CN-120059205-B - Preparation method and application of cadmium-cobalt bimetallic organic framework

Abstract

The invention discloses a preparation method and application of a cadmium-cobalt bimetallic organic frame, belonging to the technical field of bimetallic organic frame synthesis, wherein the method comprises the following steps of S1, synthesizing the cadmium-cobalt bimetallic organic frame; S2, cdCoBTCHx crystal property analysis, which can be used for identifying sulfur-containing amino acid, has the beneficial effects that the existence of two oxidation states of Co (II) and Co (III) in the cadmium cobalt bimetallic organic framework CdCoBTCHx, cdCoBTCHx is synthesized, the detection signals of cysteine and methionine are obviously enhanced, good selectivity is shown for the sulfur-containing amino acid, and in addition, the variable valence state of cobalt in CdCoBTCHx promotes obvious electron transfer in the identification process, so that the color of the solution is changed from colorless to yellow, thereby providing visual identification effect. Provides technical reference for realizing rapid visual detection of the sulfur-containing compound kit, and has important significance in the fields of biological medicine, food detection and the like.

Inventors

• CAI HONG
• LI JINGYUN
• XIAO SIQI

Assignees

• 韩山师范学院

Dates

Publication Date

20260512

Application Date

20250112

Claims (8)

1. 1. The preparation method of the cadmium cobalt bimetallic organic framework is characterized by comprising the following steps of: s1, synthesizing a cadmium cobalt bimetallic organic framework; Cd (NO 3 ) 2 ·4H 2 O、Co(NO 3 ) 2 ·6H 2 O, hx and H 3 BTC are placed in DMF solvent according to the ratio of 2:1:2:1, pH value is regulated by HNO 3 , then the mixture is sealed in a polytetrafluoroethylene high-pressure reaction kettle for constant-temperature heating, then the mixture is cooled to room temperature, and the mixture is filtered and washed to obtain CdCoBTCHx light purple crystals; In the step S1, the concentration of HNO 3 is 1 mol/L, the constant temperature heating temperature is 140 ℃ and the time is 72 hours, and the temperature of the polytetrafluoroethylene high-pressure reaction kettle is reduced at a speed of 5 ℃/h after the constant temperature heating until the temperature is cooled to the room temperature; Wherein Hx is 6-hydroxy purine, H 3 BTC is 1,3, 5-benzene tricarboxylic acid, DMF solvent is N, N-dimethylformamide solvent, cdCoBTCHx is cadmium cobalt bimetallic organic framework; and S2, carrying out property analysis on CdCoBTCHx crystals.
2. 2. The method for preparing a cadmium cobalt bimetallic organic framework according to claim 1, wherein in the step S2, the property analysis of the crystal includes fourier transform infrared spectrometer analysis, single crystal X-ray diffraction analysis, X-ray powder diffractometer analysis, thermogravimetric analysis and X-ray photoelectron spectroscopy analysis.
3. 3. The method for preparing a cadmium cobalt bimetallic organic framework according to claim 2, wherein the fourier transform infrared spectrometer analysis is used for determining whether to synthesize CdCoBTCHx crystals.
4. 4. A method of preparing a cadmium cobalt bimetallic organic framework according to claim 3 wherein single crystal X-ray diffraction analysis is used to determine the single crystal structure of CdCoBTCHx.
5. 5. A method of preparing a cadmium cobalt bimetallic organic framework according to claim 3 wherein the X-ray powder diffractometer analysis is used to determine CdCoBTCHx purity.
6. 6. A method of preparing a cadmium cobalt bimetallic organic framework according to claim 3 wherein the thermogravimetric analysis is used to determine CdCoBTCHx thermal stability.
7. 7. A method of preparing a cadmium cobalt bimetallic organic framework according to claim 3 wherein the X-ray photoelectron spectroscopy analysis is used to determine CdCoBTCHx valence states.
8. 8. Use of a cadmium cobalt bimetallic organic framework prepared by the method of any one of claims 1 to 7 for identifying sulfur-containing amino acids.

