CN106976854B - A method of preparing carbon material - Google Patents
A method of preparing carbon material Download PDFInfo
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- CN106976854B CN106976854B CN201710247827.6A CN201710247827A CN106976854B CN 106976854 B CN106976854 B CN 106976854B CN 201710247827 A CN201710247827 A CN 201710247827A CN 106976854 B CN106976854 B CN 106976854B
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- carbonate
- carbon material
- hydride
- reactor
- preparing carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of new methods for preparing carbon material.The carbon material preparation is using carbonate as carbon source, under vacuum or inert atmosphere protection, carbonate and the metal hydride mixing of 1:0.5 ~ 10 in molar ratio is placed in reactor, 100 ~ 800 DEG C is risen to the heating rate of 0.1 ~ 50 DEG C/min, reacts 0.1 ~ 12 h.After reacting end and cooling down, solid product is taken out from reactor and is impregnated with acidic materials, filters, wash, dry, can be obtained carbon.The method of the present invention is simple and easy to control, it is efficient, at low cost, be easily industrialized production.
Description
(1) technical field
The present invention relates to a kind of methods for preparing carbon material
(2) background technique
In recent years, about the preparation of carbon material and research by everybody extensive concern.Common carbon material has fullerene, carbon
There is special pattern and structure to be widely used in lithium ion for nanotube, carbon fiber, graphene and porous carbon etc., these materials
The fields such as battery, hydrogen storage material, supercapacitor, solar battery and sensor.It is many about carbon materials preparation method for material at present
It is more, such as: graphene is prepared usually using Hummers method, and this method not only needs the strong oxidizers such as the concentrated sulfuric acid and potassium permanganate
It participates in, but also needs multistep separation that can just prepare graphene (S. Y. Zheng, Y. Wen, Y. J. Zhu, Z.
Han, J. Wang, J. H. Yang, C. S.Wang, In Situ Sulfur Reduction and
Intercalation of Graphite Oxides for Li-S Battery Cathodes, Adv. Energy
Mater., 2014,1400482).Carbon nanotube preparation generallys use CVD growth method, this method not only need high temperature but also
Catalyst is needed to participate in (Y. X. Xie, L. S. Lu, Y. Tang, F. X.Zhang, C. W. Shen, X. N.
Zang, X. R. Ding, W. H. Cai, L. W. Lin, Hierarchically nanostructured carbon
fiber-nickel-carbon nanotubes for high-performance supercapacitor electrodes,
Materials Letters, 2017,186,70-73).Porous carbon preparation generallys use template, and this method utilizes organic
Object is attached to template surface, then by carbonization and strong acid erodent template to prepare porous carbon (L. Y. Zhang, H.
Huang,Y. Xia, C. Liang, W. K. Zhang, J. M. Luo, Y. P. Gan, J. Z, X. Y. Tao,
H. J. Fan, High-content sulfur uniform embedded in mesoporous carbon:A new
Electrodeposition synthesis and outstanding lithiumsulfur battery cathode, J.
Mater. Chem. A., 2017,5,5905-5911).Usually there is complex process, energy consumption in these existing preparation processes
The disadvantages of higher and seriously polluted.Thus, develop a kind of efficient, inexpensive, environmental-friendly, easy to industrialized production carbon material
Preparation method is of great significance.
(3) summary of the invention
The invention aims to provide a kind of efficient, inexpensive, environmental-friendly, easy to industrialized production carbon material
Preparation method.
Technical solution of the present invention is illustrated below.
The present invention is chemically reacted using metal hydride with metal carbonate, is simple substance by the carbon conversion in carbonate
Carbon material, specific technical solution are as follows:
A kind of method preparing carbon material, preparation method includes the following steps:
(1) under vacuum or inert atmosphere protection, carbonate and metal hydride are uniformly mixed, and mixture is shifted
To closed reactor；
(2) mixture in reactor is heated to 100 ~ 800 DEG C, and keeps the temperature 0.1 ~ 12 h；
(3) after reacting end and cooling down, the solid product taken out in reactor is impregnated into diluted acid, then by its mistake
It filters, be washed with water, dry, can be obtained carbon material.
Carbonate described in step (1) is lithium carbonate, sodium carbonate, potassium carbonate, magnesium carbonate, calcium carbonate, strontium carbonate, barium carbonate
At least one of.
Metal hydride as described in step (1) be lithium hydride, sodium hydride, hydrofining, magnesium hydride, calcium hydride, hydrogenation strontium,
At least one of barium hydride.
The molar ratio of carbonate described in step (1) and metal hydride is 1:0.5 ~ 10.
