CN117225475A - UiO-66-NH 2 Preparation of IISERP-COF12 composite material and photocatalytic carbon dioxide reduction - Google Patents
UiO-66-NH 2 Preparation of IISERP-COF12 composite material and photocatalytic carbon dioxide reduction Download PDFInfo
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- CN117225475A CN117225475A CN202311176959.6A CN202311176959A CN117225475A CN 117225475 A CN117225475 A CN 117225475A CN 202311176959 A CN202311176959 A CN 202311176959A CN 117225475 A CN117225475 A CN 117225475A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 230000009467 reduction Effects 0.000 title claims abstract description 21
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 20
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 16
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims description 10
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 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 4
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 4
- 229960001553 phloroglucinol Drugs 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000007872 degassing Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000010257 thawing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 239000012621 metal-organic framework Substances 0.000 abstract description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 abstract description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract description 2
- 230000006798 recombination Effects 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 229910052724 xenon Inorganic materials 0.000 abstract 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000013310 covalent-organic framework Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- SKQLOMUIRYYJEZ-UHFFFAOYSA-N 2,6-diaminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC(N)=C1C(O)=O SKQLOMUIRYYJEZ-UHFFFAOYSA-N 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Abstract
The invention aims to solve the problems of low photocatalytic carbon dioxide reduction efficiency and easy recombination of photo-generated electrons and holes of the existing material, and provides a UiO-66-NH 2 Preparation of the IISERP-COF12 composite material and photocatalytic carbon dioxide reduction. The method comprises the following steps: 1. method for preparing UIO-66-NH by solvothermal method 2 MOFs materials; 2. by in situ addition of UiO-66-NH 2 Synthesis of UiO-66-NH 2 IISERP-COF12 composite. The invention provides a UiO-66-NH 2 Carbon dioxide reduction photocatalyst material of/IISERP-COF 12 composite material has carbon monoxide generation rate of up to 109.21 mu mol under irradiation of 300W xenon lamp visible light·g‑ 1 ·h ‑1 Is UiO-66-NH 2 22.66 times the material is 3.5 times the IISERP-COF12 material. The invention can improve the problem that the photo-generated electrons and the holes are easy to be combined and remarkably improve the reduction efficiency of the whole material.
Description
Technical Field
The invention relates to a UiO-66-NH 2 Preparation of the IISERP-COF12 composite material and photocatalytic carbon dioxide reduction.
Background
At present, along with the rapid development of global economy and the continuous increase of global population, the demand for global energy is continuously increased, and the massive combustion of fossil energy and the massive emission of automobile tail gas have great influence on global energy and environmental problems, so that the energy shortage and environmental pollution become the common problems of people worldwide. Wherein the main substance responsible for this situation is CO 2 In the followingIn this context, it is becoming more urgent to find clean and renewable energy sources to replace increasingly depleted fossil energy sources. And CO 2 There are many conversion processes for CO by photocatalysis in recent years 2 The transformation is undoubtedly the most cleanly efficient way. However, the existing photocatalyst has low light utilization rate, electrons and holes are easy to recombine, and the utilization of solar energy is limited. Therefore, it is urgent to develop a novel high-efficiency photocatalyst capable of maximally utilizing visible light.
The metal organic frameworks (Metal OrganicFrameworks, MOFs for short) are organic-inorganic hybrid porous crystalline materials with two-dimensional or three-dimensional structures, which are coordination compounds formed by taking metal ions or metal clusters as connecting points and coordinating with organic ligands. Due to its unique electronic band structure, customizable light absorption, high CO 2 Adsorption and high specific surface area, MOFs materials are often used as supports for photocatalysts or photocatalytic applications. Its unique electronic band structure also provides suitable conditions for the formation of heterostructures.
Covalent Organic Frameworks (COFs) are porous crystalline polymers with modularization, porosity, crystallinity, structural adjustability and semiconductor characteristics, so that COFs have potential application prospects in various fields of gas adsorption and separation, catalysis, sensing, energy storage, photoelectric conversion and the like and are widely developed. However, the COFs photocatalyst of the individual component has a problem of low visible light utilization, which limits the catalysis of CO by the COFs photocatalyst 2 Further improvement of the reduction activity. Thus, a photocatalytic CO was developed 2 Materials with high reduction efficiency have become a research hotspot.
Disclosure of Invention
The invention aims to solve the problems of low photocatalytic carbon dioxide reduction efficiency and easy recombination of photo-generated electrons and holes of the existing material, and provides a UiO-66-NH 2 Preparation of the IISERP-COF12 composite material and photocatalytic carbon dioxide reduction.
