Preparation method and application of tetra-amido macrocyclic ligand and metal chelate thereof

A metal chelate and macrocyclic ligand technology, applied in the restoration of polluted soil, organic chemistry, etc., can solve the problems of complex synthesis steps, environmental and human hazards, complex synthesis process, etc., and achieve easy control of synthesis conditions, The effect of improving economic efficiency and simple synthetic route

Inactive Publication Date: 2020-07-10
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acid resistance and reaction stability of the synthesized composite material are significantly enhanced, and the reactivity is improved, which solves the problem that the activity of the tetraamidohexamethylphenylcycloiron in the prior art has a strong dependence on pH. It is significantly reduced under acidic and neutral conditions, especially under acidic conditions, it is prone to demetallization and irreversible deactivation
This invention promotes the low-cost application of tetraamidohexamethylphenyl ring iron in the actual treatment of wastewater with a wide range of pH, and i

Method used

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  • Preparation method and application of tetra-amido macrocyclic ligand and metal chelate thereof
  • Preparation method and application of tetra-amido macrocyclic ligand and metal chelate thereof
  • Preparation method and application of tetra-amido macrocyclic ligand and metal chelate thereof

Examples

Experimental program
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Embodiment 1

[0067] This embodiment provides a method for preparing a tetraamido macrocyclic ligand, comprising the following steps:

[0068] (1) In a 500mL round-bottomed flask, add 70mL of triethylamine into the ethanol solution, and use the ethanol solution to adjust the volume to 300mL; In the ethanol solution, heat at 60°C in a water bath, and use magnetic stirring under reflux at a speed of 800rpm to obtain a mixed solution A; in another 500mL round bottom flask, mix 52g dimethylmalonic acid with 211.5 g dicycloethylcarbodiimide was mixed in 300mL ethanol solution to obtain mixed solution B.

[0069] (2) Add the mixed solution B dropwise to the mixed solution A at a speed of 1 drop per second, and stir at a speed of 800rpm for 5h; After stirring, the solution was stirred for another 4h after the addition, and allowed to settle for 24h.

[0070] (3) Add deionized water to the above solution drop by drop until the top layer of the crystal is dissolved, vacuum filter the solution thro...

Embodiment 2

[0072] This embodiment provides a method for preparing a transition metal tetraamide-based macrocyclic ligand oxidation catalyst, comprising the following steps:

[0073] (1) Weigh 4.06 g of the tetraamido-macrocyclic ligand synthesized in Example 1 and put it in a 500 mL Schlenk bottle, add 160 mL of tetrahydrofuran distilled from water at the same time, stir at a speed of 500 rpm, and feed nitrogen As a protective gas, the flow rate is 100mL / min, then quickly add 10mL of n-butyllithium, keep stirring in the ice-water bath for 15min, then remove the ice-water bath, and stir at 25°C for 15min.

[0074] (2) Add 1.5g of anhydrous ferrous chloride to the above system, stir for 12h with a rotating speed of 500rpm, turn off the nitrogen protection, continue to stir for 3h in the air, filter to obtain a solid, wash 5 times with dichloromethane, and finally obtain the formula ( A) Iron tetraamido macrocyclic ligand oxidation catalyst shown.

[0075]

Embodiment 3

[0077] This example provides a method for preparing a transition metal tetraamide-based macrocyclic ligand oxidation catalyst, the difference between the preparation method and Example 2 is that 1.5g of anhydrous ferrous chloride is replaced by 1.67g of anhydrous cupric chloride , keeping other conditions unchanged.

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Abstract

The invention relates to a preparation method and application of a tetra-amido macrocyclic ligand and a metal chelate thereof. The preparation method comprises the following steps: (1) mixing a compound shown as formula (I) with organic alkali to obtain a mixed solution A; mixing the compound shown as formula (II) with a carboxyl activating agent to obtain a mixed solution B; and (2) mixing the mixed solution A with the mixed solution B obtained in the step (1), and then mixing the mixing product with a strong acid solution to obtain the tetra-amido macrocyclic ligand shown as formula (III). Compared with a synthesis method in the prior art, the synthesis method provided by the invention is greener, lower in toxicity, simpler in synthesis route, easy to control synthesis conditions, higherin synthesis efficiency and lower in cost, and can easily achieve industrial production and improve economic benefits. The tetra-amido macrocyclic ligand can be further chelated with a transition metal to obtain an oxidation catalyst, which can be used for treating industrial wastewater of papermaking, printing and dyeing, pharmacy, organic chemical engineering and the like and remediating polluted soil.

Description

technical field [0001] The invention belongs to the technical field of synthesis of environmental functional materials, and in particular relates to a preparation method and application of a tetraamide macrocyclic ligand and a metal chelate thereof. Background technique [0002] At present, the catalytic technology based on the oxidation of hydrogen peroxide has received extensive attention in the field of environment and catalysis, but the biggest shortcoming of this natural oxidant in practical applications is its low activity and low selectivity when reacting with substrates, so it is necessary to develop A catalyst that can improve the oxidation activity of oxidants such as hydrogen peroxide, thereby reducing the harm to the environment. Due to its unique physical and chemical properties, the transition metal tetraamide-based macrocyclic ligand catalytic oxidant has strong catalytic performance, and the degraded product is environmentally friendly, and can be used as an ...

Claims

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Application Information

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IPC IPC(8): C07D257/10B09C1/08
CPCB09C1/08C07D257/10
Inventor 李庭刚韦漩
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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