CN106955727B - A kind of g-C that surface is modified3N4Preparation method - Google Patents
A kind of g-C that surface is modified3N4Preparation method Download PDFInfo
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- CN106955727B CN106955727B CN201710242684.XA CN201710242684A CN106955727B CN 106955727 B CN106955727 B CN 106955727B CN 201710242684 A CN201710242684 A CN 201710242684A CN 106955727 B CN106955727 B CN 106955727B
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- 238000000034 method Methods 0.000 title abstract description 9
- -1 sodium halide Chemical class 0.000 claims abstract description 33
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 14
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 11
- 239000011591 potassium Substances 0.000 claims abstract description 11
- 239000011734 sodium Substances 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 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
- 239000000460 chlorine Substances 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 1
- 238000005286 illumination Methods 0.000 claims 1
- 239000011630 iodine Substances 0.000 claims 1
- 229910052740 iodine Inorganic materials 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000000804 electron spin resonance spectroscopy Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical group C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8634—Ammonia
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention belongs to materials and catalytic field, are related to a kind of g-C that surface is modified3N4Preparation method.For the first time creatively directly with the mixture and g-C of sodium halide, potassium halide or these salt3N4Pyroreaction is carried out, the introducing of water in reaction process, so that modified g-C3N4Containing hydroxyl, and in modified g-C3N4Corresponding metal ion in surface modification.This method not only have it is easy to operate, be easily achieved, reaction raw materials are cheap and easy to get, environmental-friendly, modified g-C3N4The features such as yield is high, and modified g-C3N4Surface hydroxyl abundant and pore structure abundant, can generate hydroxyl radical free radical abundant under visible light.These features are modified g-C3N4It lays the foundation in the practical application of photocatalysis field.
Description
Technical field
The invention belongs to materials and catalytic science field, and in particular to a kind of g-C that surface is modified3N4Preparation method.It should
Method is by simple pyroreaction method, in g-C3N4Material surface forms hydroxyl group, and loaded metal ion.This method is
It realizes for the first time.The modified g-C in a large amount of surface can be prepared quickly, in bulk by this method3N4, in solar battery, more
Mutually the fields such as catalysis, degradation of organic substances have extensive prospect.
Background technique
g-C3N4(Graphitic Carbon Nitride, is abbreviated as g-C3N4) it is a kind of with similar graphite-structure
Organic semiconducting materials.From 2009 it is found that its with photocatalysis hydrogen evolution activity since, since it is with stable physics
Chemical stability, small band gap (2.7eV), the features such as preparation method is simple, receive the extensive research of people.But
The g-C prepared due to traditional one kettle way3N4It is small with specific surface area, it is seen that the disadvantages such as light abstraction width is narrow, catalytic activity is low
It is limited in the application of catalytic field, therefore people have carried out a large amount of study on the modification to it, including topographic design, metal from
Sub- doping, organic molecule combined polymerization, building heterojunction semiconductor etc., make some progress.But due to g-C3N4High
Physical and chemical stability, people are but seldom to the modified research in its surface, and surface amido defect group abundant can be to change
Journal of Sex Research provides may.Therefore, to g-C3N4It is imperative to carry out surface modification, there is highly important theory significance and reality
Application value.
Summary of the invention
A kind of g-C that surface is modified3N4Preparation, which is characterized in that the mixing of sodium halide, potassium halide or these halide salts
Object and g-C3N4It is chemically reacted at high temperature, surface introduces corresponding metal ion, and the introducing of water makes modified g-
C3N4Contain hydroxyl group in surface.The preparation method realizes that before this, people do not utilize g-C for the first time3N4Surface amine groups
Defect is reacted at high temperature with above-mentioned halide salt to be modified.This method not only have it is easy to operate, be easy to real
Now, reaction raw materials g-C cheap and easy to get, environmental-friendly, modified3N4The features such as yield is high, and modified g-C3N4Surface hydroxyl abundant
Base and gap structure abundant, these features are modified g-C3N4It lays the foundation in the practical application of photocatalysis field.
