Immobilized metal phthalocyanines catalyst prepared by aid of synchronous synthesis and immobilization processes and methods for preparing and applying immobilized metal phthalocyanines catalyst

A metal phthalocyanine and catalyst technology, which is applied in the field of immobilized metal phthalocyanine catalysts, can solve the problems of difficult preparation process and low immobilization capacity of metal phthalocyanine catalysts, and achieve simple process, low cost and improved thermal stability Effect

Inactive Publication Date: 2016-10-12
ZHONGBEI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the defects of low immobilization capacity and difficult preparation process of metal phthalocyanine catalysts in the prior art, the present invention provides: (1) a metal phthalocyanine catalyst immobilized on a polymer / silica gel hybrid material, which can be irradiated by visible light Effectively degrades organic dye pollutants in wastewater, and can also catalyze the oxidation of styrene with oxygen; (2) A preparation method of an immobilized metal phthalocyanine catalyst, (3) An application method of an immobilized metal phthalocyanine catalyst

Method used

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  • Immobilized metal phthalocyanines catalyst prepared by aid of synchronous synthesis and immobilization processes and methods for preparing and applying immobilized metal phthalocyanines catalyst
  • Immobilized metal phthalocyanines catalyst prepared by aid of synchronous synthesis and immobilization processes and methods for preparing and applying immobilized metal phthalocyanines catalyst
  • Immobilized metal phthalocyanines catalyst prepared by aid of synchronous synthesis and immobilization processes and methods for preparing and applying immobilized metal phthalocyanines catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: In a four-necked flask, add 1.0 g of hybrid material PGMA / SiO 2 and 40 mL of N,N-dimethylformamide, fully soaked and swollen, added 0.30 g of CPPN and 1.5 mL of triethylamine, raised the temperature to 100 ° C under the protection of nitrogen, and reacted at constant temperature for 8 hours, filtered, absolute ethanol and The microspheres were fully washed with distilled water and dried in vacuum to obtain CPPN-PGMA / SiO particles bonded with CPPN 2 , The bonding amount of CPPN is 3.8g / 100g.

[0029] In a four-necked flask, 1.0 g CPPN-PGMA / SiO 2 Soak in 30 mL of n-pentanol to fully swell the particles, then add 0.6 g of 4-nitrophthalonitrile and 0.35 g of cobalt acetate hydrate, and add a certain amount of 2.5 mL of 1, 8-diazacyclo[5, 4, 0] Undec-7-ene, reflux reaction for 12 h under nitrogen protection, cooling and filtering, and repeatedly washing the product particles with methanol, then soaking in concentrated sulfuric acid and washing with distilled wat...

Embodiment 2

[0030] Example 2: In a four-neck flask, add 1.2 g of hybrid material PGMA / SiO 2 and 38 mL of dimethyl sulfoxide, fully soaked and swollen, added 0.35g CPPN and 0.26g NaOH, heated to 90°C under nitrogen protection, reacted at constant temperature for 9h, filtered, fully washed the microspheres with absolute ethanol and distilled water, and dried in vacuum , to get CPPN-PGMA / SiO particles bonded with CPPN 2 , the bonding amount of CPPN is 3.3g / 100g.

[0031] In a four-necked flask, 1.1 g CPPN-PGMA / SiO 2 Soak in 28 mL of n-pentanol to fully swell the particles, then add 0.55 g of 4-nitrophthalonitrile and 0.33 g of manganese acetate hydrate, and add 2.6 mL of 1, 8-diazacyclo[5,4,0 ] Undec-7-ene, reflux reaction under nitrogen protection for 11 h, cooling and filtering, and repeatedly washing the product particles with methanol, then soaking in concentrated sulfuric acid and washing with distilled water to neutrality, and finally using N,N-dimethyl Slightly boil formamide, wash...

