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Three metal organic frames based on Co(II) ion as well as synthesis method and application thereof

A metal-organic framework and synthesis method technology, applied in cobalt organic compounds, organic chemistry, chemical instruments and methods, etc., to achieve the effects of low cost, rapid response, and effective separation

Inactive Publication Date: 2013-04-24
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, easy-to-operate, low-cost visualized anion sensors and separators remain a major challenge

Method used

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  • Three metal organic frames based on Co(II) ion as well as synthesis method and application thereof
  • Three metal organic frames based on Co(II) ion as well as synthesis method and application thereof
  • Three metal organic frames based on Co(II) ion as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1: Preparation of three metal-organic frameworks (MOFs) of Co(II) ions

[0060] 1. 6.05g (30mmol) of 3-bromo-4methylbenzoic acid, 3.77g (30mmol) of semicarbazide hydrochloride, 50g of polyphosphoric acid in a 250mL beaker, react at 160-170°C for 6h, cool, and use 10% NaOH aqueous solution Neutralize until the pH is 8-9, filter with suction, and dry in the air to obtain a crude product. Separation by column chromatography (dichloromethane: ethyl acetate = 20:1) gave white intermediate A4.28g, yield: 68.9%.

[0061] 2. Intermediate A4.08g (10mmol), pyridine-3-boronic acid 2.95g (24mmol), anhydrous potassium carbonate 4.15g (30mmol), tetrakis-(triphenylphosphine) palladium 1.16g (1mmol), 150mL (EtOH :H 2 O:toluene=1:1:1) mixed solution in 250mL there-necked bottle, N 2 Under protection, heat to reflux for 48h. Cool, separate liquids, discard the water phase, and distill off the solvent under reduced pressure to obtain a crude product, which was separated by col...

Embodiment 2

[0068] Example 2: Anion exchange-induced structural transformation and color change of metal-organic frameworks (MOFs)

[0069] a.Cl - Exchange NO in compound 1 3 - :

[0070] 0.05M K Cl saturated methanol solution stirred compound 1, IR tracking ( Figure 2-0 ), found that after 1h, no NO 3 - Peak, Cl - The exchange is complete, and the powder color changes from red to purple ( Figure 13 ). XRD trace ( figure 2 ), with the exchange of anions, the metal-organic framework undergoes transformation, gradually changing from compound 1 to compound 2. Simultaneous TGA ( image 3 ) data show that the solvent changed from 2 THF (tetrahydrofuran) to 2 CH 3 OH (methanol). After the exchange was completed, Cl was measured by ion chromatography - The percentage content is 6.94%, and the theoretical CoL 2 Cl 2 ·2CH 3 Cl in OH - The percentage content of 7.07% is basically consistent. In summary, it can be considered that NO 3 - 100% converted to Cl - .

[0071] b.Br ...

Embodiment 3

[0074] Embodiment 3: the selectivity of compound 1 to different anions

[0075] a.0.03M Cl - ,Br - ,I - mixed methanol solution (Cl - :Br - : I - =1:1:1) Stir the compound for 12h. IR ( Figure 7 ) show no NO 3 - Peak, the exchange is complete. XRD ( Figure 8 ) tracking reveals that the metal-organic framework undergoes transformation with the exchange of anions. TGA ( Figure 9 ) data confirmed that the solvent changed from 2 THF (tetrahydrofuran) to 1.7 CH 3 OH (methanol). XPS ( Figure 10 ) shows that only Cl - ,Br - , Cl measured by ion chromatography - , Br - The contents are 3.95% and 6.02% respectively. . by Cl - ,Br - The content is deduced that the molecular formula is CoL 2 Cl 1.21 Br 0.79 ·1.7CH 3 OH (theoretical Cl - ,Br - The contents are 4.17%, 6.14% respectively). Converted to molar ratio n(Cl - ): n(Br - )=1.53:1. Can be regarded as NO 3 - 60.5% converted to Cl - ,39.5% converted to Br - .

[0076] b.0.03M Cl - ,Br - mixe...

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Abstract

The invention discloses an organism for synthesizing metal organic frame based on Co(II) ion. The structural formula is shown in the specification. The invention further provides a synthesis method of the organism. The synthesis method comprises the following steps of: firstly, carrying out cyclization reaction on 3-bromine-4-methyl benzoic acid and semicarbazide hydrochloride so as to prepare a midbody A; and secondly, carrying out SuZuki reaction on the midbody A with pyridine-3-boric acid so as to prepare the organism. The invention further respectively provides three metal organic frames based on the Co(II) ion, a preparation method of the metal organic frames, and an application of the metal organic frames as an initiator in anion exchange. The organism has the beneficial effects that the compound belongs to organic-inorganic composite super-molecule materials, is simple to operate, low in cost and rapid in response, and realizes visible sensation of anions and the effective separation of the anions.

Description

technical field [0001] The present invention relates to three metal-organic frameworks (MOFs) based on Co(II) ions, their synthesis method, anion exchange-induced structural transformation, color change and fluorescence response and their response to different anions (Cl - ,Br - , I - ) selectivity. Background technique [0002] Since anions are ubiquitous and play an important role in organisms, environmental pollutants, and chemical reaction processes, the simple and rapid identification of anions is of great significance in the fields of biochemistry and environmental protection research. However, easy-to-operate and low-cost visualized anion sensors and separators remain a major challenge. Compared with most anion sensors and separators, such as those based on nanoparticles, metal-organic frameworks (MOFs) have significant advantages as anion sensors and separators. Anions generally occupy the voids in metal-organic frameworks (MOFs), and sometimes interact weakly wi...

Claims

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Application Information

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IPC IPC(8): C07D413/14C07F15/06C09K11/06G01N21/76
Inventor 董育斌侯珊刘启奎
Owner SHANDONG NORMAL UNIV
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