CN109809387A - A kind of porous carbon materials and preparation method thereof - Google Patents

A kind of porous carbon materials and preparation method thereof Download PDF

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Publication number
CN109809387A
CN109809387A CN201910299120.9A CN201910299120A CN109809387A CN 109809387 A CN109809387 A CN 109809387A CN 201910299120 A CN201910299120 A CN 201910299120A CN 109809387 A CN109809387 A CN 109809387A
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zinc
preparation
porous carbon
carbon materials
base compound
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CN201910299120.9A
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冯金奎
安永灵
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Shandong University
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Shandong University
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Abstract

The invention discloses a kind of preparation methods of porous carbon materials, the method includes being heated at high temperature under vacuum conditions using zinc-base compound as presoma, can be obtained porous carbon materials by one-step method.It does not need to be cleaned using acid solution or lye in porous carbon preparation method of the present invention, the method is simple and easy, production cost can be effectively reduced, preparation-obtained porous carbon specific surface with higher simultaneously, suitable aperture structure, therefore the prospect of the value with good practical application and industrial applications.

Description

A kind of porous carbon materials and preparation method thereof
Technical field
The invention belongs to porous carbon preparation technical fields, and in particular to a kind of porous carbon materials and preparation method thereof.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art Art.
Porous carbon has many advantages, such as high specific surface, stable electric conductivity and pore structure abundant chemically, high, therefore It is largely studied by people, is widely used in the various aspects such as energy storage, catalysis, filtering, heat-insulated.
The preparation method of existing porous carbon has soft mode method, hard mold method, bimodulus method etc., the aperture of the porous carbon materials of synthesis It can also regulate and control in the ranges such as macropore, mesoporous, micropore.However, it is found by the inventors that there are some problems urgency for existing preparation method When needing to solve, such as preparing porous carbon materials as template using silica material, need to be removed with alkalinity or acidic materials Template, acid used pollute the environment, and harmful to operator, in addition, the template dissolved cannot recycle, increase system Standby cost is not easy to be mass produced so that the preparation of porous carbon materials is appreciably restricted.
Summary of the invention
In view of the above shortcomings of the prior art, the present invention provides a kind of porous carbon materials and preparation method thereof, specifically, its Using zinc-base compound as presoma, directly under the conditions of vacuum high-temperature one-step method generate porous carbon materials, do not need using Acid solution or lye are cleaned, and the method is simple and easy, production cost can be effectively reduced, while preparation-obtained porous Carbon specific surface with higher, suitable aperture structure, therefore with good practical application value and industrial applications it Prospect.
The present invention is based on following technical schemes to realize above-mentioned technical purpose:
The first aspect of the invention provides a kind of preparation method of porous carbon materials, and the method includes multiple with zinc-base Object is closed as presoma, heats at high temperature under vacuum conditions, porous carbon materials can be obtained by one-step method.
Further, the zinc-base compound includes zinc citrate, zinc acetate, zinc gluconate, basic zinc carbonate, oxalic acid The mixture of one or more of metal organic framework compound of zinc, zinc carbonate, trifluoromethanesulfonic acid zinc and zinc etc.;
Further, the zinc-base compound includes zinc citrate, zinc acetate, zinc gluconate, basic zinc carbonate, grass Any one of sour zinc, zinc carbonate, trifluoromethanesulfonic acid zinc;
Further, the high-temperature temperature control is 500 DEG C -1000 DEG C;
High-temperature time control is 0.1h-24h.
The second aspect of the invention provides the porous carbon materials that above-mentioned preparation method is prepared.Experiment proves that can Know, it is prepared by the present invention to obtain porous carbon materials specific surface with higher and suitable aperture structure.
The advantages and positive effects of the present invention:
(1) under vacuum conditions, by suitable temperature can one-step method evaporate Zn-ef ficiency, obtain porous carbon materials, It does not need to be melted away template, therefore this method environment-friendly and green with alkalinity or pickling substance, and the Zn-ef ficiency volatilized can recycle It utilizes, reduces production cost.
(2) presoma such as zinc citrate, zinc gluconate etc. that the present invention uses, this substance is simple and easy to get, therefore easily In large-scale production, while the porous carbon materials specific surface with higher being prepared and suitable aperture structure.Therefore Value with good practical application.
Detailed description of the invention
The Figure of description for constituting a part of the invention is used to provide further understanding of the present invention, and of the invention shows Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
Fig. 1 is the nitrogen support adsorption curve figure for the porous carbon that embodiment 1 is prepared;
