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Magnetic supported catalyst and application thereof in preparing polyphenyleneoxide in aqueous medium

A supported catalyst and magnetic technology, which is applied in the field of polymer metal complex catalysts, can solve the problems that the filtrate cannot be recycled, the catalyst cannot be recycled and reused, and the catalyst and polyphenylene ether products cannot be separated, so as to achieve high catalytic efficiency, Ease of recycling

Inactive Publication Date: 2012-11-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent application 200910097970.7 discloses the preparation method of metal ion-polyvinylimidazole complex catalyst and its application in the preparation of polyphenylene ether in aqueous medium. It is found that its catalytic efficiency is better than that of metal ion-low molecular weight ligand complexation Although the catalyst has high catalytic efficiency, there is still the problem that the catalyst cannot be recycled and reused.
However, catalyst, emulsifier and metal salt for demulsification are all present in the filtrate, and the filtrate containing catalyst cannot be recycled; and if the traditional method is adopted to load the catalyst on an inert carrier (polymer or silica gel), the loaded Catalyst and polyphenylene ether product cannot be separated
Therefore, the recovery and reuse of catalysts for preparing PPO in aqueous media is still an unsolved technical problem.

Method used

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  • Magnetic supported catalyst and application thereof in preparing polyphenyleneoxide in aqueous medium
  • Magnetic supported catalyst and application thereof in preparing polyphenyleneoxide in aqueous medium
  • Magnetic supported catalyst and application thereof in preparing polyphenyleneoxide in aqueous medium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Example 1 Preparation of Magnetically Supported Polyvinylimidazole Ligand-Metal Ion Complex Catalyst

[0072] (1) Preparation of nano-ferric oxide

[0073] Prepare 250 mL of 0.5 mol / L sodium hydroxide aqueous solution and add it to a three-necked flask. Under the protection of nitrogen, the temperature was raised to 80°C. Prepare FeCl 3 ·6H 2 O concentration is 1mol / L, FeCl 2 4H 2 25 mL of an aqueous solution with an O concentration of 0.5 mol / L and an HCl concentration of 0.4 mol / L was added dropwise to the above aqueous sodium hydroxide solution under mechanical stirring at 1200 rpm. React for 30 minutes. After the reaction, wash with distilled water and ethanol for 5 times respectively, separate the obtained solid by applying an external magnetic field, and dry it in vacuum at room temperature for 24 hours to prepare black nanometer ferric oxide.

[0074] (2) Synthesis of polyvinylimidazole ligands with a silane coupling agent at one end

[0075] Dissolve 2.7...

Embodiment 2～4

[0082] Except that the mixture of N-vinylimidazole monomer and water-soluble comonomer is used to replace the N-vinylimidazole in Example 1, the rest of the operations are the same as in Example 1 to prepare polyethylene with a silane coupling agent at one end imidazole ligands, see Table 1 for specific parameters, and finally obtain a magnetically supported polyvinyl imidazole ligand-metal ion complex catalyst.

[0083] Table 1

[0084]

Embodiment 5～6

[0086] Except for changing the feeding ratio of N-vinylimidazole and 3-mercaptopropyltrimethoxysilane, the rest of the operations are the same as in Example 1 to prepare a polyvinylimidazole ligand with a silane coupling agent at one end. The specific parameters As shown in Table 2, a magnetically supported polyvinylimidazole ligand-metal ion complex catalyst was finally obtained.

[0087] Table 2

[0088] Example serial number

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Abstract

The invention discloses a magnetic supported catalyst, which is a complex of a nano magnetic particle surface grafted polyvinyl imidazol ligand and metal ions. A molar ratio of imidazol groups to the metal ions in the complex is (0.5-300):1; and the polyvinyl imidazol ligand is homopolymer of N-polyvinyl imidazol monomers or copolymer of N-polyvinyl imidazol monomers and one or more types of water-soluble monomers. The catalyst has high catalytic efficiency, and can be separated from a reaction medium by applying a magnetic field, so that the catalyst is recycled, and solves the problem that the conventional catalyst has low catalytic efficiency of preparing polyphenyleneoxide (PPO) in a reaction medium, particularly in an aqueous medium, and is difficult to recycle. The invention also discloses a preparation method and application of the magnetic supported catalyst. The preparation method is easy to operate and control, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of polymer metal complex catalysts, in particular to a magnetic-loaded catalyst, a preparation method thereof, and an application of the magnetic-loaded catalyst to prepare polyphenylene ether in an aqueous medium. Background technique [0002] Catalyst recovery and recycling technology can greatly reduce the production cost of products, so it has been extensively and deeply studied. The usual method is to load a homogeneous catalyst on an inert carrier (usually a micron-sized carrier) to form a heterogeneous catalyst. After the reaction is completed, the catalyst is separated and recovered by simple filtration or centrifugation, and further recycled. However, compared with homogeneous catalysts, the catalytic activity and selectivity of the heterogeneous catalysts obtained after loading have a large decline. Reducing the size of the carrier to the nanoscale range can make the supported catalyst basically maintain th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/44C08F26/06
CPCY02P20/584
Inventor 张文丽王奂申屠宝卿翁志学
Owner ZHEJIANG UNIV
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