CN108502856A - A kind of green economy preparation method of two dimension carbonitride - Google Patents
A kind of green economy preparation method of two dimension carbonitride Download PDFInfo
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- CN108502856A CN108502856A CN201810614015.5A CN201810614015A CN108502856A CN 108502856 A CN108502856 A CN 108502856A CN 201810614015 A CN201810614015 A CN 201810614015A CN 108502856 A CN108502856 A CN 108502856A
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
Abstract
The invention discloses a kind of green economy preparation methods of two-dimentional carbonitride, include the following steps：Melamine and urea that molar ratio is 0.33 ~ 3 are mixed, deionized water is added and stirs evenly, adds or be not added with gaseous state remover, dry evaporating water in gained mixture；Dry gained powder is added in crucible, and crucible is placed in Muffle furnace, is warming up to 500 ~ 550 DEG C of 3 ~ 5 h of heat preservation, and then room temperature cools down, grind into powder；Powder is added deionized water and forms even suspension solution, and stripping additive, 2 ~ 8 h of sonic oscillation is added；6 ~ 12 h are stood after ultrasound, supernatant is then taken to be centrifuged in 3000 ~ 5000 rmp, are retained the supernatant after centrifugation and are stood；Supernatant is centrifuged in rotating speed for 10000 ~ 15000 rmp, after removing supernatant liquor, centrifugation substrate is added water washing, then freeze-drying obtains product.Of low cost, easy to operate, green non-pollution of the invention and it is easy to mass production.
Description
Technical field
The invention belongs to field of nanometer material technology, are related to a kind of green economy preparation method of two-dimentional carbonitride.
Background technology
Graphene is the two-dimensional slice material obtained from graphite stripping, and grinding of paying close attention to the most of scientific research personnel at present
Study carefully one of direction, has been widely used in industrial production and life.Two-dimentional azotized carbon nano sheet layer material have with
The similar structure of graphene is also gradually applied to energy conversion, photoelectric device and ring as two-dimensional semiconductor sheet layer material
The numerous areas such as border protection.The hexa-atomic piperazine ring of carbon atom list bridge knot is the basic structural unit of carbonitride, carbonitride single layer structure
Mainly constituted with the triazine ring of different polymerization degree and seven piperazine rings.The interlayer predominant intermolecular forces of carbonitride are interlayer hydrogen bond, Fan Dewa
Er Sili and π-π superpositions, therefore the interlaminar action power of carbonitride is compared with graphite layers active force bigger.The larger layer of carbonitride
Intermolecular forces are to prepare the huge obstruction of two-dimentional carbonitride sheet layer material, therefore the efficient two-dimentional carbonitride preparation method of exploration is
The difficult point of two dimension carbonitride research at present, and the widely applied huge bottleneck of the two-dimentional carbonitride of limitation.
As that studies two-dimensional material gos deep into, scientific research personnel has developed two dimension on the basis of graphene preparation method
The preparation method of carbonitride.The preparation method of two-dimentional carbonitride is broadly divided into stripping from top to bottom and prepares two plans from bottom to top
Slightly.Method is to be removed to body phase material, and rule is to utilize template forming from bottom to top from top to bottom（J Zhang, Y
Chen, X Wang, Energy Environ. Sci., 2015, 8(11), 3092）.Stripping method mainly has directly from top to bottom
Connect oxidizing process, liquid phase stripping method and oxidation-liquid phase stripping auxiliary law.Niu Ping et al. carries out carbonitride using directly thermal oxidation method
Stripping, as a result, it has been found that can obtain the less two-dimentional azotized carbon nano lamella of the number of plies using the method, but that there are yields is relatively low for the method
With the higher problem of cost（P Niu, L Zhang, G Liu and H M Cheng, Adv. Funct. Mater.,
2012, 22(22), 4763）.Xie Yi seminars also prepare ultra-thin two-dimension carbonitride using liquid phase stripping method, but this method
It needs to consume a large amount of organic solvents, it is very unfavorable to environmental ecology（X Zhang, X Xie, H Wang, J Zhang, B
Pan and Y Xie, J. Am. Chem. Soc., 2013, 135(1), 18）.The preparation method includes mainly mould from bottom to top
Plate assists synthetic method, hetero atom medium synthetic method and additive mediator method etc., and core is the template action in building-up process.
Wherein template has a gas phase soft template and solid phase antitemplate, the gas phase of the forming of solid phase template and gas phase template stripping in preparation process
Effect is the important link of the preparation method from bottom to top（M Wu, J M Yan, X N Tang, M Zhao and Q Jiang,Chemsuschem, 2015, 7(9), 2654）.Although the technology of preparing of two-dimentional carbonitride is more and more diversified, existing
Methods and techniques remain that can not to solve technique complicated in preparation process and high pollution, high cost and efficiency simultaneously low etc.
