CN115672371A - Preparation method of aminated graphite-phase carbon nitride nanosheet and application of aminated graphite-phase carbon nitride nanosheet in carbon dioxide reduction - Google Patents
Preparation method of aminated graphite-phase carbon nitride nanosheet and application of aminated graphite-phase carbon nitride nanosheet in carbon dioxide reduction Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002135 nanosheet Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 230000009467 reduction Effects 0.000 title claims abstract description 16
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 8
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 22
- 239000010439 graphite Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 230000021523 carboxylation Effects 0.000 claims description 3
- 238000006473 carboxylation reaction Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 239000002064 nanoplatelet Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000010757 Reduction Activity Effects 0.000 description 2
- -1 amino graphite Chemical compound 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The invention relates to a preparation method of an aminated graphite phase carbon nitride nanosheet and application thereof in carbon dioxide reduction, wherein in the method, bulk graphite phase carbon nitride CN is prepared firstly; the obtained bulk graphite phase carbon nitride CN and HNO 3 Placing the mixture into a reaction container, and reacting in a reflux device to obtain carboxylated CN nano-sheets X-CCN; dispersing X-CCN in toluene; and adding Ethylenediamine (EDA) and N, N-Dicyclohexylcarbodiimide (DCC) into the X-CCN dispersion liquid under stirring, and reacting in an oil bath under the atmosphere of inert gas to obtain the aminated graphite phase carbon nitride nanosheet X-CN-EDA. The surface of the X-CN-EDA prepared by the invention is rich in amino and is rich in CO 2 Adsorption energy ofStrong force, photocatalysis CO 2 Excellent reduction performance and good application prospect.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a preparation method of an amino graphite phase carbon nitride nanosheet and application thereof in carbon dioxide reduction.
Background
The global energy supply mainly depends on carbon-rich fossil fuels, and inevitably discharges a large amount of carbon dioxide CO 2 Thereby causing global warming. Introducing CO 2 Photocatalytic reduction to energy fuels is believed to reduce CO 2 An effective way for discharging and solving the energy crisis. The graphite carbon nitride CN has good stability, proper band gap and visible light response, and is a promising metal-free photocatalyst. Unfortunately, CO of CN 2 The reduction activity is very mild and is not comparable to current noble metal-based photocatalysts. CO 2 2 The main limitation of photoreduction is CO 2 Weak adsorption capacity, narrow visible light absorption range and low separation rate of photon-generated carriers. Even at high CO 2 In a reactive atmosphere of concentration, CO 2 Adsorption as a prerequisite step also affects the final efficiency of the photoreduction.
To increase g-C 3 N 4 The researchers have done a lot of modification work on the photocatalytic performance of the catalyst. However, most of the modification works, including the modulation of morphology structure, the optimization of electronic structure, and the preparation of composite photocatalyst, etc., focus on the broadening of g-C 3 N 4 And enhance the separation rate of photogenerated carriers. For CO 2 Construction of g-C by adsorption 3 N 4 Relatively few studies have been made of base photocatalysts.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of aminated graphite-phase carbon nitride nanosheets with simple process and application thereof in photocatalysis of CO 2 And (3) application of reduction direction.
In order to realize the purpose, the technical scheme provided by the invention is as follows:
the preparation method of the aminated graphite phase carbon nitride nanosheet comprises the following steps:
step (1): heating urea from room temperature to a calcination temperature at a certain rate, and calcining for 2-4 h, wherein the calcination temperature is 450-600 ℃; after calcining, centrifugally washing and drying to obtain bulk graphite phase carbon nitride CN;
step (2): the bulk graphite phase carbon nitride CN with certain mass obtained in the step (1) and HNO with certain concentration 3 Placing in a reaction container, stirring in a reflux device at a certain temperature for a period of time, cooling to room temperature, centrifugingWashing and drying to obtain carboxylated CN nano sheet X-CCN, wherein X represents CN in HNO 3 Wherein C represents carboxylation;
and (3): dispersing the X-CCN with a certain mass obtained in the step (2) in a certain volume of toluene; adding Ethylenediamine (EDA) with a certain volume and N, N-Dicyclohexylcarbodiimide (DCC) with a certain mass into the X-CCN dispersion liquid under stirring, and reacting for a period of time in an oil bath at 80-100 ℃ in an inert gas atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated graphite-phase carbon nitride nanosheet X-CN-EDA.
