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Immobilized metal phthalocyanine catalyst prepared by synchronous synthesis and immobilization method and its preparation and application method

A metal phthalocyanine and catalyst technology, which is applied in the field of solid-supported metal phthalocyanine catalysts, can solve the problems of low solid loading of metal phthalocyanine catalysts, difficult preparation process, etc., and achieves low cost, simple process, and improved thermal stability. Effect

Inactive Publication Date: 2019-01-22
ZHONGBEI UNIV
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  • Summary
  • 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 phthalocyanine catalyst prepared by synchronous synthesis and immobilization method and its preparation and application method
  • Immobilized metal phthalocyanine catalyst prepared by synchronous synthesis and immobilization method and its preparation and application method
  • Immobilized metal phthalocyanine catalyst prepared by synchronous synthesis and immobilization method and its preparation and application method

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 solid-supported metal phthalocyanine heterogeneous catalysts, and specifically relates to a solid-supported metal phthalocyanine catalyst prepared by simultaneous synthesis and solid-supporting methods, which is a solid-supported polyglycidyl methacrylate / silica gel solid-supported catalyst. The metal phthalocyanine catalyst is first bonded with 4-(4-carboxyphenoxy) phthalonitrile on a polyglycidyl methacrylate / silica gel carrier to prepare modified particles bonded with phthalonitrile. Then, the modified particles are reacted with the substituted phthalonitrile and the metal salt in the solution to form a ring, and the metal phthalocyanine is simultaneously synthesized and immobilized. The invention has simple preparation process, low cost, wide source of selected raw materials, simple post-processing, is suitable for industrial production, improves the thermal stability of the catalyst, facilitates the separation of the catalyst from the reaction medium, and allows the catalyst to be reused, etc. , greatly improving the efficiency of the catalytic process. The prepared solid-supported metal phthalocyanine can effectively degrade methylene blue in wastewater using visible light, and can catalyze the green and efficient oxidation of styrene with oxygen.

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 Patents(China)
IPC IPC(8): B01J31/22C07D303/04C07D301/06A62D3/17A62D101/28
CPCA62D3/17C07D301/06C07D303/04B01J31/1658B01J31/183A62D2101/28B01J2531/72B01J2531/842B01J2531/845B01J2531/025B01J2531/16B01J2231/72B01J35/39Y02P20/50
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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