Key technical problem.
Invention content
It is an object of the invention to be directed to many deficiencies present in existing method, a kind of of low cost, operation letter is provided
The green economy preparation method of two-dimentional carbonitride that is single, environmentally safe and being easy to mass production.
A kind of green economy preparation method of two dimension carbonitride, it is characterised in that include the following steps：
1）Melamine and urea that molar ratio is 0.33 ~ 3 are mixed, deionized water is added and stirs evenly；
2）In step 1）Add or be not added with gaseous state remover, dry evaporating water in gained mixture；
3）By step 2）Dry gained powder is added in crucible, and it is 50 ~ 80% to keep the crucible filling rate of half opening state；
4）By step 3）Crucible be placed in Muffle furnace, 3 ~ 5 h are kept the temperature after being warming up to 500 ~ 550 DEG C, then room temperature cools down, and grinds
It clays into power（Few layer carbonitride）, for use；
5）By step 4）Middle powder is added deionized water and forms even suspension solution, and stripping additive is added, and then ultrasound is shaken
Swing 2 ~ 8 h；
6）6 ~ 12 h are stood after ultrasound, then take supernatant in 3000 ~ 5000 rmp（It is preferred that 3000 rmp）It centrifuges,
Retain the supernatant after centrifugation to stand；
7）By step 6）Supernatant rotating speed be 10000 ~ 15000 rmp（It is preferred that 15000 rmp）It centrifuges, removes upper layer
After clear liquid, centrifugation substrate is added into water washing, then freeze-drying obtains product.
Step 1）Described in melamine and urea molar ratio be 0.5 ~ 2；It is preferred that described in when aerating state remover
The molar ratio of melamine and urea is 1；The molar ratio of melamine and urea described in when being not added with gaseous state remover is 0.5.
Step 2）Described in gaseous state remover be ammonium chloride, at least one of sodium bicarbonate；The above solid is by thermal energy
It is decomposed into ammonia or carbon dioxide, a small amount of washable removal of solid residue also can guarantee and generate enough gas flow and impact force,
Carbonitride is enable to realize that gas phase is removed in the course of the polymerization process.
Step 2）Described in gaseous state remover additive amount and melamine mass ratio be 0 ~ 1.
Step 4）Described in heating rate be 3 ~ 5 DEG C/min.
Step 5）Described in even suspension solution concentration be 1 ~ 10 mg/mL.
Step 5）Described in stripping additive a concentration of 1 ~ 5 mg/mL.
Step 5）Described in stripping additive be Macrogol 600, neopelex and cetyl front three
At least one of ammonium chloride.
Step 5）Described in sonic oscillation be 6 h.
Compared with prior art, the present invention has the following advantages：
1）The present invention is less using the gas phase stripping preparation number of plies in heat polymerization process as presoma using melamine and urea
Carbonitride.Then, the stripping of remover ultrasound is added in water phase and further prepares two-dimentional carbonitride.Both disappearing for the energy had been reduced
Consumption, also avoids a series of use of organic solvents, green pollution-free.
2）The method that the present invention prepares two-dimentional carbonitride is based on stripping in situ and liquid phase removes two kinds of release effects, efficiently
Ground realizes carbonitride stripping at two-dimentional carbonitride, so that preparing for two-dimentional carbonitride is highly efficient quick.
3）Operating process of the present invention is simple, has the advantages that at low cost, easy popularization, is particularly suitable for large-scale industry life
Production.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of two-dimentional carbonitride（SEM schemes, 1 μm of scale）, wherein（a）For two-dimentional carbonitride lamella shape
Looks；（b）For two-dimentional carbonitride lamella fold pattern.
Fig. 2 is the transmission electron microscope picture of two-dimentional carbonitride（TEM schemes, 50 nm of scale）.
Fig. 3 is two-dimentional carbonitride character figure（Solid-state character and solution dispersed）.
Fig. 4 is two-dimentional carbonitride preparation efficiency and react initial molar ratio relational graph.
