CN109775704A - It is a kind of using oat as nitrating porous carbon of raw material and its preparation method and application - Google Patents
It is a kind of using oat as nitrating porous carbon of raw material and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to technical field of nano material, and in particular to a kind of using oat as nitrating porous carbon of raw material and its preparation method and application.It is the preparation method of the nitrating porous carbon of raw material the following steps are included: step 1 using oat: oat is dry, milled processed carries out heating stirring at powdered rear be added in dispersing agent, activator and nitrogen source are added after mixing evenly, continue heating stirring until being uniformly mixed, obtains presoma after drying；Step 2: the presoma that step 1 obtains being calcined under atmosphere of inert gases, the processing of progress acid obtains a kind of using oat as the nitrating porous carbon of raw material after calcining.The present invention uses chemical activation method, carries out activation pore-forming to cheap, reproducible biomass using environmentally protective, corrosion-free, inexpensive activator, prepare rich nitrogen, high-specific surface area, superior performance nitrating meso-porous carbon material.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of using oat as the nitrating porous carbon and its system of raw material
Preparation Method and application.
Background technique
Porous carbon materials refer to the carbon material with Different Pore Structures, and aperture can be carried out according to the requirement of practical application
Regulation makes its size be in nanometer level microporous between micron order macropore.Porous carbon materials have the property of carbon material, such as chemistry
Stability height, good conductivity, it is cheap the advantages that；Meanwhile the introducing of pore structure makes it while having than table and long-pending big, duct
The features such as structure-controllable, adjustable aperture.Porous carbon materials in gas separation, the purification of water, chromatography, catalysis and photocatalysis and
The fields such as energy stores are widely used.In addition, the study found that if suitably adulterating other members in porous carbon materials
Element, thus it is possible to vary the crystal structure and electronic structure of carbon material, to make its physics, chemical property better than common porous carbon materials
Material, expands its application potential in energy storage, conversion equipment.
Although the porous carbon of doping is since its excellent performance is increasingly interested by researchers, Traditional dopant is more
Hole carbon based on complicated organic synthesis, passes through under severe reaction conditions generally using expensive organic compound as raw material
High temperature cabonization preparation is crossed, although can also obtain preferable effect, step is complex, therefore is difficult to be commercially produced.
Biomass is the organic matter that plant is synthesized by photosynthesis, itself contains a large amount of cellulose, hemicellulose and lignin, is
Produce the extraordinary raw material of porous carbon.Porous carbon is prepared with this renewable resource low in cost, being available anywhere not only to solve
The problem of biomass disposition, and biomass is re-used, compared to by its directly burning, compost etc.
Reason has higher resource reclaim value.Biomass efficient is converted into biomass-based carbon material, there are wide development and utilization
Prospect.
The preparation of biomass carbon material is broadly divided into three kinds, is physical activation method, chemical activation method and physical chemistry respectively
Co-activating.Physical activation method, as activator, is had using the oxygen-containing gas such as vapor, flue gas, air or mixed gas
Activation temperature is high, and the time is long, the high disadvantage of energy consumption.Chemical activation method common chemical activating agent has alkali metal, alkaline-earth metal
Hydroxide and number acid, application it is more mature have KOH, ZnCl2、H3PO4It is that activator level is big, corrosion is set Deng, disadvantage
Standby, pollution environment, activator residual are difficult to remove.Physical chemistry co-activating rule is the combination of the two, but obviously do not change
Some inherent defects of kind physical activation method and chemical activation method.
Summary develops that environmentally protective, process is simple, low-cost to prepare nitrating mesoporous as it can be seen that using biomass as raw material
The method of carbon, which becomes, works as the next item down urgent problem to be solved.This patent mainly uses chemical activation method, and utilization is environmentally protective, without corruption
Erosion, inexpensive activator carry out activation pore-forming to cheap, reproducible biomass, prepare rich nitrogen, high-specific surface area, performance
Superior nitrating meso-porous carbon material.
Summary of the invention
Technical problem solved by the invention is to provide a kind of using oat as the nitrating porous carbon of raw material and its preparation side
Method and application solve and prepare the problems such as nitrating porous carbon is at high cost, process is complicated and environmental pollution is serious in the prior art.
