CN108864437B - Synthetic method of aromatic carboxylic acid transition metal silver complex - Google Patents
Synthetic method of aromatic carboxylic acid transition metal silver complex Download PDFInfo
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Abstract
The invention discloses a synthesis method of an aromatic carboxylic acid transition metal silver complex, which comprises the steps of adding deionized water into zinc oxide powder, performing ultrasonic dispersion to obtain a suspension A, preparing an alcohol-water solution of aromatic carboxylic acid, adding the alcohol-water solution into the suspension A to obtain a solution B, finally dropping a silver nitrate solution into the solution B, aging at the temperature of 25-100 ℃ for 10 min-24 h, centrifuging, cleaning and activating to obtain the aromatic carboxylic acid silver complex. The synthesis method is simple, rapid and efficient, and can realize the crystal morphology and size regulation of the aromatic carboxylic acid transition metal silver complex.
Description
Technical Field
The invention belongs to the technical field of metal-organic frameworks, and particularly relates to a synthesis method of an aromatic carboxylic acid transition metal silver complex.
Background
Metal-organic frameworks (MOFs) are hybrid organic-inorganic materials with intramolecular pores formed by self-assembly of organic ligands and metal ions or clusters through coordination bonds. In the MOFs, the arrangement of organic ligands and metal ions or clusters has obvious directionality, and different framework pore structures can be formed, thereby showing different adsorption performance, optical properties and electromagnetic properties. A common ligand is a benzoic acid ligand which has a benzene ring conjugated structure, so that electrons are favorably transmitted to metal ions through the benzene ring.
The conventional synthesis methods for MOFs materials mainly include hydrothermal/solvothermal methods, microwave synthesis methods, ultrasonic synthesis methods, ionothermal synthesis methods, electrochemical synthesis methods, and the like. In recent years, in view of the wide application prospect of the MOFs, researchers do much work on the aspects of morphology and structure regulation of the MOFs material, so as to further improve the performance of the MOFs material. However, designing and synthesizing MOFs materials with complex structures (e.g., one-dimensional, two-dimensional, three-dimensional structures) remains a great challenge compared to the diversity of inorganic metal oxide structures.
Disclosure of Invention
The invention aims to solve the technical problems of low synthesis efficiency and long time consumption of the existing metal-organic framework, provides a synthesis method of an aromatic carboxylic acid type transition metal silver complex, and the method is simple, rapid and efficient, and can realize crystal morphology and size regulation of the aromatic carboxylic acid type transition metal silver complex.
The technical scheme is as follows:
the synthesis method of the aromatic carboxylic acid transition metal silver complex comprises the following steps:
step 1, adding deionized water into zinc oxide powder, and performing ultrasonic dispersion to obtain a suspension A;
step 2, taking a mixed solution of alcohol and water as a solvent, preparing an alcohol-water solution of aromatic carboxylic acid, and adding the alcohol-water solution into the suspension A to obtain a suspension B;
and 3, dripping a silver nitrate solution into the B, aging for 10 min-24 h at the temperature of 25-100 ℃, centrifuging, cleaning and activating to obtain the aromatic carboxylic acid silver complex.
Further, the dosage ratio of the zinc oxide powder to the deionized water in the step 1 is 10-30 mg/mL.
Further, the aromatic carboxylic acid is selected from one or more of trimesic acid or derivatives thereof, phthalic acid or derivatives thereof, mellitic acid or derivatives thereof, diphenic acid or derivatives thereof, and pyromellitic acid or derivatives thereof.
Further, the molar ratio of the aromatic carboxylic acid to the zinc oxide powder is 0.2 to 2.5.
Further, the molar ratio of silver nitrate to aromatic carboxylic acid is 2.0-5.0.
Further, the volume ratio of the total water to the alcohol in the system is 1: 1.
the synthesis method is simple, rapid and efficient, and can realize the crystal morphology and size regulation of the aromatic carboxylic acid transition metal silver complex.
Drawings
FIG. 1 is an electron micrograph of a silver monobasic trimesate complex according to example 1;
FIG. 2 is an electron micrograph of a three-dimensional silver phthalate complex of example 2;
FIG. 3 is an electron micrograph of a silver phthalate complex of example 3.
Detailed Description
The technical solution of the present invention is further explained below with reference to the specific embodiments and the accompanying drawings.
