CN115672371B - Preparation method of aminated graphite phase carbon nitride nanosheets and application of aminated graphite phase carbon nitride nanosheets in reduction of carbon dioxide - Google Patents
Preparation method of aminated graphite phase carbon nitride nanosheets and application of aminated graphite phase carbon nitride nanosheets in reduction of carbon dioxide Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002135 nanosheet Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000009467 reduction Effects 0.000 title claims abstract description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 7
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 20
- 239000010439 graphite Substances 0.000 claims abstract description 20
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 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 21
- 238000005406 washing Methods 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 5
- 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
- 230000021523 carboxylation Effects 0.000 claims description 3
- 238000006473 carboxylation reaction Methods 0.000 claims description 3
- 239000002064 nanoplatelet Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 27
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 125000003277 amino group Chemical group 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- -1 carbon nitrides Chemical class 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 12
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002055 nanoplate Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
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- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000003197 catalytic effect Effects 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
- 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
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
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- 238000007146 photocatalysis Methods 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 nano-sheet and application thereof in carbon dioxide reduction, wherein bulk graphite phase carbon nitride CN is prepared firstly; the obtained bulk graphite phase carbon nitrides CN and HNO 3 Placing the mixture in a reaction container, and reacting in a reflux device to obtain carboxylated CN nanosheets X-CCN; dispersing X-CCN in toluene; ethylenediamine EDA and N, N-dicyclohexylcarbodiimide DCC are added into the X-CCN dispersion liquid under stirring, and react in an oil bath under the inert gas atmosphere to obtain the aminated graphite phase carbon nitride nano-sheet X-CN-EDA. The surface of the X-CN-EDA prepared by the invention is rich in amino groups, and is opposite to CO 2 Has strong adsorption capacity and can catalyze CO 2 Excellent reducing 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 aminated graphite phase carbon nitride nano sheet and application thereof in carbon dioxide reduction.
Background
Global energy supply relies mainly on carbon-rich fossil fuels, inevitably emitting large amounts of carbon dioxide CO 2 Thereby causing global warming. CO is processed by 2 Photocatalytic reduction to energy fuels is believed to reduce CO 2 An effective way of 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, the CO of CN 2 The reduction activity is very mild, and is not comparable to current noble metal-based photocatalysts. CO 2 The main limitation of photoreduction is CO 2 Weak adsorption capability, narrow visible light absorption range and low separation rate of photogenerated carriers. Even at high CO 2 In a reaction atmosphere of concentration, CO 2 Adsorption as a precondition also affects the final efficiency of the photoreduction.
To increase g-C 3 N 4 A great deal of modification work was done by researchers. However, most of themThe number modification work comprises morphology structure modulation, electronic structure optimization, preparation of a composite photocatalyst and the like, and focuses on widening g-C 3 N 4 And enhance the separation rate of photogenerated carriers. For CO 2 Adsorption construction of g-C 3 N 4 The basic photocatalyst has been relatively rarely studied.
Disclosure of Invention
The invention aims at providing a preparation method of an aminated graphite phase carbon nitride nano-sheet with simple process and a photocatalytic CO (carbon monoxide) prepared by the preparation method 2 Application of the reduction direction.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
the preparation method of the aminated graphite phase carbon nitride nano-sheet comprises the following steps:
step (1): heating urea from room temperature at a certain rate to a calcination temperature, and calcining for 2-4 h, wherein the calcination temperature is 450-600 ℃; after the calcination is finished, centrifugally washing and drying to obtain bulk phase graphite phase carbon nitride CN;
step (2): the bulk graphite phase carbon nitride CN with certain quality and HNO with certain concentration obtained in the step (1) are mixed 3 Placing in a reaction vessel, stirring at a certain temperature in a reflux device for a period of time, cooling to room temperature, centrifuging, washing, and oven drying to obtain carboxylated CN nanosheets X-CCN, wherein X represents CN in HNO 3 Wherein C represents carboxylation;
step (3): dispersing the X-CCN with a certain mass obtained in the step (2) in toluene with a certain volume; adding a certain volume of ethylenediamine EDA and a certain mass of N, N-dicyclohexylcarbodiimide DCC into the X-CCN dispersion liquid under stirring, and reacting for a period of time in an oil bath at 80-100 ℃ under the atmosphere of inert gas; 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 rising rate is 2 ℃/min.
Preferably, in step (1), the calcination temperature is 550 ℃.
As a best effortIn the optional scheme, in the step (2), HNO 3 The concentration is 2 to 5mol/L, and the bulk graphite phase carbon nitride CN and HNO are 2 to 5mol/L 3 The mass/volume ratio of (c) is: 0.8 to 1.2:100g/mL.
In the step (2), the temperature of stirring in the reflux device is 50-100 ℃, and the stirring time is 4-24 hours.
Preferably, in the step (3), the mass/volume/mass ratio of the addition of X-CCN, toluene, ethylenediamine, N-dicyclohexylcarbodiimide is 0.1 to 0.3: 5-15: 10-30: 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 h.
