Method for preparing composite magnetic catalyst of magnetic solid sulfonic acid loaded amine catalyst and application thereof

A composite magnetism and catalyst technology, which is applied in the preparation of organic compounds, catalytic reactions, and preparation of carboxylic acid nitriles, etc., to achieve the effects of high product yield, improved activity, and high catalytic efficiency

Active Publication Date: 2018-08-24
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of preparation method of the composite magnetic catalyst of magnetic solid sulfonic acid load amine-based catalyst for the existing problem of the catalyst that is used for Knoevenagel condensation reaction

Method used

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  • Method for preparing composite magnetic catalyst of magnetic solid sulfonic acid loaded amine catalyst and application thereof
  • Method for preparing composite magnetic catalyst of magnetic solid sulfonic acid loaded amine catalyst and application thereof
  • Method for preparing composite magnetic catalyst of magnetic solid sulfonic acid loaded amine catalyst and application thereof

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Experimental program
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Effect test

Embodiment 1

[0033] Preparation and application of embodiment 1, composite catalyst MSA / A1

[0034] Fe 3 o 4 Preparation of magnetic particles: Take 2.6 g FeCl 3 •6H 2 O was dissolved in 50 mL of ethylene glycol solution with vigorous stirring to form a clear solution, and then 5.75 g of NaAc and 1.0 g of polyethylene glycol were added. The mixture was magnetically stirred for 30 min to obtain a dark brown-yellow viscous liquid. Afterwards, the liquid was transferred into a 50 mL polytetrafluoroethylene-lined stainless steel reaction kettle, and the temperature was raised to 200 °C in a constant temperature blast drying oven. After 8 h of reaction, it was naturally cooled to room temperature. After taking out the solution in the kettle, wash it several times with absolute ethanol and deionized water, and dry it under vacuum at 60° C. to obtain a black powder. References (Li Y D, Deng H, Li XL, Peng Q, Wang X, Chen J P. Angew. Chem. Int. Ed , 2005, 44 , 2782- 2785.) Preparation of F...

Embodiment 2

[0047] The preparation and application of embodiment 2, composite catalyst MSA / A2

[0048] Fe 3 o 4 Preparation of magnetic particles: same as Example 1;

[0049] Mercapto-coated spherical Fe3O4 3 o 4 @SiO 2 -The preparation of SH: with embodiment 1

[0050] The preparation of magnetic sulfonic acid MSA: with embodiment 1;

[0051] Preparation of composite catalyst MSA / A2: magnetic sulfonic acid MSA (1.0 g, 0.5 mmol) was suspended in CH 2 Cl 2 (20 mL), and the reaction mixture was stirred at room temperature for 15 minutes. then add N 1 ,N 1 ,N 2 ,N 2 - Tetramethylethane-1,2-diamine (A2) (70 mg, 0.6 mmol), and the resulting mixture was stirred at room temperature for 0.5 hours. Use an external magnet to attract and separate the catalyst, and use CH 2 Cl 2 washing. The resulting solid was dried under vacuum overnight at room temperature to afford MSA / A2 in 97% yield. Its reaction formula is as follows:

[0052]

[0053] Knoevenagel condensation reaction: p-...

Embodiment 3

[0054] The preparation of embodiment 3, composite catalyst MSA / A3

[0055] Fe 3 o 4 Preparation of magnetic particles: same as Example 1;

[0056] Mercapto-coated spherical Fe3O4 3 o 4 @SiO 2 -The preparation of SH: with embodiment 1

[0057] The preparation of magnetic sulfonic acid MSA: with embodiment 1;

[0058] Preparation of composite catalyst MSA / A3: magnetic sulfonic acid MSA (1.0 g, 0.5 mmol) was suspended in CH 2 Cl 2 (20 mL), and the reaction mixture was stirred at room temperature for 15 minutes. 4-Dimethylaminopyridine (A3) was then added. (73 mg, 0.6 mmol), and the resulting mixture was stirred at room temperature for 0.5 hours. Use an external magnet to attract and separate the catalyst, and use CH 2 Cl 2 washing. The resulting solid was dried under vacuum overnight at room temperature to afford MSA / A3 in 98% yield. Its reaction formula is as follows:

[0059]

[0060] Knoevenagel condensation reaction: p-chlorobenzaldehyde (0.5mmol), ethyl cya...

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Abstract

The invention discloses a method for preparing a composite magnetic catalyst of a magnetic solid sulfonic acid loaded amine catalyst. A one-kettle method is used for preparing mercapto coated ball ferriferrous oxide Fe3O4-coated SiO2-SH, hydrogen peroxide is employed for oxidizing a mercapto group (-SH) in Fe3O4-coated SiO2-SH to obtain magnetic sulfonic acid MSA, then magnetic solid sulfonic acidis taken as a carrier, an organic micromolecule amine catalyst is subjected to non covalent loading through acid-base effect, and a magnetic solid sulfonic acid-loaded diamine composite catalyst is prepared. The magnetic solid sulfonic acid of the composite catalyst can be used as the carrier, and a catalytic process can be directly participated and influenced through soda acid effect, so that activity of the composite catalyst for catalysis of a Knoevenagel condensation reaction is effectively increased; through an external magnet, direct attraction and separating can be realized, multitimecycle utilization is realized, and the problems of immobilization, separating recovery and reuse of the catalyst can be effectively solved.

Description

technical field [0001] The invention relates to a preparation method of a composite magnetic catalyst loaded with magnetic solid sulfonic acid diamine, which is mainly used in the Knoevenagel condensation reaction system of aldehyde and active methylene as a catalyst. Background technique [0002] The Knoevenagel condensation reaction is the reaction of aldehydes or ketones with active methylene-containing compounds to form unsaturated compounds and water, which have been widely used as intermediates in the synthesis of natural products, drugs and organic photovoltaic materials. Currently, organic bases and acids as well as ionic liquids are used as catalysts to catalyze the Knoevenagel condensation reaction. However, most of these catalysts are not recyclable and use organic solvents in the catalytic system. The use of microwave radiation and ultrasonic conditions can promote the solvent-free Knoevenagel condensation reaction, but high-power microwave and ultrasonic condit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02B01J31/28C07C253/30C07C255/41C07C255/35C07C255/37C07C255/36C07C255/34C07D307/54C07B37/00
CPCB01J31/0237B01J31/0244B01J31/0275B01J31/28B01J35/0033B01J2231/4205C07B37/00C07C253/30C07D307/54C07C255/41C07C255/35C07C255/37C07C255/36C07C255/34
Inventor 周鹏鑫宋靖靖张鹏兵张哲霍淑慧
Owner NORTHWEST NORMAL UNIVERSITY
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