CN109046422A - A kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof - Google Patents
A kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof Download PDFInfo
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- CN109046422A CN109046422A CN201810836984.5A CN201810836984A CN109046422A CN 109046422 A CN109046422 A CN 109046422A CN 201810836984 A CN201810836984 A CN 201810836984A CN 109046422 A CN109046422 A CN 109046422A
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- carbon nitride
- class graphite
- phase carbon
- graphite phase
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 26
- 239000010439 graphite Substances 0.000 title claims abstract description 26
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 10
- 229920000877 Melamine resin Polymers 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 9
- 239000005416 organic matter Substances 0.000 claims description 7
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 7
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims 2
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 238000001354 calcination Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229960000789 guanidine hydrochloride Drugs 0.000 description 1
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
Abstract
The present invention relates to a kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof.The g-C prepared3N4With laminar structured.Present invention process process is simple, and raw material sources are extensive, and product is easily prepared, reproducible, and by controlling graphite type carbon nitride well-crystallized, the purity is high that calcination temperature is prepared, yield is big, and preparation efficiency is high.Products obtained therefrom is not only suitable for further preparing experiment synthesis and the performance study of magnanimity high density nitridation carbon phase as precursor, can also obtain visible light catalyst, further expand its application range by metal ion-modified.
Description
Technical field
The present invention relates to a kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof belongs to material preparation
And energetic material technical field.
Background technique
Graphite phase carbon nitride is concerned as a kind of emerging important organic polymer catalysis material；There is reality
Verifying is real, and graphite phase carbon nitride has good in terms of organic pollutant degradation, water decomposition and photocatalysis carbon dioxide reduction
Effect, photocatalysis field with good application prospect.
The carbonitride capability and performance that existing carbonitride preparation method is prepared is unstable, is easy to that quality fluctuation occurs,
Crystallinity, purity etc. are not satisfactory, need to be improved.
Summary of the invention
The present invention is in view of the foregoing drawbacks, and it is an object of the present invention to provide a kind of process flow is simple, raw material sources are extensive, product is easy to
A kind of sheet class graphite phase carbon nitride g-C of preparation3N4Material and preparation method thereof.
Thus the technical solution adopted by the present invention is that: a kind of sheet class graphite phase carbon nitride g-C3N4Material is prepared
g-C3N4With laminar structured.
A kind of sheet class graphite phase carbon nitride g-C3N4The preparation method of material during the preparation process will be after ball milling
Amino-containing organic matter predecessor prepared by the way of repeatedly roasting, maturing temperature successively improves preparation.
A kind of sheet class graphite phase carbon nitride g-C3N4The preparation method of material, comprising the following steps:
(1) amino-containing organic matter predecessor is added in ball mill, abundant ball milling;
(2) predecessor after ball milling is taken to roast at a certain temperature;
(3) obtained solid in step (2) washed, dried;
(4) by gained drying solid in step (3), improve after temperature that roasting must there can be sheet class graphite-phase to nitrogenize again
Carbon g-C3N4。
Amino-containing organic matter predecessor in step (1) is selected from cyanamide, dicyandiamide, melamine, cyanuric acid sulphur
At least one of urea, guanidine hydrochloride and urea.
Ball-milling Time in step (1) is 0.5-10 hours.
Predecessor is 370-410 DEG C in the temperature of Muffle kiln roasting after step (2) ball milling, and the time is 0.25-12 hours.
Solid in step (3) is 5-50 g, is washed using second alcohols solvent, and second alcohols solvent is 50-500 ml；
The dosage of two kinds of substances zooms in or out in proportion according to above-mentioned content.
Washing times in step (3) are 2-6 times, and drying temperature is 105 DEG C.
Drying solid in step (4) is 510-610 DEG C in the temperature of Muffle kiln roasting, and the time is 0.25-12 hours.
In step (2) and (4) sample the atmosphere of Muffle kiln roasting can be selected from air, logical nitrogen, logical argon gas and
At least one vacuumized.
The invention has the advantages that present invention process process is simple, raw material sources are extensive, and product is easily prepared, reproducible,
By controlling graphite type carbon nitride well-crystallized, the purity is high that calcination temperature is prepared, yield is big, and preparation efficiency is high.Gained produces
Product are not only suitable for further preparing experiment synthesis and the performance study of magnanimity high density nitridation carbon phase as precursor, can also pass through gold
Belong to ion modification, obtains visible light catalyst, further expand its application range.
Detailed description of the invention
Fig. 1 is that SEM schemes (melamine).
Fig. 2 is SEM figure (intermediate: gained drying solid in step (3)).
