Hybrid material of polypyridine zinc complex modified MIL-101, preparation method and application in catalyzing degradation of organic phosphorus

A polypyridine zinc and hybrid material technology, which is applied in the field of organic hybrid materials, can solve the problems of unstable existence of active species LM-OH, low catalytic hydrolysis rate and efficiency, and achieve good catalytic cycle stability.

Active Publication Date: 2020-05-26
ANHUI NORMAL UNIV
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  • Description
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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 ...

Method used

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  • Hybrid material of polypyridine zinc complex modified MIL-101, preparation method and application in catalyzing degradation of organic phosphorus
  • Hybrid material of polypyridine zinc complex modified MIL-101, preparation method and application in catalyzing degradation of organic phosphorus
  • Hybrid material of polypyridine zinc complex modified MIL-101, preparation method and application in catalyzing degradation of organic phosphorus

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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 N-ethylmorpholine buffer solution with pH 7.0: Weigh 288mg of N-ethylmorpholine into a beaker filled with 45ml 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, a small amount of water for rinsing the flask was also added to the volumetric flask, and the volume was adjusted to 50 ml. Then use a small amount of 1mol / L hydrochloric acid or 1mol / L sodium hydroxide to adjust the pH of the solution to 7.0.

[0045] 50mM N-ethylmorpholine buffer solution with pH 8.0: Weigh 288mg of N-ethylmorpholine into a beaker containing 45ml 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, a small amount of water for rinsing the flask was also added t...

Embodiment 1

[0049] A kind of preparation method of the hybrid material of polypyridine zinc complex modification MIL-101, comprises the following steps:

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

Embodiment 2

[0056] A kind of preparation method of the hybrid material of polypyridine zinc complex modification MIL-101, comprises 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 Add 55.8 mg of MIL-101 activated by the above steps, ultrasonically disperse for 5 minutes, then reflux at 378K for 16 hours, centrifuge, wash with toluene and ethanol three times respectively, put it in a vacuum oven at 353K after centrifugation, and dry 12 hours.

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

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Abstract

The invention discloses a hybrid material of polypyridine zinc complex modified MIL-101, a preparation method and application in catalyzing degradation of organic phosphorus. A zinc complex capable ofcarrying out site separation is modified on a node of an activated chromium-based metal organic framework compound, a composite catalyst with multiple active centers is constructed, lewis acid activation of organic phosphorus by the zinc complex and MOFs hybrid material and catalytic breaking of P-O bonds by lewis base of the zinc complex on an MOF node are realized under a weakly alkaline condition, and the catalyst is used for degrading organic phosphorus. The hybrid material prepared by the method disclosed by the invention is relatively high in hydrolysis activity of catalyzing diethyl p-nitrophenol phosphate; the catalytic turnover frequency TOF of the hybrid material is 0.244 h<-1> and is improved by 40.2% compared with that of unmodified MIL-101, the hybrid material shows good catalytic cycle stability, the activity of the hybrid material is still kept at 95.7% after five cycles, and the hybrid material can be applied to degradation of organic phosphine poison.

Description

technical field [0001] The invention belongs to the technical field of organic hybrid materials, and in particular relates to a hybrid material for modifying MIL-101 with polypyridyl zinc complexes, a preparation method thereof and an application for 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. Organic phosphines can inhibit nerve sodium channels or acetylcholinesterase, and have direct or indirect toxic effects on non-target organisms such as humans; they have certain effects on the activity of adenosine triphosphatase widely distributed on cell membranes; most of organic phosphines are A weak alkylating agent that can methylate guanine bases. Organic phosphine usually contains (thio) phosphate bonds, which are very stable in neutral solution and room temperature, and it takes about 2 mill...

Claims

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Application Information

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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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