CN107840322A - A kind of method for preparing nitrogenous grapheme material using chitosan for raw material - Google Patents
A kind of method for preparing nitrogenous grapheme material using chitosan for raw material Download PDFInfo
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- CN107840322A CN107840322A CN201710767152.8A CN201710767152A CN107840322A CN 107840322 A CN107840322 A CN 107840322A CN 201710767152 A CN201710767152 A CN 201710767152A CN 107840322 A CN107840322 A CN 107840322A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention discloses a kind of method for preparing nitrogenous grapheme material using chitosan for raw material.This method is by chitosan in N2400-900 DEG C is warming up under atmospheric condition, is incubated 0.5~2 hour；25~35 DEG C then are slowly dropped to, obtains pre- carbonized product；The pre- carbonized product of gained is mixed with regulation and control agglomerator, pre- carbonized product is 1 with regulation and control agglomerator weight ratio：1~4, in N2400~500 DEG C are warming up under atmospheric condition, is incubated 1~2 hour；Continue to be warming up to 900~1100 DEG C, be incubated 0.5~2 hour, be then slowly dropped to room temperature, obtain nitrogenous chitosan graphene.Nitrogenous graphene prepared by the present invention, each peak of D, G and 2D is unimodal in Raman collection of illustrative plates；Preparation technology of the present invention is simple to operate, avoids and largely uses the concentrated sulfuric acid, it is not necessary to additionally adds nitrogen source material, therefore preparation cost is cheap, safety and environmental protection；The achievable continuous industrial production of the present invention.
Description
Technical field
The present invention relates to nitrogenous graphene, and nitrogenous graphene is prepared using serial chitosan for raw material more particularly to one kind
The method of material, belong to nitrogenous field of preparation of graphene.
Background technology
Graphene has excellent electric conductivity, larger specific surface area and high heat/change as a kind of new carbon
The features such as learning stability, the electrode material as fuel cell is by extensive concern.Carrying out N doping to graphene can be effective
Its Surface structure and property of ground modulation, so that the nitrogenous graphene of generation shows the performance more excellent than pure graphene and more
Wide application prospect.Typically with native graphite (G) for raw material, aniline is nitrogenous precursor, using Hummers methods, original position
Trigger aniline polymerization and be prepared for nitrogen-doped graphene (N-G) [tight auspicious brightness *, illiteracy crape myrtle, Lee in the heat treatment of nitrogen high temperature
Dimension is brave, Liu Jia；Nitrogen-doped graphene be used for alkaline fuel cell production hydrogen peroxide, modern chemical industry, the 5th phase of volume 2017,37,
62-66].On the one hand nitrogen modification to grapheme material can improve the chemical inertness on surface, there is provided may participate in catalytic reaction
Avtive spot.On the other hand, the electronic structure of carbon surface can be changed, improving electric conductivity, [Zhao Wei virtue Guo Meng common vetch Zhu Zhen great waves are perhaps beautiful
The Chen Zhi Cao Jian fine jade；One step pyrolysis synthesis nitrogen-doped graphene carries cobalt nanometer particle and its electrocatalysis to oxygen reduction reaction
Can, New Chemical Materials, the 5th phase of volume 2017,45,84-89].Also have using natural flake graphite as raw material, use is improved
Hummers methods are prepared for graphene oxide (GO), be then reducing agent using GO as carbon source, hydrazine hydrate, ammoniacal liquor be nitrogen source, use hydro-thermal
[neat sub- pretty young woman official repaiies handsome Xu Dong slopes Xu Li and appoints snowy peaks the nitrogenous graphene (N-G) that method is prepared for having different electro catalytic activities；Nitrating
The preparation of graphene and its electro catalytic activity of modified electrode, New Chemical Materials, the 4th phase of volume 2017,45,44-46].
Industrialize nitrogenous graphene product and can not meet specific demand of the various application fields to nitrogenous graphene, serious resistance
Nitrogenous graphene high-performance, the large-scale application of high added value are hindered.Secondly, the modified Hummers methods production of graphite powder contains
During nitrogen graphene, in addition to using nitrogen source material, substantial amounts of acid waste water can be produced by producing nitrogenous graphene product process
Huge pollution is caused to environment, if will necessarily using caused waste water in traditional method of wastewater treatment processing production process
Consume huge manpower and financial resources cost so that nitrogenous graphene holds at high price, and seriously hinders nitrogenous graphene
Large-scale application and popularization.Only develop green nitrogenous graphene production technology, can just be effectively reduced nitrogenous stone
The production cost of black alkene, the development of nitrogenous graphene industrialized production is promoted rapidly.