The invention relates to a UiO-66-NH 2 Preparation of IISERP-COF12 composite material and photocatalysisThe reduction of carbon dioxide is accomplished by the following steps:
step one, uiO-66-NH 2 Preparation of materials: zirconium chloride (ZrCl) was added in sequence to the beaker 4 ) 2-Amino Terephthalic Acid (ATA), modifier (3, 5-diamino terephthalic acid (2 ABA)), 5ml DMF. And carrying out ultrasonic treatment on the obtained solution for 30min to uniformly disperse the solution. The sample in the beaker was transferred to a polytetrafluoroethylene autoclave, 0.6mL of glacial acetic acid was added and placed in an oven for heating. Filtering the obtained product, and washing with DMF, etOH and deionized water respectively to obtain yellowish solid powder, denoted as UiO-66-NH 2 。
Step two, uiO-66-NH 2 Preparation of the IISERP-COF12 composite by reacting 5,5- (1, 3, 5-triazin-2, 4, 6-triyl) tris (pyridin-2-amine), 1,3, 5-trialdehyde phloroglucinol with UiO-66-NH obtained in step one 2 Placing into a heat-resistant glass tube, sequentially adding dimethyl sulfoxide (DMSO) and ethanol solution, performing ultrasonic treatment at ultrasonic frequency of 35-45 KHz for 30-35 min, and then adding 6mol.L -1 Degassing acetic acid solution in liquid nitrogen bath for three times of freeze thawing cycle, sealing, heating at 120deg.C for 72 hr, filtering, washing with DMSO and ethanol for several times, and drying to obtain UiO-66-NH 2 IISERP-COF12 composite;
the zirconium chloride (ZrCl) in step one 4 ) The molar ratio to the 2-amino terephthalic acid ATA is 1:1, a step of;
heating the sealed glass at 120 ℃ for 24 hours;
in the second step, the molar ratio of the 5,5- (1, 3, 5-triazine-2, 4, 6-triyl) tris (pyridine-2-amine) to the 1,3, 5-trialdehyde phloroglucinol is 1:1, a step of;
in the second step, the volume ratio of DMSO, ethanol and acetic acid is 1:1:0.3;
the concentration of the acetic acid solution used in the second step is 6mol.L -1 ；
Heating the sealed steel plate at 120 ℃ for 72 hours;
the above UiO-66-NH 2 Use of a/IISERP-COF 12 composite in photocatalytic carbon dioxide reduction.
The invention has the beneficial effects that:
the invention adopts a solvothermal method and adopts zirconium chloride (ZrCl) 4 ) 2-Amino Terephthalic Acid (ATA) is used as raw material to successfully synthesize UiO-66-NH 2 However, the material has low carbon dioxide reduction efficiency under visible light, which is only 4.82 mu mol.h -1 ·g -1 . Therefore, the invention will be UiO-66-NH 2 Compounding with IISERP-COF12 to synthesize a new composite material UiO-66-NH 2 The IISERP-COF12 material effectively improves the reduction performance of photocatalytic carbon dioxide, and UiO-66-NH 2 The photocatalytic carbon dioxide efficiency of the/IISERP-COF 12 composite material is 109.21 mu mol.h -1 ·g -1 。
Drawings
FIG. 1 is a diagram of UiO-66-NH 2 X-ray powder diffraction pattern of the IISERP-COF12 material;
FIG. 2 is a diagram of UiO-66-NH 2 Ultraviolet-visible absorption spectrum of the/IISERP-COF 12 material;
FIG. 3 is a diagram of UiO-66-NH 2 Band structure diagram of/IISERP-COF 12 material;
FIG. 4 is a diagram of UiO-66-NH 2 Performance profile of IISERP-COF12 material
Detailed Description
The invention is further illustrated by the following examples, which are only illustrative of the method of the invention and are not intended to limit the scope of the invention in any way.
Example 1: uiO-66-NH of the present embodiment 2 The preparation of the IISERP-COF12 material is completed according to the following steps:
step one, uiO-66-NH 2 Is prepared from the following steps: first 11.65mg of zirconium chloride (ZrCl) 4 ) 9.05mg of 2-Amino Terephthalic Acid (ATA) was added to the beaker, and after adding 5ml of the solution of LDMF, the resulting solution was sonicated for 30min to disperse it uniformly. Transferring the mixed solution into a high-pressure reaction kettle, adding 0.6mL of glacial acetic acid, reacting the high-pressure reaction kettle in an oven at 120 ℃ for 24 hours, filtering the obtained product, washing the product with DMF, etOH and deionized water respectively to obtain light yellow solid powder, and recording the light yellow solid powder as UiO-66-NH 2 ；
Step two, uiO-66-NH 2 IISERP-COF12 complexPreparation of materials: combining 5,5- (1, 3, 5-triazin-2, 4, 6-triyl) tris (pyridin-2-amine), 1,3, 5-trialdehyde phloroglucinol with UiO-66-NH obtained in step one 2 Placing into a heat-resistant glass tube, sequentially adding dimethyl sulfoxide (DMSO) and ethanol solution, performing ultrasonic treatment at ultrasonic frequency of 35-45 KHz for 30-35 min, and then adding 6mol.L -1 Degassing acetic acid solution in liquid nitrogen bath for three times of freeze thawing cycle, sealing, heating at 120deg.C for 72 hr, filtering, washing with DMSO and ethanol for several times, and drying to obtain UiO-66-NH 2 IISERP-COF12 composite.
