CN110327976B - Photocatalyst and preparation method and application thereof - Google Patents
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Abstract
本发明涉及一种光催化剂及其制备方法和应用。所述制备方法包括如下步骤：将配体溶液与钛酸酯混合，搅拌，进行水热反应即得所述光催化剂；所述配体溶液为2‑氨基对苯二甲酸和3氨基间苯甲酸的混合溶液，所述配体中3氨基间苯甲酸的摩尔分数为4～6％。本发明利用混合配体法制备出新型的MOFs光催化材料，通过调节两种配体的比例可以调节光催化剂的光催化性能，提供了一种新型的光催化剂的合成方法，有效地提高了MOFs光催化剂的催化活性和对其形貌进行调控。相较于纯的MOFs光催化剂，根据本发明制备方法所得的缺陷MOFs光催化性能明显得到提高，同时制备过程工艺简单。
The present invention relates to a photocatalyst and its preparation method and application. The preparation method includes the following steps: mixing a ligand solution with titanate, stirring, and performing a hydrothermal reaction to obtain the photocatalyst; the ligand solution is 2-aminoterephthalic acid and 3-aminoisobenzoic acid The mixed solution, the mole fraction of 3-aminoisobenzoic acid in the ligand is 4-6%. The invention uses a mixed ligand method to prepare a new type of MOFs photocatalytic material, and the photocatalytic performance of the photocatalyst can be adjusted by adjusting the ratio of the two ligands, thereby providing a new synthesis method of the photocatalyst and effectively improving the MOFs. The catalytic activity of photocatalysts and the regulation of their morphology. Compared with the pure MOFs photocatalyst, the photocatalytic performance of the defective MOFs obtained by the preparation method of the present invention is obviously improved, and the preparation process is simple.
Description
Technical Field
The invention relates to the field of photocatalysis, in particular to a photocatalyst and a preparation method and application thereof.
Background
Photocatalysis is an environment-friendly and economic technology, and is considered to be one of the most promising technologies for solving the energy crisis in the 21 st century because of the effective utilization of solar energy. The method is applied to the fields of sewage treatment, air purification, carbon dioxide reduction, water decomposition hydrogen production and the like. Metal-Organic Frameworks (MOFs) are porous materials formed by Metal clusters and Organic ligands through coordination bonds. Due to the unique structure of the MOFs, the porosity, specific surface area and chemical properties can be changed by changing the kind of metal clusters or ligands. Currently, MOFs have been widely used in the fields of gas adsorption, gas separation, gas storage, and catalysis. In the field of catalysis, MOFs are mainly applied to organic matter catalytic reaction, and certain achievements have been achieved. However, the application of MOFs in photocatalysis, particularly in the field of hydrogen production by photocatalytic water splitting, is still in the beginning, and more intensive systematic studies are required for the application of MOFs in hydrogen production by photocatalytic water splitting. According to the previous research results, the introduction of defects can effectively improve the performance of MOFs materials in the fields of gas adsorption, gas separation, organic compound catalysis and the like.
Therefore, constructing a defective MOFs photocatalytic system is a potential feasible method for improving the catalytic performance of the MOFs.
Disclosure of Invention
The invention aims to overcome the shortage of research aiming at the application of MOFs in photocatalytic water splitting to produce hydrogen and provides a preparation method of a photocatalyst. The invention prepares the novel MOFs photocatalytic material by using a mixed ligand method, can adjust the photocatalytic performance of the photocatalyst by adjusting the proportion of two ligands, provides a novel synthesis method of the photocatalyst, and effectively improves the catalytic activity of the MOFs photocatalyst and adjusts and controls the morphology of the MOFs photocatalyst. Compared with pure MOFs photocatalyst, the defect MOFs photocatalyst obtained by the preparation method provided by the invention has obviously improved photocatalytic performance, and the preparation process is simple.
Another object of the present invention is to provide a photocatalyst.
Another object of the present invention is to provide the use of the above photocatalyst in the field of photocatalysis.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a photocatalyst comprises the following steps: mixing the ligand solution with titanate, stirring, and carrying out hydrothermal reaction to obtain the photocatalyst;
the ligand solution is a mixed solution of 2-amino terephthalic acid and 3-amino m-benzoic acid, and the mole fraction of the 3-amino m-benzoic acid in the ligand is 4-6%.
The invention utilizes a mixed ligand method to prepare a novel MOFs photocatalytic material, titanium is used as a metal group, 2-amino terephthalic acid and 3-amino isophthalic acid are used as mixed ligands, the photocatalytic performance of the photocatalyst can be adjusted by adjusting the proportion of the two ligands, a novel synthesis method of the photocatalyst is provided, and the catalytic activity of the MOFs photocatalyst is effectively improved and the morphology of the MOFs photocatalyst is adjusted. Compared with pure MOFs photocatalyst, the defect MOFs photocatalyst obtained by the preparation method provided by the invention has obviously improved photocatalytic performance, and the preparation process is simple.