The content of the invention
The object of the present invention is to overcome the problems of the prior art, there is provided a kind of cost is low, safety and environmental protection, is producing
During without using the concentrated sulfuric acid, high efficiency prepares the side of nitrogenous grapheme material using resourceful natural nitrogenous chitosan
Method, the nitrogenous graphene of gained are sandwich construction.
Chitin (β-(Isosorbide-5-Nitrae) -2- acetylaminohydroxyphenylarsonic acids 2-deoxy-D-glucose) is the nitrogenous organic of quantity maximum on the earth
One of compound, is primarily present in arthropod such as shrimp, crab etc. in nature, and chitosan (Chitosan) is also known as deacetylated several
Ding Zhi, poly glucosamine, soluble chitin and Flonac N, become by chitin through deacetylation conversion
Molecular weight is 12~590,000 large biological molecule.Chemical entitled poly- (the 1,4) -2- amino -2- deoxidation-β-D- Portugals of chitosan gather
Sugar, because deacetylation not exclusively usually contains two kinds of structure lists of 2- acetylglucosamines and 2- Glucosamines in its strand
Member, both ratios are different with degree of deacetylation [He Lijian, to discard shrimp, crab shell prepares chitosan craft discussion, Xiamen section
Skill, 2014,2,38-45].As the natural macromolecular material of function admirable, the research of chitin development of resources and application by
The extensive attention of external, domestic scholars and business circles.Its scope applied has been directed to industry, agricultural, medical and health, dailyization
The various fields such as work, food, environmental protection [Qi Aijiu, Li Wanhai, Wang Hong, Guo Jinghai, Li Qiang, Dong Shi, Meng Xianyong；By shrimp and crab shells system
Take natural macromolecule flocculating agent chitosan, Jilin Institute of Chemical Technology journal, 2006, the 1st phase of volume 23,15-18].But by series
The method that chitosan is prepared into nitrogenous grapheme material has no report.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for preparing nitrogenous grapheme material using chitosan for raw material, comprises the following steps：
1) by chitosan in N2400-900 DEG C is warming up under atmospheric condition, is incubated 0.5~2 hour；Then it is slowly dropped to 25
~35 DEG C, obtain pre- carbonized product；
2) pre- carbonized product obtained by step 1) is mixed with regulation and control agglomerator, pre- carbonized product and regulation and control agglomerator weight ratio
For 1：1~4, in N2400~500 DEG C are warming up under atmospheric condition, is incubated 1~2 hour；Continue to be warming up to 900~1100 DEG C, protect
Temperature 0.5~2 hour, is then slowly dropped to room temperature, obtains nitrogenous chitosan graphene；The regulation and control agglomerator is Al (NO3)3﹑
KOH and Zn (NO3)2In one or more.
Further to realize the object of the invention, it is preferable that the chitosan is viscosity 200mPa.s low viscosity Ke Ju Tang ﹑
Viscosity 200-400mPa.s middle viscosity Ke Ju Tang ﹑ viscosity 100-200mpa.s chitosan, viscosity>400mPa.s
High-viscosity chitosan or carboxyl chitosan BR.Acetyl group be present containing part in chitosan of the present invention, the present invention selects
Chitosan >=95%.Chitin molecule formula is β-(Isosorbide-5-Nitrae) -2- acetylaminohydroxyphenylarsonic acid 2-deoxy-D-glucoses, chitosan
Molecular formula is Chitosan (1-4) -2- amino-B-D glucose；Chitosan is chitin deacetylation product, deacetylation
Purpose be water-soluble in order to increase its；The acetyl group in chitin is sloughed and how much can determined simultaneously.
Preferably, it is described be warming up to 400-500 DEG C control programming rate be 0.5~1.0 DEG C/min；It is described to continue to heat up
It is 3.0~5.0 DEG C/min to control programming rate to 900~1100 DEG C.
Preferably, step 1) is described is slowly dropped to be slowly dropped to room temperature control cooling rate described in 25~35 DEG C and step 2)
For 3~5 DEG C/min.
Preferably, the step 1) chitosan is dry chitosan；Dry chitosan also includes crushing, and crushed 50
~100 mesh sieves.