Compared with prior art, the present invention its advantages are mainly reflected in:
(1) chemical reaction occurs using metal carbonate and metal hydride in the present invention and prepares carbon material, compensate for
Carbonate is the blank that carbon source prepares this technology of carbon material.
(2) the method for the present invention it is simple and easy to control, it is efficient, at low cost, be easily industrialized production.
(3) the method for the present invention can prepare the carbon material of a variety of microscopic appearances, the carbon material by controlling reaction condition
It can be applicable to the numerous areas such as lithium ion battery, supercapacitor, hydrogen storage, catalysis.
(4) Detailed description of the invention
The scanning electron microscope diagram of carbon material prepared by Fig. 1 embodiment of the present invention 1；
The energy spectrum diagram of carbon material prepared by Fig. 2 embodiment of the present invention 1；
The scanning electron microscope diagram of carbon material prepared by Fig. 3 embodiment of the present invention 2.
(5) specific implementation method
With specific embodiment, technical scheme is described further below, but protection scope of the present invention is unlimited
In this.
Embodiment 1
Under an argon atmosphere, 0.039 mol is hydrogenated into powder for lithium and 0.0095 mol carbonic acid powder for lithium mixes, and shifted
To reactor.Mixture in reactor is risen to 550 DEG C with the heating rate of 0.5 DEG C/min, keeps the temperature 5 h.Wait react knot
After beam and cooling, taking out solid product to the concentration in reactor is to impregnate 12 h in 10wt% dilute hydrochloric acid, then by its mistake
It filters, be washed with water, dry, can be obtained carbon material.
Embodiment 2
Under vacuum conditions, 0.075 mol is hydrogenated into powder for lithium and 0.02 mol carbonic acid powder for lithium mixes, and be transferred to
Reactor.Heater is sealed and vacuumized, then rises to 550 DEG C with the heating rate of 10 DEG C/min, reacts 1 h.Wait react
After terminating and being cooling, taking out solid product to the concentration in reactor is to impregnate 10 h in 15 wt% dilute hydrochloric acid, then by it
It filters, be washed with water, dry, can be obtained carbon material.
Embodiment 3
Under helium/argon gas mixed atmosphere, 0.042 mol sodium hydride powder and 0.026 mol sodium carbonate powder are mixed
It closes, and is transferred to reactor.Heater is risen to 400 DEG C with the heating rate of 2 DEG C/min, reacts 3 h.To the end of reacting and
After cooling, taking out solid product to the concentration in reactor is to impregnate 18 h in 8 wt% dilute sulfuric acids, is then filtered, is used
Water washing, drying, can be obtained carbon material.
Embodiment 4
Under helium atmosphere, 0.09 mol magnesium hydride powder and 0.18 mol magnesium carbonate powder are mixed, and are transferred to anti-
Answer device.Heater is risen to 650 DEG C with the heating rate of 15 DEG C/min, reacts 6 h.After reacting end and cooling, take out
Solid product to concentration in reactor is to impregnate 10 h in 12 wt% dust technologies, is then filtered, be washed with water, dried
It is dry, it can be obtained carbon material.
Embodiment 5
Under an argon atmosphere, 0. 2 mol calcium hydride powders and 0.02 mol barium carbonate powder are mixed, and are transferred to anti-
Answer device.Heater is risen to 350 DEG C with the heating rate of 20 DEG C/min, reacts 5 h.After reacting end and cooling, take out
Solid product to concentration in reactor is to impregnate 18 h in 15 wt% dilute hydrochloric acid, is then filtered, be washed with water, dried
It is dry, it can be obtained carbon material.
Embodiment 6
Under vacuum conditions, 0.063 mol lithium hydride, 0.042 mol sodium hydride and 0.029 mol potassium carbonate powder are mixed
It closes, is placed in heater.Heater is risen to 450 DEG C with the heating rate of 10 DEG C/min, reacts 8 h.To the end of reacting and
After cooling, taking out solid product to the concentration in reactor is to impregnate 24 h in 7 wt% dilute hydrochloric acid, is then filtered, is used
Water washing, drying, can be obtained carbon material.
Embodiment 7
Under an argon atmosphere, by 0.042 mol sodium hydride, 0.025 mol hydrofining, 0.027 mol lithium carbonate and 0.025
The mixing of mol potassium carbonate mixed powder, and it is transferred to reactor.Heater is risen to 500 DEG C with the heating rate of 3 DEG C/min,
React 6 h.After reacting end and cooling, taking out solid product to the concentration in reactor is to impregnate in 10 wt% dilute hydrochloric acid
Then 18 h are filtered, are washed with water, are dried, can be obtained carbon material.