Preferably, the molar fraction of 3 amino-m-benzoic acid in the ligand is 5%.
Preferably, the solvent used for the ligand solution is a mixed solution of methanol and N, N-dimethylformamide.
More preferably, the volume ratio of the methanol to the N, N-dimethylformamide is 1: 5-15.
Titanates conventional in the art may be used in the present invention.
Preferably, the titanate is one or more of tetrabutyl titanate, tetraethyl titanate or tetraisopropyl titanate.
Preferably, the molar ratio of the titanate to the ligand is 1: 1-4.
Preferably, the stirring time is 0.1-0.5 h.
Preferably, the temperature of the hydrothermal reaction is 100-180 ℃ and the time is 16-72 h.
The photocatalyst is prepared by the preparation method.
Preferably, the photocatalyst is a decahedral structure.
The application of the photocatalyst in the field of photocatalysis is also within the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
the invention prepares the novel MOFs photocatalytic material by using a mixed ligand method, can adjust the photocatalytic performance of the photocatalyst by adjusting the proportion of two ligands, provides a novel synthesis method of the photocatalyst, and effectively improves the catalytic activity of the MOFs photocatalyst and adjusts and controls the morphology of the MOFs photocatalyst. Compared with pure MOFs photocatalyst, the defect MOFs photocatalyst obtained by the preparation method provided by the invention has obviously improved photocatalytic performance, and the preparation process is simple.
Drawings
FIG. 1 is a series NH2-graph of photocatalytic performance of different photocatalysts of MIL-125;
FIG. 2 shows pure NH2-scanning electron microscopy of MIL-125 photocatalyst;
FIG. 3 shows a defect NH2-scanning electron microscopy of MIL-125 photocatalyst.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Example 1
This example provides a series of photocatalysts NH2MIL-125, prepared as follows.
10mL of a mixed solution (V) of N, N-dimethylformamide and methanol is preparedN, N-dimethylformamide:VMethanol1) adding a mixed ligand of 2-aminoterephthalic acid and 3-aminoisophthalic acid with the total mole number of 3mmol (the molar ratio of 3-aminoisophthalic acid in the ligand is x), fully stirring and dissolving, adding 1mmol of tetrabutyl titanate, stirring at room temperature for 30min, transferring to a 50mL polytetrafluoroethylene hydrothermal reaction kettle, and reacting at 150 ℃ for 3 days. After the hydrothermal reaction is finished, the product is filtered and separated, N-dimethylformamide and methanol are respectively used for cleaning for 3 times, and the obtained product is placed in a blast oven for drying for 1 day at the temperature of 120 ℃ to obtain defect NH2-MIL-125-x photocatalyst, x being the molar proportion of 3-amino-m-benzoic acid in the ligand, in particular 0% (i.e. pure NH)2-MIL-125)、4％(NH2-MIL-125-4％)、5％(NH2-MIL-125-5%) and 6% (NH)2-MIL-125-6％)。
Example 2
This example provides a photocatalyst NH2-MIL-125-5%, and its preparation method is as follows.
The preparation of 10mL of N, N-dimethylformylAmine and methanol mixed solution (V)N, N-dimethylformamide:VMethanol1), adding a mixed ligand of 2-aminoterephthalic acid and 3-aminoisophthalic acid with the total mole number of 1mmol (the mole ratio of 3-aminoisophthalic acid in the mixed ligand is 5%), fully stirring to dissolve, adding 1mmol of tetraethyl titanate, stirring at room temperature for 30min, transferring to a 50mL polytetrafluoroethylene hydrothermal reaction kettle, and reacting at 180 ℃ for 16 h. After the hydrothermal reaction is finished, the product is filtered and separated, N-dimethylformamide and methanol are respectively used for cleaning for 3 times, and the obtained product is placed in a blast oven for drying for 1 day at the temperature of 120 ℃ to obtain defect NH2-MIL-125-5% photocatalyst.
Example 3
This example provides a photocatalyst NH2-MIL-125-5%, and its preparation method is as follows.