Further, in the step (1), the temperature rise rate is 2 ℃/min.
Preferably, in step (1), the calcination temperature is 550 ℃.
Preferably, in step (2), HNO 3 The concentration is 2-5 mol/L, the bulk graphite phase carbon nitride CN and 2-5 mol/L HNO 3 The mass/volume ratio of (A) is: 0.8 to 1.2:100g/mL.
Further, in the step (2), the stirring temperature in the reflux device is 50-100 ℃, and the stirring time is 4-24 h.
Preferably, in the step (3), the mass/volume/mass ratio of the X-CCN, the toluene, the ethylenediamine and the N, N-dicyclohexylcarbodiimide added is 0.1-0.3: 5 to 15:10 to 30: 0.1-0.3 g/mL/mL/g.
Further, in the step (3), the reaction time in the oil bath is 12 to 36 hours.
Further, in the step (1), the step (2) and the step (3), the drying temperature is 30-60 ℃, and the drying time is 6-12 hours.
Further, the inert gas is N 2 。
The invention also protects the application of the amino graphite phase carbon nitride nanosheet prepared by the method in carbon dioxide reduction.
Compared with the prior art, the invention has the beneficial effects that:
(1) The raw materials of the invention have low price, the preparation method has simple operation, and the invention can be prepared in large scale;
(2) The surface of the X-CN-EDA is rich in amino and CO 2 Has strong adsorption capacity and can catalyze CO by light 2 The reduction performance is excellent.
Therefore, the preparation of the aminated graphite-phase carbon nitride nanosheet has a good application prospect.
Drawings
FIG. 1: a forming process diagram of X-CN-EDA;
FIG. 2: XRD patterns of CN and X-CN-EDA;
FIG. 3: CO of CN and 24-CN-EDA 2 Adsorption isotherms;
FIG. 4: photocatalytic CO of CN and X-CN-EDA 2 And (4) measuring the reduction performance.
Detailed Description
The present invention is described in more detail below by way of examples, but it should not be construed that the scope of the subject matter of the present invention is limited to the examples below, and that techniques realized based on the above contents of the present invention are within the scope of the present invention.
The experimental procedures used in the examples below are conventional procedures unless otherwise specified, and the reagents, methods and equipment used therein are conventional in the art unless otherwise specified.
The invention provides a preparation method of aminated graphite-phase carbon nitride nanosheets, which comprises the following steps of:
step (1): heating urea from room temperature to a calcination temperature at a certain rate, and calcining for 2-4 h, wherein the calcination temperature is 450-600 ℃; after calcining, centrifugally washing and drying to obtain bulk graphite phase carbon nitride CN;
step (2): the bulk graphite phase carbon nitride CN with certain mass obtained in the step (1) and HNO with certain concentration 3 Placing in a round-bottom flask, stirring at a certain temperature in a reflux device for a period of time, cooling to room temperature, centrifuging, washing and drying to obtain carboxylated CN nanosheet X-CCN, wherein X represents CN in HNO 3 Wherein C represents carboxylation;
and (3): certain of the results obtained in step (2)The mass of X-CCN is dispersed in a volume of toluene; adding a volume of Ethylenediamine (EDA) and a mass of N, N-Dicyclohexylcarbodiimide (DCC) to the X-CCN dispersion under stirring and adding a solution of Ethylenediamine (EDA) and N, N-Dicyclohexylcarbodiimide (DCC) to the X-CCN dispersion under stirring 2 Reacting for a period of time in an oil bath at the temperature of 80-100 ℃ under the atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano sheet X-CN-EDA.
The forming process diagram of the X-CN-EDA of the invention is shown in figure 1.
Example 1: preparation of bulk graphite phase carbon nitride CN
Heating urea with a certain mass from room temperature at a heating rate of 2 ℃/min to a calcination temperature, and calcining for 2-4 h, wherein the calcination temperature is 450-600 ℃; after the calcining and sintering, centrifugally washing and drying to obtain bulk graphite phase carbon nitride CN;
example 2: preparation of 24-CCN-EDA
0.8 to 1.2g of bulk graphite phase carbon nitride CN obtained in example 1 and 100mL of HNO of 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 24 hours at the temperature of between 50 and 100 ℃ in a reflux device, cooling the mixture to room temperature, centrifuging, washing and drying the cooled mixture to obtain carboxylated CN nano-sheets 24-CCN;
dispersing 0.1-0.3 g of the obtained 24-CCN in 5-15 mL of toluene; 10 to 30mL of ethylenediamine EDA and 0.1 to 0.3g of N, N-dicyclohexylcarbodiimide DCC were added to the 24-CCN dispersion with stirring, and the mixture was stirred in N 2 Reacting for 24 hours in an oil bath at the temperature of 80-100 ℃ under the atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-sheet 24-CCN-EDA.
