CN106976854A - A kind of method for preparing carbon material - Google Patents
A kind of method for preparing carbon material Download PDFInfo
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- CN106976854A CN106976854A CN201710247827.6A CN201710247827A CN106976854A CN 106976854 A CN106976854 A CN 106976854A CN 201710247827 A CN201710247827 A CN 201710247827A CN 106976854 A CN106976854 A CN 106976854A
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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 method for preparing carbon material.The carbon material is prepared using carbonate as carbon source, under vacuum or inert atmosphere protection, by carbonate and metal hydride in molar ratio 1:0.5 ~ 10 mixing, is placed in reactor, and 100 ~ 800 DEG C are risen to 0.1 ~ 50 DEG C/min heating rate, reacts 0.1 ~ 12 h.After question response terminates and cooled down, solid product is taken out and soaked with acidic materials from reactor, filters, wash, dry, you can obtain carbon.The inventive method is simple and easy to control, efficient, cost is low, be easily achieved industrialized production.
Description
（One）Technical field
The present invention relates to a kind of method for preparing carbon material
（Two）Background technology
In recent years, the preparation and research on carbon material are by everybody extensive concern.Common carbon material has fullerene, carbon nanometer
There is pipe, carbon fiber, graphene and porous carbon etc., these materials special pattern and structure to be widely used in lithium-ion electric
The fields such as pond, hydrogen storage material, ultracapacitor, solar cell and sensor.It is numerous on carbon materials preparation method for material at present,
For example：Graphene is prepared usually using Hummers methods, and this method not only needs the strong oxidizers such as the concentrated sulfuric acid and potassium permanganate to join
With, and also need to multistep separation 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）.CNT prepares and generally uses CVD growth method, and this method not only needs high temperature but also also needs to catalyst participation
（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 prepares and generally uses template, and this method utilizes organic
Thing is attached to template surface, then by carbonization and strong acid Erodent Algorithm so as 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）.Generally there is complex process, energy consumption in these existing preparation technologies
Higher and seriously polluted the shortcomings of.Thus, develop a kind of carbon material that is efficient, inexpensive, environment-friendly, being easy to industrialized production
Preparation method is significant.
（Three）The content of the invention
The invention aims to provide a kind of carbon material preparation that is efficient, inexpensive, environment-friendly, being easy to industrialized production
Method.
Technical scheme 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, concrete technical scheme is as follows：
A kind of described method for preparing carbon material, its preparation method comprises the following steps：
（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 is incubated 0.1 ~ 12h；
（3）After question response terminates and cooled down, the solid product taken out in reactor soaks into diluted acid, is then filtered, used
Water washing, drying, you can obtain carbon material.
Step（1）Described in carbonate be lithium carbonate, sodium carbonate, potassium carbonate, magnesium carbonate, calcium carbonate, strontium carbonate, barium carbonate
At least one of.
Step（1）Described in metal hydride for lithium hydride, sodium hydride, hydrofining, magnesium hydride, calcium hydride, hydrogenation strontium,
At least one of barium hydride.
Step（1）Described in carbonate and metal hydride mol ratio be 1:0.5~10.
Compared with prior art, its advantage is mainly reflected in the present invention：
（1）Occur chemical reaction using metal carbonate and metal hydride in the present invention and prepare carbon material, compensate for carbonic acid
Salt is the blank that carbon source prepares this technology of carbon material.
（2）The inventive method is simple and easy to control, efficient, cost is low, be easily achieved industrialized production.
（3）The inventive method can be by controlling reaction condition to prepare the carbon material of a variety of microscopic appearances, the carbon material
It can be applicable to the numerous areas such as lithium ion battery, ultracapacitor, hydrogen storage, catalysis.
（Four）Brief description of the drawings
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.
（Five）Specific implementation method
Technical scheme is described further with specific embodiment below, but protection scope of the present invention is not limited to
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 is mixed, and be transferred to anti-
Answer device.Mixture in reactor is risen to 550 DEG C with 0.5 DEG C/min heating rate, 5 h are incubated.Question response terminate and
After cooling, the solid product in reactor is taken out to concentration to soak 12 h in 10wt% watery hydrochloric acid, is then filtered, used
Water washing, drying, you can obtain carbon material.
Embodiment 2
Under vacuum, 0.075 mol is hydrogenated into powder for lithium and 0.02 mol carbonic acid powder for lithium is mixed, and be transferred to reaction
Device.Heater is sealed and vacuumized, then 550 DEG C are risen to 10 DEG C/min heating rate, 1 h is reacted.Question response terminates
After cooling, take out reactor in solid product to concentration be 15 wt% watery hydrochloric acid in soak 10 h, then filtered,
It is washed with water, dries, you can obtains carbon material.
Embodiment 3
Under helium/argon gas mixed atmosphere, 0.042 mol sodium hydrides powder and 0.026 mol sodium carbonate powder are mixed, and
It is transferred to reactor.Heater is risen to 400 DEG C with 2 DEG C/min heating rate, 3 h are reacted.Question response terminates and cooled down
Afterwards, the solid product in reactor is taken out to concentration to soak 18 h in 8 wt% dilute sulfuric acids, is then filtered, is washed with water
Wash, dry, you can obtain carbon material.
