds the 3g nano-calcium carbonate again and stirs, and is cooled to room temperature and congeals, and it is taken out from beaker, and drying is cut into small pieces.850 ℃ of roastings are 1 hour under nitrogen protection, and stove takes out after reducing to room temperature, sloughs template with 0.5mol/L dilute hydrochloric acid, and distilled water wash is to neutral, and drying can obtain porous carbon materials, and the aperture is 50-100nm, and the electromicroscopic photograph of resulting material is seen Fig. 1.
Embodiment 3
Weighing 9g gelatin is in 36g distilled water, and at room temperature swelling is heated to 60 ℃ of dissolvings then and makes aqueous gelatin solution, adds the 1g nano-calcium carbonate again and stirs, and is cooled to room temperature and congeals, and it is taken out from beaker, and drying is cut into small pieces.850 ℃ of roastings are 1 hour under nitrogen protection, and stove takes out after reducing to room temperature, sloughs template with 0.5mol/L dilute hydrochloric acid, and distilled water wash is to neutral, and drying can obtain porous carbon materials, and the aperture is 50-100nm, and the electromicroscopic photograph of resulting material is seen Fig. 2.
Embodiment 4
Weighing 9g gelatin is in 9g distilled water, and at room temperature swelling is heated to 60 ℃ of dissolvings then and makes aqueous gelatin solution, adds the 6g nano-calcium carbonate again and stirs, and is cooled to room temperature and congeals, and it is taken out from beaker, and drying is cut into small pieces.1100 ℃ of roastings are 1 hour under nitrogen protection, and stove takes out after reducing to room temperature, sloughs template with 0.5mol/L dilute hydrochloric acid, and the distilled water wash drying can obtain porous carbon materials.
In addition, adopt SX1934 (SZ-82) four point probe digital testing system to measure the electric conductivity of the porous carbon of embodiment 2 preparations, and itself and commercially available graphitized carbon black are compared, the result is as shown in table 1.
The conductivity of table 1 carbon material relatively
Data in the table 1 show that the porous carbon materials of this law preparation has good electrical conductivity.
Claims (4)
1. the preparation method of a porous carbon materials is characterized in that with the gelatin being the presoma of carbon, and lime carbonate is template, may further comprise the steps:
1) be mixed with certain density aqueous gelatin solution with gelatin is water-soluble, wherein the concentration of gelatin is at 1-50wt%;
2) gelatin solution and nano-calcium carbonate are mixed with certain mass ratio, be cooled to that room temperature is congealed and dry, wherein the mass ratio of gelatin and nano-calcium carbonate is greater than 0.5;
3) with above-mentioned gelatin and nano-calcium carbonate mixing after drying thing in 500-1200 ℃, carbonization under the nitrogen protection;
4) carbon material that obtains after the carbonization be soaked in slough template in the dilute hydrochloric acid solution, and with distilled water flush away residual hydrochloric acid to neutral, drying.
2. according to the preparation method of claim 1, the mass ratio that it is characterized in that gelatin and lime carbonate is 1-10.
3. according to the preparation method of the porous carbon materials of right 1, it is characterized in that gelatin and nano-calcium carbonate mixing after drying thing in 850-1200 ℃, carbonization under the nitrogen protection;
4. according to the preparation method of claim 1, be characterised in that described gelatin is for being the gelatin of feedstock production with animal skin, bone, muscle or phosphorus.
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| CN2009101365882A CN101880037A (en) | 2009-05-08 | 2009-05-08 | Preparation method of porous carbon material |
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| CN2009101365882A CN101880037A (en) | 2009-05-08 | 2009-05-08 | Preparation method of porous carbon material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617296A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Method for preparing mesoporous carbon coated LiFePO4 electrode material |
| CN105621386A (en) * | 2014-10-30 | 2016-06-01 | 中国石油化工股份有限公司 | Method for preparing carbon material |
| CN106374092A (en) * | 2016-11-04 | 2017-02-01 | 中南大学 | Preparation method of foamed nitrogen-doped carbon composite material and application thereof in sodium ion battery |
| CN106674830A (en) * | 2015-11-11 | 2017-05-17 | 重庆润泽医药有限公司 | Porous non-metallic material |
| CN106732352A (en) * | 2016-11-16 | 2017-05-31 | 广州大学 | A kind of multiporous biological charcoal and its synthetic method and application |
| CN107032323A (en) * | 2016-02-02 | 2017-08-11 | 上海交通大学 | A kind of preparation method of flake porous nano material |
| CN107680826A (en) * | 2017-11-13 | 2018-02-09 | 扬州大学 | A kind of preparation method of layering porous active carbon electrode material for ultracapacitor |
| CN109336080A (en) * | 2018-08-21 | 2019-02-15 | 浙江工业大学 | A kind of preparation method of adjustable grading porous foam Carbon Materials |
| CN110021484A (en) * | 2019-02-26 | 2019-07-16 | 贵州大学 | A kind of method and application of controllable preparation nitrogen-doped porous carbon material |
| CN114229824A (en) * | 2021-12-14 | 2022-03-25 | 中国石油大学(华东) | Porous carbon material and preparation method thereof, lithium-sulfur battery modified diaphragm and preparation method thereof, and lithium-sulfur battery |
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2009
- 2009-05-08 CN CN2009101365882A patent/CN101880037A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621386A (en) * | 2014-10-30 | 2016-06-01 | 中国石油化工股份有限公司 | Method for preparing carbon material |
| CN105621386B (en) * | 2014-10-30 | 2017-06-06 | 中国石油化工股份有限公司 | A kind of method for preparing carbon material |
| CN104617296A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Method for preparing mesoporous carbon coated LiFePO4 electrode material |
| CN106674830A (en) * | 2015-11-11 | 2017-05-17 | 重庆润泽医药有限公司 | Porous non-metallic material |
| CN107032323A (en) * | 2016-02-02 | 2017-08-11 | 上海交通大学 | A kind of preparation method of flake porous nano material |
| CN106374092A (en) * | 2016-11-04 | 2017-02-01 | 中南大学 | Preparation method of foamed nitrogen-doped carbon composite material and application thereof in sodium ion battery |
| CN106732352A (en) * | 2016-11-16 | 2017-05-31 | 广州大学 | A kind of multiporous biological charcoal and its synthetic method and application |
| CN107680826A (en) * | 2017-11-13 | 2018-02-09 | 扬州大学 | A kind of preparation method of layering porous active carbon electrode material for ultracapacitor |
| CN109336080A (en) * | 2018-08-21 | 2019-02-15 | 浙江工业大学 | A kind of preparation method of adjustable grading porous foam Carbon Materials |
| CN110021484A (en) * | 2019-02-26 | 2019-07-16 | 贵州大学 | A kind of method and application of controllable preparation nitrogen-doped porous carbon material |
| CN114229824A (en) * | 2021-12-14 | 2022-03-25 | 中国石油大学(华东) | Porous carbon material and preparation method thereof, lithium-sulfur battery modified diaphragm and preparation method thereof, and lithium-sulfur battery |
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Application publication date: 20101110 |