CN109650372A - A kind of method that a step prepares porous N doping Carbon Materials - Google Patents
A kind of method that a step prepares porous N doping Carbon Materials Download PDFInfo
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- CN109650372A CN109650372A CN201910026389.XA CN201910026389A CN109650372A CN 109650372 A CN109650372 A CN 109650372A CN 201910026389 A CN201910026389 A CN 201910026389A CN 109650372 A CN109650372 A CN 109650372A
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- C01B32/00—Carbon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses a kind of methods of step controllable preparation even porous N doping Carbon Materials, using organic sugar and urea as raw material, organic sugar and urea are melted in proportion and form homogeneous system, then it carries out drying preliminary quickly removal residual solvent, carrying out high-temperature process again makes organic sugar polymerize charing at high temperature, urea decomposes, and realizes the one-step synthesis of porous N doping Carbon Materials.The raw material that this method is related to is cheap and easy to get, and synthesis process is simple and easy environmental-friendly；Gained Carbon Materials have micropore and mesoporous classification hole, and it can realize the controllable adjustment of N doping amount, porosity and specific surface area, have excellent optics, machinery, electronics, energy storage capacity, the fields such as absorption, electrode material, catalyst carrier of sulfur-bearing and nitrogen substance have good application prospect in gas absorption, oil.
Description
Technical field
The invention belongs to new material technology fields, and in particular to a kind of method that a step prepares porous N doping Carbon Materials.
Background technique
Carbon Materials have biggish specific surface area and hole abundant and hold structure and surface functional group abundant, make its
Many fields have a wide range of applications；And the Carbon Materials of the especially N doping of Heteroatom doping are contained due to rich in
Nitrogen functional group can further improve the electric conductivity and electro catalytic activity of porous carbon material, have excellent optics, machinery, electronics,
Energy storage capacity, the fields such as absorption, electrode material, catalyst carrier of sulfur-bearing and nitrogen substance have very in gas absorption, oil
Good application prospect.
The preparation process that conventional porous Carbon Materials (especially micropore carbon material) are related to is more complicated, generally includes to be vapor-deposited
Method, hydro-thermal method and template etc..Vapour deposition process mainly reacts gaseous feed in reaction chamber, and is deposited on chip and is formed
Required Carbon Materials；Hydro-thermal method is that usually charcoal source presoma is dissolved in aqueous solution, under certain temperature and pressure, so that reaction
System reaches subcritical or Supercritical Conditions, to form a series of Carbon Materials in ducts；Template is usually by charcoal
Source is injected into the duct of template or occupies template, then washes away to obtain by template by being heat-treated after fixed carbon structure
Required porous carbon material is arrived.And introduce nitrogen in Carbon Materials and generally include the following two kinds method: one is in harsh item
Carbon Materials are formed under part, then Carbon Materials are subjected to high-temperature process in nitrogenous gas or liquid；Another kind is that have nitrogenous
Machine object is added in Carbon Materials during synthesis as precursor material.
Currently, the preparation method of traditional Carbon Materials there are synthesis procedures complicated, process not environmentally, aperture is unable to control, no
The problems such as suitable for producing in enormous quantities, more increases technology difficulty, and step becomes more numerous especially after introducing nitrogen source
Trivial, cost also correspondinglys increase.Therefore, a kind of method that N doping Carbon Materials are synthesized by the easy method of green with cheap raw material
As demand most urgent now.
Summary of the invention
It is a primary object of the present invention in view of the deficienciess of the prior art, a step controllable preparation even porous N doping
The method of Carbon Materials, it is charcoal source, urea as nitrogen source using organic sugar, and urea is used as gas template and pore creating material simultaneously, is realized
One step in-situ preparation has the N doping Carbon Materials of even porous structure, and gained N doping Carbon Materials have uniform and abundant micro-
The mesoporous classification cellular structure in hole-, specific surface area is high and is easy to adjustable, has important research and application value.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of method that a step prepares porous N doping Carbon Materials, includes the following steps:
1) carbohydrate and urea are mixed and heated thawing, obtain jelly；
2) gained jelly is stirred heating, obtains transparent clear colloidal solution；
3) gained colloidal solution is dried, forms the fluffy foaming solid of black；
4) gained foaming solid is ground, is then calcined in protective atmosphere, it is cooling to get porous N doping charcoal
Material.