Specific implementation mode
Embodiment 1
Melamine and urea are sufficiently mixed for 1 in molar ratio, and deionized water is added and stirs evenly.Then mixed
Close the gaseous state remover NH being added in object with quality such as melamines4Cl, by the water in mixture in electric drying oven with forced convection
Divide and is evaporated completely.Dry powder is added in crucible, it is 50 ~ 80% to keep the crucible filling rate of half opening state, and crucible is set
In Muffle furnace, with the temperature programming of 3 DEG C/min heating rates to 550 DEG C, and 3 h are kept the temperature, sample room temperature natural cooling is used in combination
Mortar grinder is for use at powder.Sample powder is added deionized water and forms 2 mg/mL even suspension solution, and stripping addition is added
Agent hexadecyltrimethylammonium chloride makes its a concentration of 1 mg/mL in the solution, then 6 h of sonic oscillation.After ultrasound
6 h are stood, supernatant is then taken to be centrifuged in 3000 rmp, retains the supernatant after centrifugation and stands overnight.It will be above-mentioned upper
Clear liquid is centrifuged in rotating speed for 15000 rmp, after removing supernatant liquor, is added water washing multiple centrifugation substrate, is then freezed
It is dried to obtain product.The pattern of the two-dimentional carbonitride obtained by above method is as depicted in figs. 1 and 2, and preparation efficiency is
17.01%。
Embodiment 2
By " melamine and urea being sufficiently mixed for 1 in molar ratio, and deionized water is added and stirs in embodiment 1
It mixes uniformly." to change into " be 0.5 to be sufficiently mixed, and deionized water is added and stirs equal in molar ratio by melamine and urea
It is even.”.Then " the gaseous state remover NH with quality such as melamines will then be added in the mixture again4Cl, in electric heating air blast
The moisture in mixture is evaporated completely in drying box." change into " it is then added without any gaseous state remover in the mixture,
The moisture in mixture is evaporated completely in electric drying oven with forced convection.”.Other preparation conditions obtain two dimension with embodiment 1
Carbonitride, preparation efficiency 16.08%.
Embodiment 3
By in embodiment 1 " sample powder be added deionized water formed 2 mg/mL even suspension solution, and be added stripping addition
Agent hexadecyltrimethylammonium chloride makes its a concentration of 1 mg/mL in the solution, then 6 h of sonic oscillation." change " sample into
Powder is added deionized water and forms 2 mg/mL even suspension solution, and stripping additive hexadecyltrimethylammonium chloride is added,
Make its a concentration of 1 mg/mL in the solution, then 2 h of sonic oscillation.” .Other preparation conditions obtain two-dimentional nitrogen with embodiment 1
Change carbon, preparation efficiency 5.78%.
Embodiment 4
By " melamine and urea being sufficiently mixed for 1 in molar ratio, and deionized water is added and stirs in embodiment 1
It mixes uniformly." to change into " be 0.5 to be sufficiently mixed, and deionized water is added and stirs equal in molar ratio by melamine and urea
It is even.”.Then again by " sample powder is added deionized water and forms 2 mg/mL even suspension solution, and stripping additive ten is added
Six alkyl trimethyl ammonium chlorides make its a concentration of 1 mg/mL in the solution, then 6 h of sonic oscillation." change " sample powder into
Deionized water is added and forms 2 mg/mL even suspension solution, and stripping additive hexadecyltrimethylammonium chloride is added, makes it
A concentration of 1 mg/mL in the solution, then 4 h of sonic oscillation.”.Other preparation conditions obtain two-dimentional nitridation with embodiment 2
Carbon, preparation efficiency 9.0%.The two-dimentional carbonitride character such as Fig. 3 being prepared, is from left to right corresponding in turn to body phase nitrogen
Change carbon solid-state and dispersion liquid character, few layer carbonitride solid-state and dispersion liquid character, two-dimentional carbonitride solid-state and dispersion liquid character.It can
To find out that the reduction with the carbonitride number of plies, the solid-state and dispersion liquid color of carbonitride gradually become shallower as.And with the drop of the number of plies
Low, the time existing for dispersion stable gradually increases, two-dimentional carbonitride dispersion liquid can stablize at ambient temperature holding 7 days with
On.
Embodiment 5
By " melamine and urea being sufficiently mixed for 1 in molar ratio, and deionized water is added and stirs in embodiment 1
It mixes uniformly." to change into " be 0.5 to be sufficiently mixed, and deionized water is added and stirs equal in molar ratio by melamine and urea
It is even.”.Then again by " sample powder is added deionized water and forms 2 mg/mL even suspension solution, and stripping additive ten is added
Six alkyl trimethyl ammonium chlorides make its a concentration of 1 mg/mL in the solution, then 6 h of sonic oscillation." change that " sample powder adds into
Enter deionized water and form 2 mg/mL even suspension solution, and stripping additive neopelex is added, makes it in solution
In a concentration of 1 mg/mL, then 6 h of sonic oscillation.”.Other preparation conditions obtain two-dimentional carbonitride with embodiment 2, prepare
Efficiency is 7.83%.