Embodiment 4
Under helium atmosphere, 0.09 mol magnesium hydrides powder and 0.18 mol magnesium carbonate powder are mixed, and be transferred to reactor.
Heater is risen to 650 DEG C with 15 DEG C/min heating rate, 6 h are reacted.After question response terminates and cooled down, reactor is taken out
Interior solid product, to soak 10 h in 12 wt% dust technologies, is then filtered, is washed with water, dried to concentration, you can
Obtain carbon material.
Embodiment 5
Under an argon atmosphere, 0. 2 mol calcium hydrides powders and 0.02 mol barium carbonate powders are mixed, and is transferred to reaction
Device.Heater is risen to 350 DEG C with 20 DEG C/min heating rate, 5 h are reacted.After question response terminates and cooled down, take out anti-
The solid product in device is answered, to soak 18 h in 15 wt% watery hydrochloric acid, then to be filtered, be washed with water, dried to concentration,
Carbon material can be obtained.
Embodiment 6
Under vacuum, 0.063 mol lithium hydrides, 0.042 mol sodium hydrides and 0.029 mol potassium carbonate powder are mixed,
It is placed in heater.Heater is risen to 450 DEG C with 10 DEG C/min heating rate, 8 h are reacted.Question response terminates and cooled down
Afterwards, the solid product in reactor is taken out to concentration to soak 24 h in 7 wt% watery hydrochloric acid, is then filtered, is washed with water
Wash, dry, you can obtain carbon material.
Embodiment 7
Under an argon atmosphere, by 0.042 mol sodium hydrides, 0.025 mol hydrofinings, 0.027 mol lithium carbonates and 0.025 mol
Potassium carbonate mixed powder is mixed, and is transferred to reactor.Heater is risen into 500 DEG C, reaction with 3 DEG C/min heating rate
6 h.After question response terminates and cooled down, take out reactor in solid product to concentration be 10 wt% watery hydrochloric acid in soak 18
H, is then filtered, is washed with water, is dried, you can obtain carbon material.
Embodiment 8
Under an argon atmosphere, 0.05 mol is hydrogenated into strontium powder and 0.012 mol calcium carbonate powders is mixed, and be transferred to reaction
Device.Mixture in reactor is risen to 100 DEG C with 0.5 DEG C/min heating rate, 12 h are incubated.Question response terminate with it is cold
But after, the solid product in reactor is taken out to concentration to soak 12 h in 12 wt% watery hydrochloric acid, is then filtered, used
Water washing, drying, you can obtain carbon material.
Embodiment 9
Under an argon atmosphere, 0.06 mol barium hydrides powder and 0.02 mol strontium carbonate powders are mixed, and is transferred to reaction
Device.Mixture in reactor is risen to 800 DEG C with 2 DEG C/min heating rate, 0.1 h is incubated.Question response terminate with it is cold
But after, the solid product in reactor is taken out to concentration to soak 12 h in 8 wt% dilute sulfuric acids, then filtered, use water
Washing, drying, you can obtain 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 area
Any change that technical staff is made within the scope of the invention as claimed is each fallen within the scope of the present invention.
Claims (4)
1. a kind of method for preparing carbon material, is mainly included the following steps that：
(1) under vacuum or inert atmosphere protection, carbonate and metal hydride are uniformly mixed, and mixture is transferred to
Closed reactor；
(2) mixture in reactor is heated to 100 ~ 800 DEG C, and is incubated 0.1 ~ 12 h；
(3) after question response terminates and cooled down, the solid product taken out in reactor soaks into diluted acid, is then filtered, used
Water washing, drying, you can obtain carbon material.
2. a kind of method for preparing carbon material as claimed in claim 1, it is characterised in that：Carbonate is described in step (1)
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 claimed in claim 1, it is characterised in that：Metal hydride described in step (1)
Thing is at least one of lithium hydride, sodium hydride, hydrofining, magnesium hydride, calcium hydride, hydrogenation strontium, barium hydride.
4. a kind of method for preparing carbon material as claimed in claim 1, it is characterised in that：Carbonate described in step (1) and
The mol ratio of metal hydride is 1:0.5~10.
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| CN201710247827.6A CN106976854B (en) | 2017-05-24 | 2017-05-24 | A method of preparing carbon material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108666569A (en) * | 2018-03-28 | 2018-10-16 | 浙江天能能源科技股份有限公司 | A kind of spongy carbon material and its preparation method and application |
| 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 |
| CN113481383A (en) * | 2021-07-21 | 2021-10-08 | 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 |
-
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 (2)
| Title |
|---|
| HUI HUANG ET AL.: "Toast-like porous carbon derived from one-step reduction of CaCO3 for electrochemical lithium storage", 《CARBON》 * |
| ZHENGSONG LOU ET AL.: "Fabrication of Y-junction carbon nanotubes by reduction of carbon dioxide with sodium borohydride", 《DIAMOND & RELATED MATERIALS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108666569A (en) * | 2018-03-28 | 2018-10-16 | 浙江天能能源科技股份有限公司 | A kind of spongy carbon material and its preparation method and application |
| 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 |
| CN113481383A (en) * | 2021-07-21 | 2021-10-08 | 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 |
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| CN106976854B (en) | 2019-04-30 |
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