Preferably, described cool to after room temperature of step 2) also includes taking out material, and eluant, eluent, cleaning are used as by the use of deionized water
For neutrality, washed repeatedly with absolute ethyl alcohol, 60-70 DEG C of drying.
Preferably, step 1) it is described by chitosan in N2It is in N by chitosan that 400-900 DEG C is warming up under atmospheric condition2Gas
Under the conditions of atmosphere, it is placed in tube furnace, is warming up to 400-900 DEG C；Step 2) is described in N2400~500 are warming up under atmospheric condition
DEG C it is in N2Under atmospheric condition, it is placed in tube furnace, is warming up to 400~500 DEG C.
Preferably, the specific surface area of the nitrogenous graphene of chitosan obtained by step 2) is 1785~2469m2/g；Chitosan contains
The D ﹑ G and 2D peaks of the Raman spectrum of nitrogen graphene are unimodal；And D/G is 0.9~0.6；The peak of PXRD collection of illustrative plates 002 and 100 is clear
It can debate.
Compared with prior art, the present invention has the advantage that：
(1) chitosan (Chitosan) is natural nitrogenous organic polymer, and high efficiency of the present invention utilizes resourceful shell
Glycan prepares nitrogenous graphene, reduces pollution environment；Preparation method of the present invention not only avoid to be needed using in oxidation-reduction method
Use the substantial amounts of concentrated sulfuric acid so that a large amount of discharge of wastewater, Wu dye Huan Jing ﹑ avoided under commercial production conditions blast danger and
Increase production cost, and reduce addition nitrogen source goods and materials technical process；
(2) the nitrogenous graphene of serial chitosan for preparing of the present invention, D/G ＜ 1, and each peaks of 2D are into unimodal, it is meant that shell
The nitrogenous graphene of glycan is sandwich construction；Nitrogenous quality of graphene is improved under commercial production conditions, is that downstream product is (conductive
Carbon pastes, graphene battery, lightweight bulletproof clothing etc.) quality assurance is provided；
(3) the nitrogenous graphene of serial chitosan prepared by the present invention, specific surface area is (1785~2469m2/ g), this and reason
By the graphene specific surface area (2620m of prediction2/ g) it is close, further prove the nitrogenous graphite of serial chitosan produced by the present invention
Alkene, ensure the quality of nitrogenous graphene.The nitrogenous graphene of serial chitosan can be made, turn into the useful electronic material of electronics industry.
Brief description of the drawings
Fig. 1 is the Raman collection of illustrative plates of the products therefrom of embodiment 1.
Embodiment
To more fully understand the present invention, below in conjunction with the accompanying drawings and embodiment is described further to this present invention, but this
The embodiment of invention is unlimited so.
Embodiment 1
It is the method that raw material prepares nitrogenous grapheme material using low viscosity chitosan, comprises the following steps：
By chitosan：Low viscosity 200mPa.s (Aladdin) crosses 50 mesh sieves, obtains low viscosity Chitosan powder；In N2Atmosphere
Under the conditions of, low viscosity Chitosan powder is placed in corundum tube furnace.It is 1.0 DEG C/min to 400 DEG C to control programming rate, is protected
Temperature 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 800 DEG C, is incubated 1 hour, cooling rate control
For 5 DEG C/min, room temperature is slowly cooled to, obtains the pre- carbonized product of low viscosity chitosan；
The pre- carbonized product of 5 grams of low viscosity chitosans and 5 grams of potassium hydroxide mixing are weighed, then adds deionized water dissolving.
Stirring, 80 DEG C of dryings, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.It is 1.0 to control programming rate
DEG C/min, 800 DEG C are warming up to, is incubated 2 hours；Continue to heat up, it is 3.0 DEG C/min to control programming rate, is warming up to 1100 DEG C
Insulation 0.5 hour, room temperature is cooled to, cooling rate control is 5 DEG C/min, and room temperature takes out sample, is washed with watery hydrochloric acid, deionization
Water is as cleaning solution, until cleaning fluid is neutrality, wash 3 times with absolute ethyl alcohol, is dried at 60 DEG C.
After tested, products therefrom specific surface area is：1758m2/g；Raman collection of illustrative plates is shown in accompanying drawing [instrument title as shown in Figure 1：
Micro-Raman spectroscopy, model：LabRAM Aramis manufacturers：French H.J.Y companies], Fig. 1 is a Raman complete graph
Spectrum, D, G and 2D are unimodal, meet the expression of graphite Raman collection of illustrative plates.The present embodiment PXRD high-visible 002 and 100 peaks,
HRTEM can be recognized；Lattice is away from respectively：0.32nm and 0.23nm.