Fig. 3 is SEM figure (according to the method for carrying out calcination in the prior art).
Fig. 4 is that SEM schemes (providing method preparation according to the present invention).
Fig. 5 is XRD diagram (melamine).
Fig. 6 is XRD diagram (intermediate: gained drying solid in step (3)).
Fig. 7 is XRD diagram (g-C3N4).
Fig. 8 is UV-visible absorption spectrum (melamine).
Fig. 9 is UV-visible absorption spectrum (intermediate).
Figure 10 is UV-visible absorption spectrum (g-C3N4).
Figure 11 is infrared spectrogram (melamine).
Figure 12 is infrared spectrogram (intermediate).
Figure 13 is infrared spectrogram (g-C3N4).
Specific embodiment
Embodiment one:
50g melamine is taken to be placed in corundum crucible, roasting 6 is small at 410 DEG C in Muffle furnace after 3 hours abundant ball millings
When, it is cooling, be successively added points for 4 times totally 400 ml ethyl alcohol washed, dry after be placed in Muffle furnace again, at 560 DEG C
Sheet class graphite phase carbon nitride g-C can must be had by roasting 6 hours again3N4。
Embodiment two:
20g melamine is taken to be placed in corundum crucible, roasting 9 is small at 390 DEG C in Muffle furnace after 6 hours abundant ball millings
When, it is cooling, be successively added points for 4 times totally 300 ml ethyl alcohol washed, dry after be placed in Muffle furnace again, at 520 DEG C
Sheet class graphite phase carbon nitride g-C can must be had by roasting 9 hours again3N4。
Embodiment three:
It takes 50g melamine to be placed in corundum crucible, roasts 12 at 370 DEG C in Muffle furnace after 8 hours abundant ball millings
Hour, it is cooling, be successively added points for 6 times totally 200 ml ethyl alcohol washed, dry after be placed in Muffle furnace again, in 530 DEG C
Under roast can must have within 7 hours sheet class graphite phase carbon nitride g-C again3N4。
The present invention is generally speaking as follows: by amino-containing organic matter predecessor after abundant ball milling in Muffle furnace in one
Determine roasting temperature, it is cooling, it is added after the washing of second alcohols solvent, drying in Muffle furnace, is roasted again after improving temperature
There must be sheet class graphite phase carbon nitride g-C3N4。
Claims (10)
1. a kind of sheet class graphite phase carbon nitride g-C3N4Material, which is characterized in that the g-C prepared3N4With sheet knot
Structure.
2. a kind of sheet class graphite phase carbon nitride g-C3N4The preparation method of material, which is characterized in that during the preparation process, will
Amino-containing organic matter predecessor after ball milling is prepared by the way of repeatedly roasting, and maturing temperature successively improves system
It is standby.
3. a kind of sheet class graphite phase carbon nitride g-C according to claim 23N4The preparation method of material, feature exist
In, comprising the following steps:
(1) amino-containing organic matter predecessor is added in ball mill, abundant ball milling;
(2) predecessor after ball milling is taken to roast at a certain temperature;
(3) obtained solid in step (2) washed, dried;
(4) by gained drying solid in step (3), improve after temperature that roasting must there can be sheet class graphite-phase to nitrogenize again
Carbon g-C3N4。
4. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature exist
In the amino-containing organic matter predecessor in step (1) is selected from cyanamide, dicyandiamide, melamine, cyanuric acid thiocarbamide, salt
At least one of sour guanidine and urea.
5. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature exist
In the Ball-milling Time in step (1) is 0.5-10 hours.
6. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature exist
In predecessor is 370-410 DEG C in the temperature of Muffle kiln roasting after step (2) ball milling, and the time is 0.25-12 hours.
7. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature exist
In the solid in step (3) is 5-50 g, is washed using second alcohols solvent, and second alcohols solvent is 50-500 ml；This two
The dosage of kind substance zooms in or out in proportion according to above-mentioned content.
8. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature exist
In the washing times in step (3) are 2-6 times, and drying temperature is 105 DEG C.
9. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature exist
In drying solid in step (4) is 510-610 DEG C in the temperature of Muffle kiln roasting, and the time is 0.25-12 hours.