Embodiment 6
In embodiment 2 " melamine and urea will be sufficiently mixed for 0.5 in molar ratio, and deionized water is added and stirs
It mixes uniformly." to change into " be 2 to be sufficiently mixed, and deionized water is added and stirs equal in molar ratio by melamine and urea
It is even.”.Other preparation conditions obtain two-dimentional carbonitride, preparation efficiency 4.43% with embodiment 2.In identical sonic oscillation
Between under, influence of the comparison initial reaction molar ratio to charge stripping efficiency, the results are shown in Figure 4.
Claims (10)
1. a kind of green economy preparation method of two dimension carbonitride, it is characterised in that include the following steps：
1）Melamine and urea that molar ratio is 0.33 ~ 3 are mixed, deionized water is added and stirs evenly；
2）In step 1）Add or be not added with gaseous state remover, dry evaporating water in gained mixture；
3）By step 2）Dry gained powder is added in crucible, and it is 50 ~ 80% to keep the crucible filling rate of half opening state；
4）By step 3）Crucible be placed in Muffle furnace, be warming up to 500 ~ 550 DEG C of 3 ~ 5 h of heat preservation, then room temperature cools down, and grinds
At powder, for use；
5）Step 4）Middle powder is added deionized water and forms even suspension solution, and stripping additive is added, then sonic oscillation 2
~8 h；
6）6 ~ 12 h are stood after ultrasound, supernatant is then taken to be centrifuged in 3000 ~ 5000 rmp, are retained upper after centrifugation
Clear liquid is stood；
7）Step 6）Supernatant rotating speed be 10000 ~ 15000 rmp centrifuge, remove supernatant liquor after, substrate will be centrifuged
Add water washing, then freeze-drying obtains product.
2. preparation method as described in claim 1, it is characterised in that step 1）Described in melamine and urea mole
Than being 0.5 ~ 2.
3. preparation method as claimed in claim 2, it is characterised in that melamine and urea described in when aerating state remover
Molar ratio be 1；The molar ratio of melamine and urea described in when being not added with gaseous state remover is 0.5.
4. preparation method as described in claim 1, it is characterised in that step 2）Described in gaseous state remover additive amount and three
The mass ratio of poly cyanamid is 0 ~ 1.
5. preparation method as described in claim 1 or 4, it is characterised in that step 2）Described in gaseous state remover be chlorination
At least one of ammonium, sodium bicarbonate.
6. preparation method as described in claim 1, it is characterised in that step 4）Described in heating rate be 3 ~ 5 DEG C/min.
7. preparation method as described in claim 1, it is characterised in that step 5）Described in even suspension solution concentration be 1 ~
10 mg/mL；A concentration of 1 ~ 5 mg/mL of the stripping additive.
8. preparation method as claimed in claim 1 or 7, it is characterised in that step 5）Described in stripping additive be poly- second two
At least one of alcohol 600, neopelex and hexadecyltrimethylammonium chloride.
9. preparation method as described in claim 1, it is characterised in that step 5）Described in the sonic oscillation time be 6 h.
10. preparation method as described in claim 1, it is characterised in that step 6）Described in centrifugation rotating speed 3000
Rmp is carried out；Step 7）Described in the rotating speed that centrifuges be 15000 rmp.
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Cited By (4)
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| CN109652160A (en) * | 2019-01-25 | 2019-04-19 | 中国科学院兰州化学物理研究所 | A kind of preparation method of water solubility carbonitride original position water base lubricant |
| CN112774714A (en) * | 2021-01-27 | 2021-05-11 | 江苏大学 | MgAl LDO/nitrogen vacancy carbon nitride based photocatalyst, preparation method and application |
| CN113929197A (en) * | 2021-09-23 | 2022-01-14 | 重庆大学 | Method for treating organic wastewater by activating peroxymonosulfate under assistance of visible light |
| CN114956016A (en) * | 2022-05-24 | 2022-08-30 | 南京林业大学 | Preparation method of triazine-heptazine-based carbon nitride and triazine-heptazine-based carbon nitride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109652160A (en) * | 2019-01-25 | 2019-04-19 | 中国科学院兰州化学物理研究所 | A kind of preparation method of water solubility carbonitride original position water base lubricant |
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| CN114956016A (en) * | 2022-05-24 | 2022-08-30 | 南京林业大学 | Preparation method of triazine-heptazine-based carbon nitride and triazine-heptazine-based carbon nitride |
| CN114956016B (en) * | 2022-05-24 | 2023-10-24 | 南京林业大学 | Preparation method of triazine-heptazinyl carbon nitride and triazine-heptazinyl carbon nitride |
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Application publication date: 20180907 |