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Environment-friendly method used for preparing azoxy compound taking MOFs derivative magnetic nanometer particles as recoverable catalyst

A technology of magnetic nanoparticles and azo oxide, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of practical application and development limitations, poor stability, etc., and reduce production costs , high yield and simple reaction conditions

Active Publication Date: 2019-06-25
湖北瀚飞新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in green chemistry, how to design the use of environmentally friendly and non-toxic metal catalysts has become the key. Metal-organic framework (MOFs) materials have been obtained due to their ordered and regular structure, high specific surface area, and structural adjustability. People's extensive attention and research, as a rapidly developing new porous material, it has more attractive application prospects than traditional porous materials. However, due to the relatively poor stability of MOFs, its practical application and development have been greatly restricted.

Method used

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  • Environment-friendly method used for preparing azoxy compound taking MOFs derivative magnetic nanometer particles as recoverable catalyst
  • Environment-friendly method used for preparing azoxy compound taking MOFs derivative magnetic nanometer particles as recoverable catalyst
  • Environment-friendly method used for preparing azoxy compound taking MOFs derivative magnetic nanometer particles as recoverable catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] a. Synthesis of ZIF-67: Dissolve 0.6g of cobalt nitrate hexahydrate and 7.31g of 2-methylimidazole in 4ml and 26 ml of deionized water respectively, slowly add the second part of the solution to the first solution, the color turns purple rapidly, Stirring at room temperature for 3 h, after the reaction was completed, the blue solid was collected by centrifugation at 8000 rpm, centrifuged for 4 min, and washed with ethanol three times. After the collected crystals were dried in vacuum for 5 h, the yield reached 61%. The ZIF-67 structure is as figure 1 Shown are polyhedral particles with a diameter of approximately 400 nm.

[0025] b. Preparation of Co@C-N catalyst: under nitrogen atmosphere, place 0.8g ZIF-67 in a muffle furnace, carbonize at 800°C, heat up at a rate of 10°C / min, hold for 2h, and cool down to room temperature naturally A Co@C-N catalyst was obtained. The structure of Co@C-N is about 100nm particles (such as figure 2 As shown in the SEM image), the p...

Embodiment 2

[0028] Example 2 is basically the same as Example 1, except that the deionized water in step (a) is replaced by methanol or ethanol, and the ethanol in step (c) is replaced by methanol. The target product was also successfully synthesized.

Embodiment 4

[0030] Example 4 is basically the same as Example 1, except that the nitrobenzene in step (c) is replaced by methylnitrobenzene. The target product was also successfully synthesized.

[0031] Example 4

[0032] Example 4 is basically the same as Example 1, except that the nitrobenzene in step (c) is replaced by p-chloronitrobenzene. The target product was also successfully synthesized.

[0033] Example 4

[0034] P-chloronitrobenzene (62.8g, 1mol) and Co / C-N (0.1g) were mixed in a round bottom flask, 500ml of methanol was added, and stirred to 50°C until p-chloronitrobenzene was completely dissolved. Then add 100g of 80% hydrazine hydrate to the above mixture. The reaction temperature was maintained at 50°C, and the reaction was monitored by thin layer chromatography. After the reaction was completed, 300ml of ethyl acetate was added, and the Co / C-N catalyst was separated by magnetic adsorption. The filtrate was concentrated under reduced pressure, and the residue was pu...

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Abstract

The invention discloses an environment-friendly method used for preparing an azoxy compound taking MOFs derivative magnetic nanometer particles as a recoverable catalyst. The characteristics of the method are that: an aromatic nitro compound and a reducing agent are subjected to oxidation reduction reaction under the effect of a Co-containing magnetic nanometer catalyst so as to obtain an azoxybenzene compound; Co@C-N is taken as a catalyst, an aromatic hydrocarbon nitro compound is taken as a raw material, hydrazine hydrate is taking a reducing agent, and the azoxybenzene compound is obtainedthrough synthesis in an alcohol solution. The magnetic catalyst adopted in the reaction can be recycled, production cost is reduced, the method is friendly to the environment, reaction conditions aresimple, and yield is high.

Description

technical field [0001] The invention relates to the field of azo oxide compounds, in particular to a method for green preparation of azo oxide compounds using MOFs derived magnetic nanoparticles as a recyclable catalyst. Background technique [0002] In recent years, azo oxide compounds have received more and more attention due to their special structure, and can be widely used in dyes, pigments, reducing agents, analytical reagents, chemical stabilizers and polymerization inhibitors, and organic synthesis intermediates, such as oxidation Azobenzene is a precursor for the Wallach rearrangement reaction, which provides a simple method for the preparation of hydroxyazobenzene. [0003] At present, the traditional method of synthesizing azoxy compounds is to use zinc, glucose, NaBH 4 Reducing the nitrobenzene compound with a reducing agent, this method will produce a large amount of alkali waste liquid, which will cause damage to the environment, and also requires relatively h...

Claims

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Application Information

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IPC IPC(8): C07C291/08B01J27/24B01J27/28B01J35/00B01J37/08
CPCY02P20/584
Inventor 刘辉李陵岚缪军锋张树
Owner 湖北瀚飞新材料科技有限公司
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