CN109046434A - A kind of preparation method of defective high-efficiency silicon nitride carbon photochemical catalyst - Google Patents
A kind of preparation method of defective high-efficiency silicon nitride carbon photochemical catalyst Download PDFInfo
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- CN109046434A CN109046434A CN201811010035.8A CN201811010035A CN109046434A CN 109046434 A CN109046434 A CN 109046434A CN 201811010035 A CN201811010035 A CN 201811010035A CN 109046434 A CN109046434 A CN 109046434A
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- carbonitride
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- phase carbon
- carbon nitride
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 230000002950 deficient Effects 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 11
- 239000003054 catalyst Substances 0.000 title claims abstract description 9
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 15
- 239000011737 fluorine Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 19
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 229920000877 Melamine resin Polymers 0.000 description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 125000004193 piperazinyl group Chemical group 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001603 reducing effect Effects 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation methods of defective high-efficiency silicon nitride carbon photochemical catalyst, comprising: (1) appropriate amount of deionized water is added in nitrogenous organic precursor, is lyophilized with liquid nitrogen, drying is then removed water in freeze drier;(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, graphite phase carbon nitride is made in cooled to room temperature.(3) by the graphite phase carbon nitride in (2) in 100-200 DEG C of fluorine gas atmosphere synthesis under normal pressure 0.5-2h, obtain containing defective carbonitride.It is high-efficient using the carbonitride carrier separation for being rich in defect prepared by method of the invention, be conducive to photocatalytic activity raising.
Description
Technical field
The present invention relates to carbonitride field of photocatalytic material, and in particular to a kind of defective high-efficiency silicon nitride carbon photochemical catalyst
Preparation method.
Background technique
Conductor photocatalysis is the effective way for solving energy crisis and problem of environmental pollution.Graphite phase carbon nitride is a kind of
2D stratiform non-metal optical catalysis material, has both visible light-responded and good stability, in Photocatalyzed Hydrogen Production, water oxygen, organic
The fields such as object degradation, photosynthesis and carbon dioxide reduction are worth with important research.However carbonitride is anti-in photocatalysis at present
The problems such as forbidden bandwidth is wider, photo-generated carrier is difficult to efficiently separate and specific surface area is low is still suffered from answering.In carbonitride
Frame in introduce defect be one of solution to the problems described above, thus the extensive concern by researcher.
Researcher research shows that the intrinsic defect of defect, especially catalyst is believed to effectively improve urges
Change performance.The defects of many report discovery carbonitrides not only improve separation of charge efficiency, and enhance photocatalysis moisture
Visible absorption in solution preocess.Therefore, the controllable carbonitride of defect level is prepared by controlling reaction condition, probes into carbonitride
Relationship between defect sturcture and level structure, catalytic activity, the photocatalytic activity for further increasing material have great grind
Study carefully meaning.
Fluorine gas is a kind of strong reducing property gas, and it is abundant that generation is reacted with the graphite phase carbon nitride that freezing processing crosses presoma
Fault of construction.By the temperature and time of control fluorine gas reaction, the defect level of carbonitride, activity of the defect as reaction are adjusted
Site, so that photocatalysis efficiency effectively improves.This method is by the defect to carbonitride and other carbon-based nonmetal catalyzed materials
Study on regulation provides new thinking, provides a kind of new side in the catalysis material of photochemistry and optical electro-chemistry for development and application
Method.
Summary of the invention
The present invention provides a kind of preparation methods of defective high-efficiency silicon nitride carbon photochemical catalyst, and specific implementation step is such as
Under:
A kind of preparation method of defective high-efficiency silicon nitride carbon photochemical catalyst, including the following steps:
(1) appropriate amount of deionized water is added in nitrogenous organic precursor, is lyophilized with liquid nitrogen, is then removed water in freeze drier
It is dry;
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, naturally cools to room
Graphite phase carbon nitride is made in temperature.
(3) by the graphite phase carbon nitride in (2) in 100-200 DEG C of fluorine gas atmosphere synthesis under normal pressure 0.5-2h, contained
Defective carbonitride.
Preferably, the nitrogenous precursor is one of dicyanodiamine, melamine or thiocarbamide or mixture.
Preferably, the fluorine gas atmosphere is the fluorine gas and nitrogen mixed gas of volume fraction 20%.
Compared with prior art, the invention has the advantages that
(1) present invention has general applicability, is not limited to a kind of synthesis nitridation carbon raw material, and can be applied to be modified other
Nonmetallic carbon-supported catalysts.
