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Cobalt-iron bimetal in-situ doped MCM-41 catalyst, and preparation method and application thereof

A MCM-41, in-situ doping technology, applied in catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of complex MCM-41 catalyst process, uneven metal dispersion, poor stability, etc. Increase activation effect, rich pores, and efficient degradation

Inactive Publication Date: 2019-07-12
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a cobalt-iron bimetallic in-situ doped MCM-41 catalyst and its preparation method and its application in degrading dye wastewater. The technical solution of the present invention can solve the process of preparing MCM-41 catalyst by other methods Complexity, poor stability and uneven metal dispersion, to achieve the purpose of preparing MCM-41 catalyst with more stable structure, higher metal dispersion and better catalytic effect, and the preparation process is simple

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  • Cobalt-iron bimetal in-situ doped MCM-41 catalyst, and preparation method and application thereof
  • Cobalt-iron bimetal in-situ doped MCM-41 catalyst, and preparation method and application thereof
  • Cobalt-iron bimetal in-situ doped MCM-41 catalyst, and preparation method and application thereof

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Embodiment 1

[0032] One, the preparation method of cobalt-iron bimetallic in-situ doped MCM-41 catalyst of the present embodiment comprises the following steps:

[0033] 1. Weigh 0.1182g Fe(NO 3 ) 3 9H 2 O and 0.0804g Co(NO 3 ) 2 ·6H 2 O was dissolved in ethanol-deionized water mixed solution (deionized water volume was 5 mL, ethanol was 2 mL), and ultrasonic treatment was performed for 5 min to prepare metal precursor solution A.

[0034] 2. Weigh 1.216g of cetyltrimethylammonium bromide (CTAB) and 0.222g of sodium hydroxide and dissolve in 50mL of deionized water, stir in a water bath at 35°C for 30min, and sonicate for 2h to form solution B.

[0035] 3. Add 6.2mL tetraethyl orthosilicate (TEOS)-ethanol mixed solution (volume of tetraethyl orthosilicate: 6.2mL, ethanol: 3mL) drop by drop while stirring under hydrothermal conditions at 35°C. Stir at room temperature for 2h.

[0036] 4. The metal precursor solution A was added dropwise to the gel C, and then poured into a polytetraf...

Embodiment 2

[0046] One, the preparation method of cobalt-iron bimetallic in-situ doped MCM-41 catalyst of the present embodiment comprises the following steps:

[0047] 1. Weigh 0.1182g Fe(NO 3 ) 3 9H 2 O and 0.0804g Co(NO 3 ) 2 ·6H 2 O was dissolved in ethanol-deionized water mixed solution (deionized water volume 5mL, ethanol 2mL), and sonicated for 5min to prepare metal precursor solution A.

[0048] 2. Weigh 1.621g CTAB and 0.2775g sodium hydroxide and dissolve in 50mL deionized water, stir in a water bath at 35°C for 30min, and ultrasonicate for 2h to form solution B.

[0049] 3. Add tetraethyl orthosilicate (TEOS)-ethanol mixed solution drop by drop while stirring under hydrothermal conditions at 40°C (volume of orthosilicate is 6.2mL, and ethanol is 3mL) to form gel C, then cool down to room temperature and stir 2h.

[0050] 4. Add the metal precursor solution A to the gel C dropwise, pour the gel into a polytetrafluoroethylene-lined reactor, and crystallize at 120°C for 72 ...

Embodiment 3

[0058] One, the preparation method of cobalt-iron bimetallic in-situ doped MCM-41 catalyst of the present embodiment comprises the following steps:

[0059] 1. Weigh 0.1182g Fe(NO 3 ) 3 9H 2 O and 0.0804g Co(NO 3 ) 2 ·6H 2 O was dissolved in ethanol-deionized water mixed solution (deionized water volume 5mL, ethanol 2mL), and sonicated for 5min to prepare metal precursor solution A.

[0060] 2. Weigh 2.027g CTAB and 0.2775g sodium hydroxide and dissolve in 50mL deionized water, stir in a water bath at 30°C for 30min, and ultrasonicate for 2h to form solution B.

[0061] 3. Add tetraethyl orthosilicate (TEOS)-ethanol mixed solution drop by drop while stirring under hydrothermal conditions at 35°C (volume of orthosilicate is 6.2mL, ethanol is 3mL) to form a gel C, then cool down to room temperature and stir 2h.

[0062] 4. Add metal precursor solution A dropwise to gel C, pour gel C into a polytetrafluoroethylene-lined reactor, and crystallize at 150°C for 48 hours.

[0...

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Abstract

The invention relates to a cobalt-iron bimetal in-situ doped MCM-41 catalyst, a preparation method thereof, and an application of the catalyst in the degradation of dye wastewater. The preparation method comprises the following steps: an ethyl orthosilicate-ethanol mixed solution is added dropwise to an aqueous solution of cetyltrimethylammonium bromide and sodium hydroxide, the obtained solutionis continuously stirred to form a gel, an ethanol-water solution of cobalt nitrate and iron nitrate is added to the gel, the obtained mixture is crystallized in a reaction kettle, and the crystallizedmixture is filtered, washed, dried and calcined to obtain the MCM-41 molecular sieve catalyst with the framework doped with CoFe. The catalyst can be used to degrade methyl orange in the dye wastewater. The CoFe / MCM-41 catalyst has the advantages of simple preparation process, good structural stability, and uniform dispersion of metals in the molecular sieve framework, and can efficiently degradethe methyl orange by activating PMS or H2O2 under the action of microwave radiation.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials and organic dye wastewater treatment, and in particular relates to an iron-cobalt double metal in-situ doped MCM-41 catalyst and its preparation method and application. Background technique [0002] With the acceleration of modern industrialization, excessive discharge of industrial wastewater containing various organic substances has caused great damage to the water ecological environment. Printing and dyeing wastewater has complex components, large changes in water quality, poor biodegradability, and high chroma. It is a typical refractory organic industrial wastewater. Azo dyes are one of the most diverse and numerous dyes, and are one of the main pollutants of dye wastewater. [0003] Advanced oxidation technology (AOPs) has the characteristics of non-selectivity and strong oxidation in the oxidation process. It can oxidize refractory organic matter in water into low-toxic or non-...

Claims

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Application Information

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IPC IPC(8): B01J29/03B01J29/04B01J37/10B01J37/34B01J37/03B01J37/08C02F1/30C02F1/72C02F101/30
CPCB01J29/0333B01J29/044B01J37/10B01J37/343B01J37/036B01J37/082C02F1/302C02F1/722C02F2305/10C02F2101/308B01J2229/18C02F2305/026
Inventor 戴萍徐东彦孙晓伟汪传生刘一
Owner QINGDAO UNIV OF SCI & TECH
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