Fig. 2 is the graph of pore diameter distribution for the porous carbon that embodiment 1 is prepared.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the present invention.Unless another It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As background technique is introduced, existing porous carbon preparation method is badly in need of solving there are some problems, such as uses When the materials such as silica prepare porous carbon materials as template, need to remove template, acid used with alkalinity or acidic materials It pollutes the environment, and harmful to operator, in addition, the template dissolved cannot recycle, increases preparation cost, so that more The preparation of hole carbon material is appreciably restricted, and is not easy to be mass produced.
In view of this, providing a kind of preparation method of porous carbon materials, institute in a kind of typical embodiment of the invention The method of stating includes being heated, being can be obtained at high temperature under vacuum conditions by one-step method using zinc-base compound as presoma Porous carbon materials.Zinc-base compound cannot use other metallic matrix composites to replace in the present invention, meanwhile, use different zinc-bases Compound, also has strict demand to reaction time and reaction temperature, otherwise can not directly remove Zn-ef ficiency, and then be directly prepared into To porous carbon materials.
In still another embodiment of the invention, the zinc-base compound includes zinc citrate, zinc acetate, gluconic acid One of metal organic framework compound of zinc, basic zinc carbonate, zinc oxalate, zinc carbonate, trifluoromethanesulfonic acid zinc and zinc etc. or Two or more mixtures.
In still another embodiment of the invention, the zinc-base compound includes zinc citrate, zinc acetate, gluconic acid Any one of zinc, basic zinc carbonate, zinc oxalate, zinc carbonate, trifluoromethanesulfonic acid zinc.Inventor is the study found that different zinc-base During its high temperature cabonization of compound, reaction temperature and time are not only to the pattern for the porous carbon products being finally prepared (packet Include specific surface and aperture) it has an impact, the removal simultaneously for elements such as zinc also has an impact, to obtain pure porous carbon Material needs especially to control reaction time and reaction temperature.
In still another embodiment of the invention, the high-temperature temperature control is 500 DEG C -1000 DEG C.
In still another embodiment of the invention, high-temperature time control is 0.1h-24h.
In still another embodiment of the invention, when the zinc-base compound is zinc citrate, specific preparation method Are as follows: under vacuum conditions, 3h is heated at 700 DEG C.
In still another embodiment of the invention, when the zinc-base compound is zinc acetate, it is specific the preparation method comprises the following steps: Under vacuum conditions, 20h is heated at 500 DEG C.
In still another embodiment of the invention, when the zinc-base compound is zinc oxalate, it is specific the preparation method comprises the following steps: Under vacuum conditions, 0.5h is heated at 1000 DEG C.
In still another embodiment of the invention, when the zinc-base compound is zinc gluconate, specific preparation side Method are as follows: under vacuum conditions, heat 5h at 800 DEG C.
In still another embodiment of the invention, when the zinc-base compound is zinc carbonate, it is specific the preparation method comprises the following steps: Under vacuum conditions, 3h is heated at 700 DEG C.
In still another embodiment of the invention, when the zinc-base compound is basic zinc carbonate, specific preparation side Method are as follows: under vacuum conditions, heat 3h at 600 DEG C.
It is specific to prepare when the zinc-base compound is trifluoromethanesulfonic acid zinc in still another embodiment of the invention Method are as follows: under vacuum conditions, heated for 24 hours at 500 DEG C.
In still another embodiment of the invention, the porous carbon materials that above-mentioned preparation method is prepared are provided.Through trying Verifying is it is found that prepared by the present invention obtain porous carbon materials specific surface with higher and suitable aperture structure.
The content of present invention is further described below with reference to embodiment, but is not limitation of the invention.
Embodiment 1:
It takes the zinc citrate of 5g as raw material, under vacuum conditions, heats 3h at 700 DEG C, porous carbon materials can be obtained.
Fig. 1 is the nitrogen support adsorption curve for the porous carbon that embodiment 1 is prepared.As seen from the figure, the corresponding ratio of porous carbon Surface area is 339m2g-1, illustrate the porous carbon specific surface with higher of synthesis.
Fig. 2 is the graph of pore diameter distribution for the porous carbon that embodiment 1 is prepared.As seen from the figure, the pore-size distribution master of porous carbon 2nm is concentrated on hereinafter, illustrating that the porous pore-size distribution of synthesis is smaller.
Embodiment 2:
It takes the zinc acetate of 2g as raw material, under vacuum conditions, heats 20h at 500 DEG C, porous carbon materials can be obtained.
Embodiment 3:
It takes the zinc oxalate of 1g as raw material, under vacuum conditions, heats 0.5h at 1000 DEG C, porous carbon can be obtained Material.
Embodiment 4:
It takes the zinc gluconate of 3g as raw material, under vacuum conditions, heats 5h at 800 DEG C, porous carbon can be obtained Material.
Embodiment 5:
It takes the zinc carbonate of 2g as raw material, under vacuum conditions, heats 3h at 700 DEG C, porous carbon materials can be obtained.
Embodiment 6:
It takes the basic zinc carbonate of 1g as raw material, under vacuum conditions, heats 3h at 600 DEG C, porous carbon can be obtained Material.
Embodiment 7:
