CN113318789A - Preparation of pyridyl COFs nanosheet for photocatalytic total hydrolysis - Google Patents
Preparation of pyridyl COFs nanosheet for photocatalytic total hydrolysis Download PDFInfo
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- 239000013310 covalent-organic framework Substances 0.000 title claims abstract description 36
- 125000004076 pyridyl group Chemical group 0.000 title claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 21
- 239000002135 nanosheet Substances 0.000 title claims abstract description 19
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000002105 nanoparticle Substances 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- QEIRCDAYPQFYBI-UHFFFAOYSA-N 6-(5-aminopyridin-2-yl)pyridin-3-amine Chemical compound N1=CC(N)=CC=C1C1=CC=C(N)C=N1 QEIRCDAYPQFYBI-UHFFFAOYSA-N 0.000 claims description 3
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 238000007872 degassing Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 3
- 229960001553 phloroglucinol Drugs 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000002055 nanoplate Substances 0.000 claims 4
- 238000000527 sonication Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000011941 photocatalyst Substances 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 3
- 230000032798 delamination Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- -1 3mLN Chemical compound 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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Abstract
The invention relates to preparation of pyridyl COFs nano-sheets for photocatalytic total hydrolysis. The invention provides a preparation method of pyridyl COFs nano-sheets for photocatalytic total hydrolysis. According to the invention, platinum nanoparticles are loaded on pyridyl COFs materials by an in-situ method, and the obtained composite material is prepared into a two-dimensional nanosheet shape by an ultrasonic delamination method. Due to the uniqueness of the structure and the shape of the material, the material can be used as a photocatalyst to carry out photocatalytic full-hydrolysis reaction, and the full-hydrolysis hydrogen production and oxygen production rate can reach 130 mu mol/g/h and 64 mu mol/g/h under the irradiation of visible light.
Description
Technical Field
The invention relates to preparation of pyridyl COFs nano-sheets for photocatalytic total hydrolysis.
Background
At present, the energy crisis and environmental pollution problem have been spread all over the world, and the exploration of new green energy technology and the adjustment of energy structure are imminent. Solar energy is an inexhaustible natural energy, and the energy irradiated to the earth per second is equivalent to the energy generated by burning 500 ten thousand tons of coal. Photocatalytic materialThe water splitting is a process of simulating green plant photosynthesis, and the water is split into hydrogen and oxygen by taking solar energy as driving force under the action of a catalyst, so that the hydrogen energy is stored and utilized. The hydrogen energy does not produce secondary pollution in the preparation, storage and utilization projects, and is the most ideal environment-friendly energy. Therefore, the photocatalytic full-hydrolysis is one of effective schemes for fundamentally solving the problems of energy shortage and environmental pollution. Although using conventional semiconductor TiO2，SrTiO3The high-efficiency full water hydrolysis under the excitation of ultraviolet light is realized, but the ultraviolet light accounts for only about 5% of the solar spectrum, so the catalytic efficiency of the catalyst is low. Therefore, designing and constructing a photocatalyst which can be effectively hydrolyzed completely under the drive of visible light and has high cyclicity is always the most challenging research direction in the field of photocatalysis.
Covalent Organic Frameworks (COFs) are emerging organic semiconductor materials, and the structure of the COFs is mainly formed by connecting light elements such as C, N, O, B through reversible covalent bonds, is in a periodic arrangement, and is a crystalline porous material with high crystallinity and porosity. COFs have excellent solvent stability and acid-base stability, and can be used as a catalyst for recycling under most severe conditions. In addition, the structural characteristics of porosity and high specific surface area furthest expose reactive active sites, shorten the transmission distance of photo-generated electrons to the active sites, and are favorable for the adsorption of substrates and the escape of products. More importantly, the energy level and the framework structure of the COFs are adjustable, and the structural units and chemical bonds of the framework are adjusted and controlled according to reaction requirements, so that the COFs structure with specific active sites and energy level structures can be synthesized in a targeted mode. Therefore, in recent years, COFs have been widely studied as ideal photocatalysts.
Disclosure of Invention
The invention aims to provide a preparation method of pyridyl COFs nano-sheets for photocatalytic total hydrolysis.
