CN104291312A - Method for preparing hierarchical porous carbon material based on sea salt template - Google Patents
Method for preparing hierarchical porous carbon material based on sea salt template Download PDFInfo
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- CN104291312A CN104291312A CN201410494525.5A CN201410494525A CN104291312A CN 104291312 A CN104291312 A CN 104291312A CN 201410494525 A CN201410494525 A CN 201410494525A CN 104291312 A CN104291312 A CN 104291312A
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- sea salt
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Abstract
The invention discloses a method for preparing a hierarchical porous carbon material based on sea salt template. The method comprises the following processes: dissolving and filtering sea salt water; adding a water-soluble carbon source to obtain a mixed solution; drying and freezing the mixed solution to obtain mixture precursor powder; heating the precursor powder under a protective atmosphere, carbonizing the carbon source, and carrying out suction filtration and washing to removal the sea salt, so as to obtain the carbon material with the hierarchical porous structure. The sea salt template-based method has the advantages that the process is simple; the raw materials are cheap and environmental friendly; and the prepared carbon material has a macropore-mesopore-micropore hierarchical structure, and is large in specific surface area, and suitable for super capacitor electrodes, lithium ion battery cathode materials and the like.
Description
Technical field
The present invention relates to a kind of method based on the classifying porous carbon material of sea salt Template preparation, belong to advanced carbon material technology of preparing.
Background technology
Graded porous carbon, refer to the carbon material with foramen magnum-mesoporous-micropore multistage-combination structure, its feature comprises: the macropore in structure is distributed with the transmission being beneficial to material, makes electrolytic solution be more prone to immerse, and can as the reaction tank of electrochemical activity ion; Mesoporously can provide large electrode-electric solution matter contact area, in this sense, be conducive to the high rate performance improving electrical condenser and battery electrode material; Microvoid structure can significant increase specific surface area, provides reactive behavior site.Numerous advantages of classifying porous carbon material make it be widely used in the field such as energy storage, catalysis.
Template prepares one of the most frequently used method of classifying porous carbon material.Traditional template uses silicon, and carbon source presoma, as template, is immersed in the space of template by the material such as silicon oxide or anodised aluminium, makes carbon source carbonization, remove template subsequently, obtain vesicular structure through certain process.But there is many defects in conventional template method, as: template needs to prepare in advance, complex process, and cost is higher; Use hydrofluoric acid, hydrochloric acid etc. to have the reagent of corrodibility or toxicity at the removal process need of template, be unfavorable for environment protection and scale operation.Have report to use sodium-chlor to be template recently, citric acid is carbon source, preparation three-dimensional network shape graphene-structured.The method technique is simple, and template is easy to get.But its three-dimensional net structure prepared only has macroporous structure, lack mesoporous and micropore composition, specific surface area is lower, and needs in preparation technology to use the metal-salts such as tin protochloride as catalyzer, has certain toxic side effect.
In sum, development of new environmental protection template, the carbon material that preparation has microscopic three-dimensional graded porous structure has high theory and practical value.About the method based on sea salt Template preparation graded porous carbon, have not yet to see relevant report.
Summary of the invention
The present invention aims to provide a kind of method based on the classifying porous carbon material of sea salt Template preparation.The method process is simple, and abundant raw material, obtained carbon material has microscopic three-dimensional graded porous structure and excellent chemical property.
The present invention is a kind of method based on the classifying porous carbon material of sea salt Template preparation realized by following technical proposals, it is characterized in that comprising following process:
1) sea salt is mixed with the aqueous solution that massfraction is 15 ~ 30 %, gained solution is carried out filtration treatment, with elimination silt, obtain clarifying salts solution;
2) solubility carbon source dextrose anhydrous, sucrose or citric acid are joined in the salts solution in step 1), it is 10 ~ 50 gL that the dense DEG C of degree being made into carbon source reaches
-1mixing solutions, mixing solutions is stirred; Carry out subsequently, in 60 ~ 100 dry or-50 DEG C of vacuum lyophilizations, obtaining precursor powder;
3) precursor powder being placed in corundum tube furnace, is 100 ~ 300 mLmin at flow
-1argon gas or nitrogen protection under, with 5 ~ 10 DEG C of min
-1temperature rise rate be heated to 600 DEG C ~ 750 DEG C, insulation 1 ~ 3 h, carrying out the carbonization of carbon source, is 100 ~ 300 mLmin at flow
-1argon gas or nitrogen under, cool to room temperature with the furnace, by product take out, grinding, obtain the mixture of carbon and salt;
4) join in deionized water by step 3) gained mixture, obtained concentration is 20 ~ 50 gL
-1suspension liquid, stir 10 ~ 30 min, use deionized water filtering and washing subsequently, obtain black powder, by its dry 10 ~ 24 h in 50 ~ 100 DEG C of loft drier, obtain the classifying porous carbon material with foramen magnum-mesoporous-micropore.
