CN115888789A - Carbon nitride photocatalyst of composite heterogeneous elements Na, P and O, preparation method and application - Google Patents
Carbon nitride photocatalyst of composite heterogeneous elements Na, P and O, preparation method and application Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 60
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 59
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011734 sodium Substances 0.000 claims abstract description 59
- ASTWEMOBIXQPPV-UHFFFAOYSA-K trisodium;phosphate;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[O-]P([O-])([O-])=O ASTWEMOBIXQPPV-UHFFFAOYSA-K 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003837 high-temperature calcination Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000013329 compounding Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 230000008859 change Effects 0.000 abstract description 4
- 239000000969 carrier Substances 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 125000004093 cyano group Chemical group *C#N 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000010571 fourier transform-infrared absorption spectrum Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention belongs to the technical field of photocatalytic materials, and discloses a carbon nitride photocatalyst for compounding heterogeneous elements Na, P and O, and a preparation method and application thereof. Using dicyanodiamine and sodium phosphate dodecahydrate as raw materials, and calcining at high temperature in a muffle furnace in an atmospheric environment; and washing the calcined product to obtain the carbon nitride of the composite heterogeneous elements Na, P and O. Compared with common carbon nitride, the carbon nitride of the composite heterogeneous elements Na, P and O prepared by the invention can effectively replace the position of a nitrogen atom in the carbon nitride and then is doped into a carbon nitride skeleton, and Na enters the gap position of the carbon nitride, so that the carbon nitride of the composite heterogeneous elements Na, P and O has a corrected conduction band position and a corrected valence band position. Meanwhile, the introduction of Na, P and O can change the electronic structure of the carbon nitride and effectively inhibit the recombination of photon-generated carriers, thereby greatly improving the photocatalytic performance of the carbon nitride. The preparation method is simple, has extremely high yield, is simple to operate, easy to control, good in repeatability, green and environment-friendly, and is beneficial to industrial large-scale production.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to a carbon nitride photocatalyst of composite heterogeneous elements of Na, P and O, and a preparation method and application thereof.
Background
In recent years, with the development of socio-economic, a larger development space is brought to the development of industrial enterprises. However, as people have a transition fell in natural resources, the problems of shortage of natural resources and environmental pollution become more serious. The photocatalysis technology is an environment-friendly green technology, can efficiently utilize solar energy to treat environmental problems, has good thermal stability and chemical stability, and is considered by broad scholars as an effective method for relieving energy crisis and solving energy problems under the conditions that environmental pollution is increasingly serious and energy is deficient. At present, tiO 2 Has become the most popular and widely used photocatalyst, but the weak activity in the visible light range greatly limits the practical application of the photocatalyst. To overcome these disadvantages, a large number of narrow Bandgap Semiconductors (BiVOs) 4 CdS and C 3 N 4 Etc.) have been developed to effectively utilize visible light.
The macromolecular carbon nitride material only consisting of carbon and nitrogen elements abundant on the earth is an attractive material due to good visible light absorption capacity and good light corrosion resistance. Suitable band position (E) CB ＝-1.3V NHE ，E VB ＝1.4V NHE PH = 7), is thermodynamically suitable for water decomposition, oxygen Reduction Reaction (ORR), and degradation of organic pollutants. However, since the carrier recombination efficiency is high, the light conversion efficiency is low. Therefore, various strategies, such as morphology control, band gap engineering, co-catalyst loading, and the combination of heterogeneous elements, have been extensively studied to improve their photocatalytic activity. Among the above strategies, complex heterogeneous elements are considered as common and effective means of modification. On the one hand, complex heterogeneous elementsCarbon nitride of Na, P, O has more positive conduction band and valence band positions. In addition, the introduction of Na, P and O heterogeneous elements can change the electronic structure of the carbon nitride and effectively inhibit the recombination of photon-generated carriers, thereby greatly improving the photocatalytic performance of the carbon nitride.
At present, carbon nitride for compounding heterogeneous elements Na, P and O is not reported.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nitride photocatalyst for compounding heterogeneous elements Na, P and O, which obtains a product after high-temperature calcination by a one-step calcination method, and can directly obtain the carbon nitride photocatalyst for compounding the heterogeneous elements Na, P and O after fully washing the product. The introduction of Na, P and O heterogeneous elements can change the electronic arrangement of the elements, thereby causing the structural change of energy bands and solving the problems that the existing photocatalyst has low utilization rate of visible light, few active sites and produces H 2 O 2 Low selectivity and efficiency, etc.