Technical problem solved by the invention is realized using following technical scheme:
One aspect of the present invention discloses a kind of using oat as the preparation method of the nitrating porous carbon of raw material, including following step
It is rapid:
Step 1: oat is dry, and milled processed carries out heating stirring at powdered rear be added in dispersing agent, stirs evenly
After add activator and nitrogen source, continue heating stirring until being uniformly mixed, obtain presoma after drying；
Step 2: the presoma that step 1 obtains being calcined under atmosphere of inert gases, acid is carried out after calcining and is handled
To a kind of using oat as the nitrating porous carbon of raw material.
Preferably, the oat is the oat grain or oatmeal of decladding.
Preferably, the activator is calcium chloride, and the nitrogen source is urea.
Preferably, the mass ratio of the oat, the activator and the nitrogen source is 1:(1~4): (1~4).
Preferably, the dispersing agent is deionized water.
Preferably, the inert gas is N2。
Preferably, the temperature of the heating stirring is 80 DEG C, and drying temperature is 120 DEG C.
Calcine technology is used in the present invention, the parameter of calcine technology can all directly affect the nitrating porous carbon ultimately generated
Quality, parameter includes calcination temperature, heating rate and calcination time etc..In the present invention, it is preferred that temperature program when calcining
Are as follows: 700 DEG C~900 DEG C are warming up to the heating rate of 5~10 DEG C/min, calcination time is 1~3h.
It is furthermore preferred that temperature program when calcining are as follows: be warming up to 800 DEG C with the heating rate of 6 DEG C/min, calcination time is
2h。
Preferably, sour treatment process in the present invention are as follows: use inorganic acid pickling at normal temperature, the inorganic acid is hydrochloric acid, nitre
One of acid, sulfuric acid, the concentration of the inorganic acid are 0.5-2mol/L, and the purpose of acid processing is to remove to be produced in calcination process
Raw metal oxide, to obtain nitrating porous carbon.In actual production, acid processing after the completion of, also to be washed, filter and
Drying can just obtain nitrating porous carbon.
It is furthermore preferred that the concentration of the inorganic acid is 1-2mol/L, the acid processing time is 1-2 days.
The second aspect of the present invention discloses the above method and nitrating porous carbon using oat as raw material is prepared.
Third aspect of the present invention discloses above-mentioned using oat as nitrating porous carbon the answering in field of nanometer material technology of raw material
With.
Foregoing invention is with the following advantages or beneficial effects:
(1) at low cost；For the present invention using oat as raw material, this raw material is renewable resource, and cheap, distribution is wide
It is general, it is resourceful, it is environmentally protective.
(2) preparation method is simple；Preparation method of the invention is low to required equipment requirement, and yield is high, is suitable for rule
Modelling production.
(3) hole is big, large specific surface area；Preparation method of the invention uses urea as nitrogen source, passes through the work of urea
With making the nitrating porous carbon hole being prepared big, large specific surface area, while playing the role of nitrating.
(4) with high purity；The porous carbon surface of the nitrating that preparation method through the invention obtains does not have metallic particles, and table
Face has a large amount of folds.
(5) excellent capacitive property；Preparation method of the invention uses nitrating technology, with unitary system for porous carbon materials
Method is compared, and the electric double layer capacitance of the nitrating porous carbon of preparation method preparation of the invention is bigger, has superior capacitive character
Can, it has broad application prospects.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention
System.
Fig. 1 is scanning electron microscope (SEM) figure of nitrating porous carbon in embodiment 1；
Fig. 2 is the SEM figure of nitrating porous carbon in embodiment 3；
Fig. 3 is x-ray photoelectron spectroscopy (XPS) figure of nitrating porous carbon in embodiment 3；
Fig. 4 is energy spectrum analysis (EDS) figure of nitrating porous carbon in embodiment 3；
Fig. 5 is the nitrogen adsorption desorption curve of nitrating porous carbon in embodiment 3；
Fig. 6 is the graph of pore diameter distribution of nitrating porous carbon in embodiment 3；
Fig. 7 is the SEM figure of nitrating porous carbon in embodiment 4.
Fig. 8 is the cyclic voltammogram in embodiment 5.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments be only used for the present invention without
For limiting the scope of the invention.