Compared with prior art, the invention has the beneficial effects as follows: technique is simple, and cost is low, and obtained graded porous carbon has three-dimensional network-like structure, and specific surface area is greater than 600 m
2g
-1, macropore diameter is wherein 1 ~ 2 μm, and mesoporous pore size is 5 ~ 20 nm, and micropore size is 0.5 ~ 2 nm.This classifying porous carbon material can be applied to electrode of super capacitor and lithium ion battery negative material etc.
Accompanying drawing explanation
The TEM figure of Fig. 1 classifying porous carbon structure obtained by the embodiment of the present invention one.
The pictorial diagram of Fig. 2 graded porous carbon prepared by the embodiment of the present invention one.
The nitrogen adsorption desorption curve figure of Fig. 3 graded porous carbon prepared by the embodiment of the present invention one.
The pore size distribution curve figure of Fig. 4 graded porous carbon prepared by the embodiment of the present invention one.
Embodiment
Below in conjunction with embodiment, the invention will be further described, and these embodiments, just for illustration of the present invention, do not limit the present invention.
Embodiment one
Weigh 25 g sea salt, be dissolved in 100 mL deionized waters, use aperture to be that 0.22 μm of filter paper enters filtration treatment to gained solution, with insoluble impurity such as elimination silts, obtain clarification sea salt solution; 1.25 g dextrose anhydrouss are joined in above-mentioned sea salt solution, mixing solutions is stirred 4 h under the speed of 200 rpm; Carry out vacuum lyophilization (condenser temperature of drying machine is-50 DEG C, air pressure <20 Pa) subsequently, obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200 mLmin at flow
-1argon gas atmosphere under, with 5 DEG C of min
-1temperature rise rate be heated to 650 DEG C, being incubated 2 h, making carbon source carbonization, is 200 mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain the mixture of carbon and salt; Gained mixture is joined obtained suspension liquid in 400 mL deionized waters, 15 min are stirred under the speed of 200 rpm, suction filtration (filter paper aperture is 0.22 μm) washing subsequently, 400 mL deionized waters are added again to obtaining powder, stir 15 min, again suction filtration, obtain black powder, by its in loft drier in 80 DEG C of drying 10 h, obtain classifying porous carbon material.Through transmission electron microscope observing, the macropore diameter of obtained carbon material is 1 ~ 2 μm.Show through the test of isothermal nitrogen adsorption desorption, obtained carbon material specific surface area is 689 m
2g
-1, based on the display of DFT pore size distribution analytical results, obtained carbon material mesoporous pore size integrated distribution is in 5 nm, and micropore size is distributed in 0.5 ~ 2 nm
Embodiment two
Weigh 25 g sea salt, be dissolved in 100 mL deionized waters, use aperture to be that 0.22 μm of filter paper enters filtration treatment to gained solution, with insoluble impurity such as elimination silts, obtain clarification sea salt solution; 1.25 g dextrose anhydrouss are joined in above-mentioned sea salt solution, mixing solutions is stirred 4 h under the speed of 200 rpm; Subsequently solution is carried out drying with 80 DEG C in loft drier, obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200 mLmin at flow
-1argon gas atmosphere under, with 8 DEG C of min
-1temperature rise rate be heated to 650 DEG C, being incubated 2 h, making carbon source carbonization, is 200 mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain the mixture of carbon and salt; Gained mixture is joined obtained suspension liquid in 400 mL deionized waters, under the speed of 200 rpm, stir 15 min, suction filtration (filter paper aperture is 0.22 μm) washing subsequently three times, obtains black powder, by its dry 10 h in 80 DEG C of loft drier, obtain classifying porous carbon material.