In above scheme, heating condition described in step 1) is 80-100 DEG C.
In above scheme, agitating and heating temperature described in step 2) is 100-120 DEG C, and stirring condition is magnetic agitation.
In above scheme, the carbohydrate is including but not limited to glucose, fructose, sucrose, maltose, starch, cellulose, core
One or more of sugar, lactose.
In above scheme, the mass ratio of the carbohydrate and urea is 1:(0.1-10).
In above scheme, the baking step is dried using normal drying case or microwave-assisted drying；Wherein normal drying
The drying temperature that case uses is 120-280 DEG C, time 4-24h；The power that microwave-assisted drying uses for 500~1000W, when
Between be 3~30min.
In above scheme, the protective atmosphere is including but not limited to one of nitrogen, argon gas, hydrogen-argon gaseous mixture.
In above scheme, the calcining step are as follows: be warming up to 240-380 DEG C of pretreatment 2-6h first, then heat to
600-900 DEG C, keep the temperature 5-10h.
According to porous N doping Carbon Materials prepared by above scheme, it (has micro- with uniform and relatively rich pore structure
Hole and mesoporous classification hole), and it can realize the controllable adjustment of N doping amount, porosity and specific surface area, specific surface area can be
400-1300m2Controllable adjustment between/g；Have excellent optics, machinery, electronics, energy storage capacity, contains in gas absorption, oil
The fields such as absorption, electrode material, the catalyst carrier of sulphur and nitrogen substance have good application prospect.
The principle of the present invention are as follows:
The present invention uses organic sugar as carbon source, using urea as nitrogen source and gas template, by organic sugar and urea one
Determine to melt in certain proportion at temperature, form homogeneous system, then carries out drying preliminary quickly removal residual solvent, then carry out
High-temperature process makes organic sugar polymerize charing at high temperature, and urea decomposes and generates gas, and gas is blown in the melting charcoal in fluid
Bubble forms uniform micro channel, synchronous building micropore carbon structure and the Effective Doping for realizing nitrogen, and then obtains porous nitrogen
Adulterate Carbon Materials；And the one-step synthesis of high surface area porous Carbon Materials can be achieved in the present invention, without additionally introducing activator activation
Carbon Materials and etc., the preparation method being related to is simple and easy to control, is worth with important research and extension.
Compared with prior art, the invention has the benefit that
1) present invention firstly provides using organic sugar as carbon source, urea is nitrogen source and gas template, and the two is melted in proportion
Melt to form homogeneous system, realize the one-step synthesis of porous N doping Carbon Materials, gained N doping Carbon Materials have uniformly and enrich
Porous structure, a new thought can be provided for the preparation of N doping porous charcoal.
2) present invention uses anhydrous synthetic system, simple and easy, reproducible, Product yields in the synthesis process being related to
Greatly, and raw material sources are wide, at low cost, environmental-friendly, are suitble to promote and apply.
3) this method can be with N doping amount, porosity and the specific surface area of flexible modulation N doping Carbon Materials, in N doping
There is important meaning in terms of the synthesis of Carbon Materials.
Detailed description of the invention
Fig. 1 is nitrogen adsorption/desorption curve of the 1 porous N doping Carbon Materials of gained of embodiment.
Fig. 2 is nitrogen adsorption/desorption curve of the 2 porous N doping Carbon Materials of gained of embodiment.