Embodiment 1
The present embodiment prepares nitrating porous carbon materials by raw material of oat, successively proceeds as follows:
(1) by oat it is dry after, milled processed disperses the powdered oat of 2.0g in the deionized water of 40mL at powdered
In, stirring a hour is followed by added 4.0g calcium chloride and 4.0g urea, continues after stirring half an hour, dries at 120 DEG C
Case is drying for one day, obtains presoma；
(2) presoma is placed in high temperature process furnances, nitrogen is passed through with the rate of 100mL/min, with the heating of 6 DEG C/min
Rate is warming up to 700 DEG C, calcines 1h, cooled to room temperature, and grinding obtains black powder；
(3) black powder is put into the hydrochloric acid that 30mL substance withdrawl syndrome is 1mol/L, is stirred a hour, stand 1
It~2 days, washs, filters, the porous carbon obtained by drying prepared using oat as raw material.
The SEM of gained nitrating porous carbon contains a large amount of hole knot as shown in Figure 1, gained sample is the carbon material of sheet
Structure, there are a large amount of defect but no metallic particles on surface.
Embodiment 2
The present embodiment prepares nitrating porous carbon materials by raw material of oat, successively proceeds as follows:
(1) by oat it is dry after, milled processed disperses the powdered oat of 2.0g in the deionized water of 40mL at powdered
In, stirring a hour is followed by added 2.0g calcium chloride and 2.0g urea, continues after stirring half an hour, dries at 120 DEG C
Case is drying for one day, obtains presoma；
(2) presoma is placed in high temperature process furnances.It is passed through nitrogen with the rate of 100mL/min, with the heating of 8 DEG C/min
Rate is warming up to 800 DEG C, calcines 2h, cooled to room temperature, and grinding obtains black powder；
(3) black powder is put into the hydrochloric acid that 30mL substance withdrawl syndrome is 1mol/L, is stirred a hour, stand 1
It~2 days, washs, filters, the porous carbon obtained by drying prepared using oat as raw material.
Embodiment 3
The present embodiment prepares nitrating porous carbon materials by raw material of oat, successively proceeds as follows:
(1) by oat it is dry after, milled processed disperses the powdered oat of 2.0g in the deionized water of 40mL at powdered
In, stirring a hour is followed by added 4.0g calcium chloride and 4.0g urea, continues after stirring half an hour, dries at 120 DEG C
Case is drying for one day, obtains presoma；
(2) presoma is placed in high temperature process furnances.It is passed through nitrogen with the rate of 100mL/min, with the liter of 10 DEG C/min
Warm rate is warming up to 900 DEG C, calcines 3h, cooled to room temperature, and grinding obtains black powder；
(3) black powder is put into the hydrochloric acid that 15mL substance withdrawl syndrome is 1.5mol/L, is stirred a hour, stood
It 1~2 day, washs, filters, the porous carbon obtained by drying prepared using oat as raw material.
The SEM of gained nitrating porous carbon contains a large amount of hole knot as shown in Fig. 2, gained sample is the carbon material of sheet
Structure, there are a large amount of defect but no metallic particles on surface.XPS test result such as Fig. 3 of sample, as the result is shown sample surfaces master
Containing C, N, O element, and Ca the and Cl element being not detected in activator.This illustrates that remaining activator is acid washed thoroughly
It eliminates.Wherein N content is up to 12.36%, this illustrates that sample is mixed with a large amount of nitrogen.The body Xiang Yuan of EDS test sample
For element composition as shown in figure 4, sample body is mutually in addition to containing C, N outside O element, also contains micro Ca and Cl.This may be to have on a small quantity
CaCl2 by carbon coating, unpicked removal.Simultaneously it was noted that body phase nitrogen content is also up to 6.52%, this illustrates nitrogen not
It is only the surface for being mixed with porous carbon, is also mixed with inside it.The test of nitrogen adsorption desorption is as shown in figure 5, sample as the result is shown
For typical porous material, BET specific surface area is up to 1384.5m2/g.Further pore analysis such as Fig. 6, as the result is shown sample
Product are provided simultaneously with aperture, mesoporous and macropore, are a kind of porous carbon materials of hierarchical porous structure.
Embodiment 4
The present embodiment prepares nitrating porous carbon materials by raw material of oat, successively proceeds as follows:
(1) by oat it is dry after, milled processed disperses the powdered oat of 2.0g in the deionized water of 40mL at powdered
In, stirring a hour is followed by added 8.0g calcium chloride and 8.0g urea, continues after stirring half an hour, dries at 120 DEG C
Case is drying for one day, obtains presoma.