Embodiment three
Weigh 25 g sea salt, be dissolved in 100 mL deionized waters, use aperture to be that 0.22 μm of filter paper enters filtration treatment to gained solution, with insoluble impurity such as elimination silts, obtain clarification sea salt solution; 1.25 g sucrose are joined in above-mentioned sea salt solution, mixing solutions is stirred 4 h under the speed of 200 rpm; Carry out vacuum lyophilization (condenser temperature of drying machine is-50 DEG C, air pressure <20 Pa) subsequently, obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200 mLmin at flow
-1argon gas atmosphere under, with 5 DEG C of min
-1temperature rise rate be heated to 750 DEG C, being incubated 2 h, making carbon source carbonization, is 200 mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain the mixture of carbon and salt; Gained mixture is joined obtained suspension liquid in 400 mL deionized waters, under the speed of 200 rpm, stir 15 min, suction filtration (filter paper aperture is 0.22 μm) washing subsequently three times, obtains black powder, by its dry 10 h in 80 DEG C of loft drier, obtain classifying porous carbon material.
Embodiment four
Weigh 25 g sea salt, be dissolved in 100 mL deionized waters, use aperture to be that 0.22 μm of filter paper enters filtration treatment to gained solution, with insoluble impurity such as elimination silts, obtain clarification sea salt solution; 2 g citric acids are joined in above-mentioned sea salt solution, mixing solutions is stirred 4 h under the speed of 200 rpm; Subsequently that solution is dry in the loft drier of 80 DEG C, obtain precursor powder; Precursor powder being placed in corundum tube furnace, is 200 mLmin at flow
-1argon gas atmosphere under, with 10 DEG C of min
-1temperature rise rate be heated to 700 DEG C, being incubated 2 h, making carbon source carbonization, is 200 mLmin at flow
-1argon gas atmosphere under cool to room temperature with the furnace, by sample take out, grinding, obtain the mixture of carbon and salt; Gained mixture is joined obtained suspension liquid in 400 mL deionized waters, under the speed of 200 rpm, stir 15 min, suction filtration (filter paper aperture is 0.22 μm) washing subsequently, obtains black powder, by its dry 10 h in 80 DEG C of loft drier, obtain classifying porous carbon material.
Claims (1)
1., based on a method for the classifying porous carbon material of sea salt Template preparation, it is characterized in that comprising following process:
1) sea salt is mixed with the aqueous solution that massfraction is 15 ~ 30 %, gained solution is carried out filtration treatment, with elimination silt, obtain clarification sea salt solution;
2) solubility carbon source dextrose anhydrous, sucrose or citric acid are joined in the salts solution in step 1), it is 10 ~ 50 gL that the concentration being made into carbon source reaches
-1mixing solutions, mixing solutions is stirred; Carry out or-50 ° C vacuum lyophilizations dry at 60 ~ 100 ° of C subsequently, obtain precursor powder;
3) precursor powder being placed in corundum tube furnace, is 100 ~ 300 mLmin at flow
-1argon gas or nitrogen protection under, with 5 ~ 10 ° of Cmin
-1temperature rise rate be heated to 600 ° of C ~ 750 ° C, insulation 1 ~ 3 h, carrying out the carbonization of carbon source, is 100 ~ 300 mLmin at flow
-1argon gas or nitrogen under, cool to room temperature with the furnace, by product take out, grinding, obtain the mixture of carbon and salt;
4) join in deionized water by step 3) gained mixture, obtained concentration is 20 ~ 50 gL
-1suspension liquid, stir 10 ~ 30 min, use deionized water filtering and washing subsequently, obtain black powder, by its dry 10 ~ 24 h in 50 ~ 100 ° of C loft drier, obtain the classifying porous carbon material with foramen magnum-mesoporous-micropore.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724693A (en) * | 2015-03-06 | 2015-06-24 | 苏州大学 | Organic-salt-based 3D porous carbon material, and preparation method and application thereof |
| CN104934581A (en) * | 2015-06-03 | 2015-09-23 | 武汉理工大学 | Three-dimensional-antimony/carbon network structure composite material, preparation method and application thereof |
| CN105390672A (en) * | 2015-10-21 | 2016-03-09 | 天津大学 | Preparation method for three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet material |
| CN105762338A (en) * | 2016-02-04 | 2016-07-13 | 天津大学 | Method for preparing lithium battery silicon carbon anode material by utilizing magnesiothermic reduction |
| CN106299368A (en) * | 2016-07-23 | 2017-01-04 | 天津大学 | A kind of method preparing N doping cellular disordered carbon material |