The preparation method of the pyridyl COFs nanosheet for photocatalytic total hydrolysis is completed according to the following steps:
firstly, adding a mixed solution consisting of 1,3, 5-trialdehyde phloroglucinol, [2,2 '-bipyridine ] -5,5' -diamine, o-dichlorobenzene, N-dimethylacetamide and a platinum nanoparticle-containing N, N-dimethylacetamide colloidal solution into a 10mL heat-resistant glass tube in sequence, carrying out ultrasonic treatment for 10-15 minutes, adding an acetic acid aqueous solution, rapidly freezing in 77K (liquid nitrogen bath), degassing through three times of freeze-thaw cycle, heating at 120-150 ℃ for 72-120 hours in a vacuum sealing state, filtering, washing with N, N-dimethylacetamide, water and acetone until the filtrate is colorless, carrying out solvent exchange with acetone, and carrying out vacuum drying at 50 ℃ for 24 hours to obtain pyridyl COFs;
dispersing the pyridyl COFs in the step one in water to form a suspension, carrying out ultrasonic treatment on the suspension to realize stripping, and drying to obtain pyridyl COFs nanosheets, wherein the pyridyl COFs nanosheets are used for photocatalytic full-water decomposition to generate hydrogen and oxygen;
step one, the volume ratio of the o-dichlorobenzene to the N, N-dimethylacetamide is 1: 3;
the concentration of the N, N-dimethylacetamide colloidal solution containing platinum nanoparticles is 2-3 mg/mL;
step one, the volume ratio of the platinum nanoparticles to the N, N-dimethylacetamide is 11.4-81.3 v/v%;
secondly, the concentration of the suspension is 5-10 mg/mL;
the ultrasonic time of the second step is 30-60 minutes;
and step two, the drying time is 12-24 hours.
The invention has the beneficial effects that:
according to the invention, platinum nanoparticles are loaded on a pyridyl COFs material by an in-situ method, and the obtained composite material is prepared into a two-dimensional nanosheet shape by an ultrasonic delamination method, so that the composite material can be used as a photocatalyst to perform photocatalytic full-splitting reaction on water due to the uniqueness of the material structure and shape, and the water is split into hydrogen and oxygen.
Drawings
FIG. 1X-ray powder diffraction pattern of an embodiment 1 of the present invention;
FIG. 2 is an infrared spectrum of an embodiment 1 of the present invention;
FIG. 3 is a diagram showing the photocatalytic full-hydrolysis performance of example 1 of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are merely illustrative of the process of the invention and are not intended to limit the scope of the invention in any way.
Example 1: the preparation method of the pyridyl COFs nanosheet for photocatalytic total hydrolysis is completed according to the following steps:
adding a mixed solution consisting of 42.0mg of 1,3, 5-trialdehyde phloroglucinol, 32.7mg of [2,2 '-bipyridine ] -5,5' -diamine, 1mL of o-dichlorobenzene, 3mLN, N-dimethylacetamide and a platinum nanoparticle-containing N, N-dimethylacetamide colloidal solution (2.2mg/mL, 0.79mL) into a 10mL heat-resistant glass tube in sequence, carrying out ultrasonic treatment for 10-15 minutes to obtain a uniform dispersion, adding 0.4mL of an acetic acid aqueous solution (6mol/L), rapidly freezing in 77K (liquid nitrogen bath), degassing through three times of circulation, heating at 120 ℃ for 72 hours in a vacuum sealing state, filtering, washing the filtrate with N, N-dimethylacetamide, water and acetone until the filtrate is colorless, carrying out solvent exchange by using acetone, carrying out vacuum drying at 50 ℃ for 24 hours to obtain pyridyl COFs, dispersing the pyridine-based COFs into water to form suspension with the concentration of 7.5mg/mL, carrying out ultrasonic treatment on the suspension for 60 minutes to realize stripping, drying for 12 hours to obtain the pyridine-based COFs nanosheet, and using the pyridine-based COFs nanosheet for photocatalytic total water decomposition to generate hydrogen and oxygen.