Example 1
Step 1, adding 20mL of deionized water into a certain amount of zinc oxide powder, wherein the dosage ratio of the zinc oxide powder to the deionized water is 15 mg/mL, and performing ultrasonic dispersion for 60min to obtain a suspension A;
step 2, taking a mixed solution of alcohol and water as a solvent, preparing an alcohol-water solution of trimesic acid with a certain concentration of 60mL, wherein the molar ratio of the trimesic acid to the zinc oxide powder is 2.0, and adding the alcohol-water solution into the suspension A to obtain B;
and 3, dropping 20mL of silver nitrate solution with a certain concentration into the B, wherein the molar ratio of silver nitrate to trimesic acid is 3.5, and the volume ratio of total water to alcohol in the system is 1: 1, then aging for 60min at the temperature of 60 ℃, centrifuging, cleaning and activating to obtain the one-dimensional silver trimesate complex.
As shown in FIG. 1, the obtained silver trimesate complex has regular and uniform shape.
Example 2
Step 1, adding 30mL of deionized water into a certain amount of zinc oxide powder, wherein the dosage ratio of the zinc oxide powder to the deionized water is 20 mg/mL, and performing ultrasonic dispersion for 60min to obtain a suspension A;
step 2, taking a mixed solution of alcohol and water as a solvent, preparing an alcohol-water solution of phthalic acid with a certain concentration of 80mL, wherein the molar ratio of the phthalic acid to the zinc oxide powder is 2.5, and adding the alcohol-water solution into the suspension A to obtain B;
and 3, dripping 30mL of silver nitrate solution with a certain concentration into the B, wherein the molar ratio of silver nitrate to phthalic acid is 4.0, and the volume ratio of total water to alcohol in the system is 1: 1, then aging for 12h at the temperature of 80 ℃, centrifuging, cleaning and activating to obtain the three-dimensional silver phthalate complex.
As shown in FIG. 2, the obtained three-dimensional silver phthalate complex has regular and uniform shape and good monodispersity.
Example 3
Step 1, adding 20mL of deionized water into a certain amount of zinc oxide powder, wherein the dosage ratio of the zinc oxide powder to the deionized water is 18 mg/mL, and performing ultrasonic dispersion for 60min to obtain a suspension A;
step 2, taking a mixed solution of alcohol and water as a solvent, preparing an alcohol-water solution of phthalic acid with a certain concentration of 40mL, wherein the molar ratio of the phthalic acid to the zinc oxide powder is 2.8, and adding the alcohol-water solution into the suspension A to obtain B;
and 3, dropping 20mL of silver nitrate solution with a certain concentration into the B, wherein the molar ratio of silver nitrate to aromatic carboxylic acid is 2.0, and the volume ratio of total water to alcohol in the system is 1: 1, then aging for 20min at the temperature of 25 ℃, centrifuging, cleaning and activating to obtain the silver bisphthalate complex.
As shown in FIG. 3, the obtained two-dimensional silver phthalate complex has a regular and uniform shape.
Claims (1)
1. The synthesis method of the aromatic carboxylic acid transition metal silver complex is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding deionized water into zinc oxide powder, wherein the dosage ratio of the zinc oxide powder to the deionized water is 10-30 mg/mL, and performing ultrasonic dispersion to obtain a suspension A;
step 2, taking a mixed solution of alcohol and water as a solvent, preparing an alcohol-water solution of aromatic carboxylic acid, and adding the alcohol-water solution into the suspension A to obtain a suspension B;
step 3, dripping a silver nitrate solution into the B, then aging for 10 min-24 h at the temperature of 25-100 ℃, centrifuging, cleaning and activating to obtain the aromatic carboxylic acid silver complex;
the aromatic carboxylic acid is selected from one or more of trimesic acid or a derivative thereof, phthalic acid or a derivative thereof, mellitic acid or a derivative thereof, biphenyldicarboxylic acid or a derivative thereof, and pyromellitic acid or a derivative thereof;
the molar ratio of the aromatic carboxylic acid to the zinc oxide powder is 0.2-2.5;
the molar ratio of silver nitrate to aromatic carboxylic acid is 2.0-5.0;
the volume ratio of the total water to the alcohol in the system is 1: 1.
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