10mL of a mixed solution (V) of N, N-dimethylformamide and methanol is preparedN, N-dimethylformamide:VMethanolAnd (9: 1), adding a mixed ligand of 2-aminoterephthalic acid and 3-amino-m-benzoic acid with the total mole number of 4mmol (the molar ratio of 3-amino-m-benzoic acid in the mixed ligand is 5%), fully stirring to dissolve, adding 1mmol of tetraisopropyl titanate, stirring at room temperature for 30min, transferring to a 50ml polytetrafluoroethylene hydrothermal reaction kettle, and reacting at 100 ℃ for three days. After the hydrothermal reaction is finished, the product is filtered and separated, N-dimethylformamide and methanol are respectively used for cleaning for 3 times, and the obtained product is placed in a blast oven for drying for 1 day at the temperature of 120 ℃ to obtain defect NH2-MIL-125-5% photocatalyst.
Performance testing
The series of photocatalysts NH prepared in example 12The photocatalytic effect experiment is carried out by taking-MIL-125 as an example.
The specific experimental process is as follows: 50mg of the photocatalyst was added to a Labsolar6A photocatalytic reaction apparatus with 98mL of deionized water, 2mL of triethanolamine was added as a sacrificial agent, and 1mL of potassium chloroplatinate at a concentration of 1mg/mL was added as a cocatalyst (platinum content was 1 w% of the catalyst). The solution was stirred well and then evacuated for 30min to remove air from the solution. After the vacuum pumping is completed, 20mL of nitrogen is added into the reaction device as a protective gas. The light source is a 300W xenon lamp with A.M 1.5.5 cut-off filter, the reaction device is cooled by 4 ℃ condensed circulating water, and 1mL of gas is taken per hour for gas chromatography analysis to determine the hydrogen generation amount.
The results of the catalytic effect experiment are shown in FIG. 1. The results show that the defect NH synthesized by the mixed ligand method2-MIL-125 ratio NH prepared using pure 2-amino terephthalic acid as ligand2MIL-125 has better photocatalytic hydrogen production performance reaching 320 mu mol h-1g-1Is about NH21.5 times of MIL-125. The defect NH prepared by the mixed ligand method can be found by scanning electron microscope pictures2MIL-125 sample with NH2Compared with the disc-type structure (fig. 2) of MIL-125, the structure has a unique decahedral structure (fig. 3).
The performance test results show that the mixed ligand method is not only used for NH2The catalytic performance of the MIL-125 is regulated and controlled, and the morphological structure of the MIL-125 can be effectively regulated and controlled.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a photocatalyst is characterized by comprising the following steps: mixing the ligand solution with titanate, stirring, and carrying out hydrothermal reaction to obtain the photocatalyst;
the ligand solution is a mixed solution of 2-aminoterephthalic acid and 3-amino-m-benzoic acid, and the mole fraction of the 3-amino-m-benzoic acid in the ligand is 4-6%;
the photocatalyst is defect NH2-MIL-125 photocatalyst.
2. The method according to claim 1, wherein the molar fraction of 3-amino-m-benzoic acid in the ligand is 5%.
3. The method according to claim 1, wherein the ligand solution is a mixed solution of methanol and N, N-dimethylformamide.
4. The preparation method according to claim 3, wherein the volume ratio of the methanol to the N, N-dimethylformamide is 1:5 to 15.
5. The preparation method according to claim 1, wherein the titanate is one or more of tetrabutyl titanate, tetraethyl titanate, or tetraisopropyl titanate.
6. The preparation method according to claim 1, wherein the molar ratio of the titanate to the ligand is 1: 1-4.
7. The preparation method according to claim 1, wherein the hydrothermal reaction is carried out at a temperature of 100 to 180 ℃ for 16 to 72 hours.
8. A photocatalyst produced by the production method according to any one of claims 1 to 7.
9. The photocatalyst according to claim 8, wherein the photocatalyst has a decahedral structure.
10. Use of a photocatalyst as claimed in any one of claims 8 to 9 in the field of photocatalysis.
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| CN111848897B (en) * | 2020-07-15 | 2021-07-30 | 上海交通大学 | Preparation method of covalent organic framework material composed of two types of octopolar conjugated structural units connected by alternating carbon-carbon double bonds |
| CN111921561B (en) * | 2020-08-18 | 2023-06-23 | 浙江工业大学 | Hierarchical hollow structure NH 2 Preparation method of MIL-125 (Ti) desulfurization catalyst |
| CN113559936A (en) * | 2021-07-30 | 2021-10-29 | 陕西科技大学 | Defective UiO-66 photocatalytic material and preparation method and application thereof |
| CN114471727B (en) * | 2022-02-10 | 2023-11-17 | 重庆工商大学 | Au@NH 2 MIL-125 (Cu/Ti) photocatalyst, and preparation method and application thereof |
| CN114950562B (en) * | 2022-04-25 | 2023-08-08 | 浙江工业大学 | A titanium-based three-dimensional nano-organic complex with adjustable defect density, its preparation method and application |
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