The 24-CN-EDA was further tested by X-ray diffraction, and the test results are shown in FIG. 2.
In the photocatalysis of CO 2 In the course of reduction, CO 2 The adsorption capacity of the catalyst is critical and is suitable for CO of 24-CN-EDA 2 The adsorption performance was tested and compared with the adsorption capacity of the original CN, and the experimental results are shown in fig. 3.
Example 3: preparation of 4-CCN-EDA
The bulk graphite phase carbon nitride CN obtained in example 1 was changed to 0.8 to 1.2g and 100mL of 2-5 mol/L HNO 3 Placing the mixture into a round-bottom flask, stirring the mixture for 4 hours at the temperature of between 50 and 100 ℃ in a reflux device, cooling the mixture to room temperature, centrifuging, washing and drying the mixture to obtain carboxylated CN nano sheets 4-CCN;
dispersing 0.1-0.3 g of the obtained 4-CCN in 5-15 mL of toluene; 10 to 30mL of ethylenediamine EDA and 0.1 to 0.3g of N, N-dicyclohexylcarbodiimide DCC were added to the 4-CCN dispersion with stirring, and the mixture was stirred in N 2 Reacting for 24 hours in an oil bath at the temperature of 80-100 ℃ under the atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-sheet 4-CCN-EDA.
The 4-CN-EDA was tested by X-ray diffraction and the results are shown in FIG. 2.
Example 4: preparation of 8-CCN-EDA
0.8 to 1.2g of bulk graphite phase carbon nitride CN obtained in example 1 and 100mL of HNO of 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 8 hours at the temperature of between 50 and 100 ℃ in a reflux device, cooling the mixture to room temperature, centrifuging, washing and drying the cooled mixture to obtain carboxylated CN nano-sheets 8-CCN;
dispersing 0.1-0.3 g of the obtained 8-CCN in 5-15 mL of toluene; 10 to 30mL of ethylenediamine EDA and 0.1 to 0.3g of N, N-dicyclohexylcarbodiimide DCC were added to the 8-CCN dispersion under stirring and stirred in the presence of N 2 Reacting for 24 hours in an oil bath at the temperature of 80-100 ℃ under the atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-sheet 8-CCN-EDA.
The 8-CN-EDA was tested by X-ray diffraction, and the test results are shown in FIG. 2.
Example 5: preparation of 12-CCN-EDA
0.8 to 1.2g of bulk graphite phase carbon nitride CN obtained in example 1 and 100mL of HNO of 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 12 hours at the temperature of between 50 and 100 ℃ in a reflux device, cooling the mixture to room temperature, centrifuging, washing and drying the cooled mixture to obtain carboxylated CN nano-sheets 12-CCN;
dispersing 0.1-0.3 g of the obtained 12-CCN in 5-15 mL of toluene; 10 to 30mL of ethylenediamine EDA and 0.1 to 0.3g of N, N-dicyclohexyl carbon are added under stirringDiimine DCC was added to the 12-CCN dispersion and washed with N 2 Reacting for 24 hours in an oil bath at the temperature of 80-100 ℃ under the atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-sheet 12-CCN-EDA.
The 12-CN-EDA was tested by X-ray diffraction and the results are shown in FIG. 2.
Example 6: preparation of 48-CCN-EDA
0.8 to 1.2g of bulk graphite phase carbon nitride CN obtained in example 1 and 100mL of HNO of 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 48 hours at 50-100 ℃ in a reflux device, cooling the mixture to room temperature, centrifugally washing the mixture and drying the mixture to obtain carboxylated CN nanosheets 48-CCN;
dispersing 0.1-0.3 g of the obtained 48-CCN in 5-15 mL of toluene; 10 to 30mL of ethylenediamine EDA and 0.1 to 0.3g of N, N-dicyclohexylcarbodiimide DCC were added to the 48-CCN dispersion under stirring and stirred in the presence of N 2 Reacting for 24 hours in an oil bath at the temperature of 80-100 ℃ under the atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-sheet 48-CCN-EDA.