Description

Preparation method and application of cadmium-cobalt bimetallic organic framework Technical Field The invention relates to the technical field of bimetal organic framework synthesis, in particular to a preparation method and application of a novel cadmium cobalt bimetal organic framework. Background Sulfur-containing amino acids play a vital role in various metabolic processes, are also amino acids with great influence on food flavor in the heat treatment process, are used as basic components of polypeptides and proteins, and are biomarkers for predicting disease risks. Metal Organic Frameworks (MOFs) are a new class of porous crystalline materials developed in the nineties of the 20 th century, and are generally formed by self-assembly of transition metal ions and multidentate organic ligands containing oxygen, nitrogen, etc., linked to each other. MOF materials of the mixed metal type generally refer to MOFs constructed with two or more different metal ions. Since the inorganic metal sites of the single metal type MOF are limited and relatively single, if other metal systems are introduced, the variety of metal sites can be increased, and the arrangement mode is more various. For example, co is doped into ZnCo-ZIF-8 synthesized in ZIF-8, and the mixture can be prepared into a side heating type gas sensor after calcination at 600 ℃, and the side heating type gas sensor shows good selectivity in acetone detection. Heterovalent bimetallic MOF materials are less common, typically as the CPM-200 series, which are heterometallic MOFs formed by matching trivalent In 3+、Ga3+ with divalent Mg 2+、Mn2+, etc., exhibiting excellent selective adsorption capacity for CO 2. However, since different metal ions have different coordination rates and coordination modes under the same conditions, autonomous assembly of the bimetallic MOF and control of the final product remains a major challenge. At present, the synthesis of the cadmium-cobalt bimetallic organic framework is blank, and the cadmium-cobalt bimetallic organic framework has good effect on the identification of sulfur-containing amino acid. Disclosure of Invention In order to solve the problems, the invention provides a preparation method and application of a novel cadmium cobalt bimetallic organic frame, and the preparation method is realized through the following technical scheme. The preparation method of the novel cadmium cobalt bimetallic organic framework is characterized by comprising the following steps of: s1, synthesizing a cadmium cobalt bimetallic organic framework; Cd (NO 3)2·4H2O、Co(NO3)2·6H2 O, hx and H 3 BTC are placed in DMF solvent according to the ratio of 2:1:2:1, pH value is regulated by HNO 3, then the mixture is sealed in a polytetrafluoroethylene high-pressure reaction kettle for constant-temperature heating, then the mixture is cooled to room temperature, and the mixture is filtered and washed to obtain CdCoBTCHx light purple crystals; Wherein Hx is 6-hydroxy purine, H 3 BTC is 1,3, 5-benzene tricarboxylic acid, DMF solvent is N, N-dimethylformamide solvent, cdCoBTCHx is cadmium cobalt bimetallic organic framework; and S2, carrying out property analysis on CdCoBTCHx crystals. Preferably, in the step S1, the concentration of HNO 3 is 1mol/L, the constant temperature heating temperature is 140 ℃ and the time is 72 hours, and the temperature of the polytetrafluoroethylene high-pressure reaction kettle is reduced at a speed of 5 ℃ after the constant temperature heating until the temperature is cooled to the room temperature. Preferably, in the step S2, the property analysis of the crystal includes fourier transform infrared spectrometer analysis, single crystal X-ray diffraction analysis, X-ray powder diffraction analysis, thermogravimetric analysis, and X-ray photoelectron spectroscopy analysis. Preferably, the fourier transform infrared spectrometer analysis is used to determine whether CdCoBTCHx crystals are synthesized. Preferably, the single crystal X-ray diffraction analysis is used to determine the single crystal structure of CdCoBTCHx. Preferably, the X-ray powder diffractometer analysis is used to determine CdCoBTCHx purity. Preferably, the thermogravimetric analysis is used to determine the thermal stability of CdCoBTCHx. Preferably, the X-ray photoelectron spectroscopy is used to determine the CdCoBTCHx valence states. An application of a cadmium-cobalt bimetallic organic framework is used for identifying sulfur-containing amino acids. The invention has the beneficial effects that the cadmium-cobalt bimetallic organic framework CdCoBTCHx is synthesized, and is prepared by 6-hydroxy purine, 1,3, 5-benzene tricarboxylic acid, metal cadmium and cobalt ions, and the existence of two oxidation states Co (II) and Co (III) in CdCoBTCHx remarkably enhances detection signals of cysteine and methionine, shows good selectivity to sulfur-containing amino acid, and an ultraviolet-visible absorption spectrum shows that remarkable electron transfe