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Catalyst of acetylacetone metal supported and carried by ion liquid, and preparation method

A technology of metal catalysts and acetylacetone, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the difficulties of extraction, easy destruction, and difficulty in catalyst recovery, etc. question

Inactive Publication Date: 2007-02-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of acetylacetonate metal catalysts in these reactions also has its inherent disadvantages. Taking oxidation reactions as an example (US4970347, US4046813), because acetylacetone metal catalysts have good solubility in the organic phase, they can be well dissolved Due to the reaction system, it brings difficulties to the aftertreatment process and the recovery of the catalyst: by the method of water washing and extraction, it is difficult to recover it due to the poor solubility of metal acetylacetone catalysts in water; by the method of rectification, due to The by-products (especially some polymerization by-products) produced during the reaction often remain in the scrap during rectification. This part of the by-products is mixed with the metal acetylacetonate catalyst, and the metal acetylacetonate catalyst should be extracted from it It is also quite difficult, and acetylacetone metal catalysts are easily destroyed during high-temperature distillation

Method used

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  • Catalyst of acetylacetone metal supported and carried by ion liquid, and preparation method
  • Catalyst of acetylacetone metal supported and carried by ion liquid, and preparation method
  • Catalyst of acetylacetone metal supported and carried by ion liquid, and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 16.4g (0.2mol) of methylimidazole and 150ml of acetone into a 250ml three-necked flask, stir and cool down to 0°C, slowly add 33.5g (0.25mol) of chloroacetylacetone dropwise within 2 hours, and then raise the temperature Stirring was continued to room temperature for 8 hours. Distill under reduced pressure to constant weight to obtain 39.3 g of chloromethylimidazole acetylacetone (yield: 91.0%).

Embodiment 2

[0019] In a 250ml three-necked flask, add 10.8g (0.04mol) ferric chloride hexahydrate and 100ml ethanol, in a constant pressure dropping funnel of 100ml, 26.0g (0.12mol) chloromethylimidazole acetylene obtained in Example 1 Dissolve acetone in 80ml of ethanol, raise the temperature to 40°C with stirring, slowly add the ethanol solution of chloromethylimidazole acetylacetone dropwise within 2 hours, and continue to keep warm and stir for 5 hours after the drop is completed. Distill under reduced pressure to constant weight to obtain 27.9 g of chloromethylimidazolium acetylacetonate iron (III) (yield: 99.2%).

Embodiment 3

[0021] Add 16.4g (0.2mol) of methylimidazole and 150ml of methanol into a 500ml three-necked flask, stir and cool down to 0°C, slowly add 33.5g (0.25mol) of chloroacetylacetone dropwise within 2 hours, and then raise the temperature Stirring was continued to room temperature for 8 hours.

[0022] In the constant pressure dropping funnel of 250ml, add the mixed solution of 18.1g (0.067mol) iron trichloride hexahydrate and 150ml methanol. The solution in the three-necked flask was heated up to 40°C with stirring, and the methanol solution of ferric chloride was slowly added dropwise within 2 hours, and continued to keep stirring for 5 hours after the drop was completed. Distill under reduced pressure to constant weight to obtain 46.2 g of chloromethylimidazolium acetylacetonate iron (III) (yield: 98.1%).

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Abstract

An ionic liquid carried acetylacetone-metal catalyst able to be easily recovered from reaction system by water washing is prepare through reaction between substituted acetylacetone and imidazole at -20-150 deg.C to obtain ionic liquid carried acetylacetone, and the complex reaction between said ionic liquid carried acetylacetone and transition metal at 0-100 deg.C.

Description

technical field [0001] The invention relates to a catalyst and a preparation method of a metal acetylacetonate supported by an ionic liquid. Background technique [0002] As everyone knows, acetylacetone metal reagent is an excellent reaction process in oxidation reaction (US4970347, US4046813, CN1425642), ring-opening polymerization reaction, graft polymerization reaction (CN1470534, CN1405192, CN1405192, CN1422876, CN1263520, CN1470535, CN1572809) etc. catalyst. However, the use of acetylacetonate metal catalysts in these reactions also has its inherent disadvantages. Taking oxidation reactions as an example (US4970347, US4046813), because acetylacetone metal catalysts have good solubility in the organic phase, they can be well dissolved Due to the reaction system, it brings difficulties to the aftertreatment process and the recovery of the catalyst: by the method of water washing and extraction, it is difficult to recover it due to the poor solubility of metal acetylacet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18B01J31/30C08F4/72C08F4/80
Inventor 李浩然胡兴邦王从敏
Owner ZHEJIANG UNIV
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