(2) presoma is placed in high temperature process furnances.It is passed through nitrogen with the rate of 100mL/min, with the heating of 5 DEG C/min
Rate is warming up to 800 DEG C, calcines 2h, cooled to room temperature, and grinding obtains black powder.
(3) black powder is put into the hydrochloric acid that 15mL substance withdrawl syndrome is 2mol/L, is stirred a hour, stand 1
It~2 days, washs, filters, the porous carbon obtained by drying prepared using oat as raw material, the quality of final product is.
The SEM of gained nitrating porous carbon contains a large amount of hole knot as shown in fig. 7, gained sample is the carbon material of sheet
Structure, there are a large amount of defect but no metallic particles on surface.
Embodiment 5
The nitrating porous carbon materials that embodiment 4 is obtained, in 6M KOH electrolyte, under the sweep speed of 100mv/s, benefit
Its specific capacitance is tested with cyclic voltammetry.Cyclic voltammetric result is as shown in figure 8, calculating its specific capacitance is 180F/g.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (10)
1. a kind of using oat as the preparation method of the nitrating porous carbon of raw material, which comprises the following steps:
Step 1: oat is dry, and milled processed carries out heating stirring at powdered rear be added in dispersing agent, after mixing evenly again
Activator and nitrogen source is added, continues heating stirring until being uniformly mixed, obtains presoma after drying；
Step 2: the presoma that step 1 obtains being calcined under atmosphere of inert gases, acid processing is carried out after calcining and obtains one
Kind is using oat as the nitrating porous carbon of raw material.
2. preparation method according to claim 1, which is characterized in that the activator is calcium chloride, and the nitrogen source is urine
Element.
3. preparation method according to claim 1, which is characterized in that the oat, the activator and the nitrogen source
Mass ratio is 1:(1~4): (1~4).
4. preparation method according to claim 1, which is characterized in that the dispersing agent is deionized water.
5. preparation method according to claim 1, which is characterized in that the inert gas is N2。
6. preparation method according to claim 1, which is characterized in that the temperature of the heating stirring is 80 DEG C, dry temperature
Degree is 120 DEG C.
7. preparation method according to claim 1, which is characterized in that in step 2, temperature program when calcining are as follows: with 5
The heating rate of~10 DEG C/min is warming up to 700 DEG C~900 DEG C, and calcination time is 1~3h.
8. preparation method according to claim 1, which is characterized in that in step 2, the sour treatment process: normal
Temperature is lower to use inorganic acid pickling, and the inorganic acid is one of hydrochloric acid, sulfuric acid, nitric acid, wherein the concentration of the inorganic acid is
0.5-2mol/L。
9. the nitrating porous carbon using oat as raw material is prepared in any one of -8 methods according to claim 1.
10. it is according to claim 9 using oat as the nitrating porous carbon of raw material field of nanometer material technology application.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299389A (en) * | 2020-09-23 | 2021-02-02 | 鸡西市唯大新材料科技有限公司 | Method for preparing sodium ion carbon negative electrode material by using nitrogen-doped porous biomass carbon |
| CN114105137A (en) * | 2021-11-04 | 2022-03-01 | 中欣环保科技有限公司 | Preparation method of composite super-capacitor carbon |
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| CN106006636A (en) * | 2016-05-19 | 2016-10-12 | 中国科学院青岛生物能源与过程研究所 | Biomass-based nitrogen-doped porous carbon material, and preparation method and application thereof |
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- 2018-11-08 CN CN201811325548.8A patent/CN109775704A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106006636A (en) * | 2016-05-19 | 2016-10-12 | 中国科学院青岛生物能源与过程研究所 | Biomass-based nitrogen-doped porous carbon material, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| JINGJIANG LIU ET AL: "Promising Nitrogen-Rich Porous Carbons Derived from One-Step Calcium Chloride Activation of Biomass-Based Waste for High Performance Supercapacitors", 《ACS SUSTAINABLE CHEM. ENG.》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299389A (en) * | 2020-09-23 | 2021-02-02 | 鸡西市唯大新材料科技有限公司 | Method for preparing sodium ion carbon negative electrode material by using nitrogen-doped porous biomass carbon |
| CN114105137A (en) * | 2021-11-04 | 2022-03-01 | 中欣环保科技有限公司 | Preparation method of composite super-capacitor carbon |
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