The technical scheme for realizing the aim of the invention is as follows:
the preparation method of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O introduces the heterogeneous elements Na, P and O in situ by a one-step calcination method to synthesize the carbon nitride of the composite heterogeneous elements Na, P and O, and comprises the following steps:
(1) Firstly, placing dicyanodiamine and sodium phosphate dodecahydrate into a mortar to be fully ground to be uniform;
(2) Adding a certain amount of uniformly ground mixture into a crucible, putting the crucible into a muffle furnace, heating the crucible to a certain temperature at a certain heating speed, and keeping the crucible for a certain time;
(3) And fully washing and drying the product after high-temperature calcination to obtain the carbon nitride of the composite heterogeneous elements Na, P and O.
In the step (1), the mass ratio of dicyanodiamine to sodium phosphate dodecahydrate is 0.5-2:0.1-2.
In the step (1), the grinding time is 15-30 min.
In the step (2), the heating temperature in the muffle furnace is 450-550 ℃, and the holding time is 2-5h; the temperature rising speed is 1-4 ℃/min.
The carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O prepared by the invention is used for preparing H 2 O 2 In particular to the preparation of H by using isopropanol as a sacrificial agent under the air condition and utilizing water and oxygen in the air 2 O 2 。
Compared with the prior art, the invention has the following remarkable advantages:
1. the material successfully introduces Na, P and O heterogeneous elements, optimizes the electronic structure and the energy band position of the material, greatly improves the separation and migration efficiency of photon-generated carriers, and improves the generation of H by the material 2 O 2 The ability of the cell to perform.
2. The preparation method of the material has no special requirements on equipment, has extremely high yield, is simple to operate, easy to control and good in repeatability, and is beneficial to industrial large-scale production.
Drawings
FIG. 1 is an X-ray diffraction pattern of the composite heterogeneous element Na, P, O carbon nitride photocatalyst prepared in this example;
FIG. 2 is a Fourier transform infrared absorption spectrum (FTIR) of the composite heterogeneous element Na, P, O carbon nitride photocatalyst prepared in this example;
FIG. 3 is the X-ray photoelectron spectrum (XPS) of the composite heterogeneous Na, P, O carbon nitride photocatalyst prepared in this example;
FIG. 4 is the valence band spectrum of X-ray photoelectron spectroscopy (XPS) of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O prepared by the present example;
FIG. 5 is the Mott Schottky curve (MS) of the composite heterogeneous Na, P, O carbon nitride photocatalyst prepared in this example;
FIG. 6 is a steady-state fluorescence spectrum (PL) of the composite heterogeneous element Na, P, O carbon nitride photocatalyst prepared in this example;
FIG. 7 is a photo current diagram of the carbon nitride photocatalyst containing heterogeneous elements Na, P and O prepared in this example;
FIG. 8 shows the photocatalytic production of H by the carbon nitride photocatalyst containing composite heterogeneous elements Na, P and O prepared in this example 2 O 2 And (4) an activity graph.
Detailed Description
The invention is explained in further detail below with reference to the drawing.
Comparative example
The first step is as follows: placing 2g of dicyanodiamine in a mortar and fully grinding the mixture until the mixture is uniform;
the second step: adding a certain amount of uniformly ground mixture into the crucible, putting the crucible into a muffle furnace, heating the crucible to 550 ℃ at the temperature rising speed of 2 ℃/min, and keeping the temperature for 4 hours;
the third step: washing the product after high-temperature calcination with distilled water for 10 times, and drying to obtain the carbon nitride CN.
Example 1
The preparation method of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O comprises the following steps:
the first step is as follows: placing 2g of dicyanodiamine and 0.25g of sodium phosphate dodecahydrate in a mortar and fully grinding the mixture until the mixture is uniform;
the second step is that: adding a certain amount of uniformly ground mixture into a crucible, putting the crucible into a muffle furnace, heating to 550 ℃ at a heating rate of 2 ℃/min, and keeping for 4 hours;
the third step: washing the product after high-temperature calcination with distilled water for 10 times, and drying to obtain the carbon nitride of the composite heterogeneous elements Na, P and O, which is marked as 0.25Na-CN.