Fig. 3 is the XPS figure of the 2 porous N doping Carbon Materials of gained of embodiment.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
A kind of porous N doping Carbon Materials, preparation method include the following steps:
1) 1g glucose is weighed respectively and 1g urea is placed in small beaker, keeps the temperature 30min under the conditions of 90 DEG C, keeps mixing solid
Body slowly melts, and forms jelly；
2) gained jelly is continuously heating to 120 DEG C, and magnetic agitation 2h or so, forms transparent clear brown colloid
Solution；
3) gained colloidal solution is placed in micro-wave oven and is consolidated with the power microwave 5min formation fluffy foam-like of black of 900W
Body obtains Tan solid after grinding；
4) it in a nitrogen atmosphere by gained Tan solid, is pre-processed 4 hours in 350 DEG C, then is warming up to 900 DEG C of processing 10
Hour, room temperature is cooled to get porous N doping Carbon Materials.
Fig. 1 is nitrogen adsorption/desorption curve of products therefrom of the present invention, it can be seen that there are hysteresis loop, illustrates that gained produces
Object has micropore and mesoporous classification hole, and the specific surface area of products therefrom is 1304.8m2/ g, micropore specific area are
1096.6m2/ g, mesopore surface area 208.2m2/g。
Embodiment 2
A kind of porous N doping Carbon Materials, preparation method include the following steps:
1) 1g glucose is weighed respectively and 2g urea is placed in small beaker, is kept the temperature 30min under the conditions of 100 DEG C, is made to mix
Solid slowly melts, and forms jelly；
2) gained jelly is continuously heating to 120 DEG C, and magnetic agitation 2h or so, forms transparent clear brown colloid
Solution；
3) gained colloidal solution is placed in micro-wave oven and is consolidated with the power microwave 5min formation fluffy foam-like of black of 900W
Body obtains Tan solid after grinding；
4) in a nitrogen atmosphere by gained Tan solid, in 350 DEG C of pretreatment 4h, then 700 DEG C of processing 10h are warming up to,
Room temperature is cooled to get porous N doping Carbon Materials.
Fig. 2 is nitrogen adsorption/desorption curve of products therefrom of the present invention, it can be seen that there are hysteresis loop, illustrates that gained produces
Object has micropore and mesoporous classification hole, and the specific surface area of products therefrom is 564.2m2/ g, micropore specific area are
533.8m2/ g, mesopore surface area 30.4m2/g。
Fig. 3 is that the XPS of the present embodiment products therefrom schemes, it can be seen that mainly with the shape of pyridine nitrogen in products therefrom of the present invention
Formula realizes N doping, is remarkably improved the electric conductivity and electrocatalysis characteristic of products therefrom.
Embodiment 3
A kind of porous N doping Carbon Materials, preparation method include the following steps:
1) 2g sucrose is weighed respectively and 1g urea is placed in small beaker, is kept the temperature 30min under the conditions of 90 DEG C, is made hybrid solid
Slowly melt, forms jelly；
2) gained jelly is continuously heating to 120 DEG C, and magnetic agitation 2h or so, forms transparent clear brown colloid
Solution；
3) gained colloidal solution is placed in micro-wave oven and is consolidated with the power microwave 5min formation fluffy foam-like of black of 900W
Body obtains Tan solid after grinding；
4) in a nitrogen atmosphere by gained Tan solid, in 350 DEG C of pretreatment 4h, then 800 DEG C of processing 10h are warming up to,
Room temperature is cooled to get porous N doping Carbon Materials.
Embodiment 4
A kind of porous N doping Carbon Materials, preparation method include the following steps:
1) 1g glucose is weighed respectively and 2g urea is placed in small beaker, is kept the temperature 30min under the conditions of 100 DEG C, is made to mix
Solid slowly melts, and forms jelly；
2) gained jelly is continuously heating to 120 DEG C, and magnetic agitation 2h or so, forms transparent clear brown colloid
Solution；
3) gained colloidal solution, which is placed in micro-wave oven, forms the fluffy foaming solid of black with the power microwave 5min of 900W,
Tan solid is obtained after grinding；
4) gained Tan solid is ground, and in a nitrogen atmosphere, in 350 DEG C of pretreatment 4h, then is warming up to 850
DEG C processing 10h, be cooled to room temperature to get porous N doping Carbon Materials.