Further, the inert gas is N 2 。
The invention also protects the application of the aminated graphite phase carbon nitride nano-sheet 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 are low in price, and the preparation method is simple to operate and can be used for mass preparation;
(2) The X-CN-EDA surface of the invention is rich in amino groups and is opposite to CO 2 Has strong adsorption capacity and can catalyze CO 2 The reduction performance is excellent.
Therefore, the preparation of the aminated graphite phase carbon nitride nano-sheet has good application prospect.
Drawings
Fig. 1: a process map of X-CN-EDA formation;
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 for CN and X-CN-EDA 2 And (5) measuring reduction performance.
Detailed Description
The above-described matters of the present invention will be further described in detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
The experimental methods used in the examples below are conventional methods, and the reagents, methods and apparatus used are conventional in the art, unless otherwise indicated.
The invention provides a preparation method of an aminated graphite phase carbon nitride nano-sheet, which comprises the following steps:
step (1): heating urea from room temperature at a certain rate to a calcination temperature, and calcining for 2-4 h, wherein the calcination temperature is 450-600 ℃; after the calcination is finished, centrifugally washing and drying to obtain bulk phase graphite phase carbon nitride CN;
step (2): the bulk graphite phase carbon nitride CN with certain quality and HNO with certain concentration obtained in the step (1) are mixed 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 oven drying to obtain carboxylated CN nanosheets X-CCN, wherein X represents CN in HNO 3 Wherein C represents carboxylation;
step (3): dispersing the X-CCN with a certain mass obtained in the step (2) in toluene with a certain volume; adding a volume of ethylenediamine EDA and a mass of N, N-dicyclohexylcarbodiimide DCC to the X-CCN dispersion with stirring, and adding the mixture to the mixture at a concentration of N 2 Reacting for a period of time in an oil bath at 80-100 ℃ under the atmosphere; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-chip X-CN-EDA.
A diagram of the formation process of the X-CN-EDA of the present invention is shown in FIG. 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 calcining temperature, and calcining for 2-4 h, wherein the calcining temperature is 450-600 ℃; after the calcination is finished, centrifugally washing and drying to obtain bulk phase graphite phase carbon nitride CN;
example 2: preparation of 24-CCN-EDA
The bulk graphite phase carbon nitride CN obtained in example 1 was treated with 0.8 to 1.2g and 100mL of HNO 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 24 hours at 50-100 ℃ in a reflux device, cooling the mixture to room temperature, and centrifugally washing and drying the mixture to obtain carboxylated CN nano-platelets 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 are added to the 24-CCN dispersion with stirring, and the mixture is stirred in N 2 Reacting for 24 hours in an oil bath at 80-100 ℃ under the atmosphere; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-plate 24-CCN-EDA.
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 process of reduction, CO 2 Is critical for the adsorption capacity of 24-CN-EDA CO 2 The adsorption performance was tested and compared to 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 treated with 0.8 to 1.2g and 100mL of HNO 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 4 hours at 50-100 ℃ in a reflux device, cooling the mixture to room temperature, and centrifugally washing and drying the mixture to obtain carboxylated CN nano-chips 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 are added to the 4-CCN dispersion with stirring, and the mixture is stirred in N 2 Reacting for 24 hours in an oil bath at 80-100 ℃ under the atmosphere; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-plate 4-CCN-EDA.
4-CN-EDA was tested using X-ray diffraction and the test results are shown in FIG. 2.
Example 4: preparation of 8-CCN-EDA
The bulk graphite phase carbon nitride CN obtained in example 1 was treated with 0.8 to 1.2g and 100mL of HNO 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 8 hours at 50-100 ℃ in a reflux device, cooling the mixture to room temperature, and centrifugally washing and drying the mixture to obtain carboxylated CN nano-chips 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 are added to the 8-CCN dispersion with stirring, and the mixture is stirred in N 2 Reacting for 24 hours in an oil bath at 80-100 ℃ under the atmosphere; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-chip 8-CCN-EDA.
8-CN-EDA was tested using X-ray diffraction and the test results are shown in FIG. 2.
Example 5: preparation of 12-CCN-EDA
The bulk graphite phase carbon nitride CN obtained in example 1 was treated with 0.8 to 1.2g and 100mL of HNO 2 to 5mol/L 3 Placing the mixture into a round-bottom flask, stirring the mixture for 12 hours at 50-100 ℃ in a reflux device, cooling the mixture to room temperature, and centrifugally washing and drying the mixture to obtain carboxylated CN nano-chips 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-dicyclohexylcarbodiimide DCC are added to the 12-CCN dispersion with stirring, and the mixture is stirred in N 2 Reacting for 24 hours in an oil bath at 80-100 ℃ under the atmosphere; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-plate 12-CCN-EDA.
The 12-CN-EDA was tested using X-ray diffraction and the test results are shown in FIG. 2.