Its preparation includes the following steps:
(1) by the mixture and g-C of sodium halide, potassium halide or these halide salts3N4It is mixed, obtains mixture, halogenation
The water added in the residual and protection gas of salt is the source of water in reaction；
(2) obtained mixture is placed in the calcining vessel of gas shield, is calcined, calcination temperature be 450 DEG C~
650 DEG C, calcination time 0-7h；
(3) product that (2) obtain is centrifuged, filtered, obtain modified g-C3N4。
In above-mentioned preparation method, in step (1), the g-C3N4Mass ratio range be 1%~90wt%.
In above-mentioned preparation method, in step (1), in the sodium halide and potassium halide halogen element be fluorine, chlorine, bromine, iodine,
The mixture of halide salt is sodium halide and potassium halide, sodium halide and sodium halide, potassium halide and a kind of halide salt of potassium halide to a variety of
The mixing of halide salt.
In above-mentioned preparation method, in step (2), the protective gas is nitrogen, argon gas, helium, carbon dioxide
In above-mentioned preparation preparation method, in step (2), the calcination temperature range is 450 DEG C~650 DEG C, and
0~7h of retention time in the temperature range.
In above-mentioned preparation method, in step (3), the modification g-C3N4Surface hydroxyl group rich in, in light
A large amount of hydroxyl radical free radical is generated according to lower, the degradation for organic matter.
In above-mentioned preparation method, in step (3), the modification g-C3N4Contain the stratiform of a large amount of 1~3nm in surface
Gap is used for CO2、NH3Absorption and catalytic reduction reaction.
Detailed description of the invention:
Fig. 1 is embodiment 1, example 2 and the made modified g-C of example 33N4And parent g-C3N4Infrared spectrum (FT-IR),
810cm-1With 1200-1700cm-1It is respectively belonging to the breathing vibration peak of triazine ring and the stretching vibration peak of three s-triazine rings.
3100cm-1Vibration peak ownership and the-NH and-NH nearby occurred2.These results and parent g-C3N4It is consistent, illustrates that high temperature changes
Property does not destroy g-C3N4Basic structure.Modified g-C3N4In 3400nm-1Nearby there is hydroxyl vibration peak, illustrates hydroxyl
Base is successfully modified to g-C3N4Surface.
Table 1 is embodiment 1, example 2 and the made modified g-C of example 33N4Surface metal ion and chloride ion content, in table 1
Containing corresponding metallic element, but without chlorine element.The result shows halide can and g-C3N4It reacts, and by metal
Ion can modify g-C3N4Surface.
| Na atm% | K atm% | Cl atm% | |
| Na-4h | 3.2 | 0 | 0 |
| K-3h | 0 | 3.7 | 0 |
| Na-K-4h | 2.7 | 3.0 | 0 |
Fig. 2 is modification g-C obtained by embodiment 33N4Electron spin resonance spectroscopy (ESR), be used to quantitative test hydroxyl from
By the yield (square that the quantity of free radical is proportional to signal peak heights) of base.Under Ar protective condition, the hydroxyl of appearance is certainly
The hydroxyl of Na-K-4h surface structure is derived from by base signal.In air, the yield of hydroxyl radical free radical is 30 under Ar protection
Times, this illustrates the O in air2Generation to its hydroxyl is very favorable.As a comparison, parent g-C3N4But it is displayed without bright
Aobvious hydroxyl signal peak.Generally, hydroxyl radical free radical is degradation of organic substances, the active material for being catalyzed organic synthesis, therefore is modified g-
C3N4It is very favorable for catalytic degradation organic matter, catalysis organic synthesis.
Fig. 3 is modification g-C obtained by embodiment 33N4Transmission electron microscope picture (TEM).It can obviously find modified g-C3N4's
Contain the stratiform gap of a large amount of 1~3nm in surface.