Embodiment 5
A kind of porous N doping Carbon Materials, preparation method include the following steps:
1) 3g glucose is weighed respectively and 5g urea is placed in small beaker, keeps the temperature 30min under the conditions of 90 DEG C, keeps mixing solid
Body slowly melts, and forms jelly；
2) gained jelly is continuously heating to 120 DEG C, and magnetic agitation 2h or so, forms transparent clear brown colloid
Solution；
3) gained colloidal solution is placed in micro-wave oven and is consolidated with the power microwave 5min formation fluffy foam-like of black of 900W
Body obtains Tan solid after grinding；
4) in a nitrogen atmosphere by gained Tan solid, in 350 DEG C of pretreatment 4h, then 900 DEG C of processing 10h are warming up to,
Room temperature is cooled to get porous N doping Carbon Materials.
Each raw material cited by the present invention can realize that the bound value of the present invention and each raw material, interval value can
Realize the present invention；Embodiment numerous to list herein.The bound value of technological parameter of the invention, interval value can realize this
Invention, embodiment numerous to list herein.
Claims (8)
1. a kind of method that a step prepares porous N doping Carbon Materials, includes the following steps:
1) carbohydrate and urea are mixed and heated thawing, obtain jelly；
2) gained jelly is stirred heating, obtains transparent clear colloidal solution；
3) gained colloidal solution is dried, forms the fluffy foaming solid of black；
4) gained foaming solid is ground, is then calcined in protective atmosphere, it is cooling to get porous N doping raw material of wood-charcoal
Material.
2. the method according to claim 1, wherein heating condition described in step 1) is 80-100 DEG C.
3. the method according to claim 1, wherein agitating and heating temperature described in step 2) be 100-120 DEG C,
Stirring condition is magnetic agitation.
4. the method according to claim 1, wherein the carbohydrate is glucose, fructose, sucrose, maltose, shallow lake
One or more of powder, cellulose, ribose, lactose.
5. the method according to claim 1, wherein the mass ratio of the carbohydrate and urea is 1:(0.1-10).
6. the method according to claim 1, wherein the baking step is dried using normal drying case or microwave
Assist drying.
7. the method according to claim 1, wherein the calcining step are as follows: be warming up to 240-380 DEG C first in advance
Handle 2-6h；600-900 DEG C is then heated to, 5-10h is kept the temperature.
8. the porous N doping Carbon Materials of any one of claim 1~7 the method preparation.
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| CN111514852A (en) * | 2020-04-29 | 2020-08-11 | 广州大学 | Method for preparing nitrogen-doped carbon adsorbent by gas-phase hydrothermal carbonization of eutectic solvent |
| CN112736252A (en) * | 2020-12-30 | 2021-04-30 | 广州流行色服饰有限公司 | Mesoporous nickel oxide loaded nitrogen-doped porous carbon negative electrode material and preparation method thereof |
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| CN111514852A (en) * | 2020-04-29 | 2020-08-11 | 广州大学 | Method for preparing nitrogen-doped carbon adsorbent by gas-phase hydrothermal carbonization of eutectic solvent |
| CN111514852B (en) * | 2020-04-29 | 2022-04-19 | 广州大学 | Method for preparing nitrogen-doped carbon adsorbent by gas-phase hydrothermal carbonization of eutectic solvent |
| CN112736252A (en) * | 2020-12-30 | 2021-04-30 | 广州流行色服饰有限公司 | Mesoporous nickel oxide loaded nitrogen-doped porous carbon negative electrode material and preparation method thereof |
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