(2) the carbonitride carrier separation rich in defect prepared is high-efficient, is conducive to photocatalytic activity raising, can be used for
Design high efficiency photocatalyst.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the carbonitride containing defect;
Fig. 2 is the X-ray diffractogram of the carbonitride containing defect;
Fig. 3 is the infrared spectrogram of the carbonitride containing defect;
Fig. 4 is the x-ray photoelectron spectroscopy figure of the carbonitride containing defect.
Specific embodiment
The present invention is described in further detail below in conjunction with the drawings and specific embodiments.It should be appreciated that described herein
Specific embodiment to explain the present invention, be not intended to limit the present invention.
Embodiment 1
(1) 30mL deionized water is added in 1g melamine, is lyophilized with liquid nitrogen, is then removed water in freeze drier dry
It is dry.
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, naturally cools to room
Graphite phase carbon nitride is made in temperature.
(3) by the 100mg graphite phase carbon nitride in (2) 150 DEG C of volume fraction 20% fluorine gas and nitrogen mixture
Synthesis under normal pressure 1h in body is obtained containing defective carbonitride 46mg.
Fig. 1 is the transmission electron microscope picture of the defect carbonitride of preparation, and there is apparent hole configurations on surface.
Fig. 2 be preparation defect carbonitride X-ray diffractogram, 13.Corresponding peak (100) is vanished from sight substantially, shows
It is destructurized in face.
Fig. 3 is the infrared spectrogram of the defect carbonitride of preparation, 3000-3500cm-1Belong to amino group or water, 1200-
1700cm-1Belong to aroma type carbon azacyclo-, 810cm-1Belong to piperazine ring, shows that carbonitride basic structure remains unchanged.
Fig. 4 is the x-ray photoelectron spectroscopy figure of the defect carbonitride of preparation, contains carbon, nitrogen, four kinds of oxygen, fluorine members in sample
Element.
Embodiment 2
(1) 30mL deionized water is added in 1g melamine, is lyophilized with liquid nitrogen, is then removed water in freeze drier dry
It is dry.
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, naturally cools to room
Graphite phase carbon nitride is made in temperature.
(3) by the 100mg graphite phase carbon nitride in (2) 120 DEG C of volume fraction 20% fluorine gas and nitrogen mixture
Synthesis under normal pressure 1h in body is obtained containing defective carbonitride 54mg.
Embodiment 3
(1) 30mL deionized water is added in 1g melamine, is lyophilized with liquid nitrogen, is then removed water in freeze drier dry
It is dry.
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, naturally cools to room
Graphite phase carbon nitride is made in temperature.
(3) by the 100mg graphite phase carbon nitride in (2) 180 DEG C of volume fraction 20% fluorine gas and nitrogen mixture
Synthesis under normal pressure 1h in body is obtained containing defective carbonitride 39mg.
Embodiment 4
(1) 30mL deionized water is added in 1g melamine, is lyophilized with liquid nitrogen, is then removed water in freeze drier dry
It is dry.
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, naturally cools to room
Graphite phase carbon nitride is made in temperature.
(3) by the 100mg graphite phase carbon nitride in (2) 150 DEG C of volume fraction 20% fluorine gas and nitrogen mixture
Synthesis under normal pressure 2h in body is obtained containing defective carbonitride 35mg.
Embodiment 5
(1) 30mL deionized water is added in 1g melamine, is lyophilized with liquid nitrogen, is then removed water in freeze drier dry
It is dry.
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h in Muffle furnace with 5 DEG C/min, naturally cools to room
Graphite phase carbon nitride is made in temperature.
(3) by the 100mg graphite phase carbon nitride in (2) 150 DEG C of volume fraction 20% fluorine gas and nitrogen mixture
Synthesis under normal pressure 0.5h in body is obtained containing defective carbonitride 59mg.
Claims (3)
1. a kind of preparation method of defective high-efficiency silicon nitride carbon photochemical catalyst, including the following steps:
(1) appropriate amount of deionized water is added in nitrogenous organic precursor, is lyophilized with liquid nitrogen, then removed water in freeze drier dry
It is dry;
(2) dried object in (1) is warming up to 550 DEG C of reaction 4h, cooled to room temperature, system in Muffle furnace with 5 DEG C/min
Obtain graphite phase carbon nitride.