Fig. 4 is modification g-C obtained by embodiment 33N4CO2And NH3Temperature programmed desorption curve (TPD).Fig. 4
It (a) and is respectively NH in Fig. 4 (b)3And CO2Temperature programmed desorption curve.Desorbing gas peak area is bigger, represents the gas of absorption
The scale of construction is more.Na-K-4h as shown in the figure has huge CO at 100 DEG C~300 DEG C2And NH3Adsorption area, parent g-C3N4
Desorbing gas area can ignore, the result shows modified g-C3N4It has broad prospects in gas absorption direction, in addition
Due to parent g-C3N4With certain catalysis CO2Reducing power, therefore, a large amount of gas absorption are beneficial to modified g-C3N4Into
Row CO2Photo catalytic reduction.
Specific embodiment
The specific embodiment taken according to the technical scheme of the invention is described as follows:
Embodiment 1
Weigh the g-C of 600mg3N4With the sodium chloride of 1200mg, mixed grinding is uniform, then in N2Protect lower 550 DEG C of calcinings
4h is then centrifuged for, washes the modified g-C of acquisition3N4(abbreviation Na-4h).
Embodiment 2
Weigh the g-C of 600mg3N4With 1200mg potassium chloride, mixture grinding is uniform, then in N2Protect lower 550 DEG C of calcinings
3h is then centrifuged for, washes the modified g-C of acquisition3N4(abbreviation K-3h).
Embodiment 3
Weigh 600mg g-C3N4, 600 sodium chloride and 600mg potassium chloride, mixed grinding is uniform, then in N2Protective condition
Lower 550 DEG C of calcinings 4h, is then centrifuged for, and washing obtains modified g-C3N4(abbreviation Na-K-4h).
Claims (7)
1. a kind of modified g-C in surface3N4Preparation method, which is characterized in that sodium halide, potassium halide or these halide salts it is mixed
Close object and g-C3N4Further mixing, calcining are chemically reacted, surface introduces corresponding potassium/sodium metal ion, and water draws
Enter to make modified g-C3N4Contain hydroxyl in surface；
Its preparation includes the following steps:
(1) by the mixture and g-C of sodium halide, potassium halide or these halide salts3N4It is mixed, obtains mixture；
(2) then obtained mixture is placed in the calcining vessel of gas shield, is calcined；
The water added in the residual and protection gas of halide salt is the source of water in reaction；
(3) product that (2) obtain is centrifuged, filtered, obtained solid, as modified g-C3N4。
2. preparation method according to claim 1, which is characterized in that g-C3N4Mass ratio range be 1%~
90wt%.
3. preparation method according to claim 1, which is characterized in that in sodium halide and potassium halide halogen be fluorine, chlorine, bromine or
Iodine.
4. preparation method according to claim 1, which is characterized in that protective gas in calcining vessel be nitrogen, argon gas,
Helium or carbon dioxide.
5. preparation method according to claim 1, which is characterized in that calcination temperature range is 450 DEG C~650 DEG C, and
0~7h of retention time in the temperature range, and calcination time is not 0.
6. preparation method according to claim 1, which is characterized in that the modification g-C3N4Hydroxyl group is contained on surface,
Hydroxyl radical free radical is generated under light illumination, the degradation for organic matter.
7. preparation method according to claim 1, which is characterized in that the modification g-C3N4Contain 1~3nm's in surface
Stratiform gap is used for CO2、NH3Absorption and catalytic reduction reaction.
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| CN108855182B (en) * | 2018-06-05 | 2020-05-22 | 中国地质大学（武汉） | Element-doped porous g-C3N4Preparation method of nanosheet |
| CN110327872B (en) * | 2019-07-08 | 2022-02-18 | 中国科学院兰州化学物理研究所 | Functional graphite-phase carbon nitride material and preparation method and application thereof |
| CN114950520B (en) * | 2022-04-11 | 2023-10-03 | 湖北工业大学 | CeO (CeO) 2 Na, K doped g-C 3 N 4 Fenton-like catalytic material and preparation method and application thereof |
| CN115010101B (en) * | 2022-07-18 | 2023-09-12 | 河南大学 | Preparation method and application of carbon nitride nano-sheet with wide spectral response and high crystallinity |
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