A kind of hybrid material of polybipyridine zinc complex modified mil-101 ​​and preparation method and application of catalytic organophosphorus degradation

A technology of zinc polypyridine and hybrid material is applied in the application of catalytic organophosphorus degradation, and the field of hybrid material and preparation of MIL-101 modified by zinc polypyridine complex can solve the problem that the active species LM-OH cannot exist stably , the problem of low catalytic hydrolysis rate and efficiency, etc., to achieve the effect of good catalytic cycle stability

Active Publication Date: 2022-08-02
ANHUI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Unfortunately, the rate and efficiency of catalytic hydrolysis of these small molecule model substances are not high, because the metal complexes in aqueous solution are easy to form hydroxyl-bridged multinuclear metal complexes LM-OH-ML, so that the active species LM-OH usually cannot stable existence

Method used

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  • A kind of hybrid material of polybipyridine zinc complex modified mil-101 ​​and preparation method and application of catalytic organophosphorus degradation
  • A kind of hybrid material of polybipyridine zinc complex modified mil-101 ​​and preparation method and application of catalytic organophosphorus degradation
  • A kind of hybrid material of polybipyridine zinc complex modified mil-101 ​​and preparation method and application of catalytic organophosphorus degradation

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preparation example Construction

[0043] The preparation method of each buffer solution involved in the present invention is as follows:

[0044] 50mM pH 7.0 N-ethylmorpholine buffer: Weigh 288 mg of N-ethylmorpholine into a beaker containing 45 ml of distilled water, adjust with 1mol / L hydrochloric acid or 1mol / L sodium hydroxide The pH of the solution was close to 7.0, transferred to a 50-ml volumetric flask, and a small amount of water from rinsing the flask was also added to the volumetric flask to make up to 50 ml. Then use a small amount of 1 mol / L hydrochloric acid or 1 mol / L sodium hydroxide to adjust the pH of the solution to 7.0.

[0045] 50mM pH 8.0 N-Ethylmorpholine buffer: Weigh 288 mg of N-Ethylmorpholine into a beaker containing 45 mL of distilled water, adjust with 1mol / L hydrochloric acid or 1mol / L sodium hydroxide The pH of the solution was close to 8.0, transferred to a 50-mL volumetric flask, and a small amount of water from rinsing the flask was also added to the volumetric flask to make ...

Embodiment 1

[0049] A preparation method of a hybrid material of MIL-101 modified by a polybipyridine zinc complex, comprising the following steps:

[0050] (1) Preparation of MIL-101 activated by decoordinated water: Weigh 4.33 g (10.82 mmol) of chromium nitrate nonahydrate and 1.80 g (10.83 mmol) of terephthalic acid and ultrasonically disperse them in 52 mL of deionized water. The ultrasonic dispersion is uniform. , and 0.3 mL (1.5 mmol) of a 42% HF aqueous solution was added dropwise. The above prepared solution was added to a polytetrafluoroethylene-lined autoclave, and heated in a 473K oven for 8 hours. In order to remove impurities in the pores of MIL-101, MIL-101 was refluxed with 450 ml of deionized water for 24 hours, filtered while hot, and then MIL-101 was refluxed with 450 ml of ethanol twice for 24 hours each time, using hot ethanol Washed and filtered, and the obtained crystals were re-used containing NH 4 The aqueous solution of F was refluxed for 24 hours, filtered while...

Embodiment 2

[0056] A preparation method of a hybrid material of MIL-101 modified by a polybipyridine zinc complex, comprising the following steps:

[0057] (1) with step (1) in embodiment 1;

[0058] (2) Preparation of MIL-101-L': Dissolve 37.2 mg of ligand L, namely 4'-(4-pyridyl)-2,2':6',2"-terpyridine in 13 ml of anhydrous toluene 55.8mg of MIL-101 activated by the above steps was added, ultrasonically dispersed for 5 minutes, and then refluxed at 378K for 16 hours, centrifuged, washed three times with toluene and ethanol, and placed in a vacuum drying box at 353K after centrifugation. 12 hours.

[0059] (3) Preparation of MIL-101-L'Zn: 32.8 mg of Zn (CH 3 COOH) 2· 2H 2 O was dissolved in a mixed solvent of 15mL methanol and water (v / v=1:1.1), under vigorous stirring, 65.5mg MIL-101-L' was added, heated under reflux at 343K for 5 hours, centrifuged, and washed three times with methanol , after centrifugation, it was placed in a vacuum drying oven at 353K and dried for 12 hours to ...

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Abstract

The invention discloses a hybrid material of MIL-101 modified by a polybipyridine zinc complex, a preparation method and an application of catalyzing the degradation of organic phosphorus. By modifying the site-separable zinc complexes on the nodes of activated chromium-based metal-organic framework compounds, a multi-active center composite catalyst was constructed to realize the pairing of zinc complexes with MOFs hybrid materials under weak alkaline conditions. Lewis acid activation of organic phosphine and Lewis base of zinc complex on MOF node catalyze the cleavage of P-O bond, as a catalyst for degrading organic phosphine, the hybrid material prepared by the method of the present invention catalyzes the hydrolysis of p-nitrophenol diethyl phosphate High activity, its catalytic conversion frequency TOF is 0.244h ‑1 , which is 40.2% higher than that of the unmodified MIL‑101. The hybrid material exhibits good catalytic cycling stability, and its activity still maintains 95.7% after five cycles, which can be applied to the degradation of organic phosphine poisons.

Description

technical field [0001] The invention belongs to the technical field of organic hybrid materials, and in particular relates to a hybrid material of polybipyridine zinc complex modified MIL-101, a preparation method and an application of catalyzing the degradation of organic phosphorus. Background technique [0002] At present, organophosphine nerve agents are a class of very toxic compounds, which are widely used in chemical pesticides and chemical warfare agents. Organophosphines can inhibit nerve sodium channels or acetylcholinesterase, and have direct or indirect toxic effects on non-target organisms such as humans; have certain effects on the activity of adenosine triphosphatase widely distributed on cell membranes; most of the organophosphines are Weak alkylating agent that can methylate guanine bases. Organophosphines usually contain (thio) phosphate bonds, which are very stable in neutral solution and room temperature, and it takes about 2 million years for about half...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22A62D3/30A62D101/04A62D101/26A62D101/28
CPCB01J31/1815B01J31/1691A62D3/30A62D2101/04A62D2101/26A62D2101/28B01J2531/0241B01J2531/26
Inventor 周映华高艾佳张凯
Owner ANHUI NORMAL UNIV
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