10. a kind of sheet class graphite phase carbon nitride g-C according to claim 33N4The preparation method of material, feature
Be, in step (2) and (4) sample the atmosphere of Muffle kiln roasting can be selected from air, logical nitrogen, logical argon gas and take out true
Empty at least one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810836984.5A CN109046422A (en) | 2018-07-26 | 2018-07-26 | A kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810836984.5A CN109046422A (en) | 2018-07-26 | 2018-07-26 | A kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof |
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| CN201810836984.5A Withdrawn CN109046422A (en) | 2018-07-26 | 2018-07-26 | A kind of sheet class graphite phase carbon nitride g-C3N4Material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233838A (en) * | 2018-11-02 | 2019-01-18 | 扬州工业职业技术学院 | A kind of Eu3+, Se codope Fe3O4/g-C3N4Material and its application in environment remediation |
| CN109647488A (en) * | 2019-01-30 | 2019-04-19 | 扬州工业职业技术学院 | A kind of modified Ag/g-C3N4The preparation method of composite material and its application in photocatalysis |
| CN109647489A (en) * | 2019-01-30 | 2019-04-19 | 扬州工业职业技术学院 | A kind of modified by silver modified graphite phase carbon nitride material and its application in photocatalysis |
| CN109725104A (en) * | 2019-01-11 | 2019-05-07 | 陕西科技大学 | A kind of catalytic activity of graphite phase carbon nitride and the research method of temperature gradient relation |
| CN111186824A (en) * | 2020-01-10 | 2020-05-22 | 山东大学 | Preparation method of high-specific-surface-area defective carbon nitride |
| CN111943152A (en) * | 2020-09-09 | 2020-11-17 | 中国地质大学（北京） | Photocatalyst and method for synthesizing ammonia by photocatalysis |
| CN111974436A (en) * | 2020-09-23 | 2020-11-24 | 中国科学技术大学 | Graphite-phase carbon nitride and preparation method thereof, and method for producing hydrogen by photocatalytic water |
| CN112608779A (en) * | 2020-12-28 | 2021-04-06 | 四川大学 | Lubricating grease based on carbonitride and preparation method thereof |
| CN113444558A (en) * | 2021-05-26 | 2021-09-28 | 无锡烯创科技有限公司 | Organic modification method for improving dispersibility of graphite-phase carbon nitride in lubricating oil |
| CN113976157A (en) * | 2021-10-19 | 2022-01-28 | 新乡医学院 | Three-dimensional porous in-situ carbon-doped g-C3N4Process for preparing catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109233838B (en) * | 2018-11-02 | 2020-06-30 | 扬州工业职业技术学院 | Eu (Eu)3+Se codoped with Fe3O4/g-C3N4Material and application thereof in environmental remediation |
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| CN109725104A (en) * | 2019-01-11 | 2019-05-07 | 陕西科技大学 | A kind of catalytic activity of graphite phase carbon nitride and the research method of temperature gradient relation |
| CN109647488B (en) * | 2019-01-30 | 2022-01-11 | 扬州工业职业技术学院 | Modified Ag/g-C3N4Preparation method of composite material and application of composite material in photocatalysis |
| CN109647488A (en) * | 2019-01-30 | 2019-04-19 | 扬州工业职业技术学院 | A kind of modified Ag/g-C3N4The preparation method of composite material and its application in photocatalysis |
| CN109647489A (en) * | 2019-01-30 | 2019-04-19 | 扬州工业职业技术学院 | A kind of modified by silver modified graphite phase carbon nitride material and its application in photocatalysis |
| CN109647489B (en) * | 2019-01-30 | 2022-03-01 | 扬州工业职业技术学院 | Silver modified graphite phase carbon nitride material and application thereof in photocatalysis |
| CN111186824A (en) * | 2020-01-10 | 2020-05-22 | 山东大学 | Preparation method of high-specific-surface-area defective carbon nitride |
| CN111943152A (en) * | 2020-09-09 | 2020-11-17 | 中国地质大学（北京） | Photocatalyst and method for synthesizing ammonia by photocatalysis |
| CN111974436A (en) * | 2020-09-23 | 2020-11-24 | 中国科学技术大学 | Graphite-phase carbon nitride and preparation method thereof, and method for producing hydrogen by photocatalytic water |
| CN112608779A (en) * | 2020-12-28 | 2021-04-06 | 四川大学 | Lubricating grease based on carbonitride and preparation method thereof |
| CN112608779B (en) * | 2020-12-28 | 2022-06-07 | 四川大学 | Lubricating grease based on carbonitride and preparation method thereof |
| CN113444558A (en) * | 2021-05-26 | 2021-09-28 | 无锡烯创科技有限公司 | Organic modification method for improving dispersibility of graphite-phase carbon nitride in lubricating oil |
| CN113976157A (en) * | 2021-10-19 | 2022-01-28 | 新乡医学院 | Three-dimensional porous in-situ carbon-doped g-C3N4Process for preparing catalyst |
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Application publication date: 20181221 |