Example 2
The preparation method of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O comprises the following steps:
the first step is as follows: 2g of dicyanodiamine and 0.75g of sodium phosphate dodecahydrate are put into a mortar and sufficiently ground to be uniform;
the second step: adding a certain amount of uniformly ground mixture into a crucible, putting the crucible into a muffle furnace, heating to 550 ℃ at a heating rate of 2 ℃/min, and keeping for 4 hours;
the third step: washing the product after high-temperature calcination with distilled water for 10 times, and drying to obtain the carbon nitride of the composite heterogeneous elements Na, P and O, which is marked as 0.75Na-CN.
Example 3
The preparation method of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O comprises the following steps:
the first step is as follows: placing 2g of dicyanodiamine and 1.25g of sodium phosphate dodecahydrate in a mortar and fully grinding to be uniform;
the second step is that: adding a certain amount of uniformly ground mixture into a crucible, putting the crucible into a muffle furnace, heating to 550 ℃ at a heating rate of 2 ℃/min, and keeping for 4 hours;
the third step: washing the product after high-temperature calcination with distilled water for 10 times, and drying to obtain the carbon nitride of the composite heterogeneous elements Na, P and O, which is marked as 1.25Na-CN.
FIG. 1 shows the X-ray diffraction patterns of the composite heterogeneous elements Na, P, O of the carbon nitride photocatalyst prepared in examples 1-3. The ordinary carbon nitride has diffraction peaks characteristic to carbon nitride at 13.1 ° and 27.3 °, whereas the diffraction peaks at 13.1 ° for carbon nitride of the complex heterogeneous elements Na, P, O are hardly observed, indicating that the carbon nitride of the complex heterogeneous elements Na, P, O has a small interlayer plane size.
FIG. 2 is a Fourier transform infrared absorption spectrum (FTIR) of the composite heterogeneous element Na, P, O carbon nitride photocatalyst prepared in the examples 1-3. Compared with common carbon nitride, the carbon nitride for compounding heterogeneous elements of Na, P and O is 2180cm -1 A distinct infrared peak appears, which is a characteristic peak of the cyano group formed due to the nitrogen defect.
Fig. 3 is an X-ray photoelectron spectrum (XPS) of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P, O prepared in this example 3. From the spectra, the presence of Na and P was confirmed. In addition, compared with common carbon nitride, the content of the O element is obviously improved.
FIG. 4 is the valence band spectrum (XPS) of the carbon nitride photocatalyst containing composite heterogeneous elements Na, P and O prepared in the example 3. It is obvious from the spectrogram that the valence band position of the carbon nitride of the composite heterogeneous elements Na, P and O is more positive than that of the common carbon nitride, and the composite heterogeneous elements have stronger oxidation capability.
FIG. 5 shows the Mott-based curves (MS) of the composite heterogeneous Na, P, O carbon nitride photocatalysts prepared in examples 1-3. From the spectrogram, the flat band potential of the carbon nitride for compounding the heterogeneous elements Na, P and O is more and more positive along with the increase of the amount of the heterogeneous elements, which shows that the conduction band position of the carbon nitride is positively shifted along with the increase of the content of the heterogeneous elements, and the fact that the energy band position of the catalyst is effectively changed by the compounding of the heterogeneous elements is fully shown.
FIG. 6 shows the steady-state fluorescence spectrum (PL) of the composite heterogeneous element Na, P, O carbon nitride photocatalyst prepared in this example 3. The spectrogram shows that the signal intensity of the carbon nitride for compounding the heterogeneous elements Na, P and O is obviously lower than that of the common carbon nitride, which shows that the carrier compounding efficiency of the carbon nitride for compounding the heterogeneous elements Na, P and O is obviously reduced, and the method is favorable for improving the photocatalytic H production 2 O 2 The efficiency of (c).
FIG. 7 is a photo current diagram of the carbon nitride photocatalyst containing heterogeneous elements Na, P and O prepared in the embodiments 1-3. The carbon nitride of the composite heterogeneous elements Na, P and O has stronger photocurrent intensity (wherein the photocurrent intensity is strongest when sodium phosphate dodecahydrate is added in an amount of 1.25 g), and also keeps good stability after the light is turned on and off for eight times, which shows that the carbon nitride has better photoelectric carrier separation efficiency, thereby promoting the photocatalytic H production 2 O 2 The efficiency of (c).