Embodiment 8
Under an argon atmosphere, 0.05 mol is hydrogenated into strontium powder and 0.012 mol calcium carbonate powder mixes, and be transferred to
Reactor.Mixture in reactor is risen to 100 DEG C with the heating rate of 0.5 DEG C/min, keeps the temperature 12 h.To the end of reacting
After cooling, taking out solid product to the concentration in reactor is to impregnate 12 h in 12 wt% dilute hydrochloric acid, then by its mistake
It filters, be washed with water, dry, can be obtained carbon material.
Embodiment 9
Under an argon atmosphere, 0.06 mol barium hydride powder and 0.02 mol strontium carbonate powder are mixed, and are transferred to anti-
Answer device.Mixture in reactor is risen to 800 DEG C with the heating rate of 2 DEG C/min, keeps the temperature 0.1 h.To the end of reacting and
After cooling, taking out solid product to the concentration in reactor is to impregnate 12 h in 8 wt% dilute sulfuric acids, is then filtered, is used
Water washing, drying, can be obtained carbon material.
The preferred embodiments of the invention are only listed above, and protection scope of the present invention is not restricted to this, this field
Made any change is each fallen in the scope of the present invention technical staff within the scope of the invention as claimed.
Claims (3)
1. a kind of method for preparing carbon material, mainly comprises the steps that
(1) under vacuum or inert atmosphere protection, carbonate and metal hydride are uniformly mixed, and mixture is transferred to close
The reactor closed；
(2) mixture in reactor is heated to 100~800 DEG C, and keeps the temperature 0.1~12h；
(3) after reacting end and cooling down, the solid product taken out in reactor is impregnated into diluted acid, is then filtered, is used
Water washing, drying, can be obtained carbon material；
The molar ratio of carbonate described in step (1) and metal hydride is 1:0.5~10.
2. a kind of method for preparing carbon material as described in claim 1, it is characterised in that: carbonate described in step (1) is
At least one of lithium carbonate, sodium carbonate, potassium carbonate, magnesium carbonate, calcium carbonate, strontium carbonate, barium carbonate.
3. a kind of method for preparing carbon material as described in claim 1, it is characterised in that: metal hydride described in step (1)
Object is at least one of lithium hydride, sodium hydride, hydrofining, magnesium hydride, calcium hydride, hydrogenation strontium, barium hydride.
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| CN201710247827.6A CN106976854B (en) | 2017-05-24 | 2017-05-24 | A method of preparing carbon material |
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| CN201710247827.6A CN106976854B (en) | 2017-05-24 | 2017-05-24 | A method of preparing carbon material |
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| CN106976854B true CN106976854B (en) | 2019-04-30 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108666569B (en) * | 2018-03-28 | 2020-09-29 | 天能帅福得能源股份有限公司 | Preparation method of spongy carbon material |
| CN110171832A (en) * | 2019-06-20 | 2019-08-27 | 浙江工业大学 | A method of porous silicon is prepared based on metal hydride reduction |
| CN113481383B (en) * | 2021-07-21 | 2022-07-19 | 合肥学院 | Preparation method of metal potassium |
| CN115784156A (en) * | 2022-12-13 | 2023-03-14 | 合肥学院 | Preparation method of potassium hydride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456554A (en) * | 2009-01-06 | 2009-06-17 | 黑龙江大学 | Method for preparing graphitization nano carbon |
| CN104269555A (en) * | 2014-10-08 | 2015-01-07 | 深圳市贝特瑞新能源材料股份有限公司 | Soft carbon anode material for lithium-ion power and energy storage battery as well as preparation method and application of soft carbon anode material |
| CN105271178A (en) * | 2015-11-18 | 2016-01-27 | 浙江工业大学 | Method for converting greenhouse gas into carbon |
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2017
- 2017-05-24 CN CN201710247827.6A patent/CN106976854B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101456554A (en) * | 2009-01-06 | 2009-06-17 | 黑龙江大学 | Method for preparing graphitization nano carbon |
| CN104269555A (en) * | 2014-10-08 | 2015-01-07 | 深圳市贝特瑞新能源材料股份有限公司 | Soft carbon anode material for lithium-ion power and energy storage battery as well as preparation method and application of soft carbon anode material |
| CN105271178A (en) * | 2015-11-18 | 2016-01-27 | 浙江工业大学 | Method for converting greenhouse gas into carbon |
Non-Patent Citations (1)
| Title |
|---|
| Fabrication of Y-junction carbon nanotubes by reduction of carbon dioxide with sodium borohydride;Zhengsong Lou et al.;《Diamond & Related Materials》;20060220;第15卷;第1540–1543页 * |
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