The 48-CN-EDA was tested by X-ray diffraction and the results are shown in FIG. 2.
Example 7: photocatalytic CO of X-CN-EDA 2 Reduction Property
Adopts Labsolar-6A type full glass automatic online trace gas analysis system produced by Beijing Pofilly science and technology Limited company, combines with Zhejiang Fuli GC 9790 II gas chromatograph to detect reduction products, and carries out photocatalytic reduction on CO (carbon monoxide) -containing X-CN-EDA (X-CN-EDA) comprising 4-CCN-EDA, 8-CCN-EDA, 12-CCN-EDA, 24-CCN-EDA and 48-CCN-EDA (carbon dioxide-containing organic acid) prepared by the embodiment of the invention 2 The performance is tested, and compared with the catalytic capability of bulk graphite phase carbon nitride CN, the detection result is shown in figure 4, and the catalytic activity of the X-CN-EDA prepared by the invention is obviously improved compared with the activity of the bulk graphite phase carbon nitride CN.
All X-CN-EDA samples in the examples showed higher photocatalytic activity than bulk CN, indicating that EDA contains amino groups that favor photocatalytic CO 2 And (4) reduction activity. The 24-CN-EDA photocatalyst showed the bestOf (2) photocatalytic CO 2 The reduction performance, CO yield, was 8.58. Mu. Mol/g, which is 5.92 times that of bulk CN (1.45. Mu. Mol/g). Notably, the 48-CN-EDA sample showed a slight decrease, but was still significantly higher than the bulk CN, probably because excess EDA functionalization would mask active sites on the bulk CN surface.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any simple modifications, equivalents and improvements made by those skilled in the art without departing from the technical scope of the present invention are all within the scope of the present invention.
Claims (10)
1. The preparation method of the aminated graphite-phase carbon nitride nanosheet is characterized by comprising the following steps: the method comprises the following steps:
step (1): heating urea from room temperature to a calcination temperature at a certain rate, and calcining for 2-4 h, wherein the calcination temperature is 450-600 ℃; after the calcining and sintering, centrifugally washing and drying to obtain bulk graphite phase carbon nitride CN;
step (2): the bulk graphite phase carbon nitride CN with certain mass obtained in the step (1) and HNO with certain concentration 3 Placing the mixture into a reaction container, stirring the mixture for a period of time at a certain temperature in a reflux device, cooling the mixture to room temperature, centrifugally washing and drying the cooled mixture to obtain carboxylated CN nano-sheet X-CCN, wherein X represents the content of CN in HNO 3 Wherein C represents carboxylation;
and (3): dispersing the X-CCN with a certain mass obtained in the step (2) in a certain volume of toluene; under stirring, adding a certain volume of Ethylenediamine (EDA) and a certain mass of N, N-Dicyclohexylcarbodiimide (DCC) into the X-CCN dispersion liquid, and reacting for a period of time in an oil bath at 80-100 ℃ in an inert gas atmosphere; and after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated graphite-phase carbon nitride nanosheet X-CN-EDA.
2. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in the step (1), the heating rate is 2 ℃/min.
3. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in the step (1), the calcination temperature was 550 ℃.
4. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in step (2), HNO 3 The concentration is 2-5 mol/L, the bulk graphite phase carbon nitride CN and 2-5 mol/L HNO 3 The mass/volume ratio of (A) is: 0.8 to 1.2:100g/mL.
5. The method of preparing aminated graphite phase carbon nitride nanosheets of claim 1, characterized by: in the step (2), the stirring temperature in the reflux device is 50-100 ℃, and the stirring time is 4-24 h.
6. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in the step (3), the mass/volume/mass ratio of the X-CCN, the toluene, the ethylenediamine and the N, N-dicyclohexylcarbodiimide added is 0.1-0.3: 5 to 15:10 to 30: 0.1-0.3 g/mL/mL/g.
7. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in the step (3), the reaction time in the oil bath is 12 to 36 hours.
8. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in the steps (1), (2) and (3), the drying temperature is 30-60 ℃, and the drying time is 6-12 h.
9. The method of preparing aminated graphite-phase carbon nitride nanosheets of claim 1, wherein: in the step (3), the inert gas is N 2 。
10. Use of aminated graphite-phase carbon nitride nanoplatelets prepared according to the process of any one of claims 1-9 in the reduction of carbon dioxide.
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