FIG. 8 shows the photocatalytic production of H by the carbon nitride photocatalyst containing heterogeneous Na, P, O elements prepared in examples 1-3 2 O 2 And (4) an activity diagram. The method specifically comprises the following steps: under the air condition, 25mg of carbon nitride of composite heterogeneous elements Na, P and O is weighed and dispersed in 25ml of mixed solvent (water: isopropanol =9 = 1) in a photocatalysis way, and the reaction system is stirred magnetically for 30min under the dark condition to reach the adsorption equilibrium. After the dark reaction is complete, the light source (300W xenon lamp lambda) is turned on>420 nm), 1mL of sample is extracted every 10min, after centrifugation, the supernatant is aspirated and measured by colour development at 551nm, and the data are recorded. The results show that: carbon nitride of complex heterogeneous elements Na, P, O exhibits greater photocatalytic production of H than ordinary carbon nitride 2 O 2 The ability of the cell to perform. After 1 hour of light, it (when 1.25g of sodium phosphate dodecahydrate was added) produced H 2 O 2 The amount of (a) is approximately 17 times that of ordinary carbon nitride.
Claims (7)
1. The preparation method of the carbon nitride photocatalyst of the composite heterogeneous elements Na, P and O is characterized in that the heterogeneous elements Na, P and O are introduced in situ by a one-step calcination method to synthesize the carbon nitride of the composite heterogeneous elements Na, P and O, and comprises the following steps:
(1) Firstly, placing dicyanodiamine and sodium phosphate dodecahydrate into a mortar and fully grinding the mixture to be uniform;
(2) Adding a certain amount of uniformly ground mixture into a crucible, putting the crucible into a muffle furnace, heating the crucible to a certain temperature at a certain heating speed, and keeping the crucible for a certain time;
(3) And fully washing and drying the product after high-temperature calcination to obtain the carbon nitride of the composite heterogeneous elements Na, P and O.
2. The method of claim 1, wherein: in the step (1), the mass ratio of dicyanodiamine to sodium phosphate dodecahydrate is 0.5-2:0.1-2.
3. The method of claim 1, wherein: in the step (1), the grinding time is 15-30 min.
4. The method of claim 1, wherein: in the step (2), the heating temperature in the muffle furnace is 450-550 ℃, and the holding time is 2-5h; the temperature rising speed is 1-4 ℃/min.
5. A carbon nitride photocatalyst which is a composite of heterogeneous elements Na, P and O, characterized in that it is produced by the production method according to any one of claims 1 to 4.
6. Use of the composite heteroelement of Na, P, O of claim 5 as a photocatalyst for the preparation of H 2 O 2 The use of (1).
7. Use according to claim 6, characterised in that water and air are used under atmospheric conditions, using isopropanol as sacrificial agentOxygen production of H 2 O 2 The use of (1).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389450A (en) * | 2020-05-13 | 2020-07-10 | 中国农业科学院烟草研究所 | Phosphorus-doped carbon nitride material and preparation method and application thereof |
| CN113457713A (en) * | 2021-07-09 | 2021-10-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon nitride based single-atom catalyst, product and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389450A (en) * | 2020-05-13 | 2020-07-10 | 中国农业科学院烟草研究所 | Phosphorus-doped carbon nitride material and preparation method and application thereof |
| CN113457713A (en) * | 2021-07-09 | 2021-10-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon nitride based single-atom catalyst, product and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| LANG DENG ET AL.: ""Improved performance of photosynthetic H2O2 and photodegradation by K-, P-, O-, and S-co-doped g-C3N4 with enhanced charge transfer ability under visible light"", 《APPLIED SURFACE SCIENCE》, vol. 597, pages 2 * |
| LULU BAI ET AL.: ""Supported Ru Single Atoms and Clusters on P-Doped Carbon Nitride as an Efficient Photocatalyst for H2O2 Production"", 《CHEMCATCHEM》, vol. 14, pages 6 * |
| SHAOWEN CAO ET AL.: ""Trace-level phosphorus and sodium co-doping of g-C3N4 for enhanced photocatalytic H2 production"", 《JOURNAL OF POWER SOURCES》, vol. 351, pages 151 - 157 * |
| 马元功等: ""磷掺杂石墨相氮化碳及其光催化性能研究"", 《化工新型材料》, vol. 48, no. 4, pages 1 * |
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