To verify the beneficial effects of the present invention, the following tests were performed:
in order to examine the photocatalytic full-hydrolysis effect of the pyridyl COFs nanosheets under visible light, the photocatalytic full-hydrolysis performance test is carried out according to the following method. The test procedure was as follows: 15mg of solid catalyst and 50mL of H were weighed2O, placed in a reactor, and the reaction system was evacuated for 30 minutes to remove dissolved gases and ensure vacuum conditions, and a photocatalytic total hydrolysis experiment was performed at 10 ℃. As shown in FIG. 3, the hydrogen and oxygen release rates reached 130. mu. mol/g/h and 64. mu. mol/g/h, respectively.
Claims (7)
1. Preparation of pyridyl COFs nano-sheet for photocatalytic total hydrolysis, which is characterized by comprising the following steps:
firstly, adding a mixed solution consisting of 1,3, 5-trialdehyde phloroglucinol, [2,2 '-bipyridine ] -5,5' -diamine, o-dichlorobenzene, N-dimethylacetamide and a platinum nanoparticle-containing N, N-dimethylacetamide colloidal solution into a 10mL heat-resistant glass tube in sequence, carrying out ultrasonic treatment for 10-15 minutes, adding an acetic acid aqueous solution, rapidly freezing in 77K (liquid nitrogen bath), degassing through three times of freeze-thaw cycle, heating at 120-150 ℃ for 72-120 hours in a vacuum sealing state, filtering, washing with N, N-dimethylacetamide, water and acetone until the filtrate is colorless, carrying out solvent exchange with acetone, and carrying out vacuum drying at 50 ℃ for 24 hours to obtain pyridyl COFs;
and secondly, dispersing the pyridyl COFs in the step one in water to form turbid liquid, carrying out ultrasonic treatment on the turbid liquid to realize stripping, and drying to obtain pyridyl COFs nano sheets which are used for photocatalytic full-water decomposition to generate hydrogen and oxygen.
2. Preparation of pyridyl COFs nanoplates according to claim 1, characterized in that the volume ratio of o-dichlorobenzene to N, N-dimethylacetamide in step one is 1: 3.
3. The preparation of pyridyl COFs nano-sheet according to claim 1, wherein the concentration of the N, N-dimethylacetamide colloidal solution containing platinum nano-particles in the step one is 2-3 mg/mL.
4. The preparation of pyridyl COFs nanoplates according to claim 1, wherein the volume ratio of the platinum nanoparticles to N, N-dimethylacetamide in the first step is 11.4-81.3 v/v%.
5. The preparation of pyridyl COFs nano-sheet according to claim 1, wherein the concentration of the suspension in the second step is 5-10 mg/mL.
6. Preparation of pyridyl COFs nanoplates according to claim 1, characterised in that the sonication time in step two is 30-60 minutes.
7. Preparation of pyridyl COFs nanoplates according to claim 1, characterised in that the drying time in step two is 12-24 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114225963A (en) * | 2021-12-18 | 2022-03-25 | 复旦大学 | Ketone enamine covalent organic framework photocatalyst and preparation method and application thereof |
| CN115007207A (en) * | 2022-06-04 | 2022-09-06 | 哈尔滨理工大学 | Preparation of BiNPs/TpBpy composite material and photocatalytic carbon dioxide reduction |
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2021
- 2021-06-29 CN CN202110727408.9A patent/CN113318789A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114225963A (en) * | 2021-12-18 | 2022-03-25 | 复旦大学 | Ketone enamine covalent organic framework photocatalyst and preparation method and application thereof |
| CN114225963B (en) * | 2021-12-18 | 2024-04-26 | 复旦大学 | Ketone enamine covalent organic framework photocatalyst and preparation method and application thereof |
| CN115007207A (en) * | 2022-06-04 | 2022-09-06 | 哈尔滨理工大学 | Preparation of BiNPs/TpBpy composite material and photocatalytic carbon dioxide reduction |
| CN115007207B (en) * | 2022-06-04 | 2023-11-21 | 哈尔滨理工大学 | Preparation of BiNPs/TpBpy composite material and photocatalytic carbon dioxide reduction |
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