Example 6: preparation of 48-CCN-EDA
The bulk graphite phase carbon nitride CN obtained in example 1 was treated with 0.8 to 1.2g and 100mL of HNO 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, and centrifugally washing and drying the mixture to obtain carboxylated CN nano-platelets 48-CCN;
dispersing 0.1-0.3 g of the obtained 48-CCN in 5-15 mL of toluene; stirring while stirring10-30 mL of ethylenediamine EDA and 0.1-0.3 g of N, N-dicyclohexylcarbodiimide DCC are added to the 48-CCN dispersion under N 2 Reacting for 24 hours in an oil bath at 80-100 ℃ under the atmosphere; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain the aminated CN nano-plate 48-CCN-EDA.
48-CN-EDA was tested using X-ray diffraction and the test results are shown in FIG. 2.
Example 7: photocatalytic CO of X-CN-EDA 2 Reduction performance
The X-CN-EDA prepared by the embodiment of the invention comprises photocatalytic reduction CO of 4-CCN-EDA, 8-CCN-EDA, 12-CCN-EDA, 24-CCN-EDA and 48-CCN-EDA by adopting a Labsorar-6A full-glass automatic online micro-gas analysis system produced by Beijing poffy science and technology limited company and combining a Zhejiang Fuli GC 9790 II gas chromatograph to detect the reduction product 2 The performance is tested and compared with the catalytic capability of the bulk graphite phase carbon nitride CN, and the detection result is shown in figure 4, so that 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 the bulk CN, indicating that the amino groups contained in EDA are beneficial for photocatalytic CO 2 Reduction activity. 24-CN-EDA photocatalyst shows optimal photocatalytic CO 2 The reduction performance, CO yield, was 8.58. Mu. Mol/g, 5.92 times that of the bulk CN (1.45. Mu. Mol/g). Notably, the 48-CN-EDA sample showed a slight decrease, but was still significantly higher than bulk CN, probably because excessive EDA functionalization would mask active sites on the bulk CN surface.
The present invention is not limited to the preferred embodiments, and any simple modification, equivalent replacement, and improvement made to the above embodiments by those skilled in the art without departing from the technical scope of the present invention, will fall within the scope of the present invention.
Claims (8)
1. The preparation method of the aminated graphite phase carbon nitride nanosheets is characterized by comprising the following steps of: the method comprises the following steps:
step (1): heating urea from room temperature at a certain rate to a calcination temperature, and calcining for 2-4 hours, wherein the calcination temperature is 450-600 ℃; after the calcination is finished, centrifugally washing and drying to obtain bulk phase graphite phase carbon nitride CN;
step (2): the bulk graphite phase carbon nitride CN with certain quality and HNO with certain concentration obtained in the step (1) are mixed 3 Placing in a reaction vessel, stirring at a certain temperature in a reflux device for a period of time, cooling to room temperature, centrifuging, washing, and oven drying to obtain carboxylated CN nanosheets X-CCN, wherein X represents CN in HNO 3 Wherein C represents carboxylation;
step (3): dispersing the X-CCN with a certain mass obtained in the step (2) in toluene with a certain volume; adding a certain volume of ethylenediamine EDA and a certain mass of N, N-dicyclohexylcarbodiimide DCC into the X-CCN dispersion liquid under stirring, and reacting for a period of time in an oil bath at 80-100 ℃ under the atmosphere of inert gas; after the reaction is finished, cooling to room temperature, centrifugally washing and drying to obtain an aminated graphite phase carbon nitride nanosheet X-CN-EDA;
HNO 3 the concentration is 2-5 mol/L, and the bulk graphite phase carbon nitride CN and HNO are 2-5 mol/L 3 The mass/volume ratio of (c) is: 0.8-1.2: 100 g/mL;
in the step (2), the temperature of stirring in the reflux device is 50-100 ℃, and the stirring time is 4-24 hours.
2. The method for preparing the aminated graphite phase carbon nitride nanosheets according to claim 1, wherein: in the step (1), the temperature rising rate is 2 ℃ per minute.
3. The method for preparing the aminated graphite phase carbon nitride nanosheets according to claim 1, wherein: in step (1), the calcination temperature was 550 ℃.
4. The method for preparing the aminated graphite phase carbon nitride nanosheets according to claim 1, wherein: in the step (3), the mass/volume/mass ratio of the addition of the X-CCN, toluene, ethylenediamine and N, N-dicyclohexylcarbodiimide is 0.1-0.3: 5-15: 10-30: 0.1 to 0.3g/mL/mL/g.
5. The method for preparing the aminated graphite phase carbon nitride nanosheets according to claim 1, wherein: in the step (3), the reaction time in an oil bath is 12-36 h.
6. The method for preparing the aminated graphite phase carbon nitride nanosheets according to claim 1, wherein: in the step (1), the step (2) and the step (3), the drying temperature is 30-60 ℃ and the drying time is 6-12 h.
7. The method for preparing the aminated graphite phase carbon nitride nanosheets according to claim 1, wherein: in the step (3), the inert gas is N 2 。
8. Use of the aminated graphite-phase carbon nitride nanoplatelets prepared by the method of any one of claims 1 to 7 in carbon dioxide reduction.
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