It takes the trifluoromethanesulfonic acid zinc of 1g as raw material, under vacuum conditions, is heated at 500 DEG C for 24 hours, porous carbon can be obtained Material.
It should be noted that above example is only used to illustrate the technical scheme of the present invention rather than is limited.Although ginseng It is described the invention in detail according to given example, but those skilled in the art can be as needed to this hair Bright technical solution is modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1. a kind of preparation method of porous carbon materials, which is characterized in that the method includes using zinc-base compound as presoma, It heats at high temperature under vacuum conditions, porous carbon materials can be obtained by one-step method.
2. a kind of preparation method of porous carbon materials as described in claim 1, which is characterized in that the zinc-base compound includes Zinc citrate, zinc acetate, zinc gluconate, basic zinc carbonate, zinc oxalate, zinc carbonate, trifluoromethanesulfonic acid zinc and zinc metal have The mixture of one or more of machine frame compound;
Preferably, the zinc-base compound includes zinc citrate, zinc acetate, zinc gluconate, basic zinc carbonate, zinc oxalate, carbon Any one of sour zinc, trifluoromethanesulfonic acid zinc;
The high-temperature temperature control is 500 DEG C -1000 DEG C;High-temperature time control is 0.1h-24h.
3. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is lemon When lemon acid zinc, specifically the preparation method comprises the following steps: under vacuum conditions, heating 3h at 700 DEG C.
4. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is vinegar When sour zinc, specifically the preparation method comprises the following steps: under vacuum conditions, heating 20h at 500 DEG C.
5. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is grass When sour zinc, specifically the preparation method comprises the following steps: under vacuum conditions, heating 0.5h at 1000 DEG C.
6. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is Portugal When grape saccharic acid zinc, specifically the preparation method comprises the following steps: under vacuum conditions, heating 5h at 800 DEG C.
7. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is carbon When sour zinc, specifically the preparation method comprises the following steps: under vacuum conditions, heating 3h at 700 DEG C.
8. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is alkali When formula zinc carbonate, specifically the preparation method comprises the following steps: under vacuum conditions, heating 3h at 600 DEG C.
9. a kind of preparation method of porous carbon materials as claimed in claim 2, which is characterized in that the zinc-base compound is three When fluorine methanesulfonic acid zinc, specifically the preparation method comprises the following steps: under vacuum conditions, being heated for 24 hours at 500 DEG C.
10. the porous carbon materials that any one of the claim 1-9 preparation method is prepared.
CN201910299120.9A 2019-04-15 2019-04-15 A kind of porous carbon materials and preparation method thereof Pending CN109809387A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110467182A (en) * 2019-09-07 2019-11-19 北方民族大学 A kind of multi-stage porous carbon sill and its preparation method and application based on reaction template
CN111924822A (en) * 2020-07-27 2020-11-13 山东理工大学 Preparation method of low-frequency efficient wave-absorbing SiC/porous carbon composite material
CN111994897A (en) * 2020-09-08 2020-11-27 许昌学院 Simple preparation method of honeycomb porous carbon with high specific surface area
CN112321315A (en) * 2020-11-19 2021-02-05 航天特种材料及工艺技术研究所 Preparation method of carbon/silicon carbide-zirconium carbide ceramic matrix composite
CN114195124A (en) * 2022-01-25 2022-03-18 山东大学 Porous carbon material, preparation method thereof and application thereof in sodium battery
CN115231550A (en) * 2022-08-05 2022-10-25 中国新型建材设计研究院有限公司 Preparation method and application of porous carbon material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107464923A (en) * 2017-07-19 2017-12-12 成都理工大学 A kind of compound high-capacity lithium ion cell material of nano zine oxide/porous carbon in situ and preparation method thereof
CN108940252A (en) * 2018-06-12 2018-12-07 江苏理工学院 A kind of zinc oxide/carbon composite photocatalyst nano material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107464923A (en) * 2017-07-19 2017-12-12 成都理工大学 A kind of compound high-capacity lithium ion cell material of nano zine oxide/porous carbon in situ and preparation method thereof
CN108940252A (en) * 2018-06-12 2018-12-07 江苏理工学院 A kind of zinc oxide/carbon composite photocatalyst nano material and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110467182A (en) * 2019-09-07 2019-11-19 北方民族大学 A kind of multi-stage porous carbon sill and its preparation method and application based on reaction template
CN111924822A (en) * 2020-07-27 2020-11-13 山东理工大学 Preparation method of low-frequency efficient wave-absorbing SiC/porous carbon composite material
CN111994897A (en) * 2020-09-08 2020-11-27 许昌学院 Simple preparation method of honeycomb porous carbon with high specific surface area
CN111994897B (en) * 2020-09-08 2023-05-02 许昌学院 Simple preparation method of honeycomb porous carbon with high specific surface area
CN112321315A (en) * 2020-11-19 2021-02-05 航天特种材料及工艺技术研究所 Preparation method of carbon/silicon carbide-zirconium carbide ceramic matrix composite
CN114195124A (en) * 2022-01-25 2022-03-18 山东大学 Porous carbon material, preparation method thereof and application thereof in sodium battery
CN115231550A (en) * 2022-08-05 2022-10-25 中国新型建材设计研究院有限公司 Preparation method and application of porous carbon material
CN115231550B (en) * 2022-08-05 2024-02-06 中国新型建材设计研究院有限公司 Preparation method and application of porous carbon material

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