(3) by the graphite phase carbon nitride in (2) in 100-200 DEG C of fluorine gas atmosphere synthesis under normal pressure 0.5-2h, obtain containing lack
Sunken carbonitride.
2. preparation method according to claim 1, which is characterized in that the nitrogenous precursor is dicyanodiamine, trimerization
One of cyanamide or thiocarbamide or mixture.
3. preparation method according to claim 1, which is characterized in that the fluorine gas atmosphere is the fluorine of volume fraction 20%
Gas and nitrogen mixed gas.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108927191A (en) * | 2017-05-22 | 2018-12-04 | 天津大学 | Fluorine-containing graphite-phase nitrogen carbide photochemical catalyst and preparation method thereof |
CN109675606A (en) * | 2019-01-14 | 2019-04-26 | 燕山大学 | A kind of photochemical catalyst and preparation method thereof |
CN113457715A (en) * | 2021-07-23 | 2021-10-01 | 吉林化工学院 | Preparation method and application of novel porous g-C3N4 with photocatalytic performance |
CN114188522A (en) * | 2021-12-10 | 2022-03-15 | 湖南宸宇富基新能源科技有限公司 | Microcrystalline graphite/CNT @ C composite material, preparation method thereof and application thereof in lithium secondary battery |
CN114188522B (en) * | 2021-12-10 | 2024-05-14 | 湖南宸宇富基新能源科技有限公司 | Microcrystalline graphite/CNT@C composite material, preparation method thereof and application thereof in lithium secondary battery |
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CN103420352A (en) * | 2013-08-08 | 2013-12-04 | 四川大学 | High-fluoride-content graphite fluoride and preparation method thereof |
CN105670620A (en) * | 2016-03-14 | 2016-06-15 | 山东农业大学 | Preparation method of doped carbon nitride fluorescent quantum dots |
CN105944748A (en) * | 2016-06-14 | 2016-09-21 | 辽宁大学 | Graphite-phase carbon nitride photocatalyst with large specific surface area and preparation method and application thereof |
CN107473191A (en) * | 2017-07-19 | 2017-12-15 | 天津大学 | Method for preparing three-dimensional graphite phase carbon nitride with cyano group by salt assistance |
CN107983388A (en) * | 2017-12-05 | 2018-05-04 | 江南大学 | A kind of nonmetal doping nitride porous carbon photochemical catalyst and preparation method thereof |
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2018
- 2018-08-31 CN CN201811010035.8A patent/CN109046434A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103420352A (en) * | 2013-08-08 | 2013-12-04 | 四川大学 | High-fluoride-content graphite fluoride and preparation method thereof |
CN105670620A (en) * | 2016-03-14 | 2016-06-15 | 山东农业大学 | Preparation method of doped carbon nitride fluorescent quantum dots |
CN105944748A (en) * | 2016-06-14 | 2016-09-21 | 辽宁大学 | Graphite-phase carbon nitride photocatalyst with large specific surface area and preparation method and application thereof |
CN107473191A (en) * | 2017-07-19 | 2017-12-15 | 天津大学 | Method for preparing three-dimensional graphite phase carbon nitride with cyano group by salt assistance |
CN107983388A (en) * | 2017-12-05 | 2018-05-04 | 江南大学 | A kind of nonmetal doping nitride porous carbon photochemical catalyst and preparation method thereof |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108927191A (en) * | 2017-05-22 | 2018-12-04 | 天津大学 | Fluorine-containing graphite-phase nitrogen carbide photochemical catalyst and preparation method thereof |
CN108927191B (en) * | 2017-05-22 | 2021-05-28 | 天津大学 | Fluorine-containing graphite phase nitrogen carbide photocatalyst and preparation method thereof |
CN109675606A (en) * | 2019-01-14 | 2019-04-26 | 燕山大学 | A kind of photochemical catalyst and preparation method thereof |
CN113457715A (en) * | 2021-07-23 | 2021-10-01 | 吉林化工学院 | Preparation method and application of novel porous g-C3N4 with photocatalytic performance |
CN114188522A (en) * | 2021-12-10 | 2022-03-15 | 湖南宸宇富基新能源科技有限公司 | Microcrystalline graphite/CNT @ C composite material, preparation method thereof and application thereof in lithium secondary battery |
CN114188522B (en) * | 2021-12-10 | 2024-05-14 | 湖南宸宇富基新能源科技有限公司 | Microcrystalline graphite/CNT@C composite material, preparation method thereof and application thereof in lithium secondary battery |
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Application publication date: 20181221 |