| CN106328905A (en) * | 2016-11-04 | 2017-01-11 | 中南大学 | Preparation method for coralline nitrogen and phosphorus co-doped carbon composite material and application of composite material in sodium-ion battery |
| CN106744858A (en) * | 2017-01-16 | 2017-05-31 | 深圳大学 | A kind of three-dimensional grapheme and preparation method and application |
| CN109553098A (en) * | 2018-09-04 | 2019-04-02 | 四川大学 | A kind of method and application preparing the foramen magnum-mesoporous carbon of high-specific surface area using salt template |
| CN110028051A (en) * | 2019-04-24 | 2019-07-19 | 陕西科技大学 | A method of sodium-ion battery is prepared with porous carbon negative pole material based on sucrose |
| CN110155980A (en) * | 2019-05-20 | 2019-08-23 | 北京化工大学 | A kind of preparation method of the three-dimensional porous carbon material of honeycomb |
| CN110386626A (en) * | 2018-04-16 | 2019-10-29 | 中国科学技术大学 | A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic |
| CN110449149A (en) * | 2019-06-27 | 2019-11-15 | 天津大学 | A kind of preparation method of carbon network supported noble metals nano-particle material |
| CN110804279A (en) * | 2019-11-27 | 2020-02-18 | 天津大学 | Preparation method of three-dimensional network carbon/epoxy resin heat-conducting composite material based on salt template |
| CN111196602A (en) * | 2020-01-09 | 2020-05-26 | 安徽大学 | Preparation method and application of porous graphene-like nano carbon sheet doped with double hetero atoms |
| CN112582623A (en) * | 2019-09-29 | 2021-03-30 | 东北大学秦皇岛分校 | Method for preparing nitrogen-doped porous carbon based on carboxymethyl modified natural high molecular compound |
| CN112794324A (en) * | 2019-11-14 | 2021-05-14 | 华南理工大学 | High-mesoporosity lignin hierarchical pore carbon material and preparation method and application thereof |
| CN113371693A (en) * | 2021-06-09 | 2021-09-10 | 中钢集团南京新材料研究院有限公司 | Cobalt-nitrogen co-doped three-dimensional structure carbon material and preparation method and application thereof |
| CN115477548A (en) * | 2022-09-01 | 2022-12-16 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
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Cited By (23)
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| CN104724693B (en) * | 2015-03-06 | 2016-09-07 | 苏州大学 | 3D porous carbon materials based on organic salt, preparation method and applications |
| CN104724693A (en) * | 2015-03-06 | 2015-06-24 | 苏州大学 | Organic-salt-based 3D porous carbon material, and preparation method and application thereof |
| CN104934581A (en) * | 2015-06-03 | 2015-09-23 | 武汉理工大学 | Three-dimensional-antimony/carbon network structure composite material, preparation method and application thereof |
| CN105390672A (en) * | 2015-10-21 | 2016-03-09 | 天津大学 | Preparation method for three-dimensional nitrogen-doped mesoporous carbon ultra-thin nanosheet material |
| CN105762338A (en) * | 2016-02-04 | 2016-07-13 | 天津大学 | Method for preparing lithium battery silicon carbon anode material by utilizing magnesiothermic reduction |
| CN106299368A (en) * | 2016-07-23 | 2017-01-04 | 天津大学 | A kind of method preparing N doping cellular disordered carbon material |
| CN106328905A (en) * | 2016-11-04 | 2017-01-11 | 中南大学 | Preparation method for coralline nitrogen and phosphorus co-doped carbon composite material and application of composite material in sodium-ion battery |
| CN106744858A (en) * | 2017-01-16 | 2017-05-31 | 深圳大学 | A kind of three-dimensional grapheme and preparation method and application |
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| CN112582623A (en) * | 2019-09-29 | 2021-03-30 | 东北大学秦皇岛分校 | Method for preparing nitrogen-doped porous carbon based on carboxymethyl modified natural high molecular compound |
| CN112794324A (en) * | 2019-11-14 | 2021-05-14 | 华南理工大学 | High-mesoporosity lignin hierarchical pore carbon material and preparation method and application thereof |
| CN110804279A (en) * | 2019-11-27 | 2020-02-18 | 天津大学 | Preparation method of three-dimensional network carbon/epoxy resin heat-conducting composite material based on salt template |
| CN111196602A (en) * | 2020-01-09 | 2020-05-26 | 安徽大学 | Preparation method and application of porous graphene-like nano carbon sheet doped with double hetero atoms |
| CN111196602B (en) * | 2020-01-09 | 2022-11-08 | 安徽大学 | Preparation method and application of double-heteroatom-doped porous graphene-like nano carbon sheet |
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| CN115477548B (en) * | 2022-09-01 | 2023-11-17 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
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