UiO-66-NH 2 Characterization of IISERP-COF12 composite:
the obtained UiO-66-NH 2 As can be seen from FIG. 1, the diffraction peak position of the composite material comprises characteristic peaks of two independent materials, and the peak height changes along with the change of the proportion, so as to meet the basic characteristics of the composite material, and demonstrate the successful synthesis of the composite material.
The obtained UiO-66-NH 2 Ultraviolet-visible absorption Spectrometry test of the/IISERP-COF 12 composite, as seen in FIG. 2, uiO-66-NH 2 The band gap width of the IISERP-COF12 is 2.83eV, the band gap width of the IISERP-COF12 is 1.95eV, and the band structure of the integral material is obtained through calculation and is shown in figure 3.
The following tests were performed to verify the beneficial effects of the present invention:
to examine uiO-66-NH 2 The photocatalytic carbon dioxide reduction effect of the IISERP-COF12 composite material was tested according to the following method. The test procedure was as follows: the gas-solid photocatalytic reaction device is adopted, and samples are required to be pretreated before being tested, and the operation is as follows: 10mg of catalyst was ultrasonically dispersed in 1mL of acetone, the dispersion was dropped into a specific glass sheet, the glass sheet was then placed in a gas-solid reactor, and 99.9% CO was introduced into the apparatus 2 And (5) sealing the reaction device after 30 min. The reaction system was put under 300WXe lamp (filter lambda>420 nm), the condensing unit is turned on to ensure that the system is at room temperature. The light source is automatically turned on for timing, and gas samples in the system are collected once every 1h and injectedThe mixture was introduced into the FID detection port of GC7920 gas chromatography to measure the CO gas content. The number of sample tests was five, and the photocatalytic reaction amounted to five hours. As shown in FIG. 4, the reduction rate of carbon dioxide to carbon monoxide can reach 109.21 mu mol g -1 ·h -1 Is UiO-66-NH 2 22.66 times the material is 3.5 times the IISERP-COF12 material.
Claims (5)
1. UiO-66-NH 2 The preparation of the IISERP-COF12 composite material and the photocatalytic carbon dioxide reduction are characterized in that the method comprises the following steps:
step one, uiO-66-NH 2 Is prepared from the following steps: first 11.65mg of zirconium chloride (ZrCl) 4 ) 9.05mg of 2-Amino Terephthalic Acid (ATA) was added to the beaker, and after adding 5ml of the solution of LDMF, the resulting solution was sonicated for 30min to disperse it uniformly. Transferring the mixed solution into a high-pressure reaction kettle, adding 0.6mL of glacial acetic acid, reacting the high-pressure reaction kettle in an oven at 120 ℃ for 24 hours, filtering the obtained product, washing the product with DMF, etOH and deionized water respectively to obtain light yellow solid powder, and recording the light yellow solid powder as UiO-66-NH 2 ；
Step two, uiO-66-NH 2 Preparation of IISERP-COF12 composite material: combining 5,5- (1, 3, 5-triazin-2, 4, 6-triyl) tris (pyridin-2-amine), 1,3, 5-trialdehyde phloroglucinol with UiO-66-NH obtained in step one 2 Placing into a heat-resistant glass tube, sequentially adding dimethyl sulfoxide (DMSO) and ethanol solution, performing ultrasonic treatment at ultrasonic frequency of 35-45 KHz for 30-35 min, and then adding 6mol.L -1 And (3) carrying out freeze thawing cycle degassing on the acetic acid solution in a liquid nitrogen bath for three times, heating at 120 ℃ for 72 hours after sealing, filtering, washing with DMSO and ethanol for several times, and drying to obtain the UiO-66-NH2/IISERP-COF12 composite material.
2. A UiO-66-NH as claimed in claim 1 2 Preparation of the IISERP-COF12 composite material and photocatalytic carbon dioxide reduction, which is characterized in that UiO-66-NH is subjected to the step two 2 In situ, to the synthesis system of IISERP-COF12 material.
3. A UiO-66-NH as claimed in claim 1 2 The preparation of the IISERP-COF12 composite material and the photocatalytic carbon dioxide reduction are characterized in that the solvent in the synthesis system in the second step is dimethyl sulfoxide (DMSO) and ethanol solution.
4. A UiO-66-NH as claimed in claim 1 2 The preparation of the/IISERP-COF 12 composite material and the photocatalytic carbon dioxide reduction are characterized in that the concentration of the acetic acid solution in the step two is 6 mol.L -1 。
5. A UiO-66-NH as claimed in claim 1 2 The preparation of the/IISERP-COF 12 composite material and the photocatalytic carbon dioxide reduction are characterized in that the volume ratio of dimethyl sulfoxide (DMSO) to ethanol solution in the second step is 1:1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311176959.6A CN117225475A (en) | 2023-09-13 | 2023-09-13 | UiO-66-NH 2 Preparation of IISERP-COF12 composite material and photocatalytic carbon dioxide reduction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311176959.6A CN117225475A (en) | 2023-09-13 | 2023-09-13 | UiO-66-NH 2 Preparation of IISERP-COF12 composite material and photocatalytic carbon dioxide reduction |
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2023
- 2023-09-13 CN CN202311176959.6A patent/CN117225475A/en active Pending
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