It can be seen from figure 1 that in the present embodiment, in Fig. 1, D/G ＜ 1, D/G ＞ 0.38, and also 2D peaks are unimodal, low viscosity shell gathers
Sugar is the nitrogenous graphene of multilayer, relative to Dan Yuan ﹑ graphite powders be raw material prepare nitrogenous graphene, simple production process, peace
Loopful is protected；The quality of downstream product can be above ensure that in application.
Embodiment 2
By chitosan：Middle viscosity 200-400mPa.s (Aladdin) crosses 100 mesh sieves, viscosity Chitosan powder in acquisition；
N2Under atmospheric condition, middle viscosity Chitosan powder is placed in tube furnace.It is 0.5 DEG C/min to control programming rate, is warming up to
500 DEG C, it is incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 1000 DEG C, is incubated 1 hour, slowly
Room temperature is cooled to, cooling rate control is 5 DEG C/min, the pre- carbonized product of viscosity chitosan in acquisition；
Weigh the pre- carbonized product of viscosity chitosan and 5 grams of Al (NO in 5 grams3)3Mixing, then adds deionized water dissolving.Stir
Mix, 90 DEG C of dryings, remove water；Mixed again with 5 grams of KOH, add deionized water dissolving.Stirring, 90 DEG C of dryings, removes water；It is remaining
Thing is in N2Under atmospheric condition, it is placed in tube furnace.It is 0.5 DEG C/min to control programming rate, is warming up to 500 DEG C, insulation 1
Hour；Continue to heat up, it is 3.0 DEG C/min to control programming rate, is warming up to 1100 DEG C, is incubated 1 hour, slowly cools to room temperature,
Cooling rate control is 5 DEG C/min, and room temperature takes out sample, by the use of watery hydrochloric acid and deionized water as eluant, eluent, until cleaning fluid is
Neutrality, washed 3 times with absolute ethyl alcohol, in 60 DEG C of drying.After tested, products therefrom specific surface area is：1876m2/ g, Raman collection of illustrative plates
It is identical with Fig. 1, determined with micro-Raman spectroscopy, LabRAM Aramis productions, French H.J.Y companies.
Embodiment 3
By chitosan：Deacetylated >=95%, viscosity 100-200mpa.s (Aladdin) crosses 50 mesh sieves, obtains deacetylated shell and gathers
Icing Sugar end；In N2Under atmospheric condition, chitosan powder is placed in tube furnace.It is 1.0 DEG C/minute to control programming rate
Clock, 500 DEG C are warming up to, are incubated 2 hours；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 900 DEG C, insulation 1
Hour, room temperature is slowly cooled to, cooling rate control is 5 DEG C/min, obtains the pre- carbonized product of chitosan；
Weigh the pre- carbonized product of 5 grams of chitosans and 10 grams of Zn (NO3)2Mixing, then adds deionized water dissolving.
Stirring dries 80 DEG C, removes water；Mixed again with 5 grams of KOH, add deionized water dissolving.Stirring, 90 DEG C of dryings, removes water；It is remaining
Thing is in N2Under atmospheric condition, it is placed in tube furnace.It is 1.0 DEG C/min to control programming rate, is warming up to 500 DEG C, insulation 1
Hour；Continue to heat up, it is 3.0 DEG C/min to control programming rate, is warming up to 1000 DEG C, is incubated 0.5 hour, slowly cools to room
Temperature, cooling rate control are 5 DEG C/min, and room temperature takes out sample, and by the use of deionized water as eluant, eluent, cleaning fluid is neutrality, with nothing
Water-ethanol washs 3 times, in 60 DEG C of drying.Specific surface area is：2087m2/ g, Raman collection of illustrative plates are determined with micro-Raman spectroscopy, [type
Number：LabRAM Aramis manufacturers：French H.J.Y companies], same Fig. 1 of Raman collection of illustrative plates obtained by the present embodiment.
