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Manganese dioxide-supported metal phthalocyanine composite material and its preparation and application in degrading antibiotics

A manganese dioxide and metal-loaded technology, which is applied in the direction of catalyst activation/preparation, oxidized water/sewage treatment, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of high energy consumption and Unfavorable catalytic center exposure, limited catalytic performance and other issues, to achieve the effect of simple and rapid mass production, mass production, and simple process

Active Publication Date: 2022-03-29
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention solves the problem that metal phthalocyanines in the prior art are prone to aggregation when used as a catalyst, which is not conducive to the exposure of the catalytic center, thereby limiting the performance of its catalytic performance, and the preparation of supported metal phthalocyanines requires high energy consumption and low efficiency.

Method used

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  • Manganese dioxide-supported metal phthalocyanine composite material and its preparation and application in degrading antibiotics
  • Manganese dioxide-supported metal phthalocyanine composite material and its preparation and application in degrading antibiotics
  • Manganese dioxide-supported metal phthalocyanine composite material and its preparation and application in degrading antibiotics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Control MnO 2 The total mass of FePc and FePc is 1.0g, and the iron phthalocyanine content is 7.5%, which is added to a dry and clean ball mill jar. The inner depth of the ball mill tank is 3.75 mm, the inner diameter of the tank mouth is 3.2 mm, and the inner volume of the tank is about 50 mL. The ball mill jar and the ball mill cover are connected by a sealing ring.

[0038] (2) Fix the ball milling jar on the ball mill, set the rotating speed of the ball milling jar to 350rpm, and carry out the ball milling reaction at normal temperature and pressure. After 20 minutes of reaction, take out the ball milling jar and collect the solid powder. The resulting solid mixture was washed with distilled water, centrifuged at 6000rpm, and dried at 60°C to obtain MnO 2 / FePc-7.5%.

[0039] (3) X-ray diffraction tests show that MnO 2 The crystal form remains unchanged before and after compounding with FePc, both are γ-MnO 2 ,like figure 1 shown. X-ray photoelectron spec...

Embodiment 2

[0043] In order to evaluate MnO 2 / Catalytic performance of FePc. The product obtained in step (2) of Example 1 was collected. 10mg MnO 2 / FePc composite material was added to 50mL 10mg L -1 Norfloxacin solution. The initial pH of norfloxacin solution was adjusted to 7.0±0.2 by adding dilute HCl or NaOH solution. Place it on a magnetic stirrer and react for 30min. After Norfloxacin is adsorbed-desorbed on the surface of the catalyst to balance, add 100μL of 50g L -1 Potassium persulfate solution starts the degradation reaction of norfloxacin. When the reaction was carried out to 1, 3, 5, 10 and 20 min respectively, 1 mL of degradation solution and 100 μL of 0.5 mol L -1 The sodium thiosulfate solution was mixed and shaken vigorously to terminate the reaction. After the catalyst was filtered out with a 0.22 μm water filter membrane, the concentration of norfloxacin remaining in the degradation solution was determined by high performance liquid chromatography (HPLC). Th...

Embodiment 3

[0045] In order to explore the effect of FePc content on MnO in composites 2 / FePc composite catalytic performance by changing FePc and MnO 2 The mass ratio of preparing phthalocyanine iron content X is respectively 2.5,5,10 and 15% MnO 2 / FePc-X composites, and use catalytic degradation of norfloxacin. The result is as image 3 Shown: As the iron phthalocyanine content increases from 2.5 to 7.5%, MnO 2 The performance of / FePc catalyzing the degradation of norfloxacin by potassium persulfate is gradually enhanced, and its quasi-first-order reaction rate constant k is from 0.24min -1 increased to 0.61min -1 ; As the iron phthalocyanine content further increased to 15%, the k value decreased to 0.28min -1 . It can be seen that MnO 2 / FePc-7.5 has the best catalytic activity.

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Abstract

The invention discloses a manganese dioxide-supported metal phthalocyanine composite material and its application in preparation and degradation of antibiotics, and belongs to the technical field of novel material preparation. The invention discloses a manganese dioxide (MnO 2 ) and metal phthalocyanine (MPc) as raw materials, MnO was prepared by mechanical ball milling 2 Loaded MPc composites (MnO 2 / MPc) and use it to catalyze the oxidative degradation of antibiotics. At normal temperature and pressure, MPc and MnO 2 Mixed and placed in a ball mill reactor, MPc was loaded on MnO by mechanical force effect 2 On the other hand, the preparation process is simple and fast, and the reaction conditions are mild without the use of organic solvents. Prepared MnO 2 The / MPc composite material has the performance of efficiently activating persulfate, and utilizes the generated reactive oxygen species to oxidatively degrade antibiotics.

Description

technical field [0001] The invention belongs to the technical field of novel material preparation, and more specifically relates to a manganese dioxide-supported metal phthalocyanine composite material and its preparation and application for degrading antibiotics, in particular to a method for preparing highly active catalysts by mechanical ball milling and for degrading antibiotics in water bodies. Background technique [0002] Phthalocyanine (Pc) is a two-dimensional aromatic porphyrin compound, and a hole with a diameter of 2.7nm is formed in the phthalocyanine ring composed of four isoindole units. The two hydrogen atoms in the center of the phthalocyanine molecule are replaced by metal ions to obtain metal phthalocyanine (MPc). The metal ions in the structure form covalent bonds with the two Ns in the phthalocyanine ring, and coordinate Binding in the form of bit keys. At present, more than 70 kinds of metal elements such as Cu have been reported 2+ ,Co 2+ , Fe 2+ e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/32C02F1/72C02F101/30C02F101/34C02F101/36C02F101/38
CPCB01J31/32B01J37/0036C02F1/725C02F2101/30C02F2101/36C02F2101/34C02F2101/38C02F2101/40
Inventor 王楠张艺凡朱丽华
Owner HUAZHONG UNIV OF SCI & TECH
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