Embodiment 3

[0032] Example 3: In a four-necked flask, add 1.1 g of hybrid material PGMA / SiO 2 and 35 mL of dimethyl sulfoxide, after fully soaking and swelling, add 0.32g CPPN and 1.00g Na 2 CO 3 , heated up to 110°C under the protection of nitrogen, reacted at constant temperature for 10 hours, filtered, washed the microspheres with absolute ethanol and distilled water, and dried in vacuum to obtain CPPN-PGMA / SiO particles bonded with CPPN 2 , The bonding amount of CPPN is 3.2g / 100g.

[0033] In a four-neck flask, 1.2 g CPPN-PGMA / SiO 2 Soak in 25 mL of n-pentanol to fully swell the particles, then add 0.5 g of 4-nitrophthalonitrile and 0.21 g of copper acetate hydrate, and add 2.4 mL of 1, 8-diazacyclo[5,4,0 ] Undec-7-ene, reflux reaction for 13 h under the protection of nitrogen, cooled and filtered, and washed the product particles repeatedly with methanol, then soaked in concentrated sulfuric acid and washed with distilled water to neutrality, and finally washed with N,N-dimethyl ...

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Abstract

The invention belongs to the technical field of immobilized metal phthalocyanines heterogeneous catalysts, and particularly relates to an immobilized metal phthalocyanines catalyst prepared by the aid of synchronous synthesis and immobilization processes. The immobilized metal phthalocyanines catalyst is a polymethylacrylic acid glycidyl ester / silica gel immobilized metal phthalocyanines catalyst. A method for preparing the immobilized metal phthalocyanines catalyst includes bonding 4-(4-carboxyl phenoxy) phthalonitrile on polymethylacrylic acid glycidyl ester / silica gel carriers to obtain modified micro-particles bonded with phthalonitrile; carrying out ring formation reaction on the modified micro-particles and substituted phthalonitrile and metal salt in solution; synchronously synthesizing and immobilizing metal phthalocyanines. The immobilized metal phthalocyanines catalyst and the method have the advantages that technologies for preparing the immobilized metal phthalocyanines catalyst are simple, the immobilized metal phthalocyanines catalyst is low in cost, selected raw materials for the immobilized metal phthalocyanines catalyst can come from wide sources, post-treatment is simple, the immobilized metal phthalocyanines catalyst and the method are applicable to industrial production, the heat stability of the immobilized metal phthalocyanines catalyst can be improved, the immobilized metal phthalocyanines catalyst is convenient to separate from reaction media and can be reused, and the efficiency of catalysis procedures can be greatly enhanced; methylene blue in wastewater can be effectively degraded by the prepared immobilized metal phthalocyanines by the aid of visible light, and oxygen can be catalyzed by the immobilized metal phthalocyanines catalyst to efficiently oxidize styrene in an environment-friendly manner.

Description

technical field [0001] The invention belongs to the technical field of solid-supported metal phthalocyanine heterogeneous catalysts, and in particular relates to a solid-supported metal phthalocyanine catalyst prepared by synchronous synthesis and immobilization method and its preparation and application method. Background technique [0002] The metal phthalocyanine compound has an aromatic conjugated macrocyclic ring with 18 π electrons. This large π bond conjugated structure makes it very stable, resistant to acids, alkalis, water, heat, light and various organic solvents , stable chemical properties. Metal phthalocyanine and its derivatives not only have unique optical, acoustic, electrical, magnetic and other properties, but also have excellent catalytic properties (the conjugated molecule is a planar structure, and the catalytic reaction can occur in the axial position; the aromatic ring contained It is both an electron donor and an electron acceptor), which can cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D303/04C07D301/06A62D3/17A62D101/28
CPCA62D3/17A62D2101/28B01J31/1658B01J31/183B01J35/004B01J2231/72B01J2531/025B01J2531/16B01J2531/72B01J2531/842B01J2531/845C07D301/06C07D303/04Y02P20/50
Inventor 王蕊欣谢美娜王晓刚焦纬洲马彦琴吴红玲陈志权朱智明
Owner ZHONGBEI UNIV
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