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Core-shell structure loaded tungsten composite catalyst, preparation method and application thereof

A composite catalyst and shell structure technology, applied in catalyst activation/preparation, chemical instruments and methods, chemical elements of heterogeneous catalysts, etc., can solve the problems of long synthesis steps, large amount of three wastes, complicated operation, etc., and achieve low production cost. , The effect of less strong alkali and simple operation

Active Publication Date: 2017-12-15
HANGZHOU NORMAL UNIVERSITY +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the synthesis of the main ring of quinolones basically requires three-step reactions to obtain its key intermediates, and then undergoes hydrolysis and substitution reactions to obtain quinolones. There are long synthesis steps, cumbersome operations, large amounts of three wastes, and high costs. advanced defects

Method used

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  • Core-shell structure loaded tungsten composite catalyst, preparation method and application thereof
  • Core-shell structure loaded tungsten composite catalyst, preparation method and application thereof
  • Core-shell structure loaded tungsten composite catalyst, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1-12

[0039] Preparation of Magnetic Separation Core-Shell Supported Tungsten Composite Catalyst WO 3 / SiO 2 / Fe 3 O 4 The preparation method is carried out according to the following steps in turn:

[0040] 1), the preparation of Fe 3 O 4 Nanoparticles

[0041] Preparation of Fe by Partial Reduction-Coprecipitation 3 O 4Nanoparticles. 16.3 g FeCl at room temperature 3 Add to 250 mL flask and dissolve with water. Under the protection of nitrogen, slowly add the reducing agent Na 2 SO 3 Solution (containing 2.7g Na 2 SO 3 ) and stirring, and 40.8 mL of ammonia water with a mass fraction of 28% was quickly added after 10 minutes, and the formation of black particles was observed. The temperature of the constant temperature water bath was raised to 70 °C, and 2 mL of oleylamine was added as a surfactant, and the stirring was continued for 6 hours. After that, the product was centrifuged and washed with deionized water for several times. Finally, the ionized water was disp...

Embodiment a1-a12

[0049] Embodiment a1-a12: the preparation method of quinolones

[0050] Put 24.6g ethyl formyl ethyl acetate sodium salt, 100mL toluene and 4g WO into the reactor 3 / SiO 2 / Fe 3 O 4 Catalyst, feed 8.7g dimethylamine under stirring, add 10g 2,4-dichloro-5-fluorobenzoyl chloride, keep the reaction for 1 hour, add cyclopropylamine dropwise at 50°C, and feed CO at the same time 2 , the control reaction pressure is 1.5-2 atmospheres. After reacting for 1 hour, 12 g of flake alkali and 200 mL of toluene were added to the reaction solution, and the temperature was raised to 100° C. with stirring, kept for half an hour, the catalyst was recovered by filtration, and the toluene was recovered under pressure to dryness. Add an appropriate amount of water, heat up to 100°C, and after the system is clarified, add hydrochloric acid dropwise to adjust the pH, and after the crystals are precipitated, centrifuge and dry to obtain the organic amine compound of formula (V).

[0051] Embodim...

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Abstract

The invention discloses a core-shell structure loaded tungsten composite catalyst, a preparation method and application thereof. Existing synthesis of the main rings of quinolone drugs mostly has the defects of long synthesis steps, tedious operation, large amount of three wastes, high cost, etc. Fe3O4 colloid and SiO2 / Fe3O4 composite nanoparticles are prepared to prepare a magnetic separation core-shell loaded tungsten composite catalyst WO3 / SiO2 / Fe3O4 used for catalytic synthesis of quinolone compounds. The invention provides an efficient quinolone compound preparation method with magnetically separable and recyclable catalyst. The catalyst prepared by the method provided by the invention can be reutilized in preparation of quinolone compounds, still maintains the original activity and is free of inactivation phenomenon, not only greatly improves the production efficiency, but also reduces environmental pollution.

Description

technical field [0001] The invention relates to a catalyst, a preparation method and its application, in particular to a magnetic separation core-shell structure supported tungsten composite catalyst, a preparation method and a preparation method applied to the synthesis of quinolone compounds. Background technique [0002] Quinolones are one of the most widely used anti-infectives in clinical practice. Quinolones have the advantages of broad antibacterial spectrum, strong antibacterial activity, convenient administration, few adverse reactions, and no cross-resistance with other antibiotics. The first choice for combination drugs, the market demand is large. [0003] In recent years, studies have found that quinolones have new curative effects in anti-malarial, anti-AIDS, anti-tumor and other diseases. It has good activity, and its activity spectrum and application range are constantly expanding. [0004] However, the synthesis of the main ring of quinolones basically req...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/888C07D215/56
CPCB01J23/888C07D215/56B01J2523/00B01J35/398B01J35/33B01J2523/41B01J2523/69B01J2523/842Y02P20/584B01J35/397B01J37/342
Inventor 章鹏飞沈超顾海宁李小玲徐骏
Owner HANGZHOU NORMAL UNIVERSITY
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