Cu(I)-based metal organic framework, and preparation method and applications thereof

A technology of metal-organic frameworks and organic ligands, applied in the direction of 1/11 organic compounds without C-metal bonds, organic chemistry, copper organic compounds, etc., to achieve low detection limits, ensure accuracy, and highly selective effects

Inactive Publication Date: 2015-11-04
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although people have developed a lot of sensors for HCl, there are few reports on high-sensitivity sensors with good specificity, easy to use, and visible to the naked eye, and it is worth continuing to study

Method used

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  • Cu(I)-based metal organic framework, and preparation method and applications thereof
  • Cu(I)-based metal organic framework, and preparation method and applications thereof
  • Cu(I)-based metal organic framework, and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] 1. Preparation of organic ligand L

[0061] Add 4.41 g of 5-(3-pyridyl) tetrazole to 3.48 g of 2,4,6-triethyl-1,3,5-trimesoyl chloride, 10 ml of anhydrous pyridine, and react at 120° C. for 2 h. After the system was cooled, 100 ml of water was added, and the dark crude product was obtained by suction filtration, dried, and column chromatography (ethyl acetate) gave 3.1 g of light yellow powder with a yield of 53%. we pass 1 The compound was characterized by H NMR and IR, and the results are shown in Figure 4 and Figure 5 . 2,4,6-Triethyl-1,3,5-trimesoyl chloride References C.-W.Zhao, J.-P.Ma, Q.-K.Liu, Y.Yu, P.Wang ,Y.-A.Li,K.Wang and Y.-B.Dong,Green Chem.,2013,15,3150-3154.

[0062]

[0063] 2. Synthesis of CuI-MOF

[0064] Dissolve 30mg of organic ligand L and 40mg of CuI in 10mL of acetonitrile respectively, mix the two evenly, and let stand at 10°C for 15 hours to obtain 53mg of metal organic framework CuI-MOF with a yield of 77% (based on L).

[0065] W...

Embodiment 2

[0082] 1. Preparation of organic ligand L

[0083] Add 3.88 g of 5-(3-pyridyl) tetrazole to 2.80 g of 2,4,6-triethyl-1,3,5-trimesoyl chloride, 9.5 mL of anhydrous pyridine, and react at 110°C for 3.5 h. After the system was cooled, 100 mL of water was added, and the dark crude product was obtained by suction filtration, dried, and column chromatography (ethyl acetate) gave 3.0 g of light yellow powder with a yield of 52%.

[0084] 2. Synthesis of CuI-MOF

[0085] Dissolve 27mg of organic ligand L and 30mg of CuI in 9mL of acetonitrile, mix the two evenly, and let stand at 30°C for 12 hours to obtain 51mg of metal organic framework CuI-MOF with a yield of 76% (based on L).

[0086] 3. I 2 Synthesis of CuI(Cl)-MOF

[0087] The CuI-MOF crystal prepared in Example 2 was placed in a 50mL container with an HCl (g) concentration of 200ppm at 25°C, taken out after 14min, and left to stand in air for 150min to obtain I 2 CuI(Cl)-MOF.

[0088] 4. Synthesis of micro-CuI-MOF

[0089] ...

Embodiment 3

[0091] 1. Preparation of organic ligand L

[0092] Add 5.51 g of 5-(3-pyridyl) tetrazole to 3.80 g of 2,4,6-triethyl-1,3,5-trimesoyl chloride, 11 mL of anhydrous pyridine, and react at 130° C. for 1.5 h. After the system was cooled, 100 mL of water was added, the dark crude product was obtained by suction filtration, dried, and column chromatography (ethyl acetate) gave 3.2 g of a light yellow powder with a yield of 55%.

[0093] 2. Synthesis of CuI-MOF

[0094] Dissolve 35mg of organic ligand L and 42mg of CuI in 12mL of acetonitrile respectively, mix the two evenly, and let stand at 10°C for 15 hours to obtain 55mg of metal organic framework CuI-MOF with a yield of 78% (based on L).

[0095] 3. I 2 Synthesis of CuI(Cl)-MOF

[0096] The CuI-MOF crystal prepared in Example 2 was placed in a 50mL container with an HCl (g) concentration of 150ppm at 25°C, taken out for 10min, and left to stand in air for 100min to obtain I 2 CuI(Cl)-MOF.

[0097] 4. Synthesis of micro-CuI-M...

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Abstract

The invention discloses a Cu(I)-based metal organic framework (MOF), and a preparation method and applications thereof. The Cu(I)-based metal organic framework CuI-MOF is capable of reacting with HCl(g) and O2 in air atmosphere so as to obtain a novel I2-containing metal organic framework I2@CuI(Cl)-MOF with obvious color variation. Reaction of CuI-MOF with HF(g), HBr(g), and HI(g) in gas phase is impossible. Micrometer-scaled micro-CuI-MOF can be taken as a naked eye visible sensor for rapid detection of HCl gas in the air. The micro-CuI-MOF sensor high reaction activity is naked eye visible compared with common organic polymer HCl sensors, and detection limit is lower. The micro-CuI-MOF sensor high reaction activity possesses high selectivity in detection of HCl, and detection accuracy is guaranteed.

Description

technical field [0001] The invention relates to a Cu(I)-based metal-organic framework, a preparation method and application thereof, and belongs to the technical field of sensor preparation. Background technique [0002] Metal-organic Framework (MOF) is a research hotspot in recent years. Compared with traditional porous materials, MOF has the characteristics of porosity, larger specific surface area and pore volume in the framework. The metal nodes, anions, and organic ligands that make up the MOF framework often have obvious photoelectric signals, making them have specific stress responses to certain external stimuli. As a porous functionalized material, it shows great advantages in sensing applications. [0003] HCl gas is a hazardous gas that is mainly produced and released into the environment by the complete incineration of chlorinated polymers. The safe concentration of HCl gas for human exposure is below 10ppm. When the concentration reaches 35ppm, it will irritate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D413/14C07F1/08C09K11/06G01N21/64
CPCC07D413/14C07F1/005C09K11/06C09K2211/1007C09K2211/1029C09K2211/1048G01N21/643
Inventor 董育斌赵朝委马建平
Owner SHANDONG NORMAL UNIV
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