Embodiment 4
By chitosan：High viscosity>400mPa.s (Aladdin) crosses 100 mesh sieves, obtains high-viscosity chitosan powder；In N2Gas
Under the conditions of atmosphere, it is placed in tube furnace.It is 1.0 DEG C/min to control programming rate, is warming up to 500 DEG C, is incubated 2 hours；Continue to rise
Temperature, it is 5.0 DEG C/min to control programming rate, is warming up to 1050 DEG C, is incubated 1 hour, slowly cools to room temperature, cooling rate control
5 DEG C/min are made as, obtains the pre- carbonized product of high-viscosity chitosan；
Weigh 5 grams of pre- carbonization high-viscosity chitosan carbon and 5 grams of Al (NO3)3Mixing, then adds deionized water dissolving.Stirring
90 DEG C are dried, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.It is 1.0 DEG C/minute to control programming rate
Clock is incubated 2 hours to 500 DEG C；Continuing to heat up, it is 5.0 DEG C/min that heating, which controls speed, is warming up to 1100 DEG C, is incubated 1 hour,
Room temperature is slowly cooled to, cooling rate control is 5 DEG C/min, and room temperature takes out sample, and elution is used as by the use of diluted acid and deionized water
Agent, until cleaning fluid for neutrality, wash 3 times with absolute ethyl alcohol, 60 DEG C dry.After testing, products therefrom specific surface area is：
2489m2/ g, the same Fig. 1 of Raman collection of illustrative plates, Raman collection of illustrative plates are determined with micro-Raman spectroscopy, [model：LabRAM Aramis factories
Family：French H.J.Y companies].
Embodiment 5：
By chitosan：Carboxylation BR (Aladdin) crosses 100 mesh sieves, obtains carboxyl chitosan BR powder；In N2Under atmospheric condition,
Carboxyl chitosan BR powder is placed in tube furnace.It is 0.5 DEG C/min to control programming rate, is warming up to 500 DEG C, insulation 2 is small
When；Continue to heat up, it is 5.0 DEG C/min to control programming rate, is warming up to 900 DEG C, is incubated 1 hour, slowly cools to room temperature, is dropped
Warm speed control is 5 DEG C/min, obtains the pre- carbonized products of carboxyl chitosan BR；
Weigh 5 grams of pre- carbonized products of carboxyl chitosan BR (pre- carbonization carboxyl chitosan BR) and 5 grams of Zn (NO3)2Mixing, so
After add deionized water dissolving.Stirring dries 90 DEG C, removes water, residue is in N2Under atmospheric condition, it is placed in tube furnace.
It is 1.0 DEG C/min to control programming rate, is warming up to 500 DEG C, is incubated 2 hours；Continue to heat up, control programming rate for 3.0 DEG C/
Minute, 900 DEG C are warming up to, is incubated 1 hour, slowly cools to room temperature, cooling rate control is 5 DEG C/min, and room temperature takes out sample
Product, it is neutrality by the use of deionized water as eluant, eluent, cleaning fluid, is washed 3 times with absolute ethyl alcohol, in 60 DEG C of drying.Specific surface area is：
2286m2/ g, the same Fig. 1 of Raman collection of illustrative plates, Raman collection of illustrative plates are determined with micro-Raman spectroscopy, [model：LabRAM Aramis factories
Family：French H.J.Y companies].
It is substantial amounts of acid relative to the oxidation-reduction method used with the nitrogenous graphene that graphite powder and nitrogen source are raw material preparation
Waste water causes huge pollution to environment, and must using caused waste water in traditional method of wastewater treatment processing production process
Huge manpower and financial resources cost can so be consumed so that nitrogenous graphene holds at high price, and seriously hinders nitrogenous graphite
The large-scale application of alkene and popularization.The invention provides the preparation method of the new nitrogenous graphene of serial chitosan, the present invention contains
The preparation method of nitrogen graphene not only avoid using needing to use the substantial amounts of concentrated sulfuric acid in oxidation-reduction method so that a large amount of waste water
Discharge, environment is polluted, while danger and the increase production cost of blast are also avoided under commercial production conditions, and the present invention
Production process reduces addition nitrogen source goods and materials technique.
The present invention realizes the preparation that serial chitosan is useful electronic material.Prepared by the serial chitosan of the present invention contains
Nitrogen graphene, D/G ＜ 1, and 2D peaks are into unimodal；It is sandwich construction that the present invention prepares nitrogenous graphene with serial chitosan, this
The nitrogenous graphene that invention obtains can be used for conductive carbon paste, ultracapacitor, the electrode material of lithium ion battery, can also add
Into resin, rubber, the physical property of reinforced resin, rubber etc..
Simple production process of the present invention, cost is cheap, safety and environmental protection, it is possible to achieve continuous industrial production, has wide
Market application foreground.
Claims (8)
- A kind of 1. method for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that comprise the following steps：1) by chitosan in N2400-900 DEG C is warming up under atmospheric condition, is incubated 0.5~2 hour；Then it is slowly dropped to 25~35 DEG C, obtain pre- carbonized product；2) pre- carbonized product obtained by step 1) is mixed with regulation and control agglomerator, pre- carbonized product is 1 with regulation and control agglomerator weight ratio： 1~4, in N2400~500 DEG C are warming up under atmospheric condition, is incubated 1~2 hour；Continue to be warming up to 900~1100 DEG C, insulation 0.5~2 hour, room temperature is then slowly dropped to, obtains nitrogenous chitosan graphene；The regulation and control agglomerator is Al (NO3)3﹑ KOH With Zn (NO3)2In one or more.
- 2. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that The chitosan is viscosity 200mPa.s low viscosity Ke Ju Tang ﹑ viscosity 200-400mPa.s middle viscosity Ke Ju Tang ﹑ viscosity 100-200mpa.s chitosan, viscosity>400mPa.s high-viscosity chitosan or carboxyl chitosan BR.
- 3. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that It is described be warming up to 400-500 DEG C control programming rate be 0.5~1.0 DEG C/min；It is described to continue to be warming up to 900~1100 DEG C of controls Programming rate processed is 3.0~5.0 DEG C/min.
- 4. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that Step 1) is described to be slowly dropped to be slowly dropped to room temperature described in 25~35 DEG C and step 2) to control cooling rate to be 3~5 DEG C/min.
- 5. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that Step 1) the chitosan is dry chitosan；Dry chitosan also includes crushing, and crushed 50~100 mesh sieves.
- 6. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that Described cools to after room temperature of step 2) also includes taking out material, by the use of deionized water as eluant, eluent, cleans as neutrality, with anhydrous second Alcohol washing is multiple, 60-70 DEG C of drying.
- 7. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that Step 1) it is described by chitosan in N2It is in N by chitosan that 400-900 DEG C is warming up under atmospheric condition2Under atmospheric condition, pipe is placed in In formula stove, 400-900 DEG C is warming up to；Step 2) is described in N2It is in N that 400~500 DEG C are warming up under atmospheric condition2Atmospheric condition Under, it is placed in tube furnace, is warming up to 400~500 DEG C.
- 8. the method according to claim 1 for preparing nitrogenous grapheme material using chitosan for raw material, it is characterised in that The specific surface area of the nitrogenous graphene of chitosan is 1785~2469m obtained by step 2)2/g；The Raman light of the nitrogenous graphene of chitosan The D ﹑ G and 2D peaks of spectrum are unimodal；And D/G is 0.9~0.6；The peak of PXRD collection of illustrative plates 002 and 100 can clearly debate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111686761A (en) * | 2020-05-20 | 2020-09-22 | 华南理工大学 | Cu/CdS/graphene composite photocatalyst and preparation method and application thereof |
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| CN103922328A (en) * | 2014-04-18 | 2014-07-16 | 山东大学 | Method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan |
| CN105417533A (en) * | 2015-12-22 | 2016-03-23 | 北京理工大学 | Preparation method for graphene with high specific surface area |
| CN105502359A (en) * | 2015-12-22 | 2016-04-20 | 福州大学 | Preparation method of low-cost porous graphene |
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- 2017-08-31 CN CN201710767152.8A patent/CN107840322A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103922328A (en) * | 2014-04-18 | 2014-07-16 | 山东大学 | Method for preparing nitrogenous hierarchical pore three-dimensional graphene by using chitosan |
| CN105417533A (en) * | 2015-12-22 | 2016-03-23 | 北京理工大学 | Preparation method for graphene with high specific surface area |
| CN105502359A (en) * | 2015-12-22 | 2016-04-20 | 福州大学 | Preparation method of low-cost porous graphene |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111686761A (en) * | 2020-05-20 | 2020-09-22 | 华南理工大学 | Cu/CdS/graphene composite photocatalyst and preparation method and application thereof |
| CN111686761B (en) * | 2020-05-20 | 2021-08-10 | 华南理工大学 | Cu/CdS/graphene composite photocatalyst and preparation method and application thereof |
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