Parachloronitrobenzene hydrogenation reduction catalyst capable of being magnetically recycled and preparation method

A technology of p-chloronitrobenzene and catalyst, which is applied in the preparation of amino compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve problems such as environmental hazards and harsh reaction conditions, and achieve adsorption and dispersion promotion, the availability of raw materials, the effect of changing the lattice structure

Inactive Publication Date: 2016-03-23
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to price and cost constraints, catalytic selectivity, environmental hazards, and harsh reaction conditions are still the main factors restricting this type of catalyst.

Method used

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  • Parachloronitrobenzene hydrogenation reduction catalyst capable of being magnetically recycled and preparation method
  • Parachloronitrobenzene hydrogenation reduction catalyst capable of being magnetically recycled and preparation method
  • Parachloronitrobenzene hydrogenation reduction catalyst capable of being magnetically recycled and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 270ml of deionized water and 40.5g of ferric chloride into a 500ml three-neck flask and stir to form a homogeneous solution. Add 0.3M KO 2 Slowly add to the solution, stir vigorously, and pass through N 2 Protected, reacted at a temperature of 343K for 2h, and continued to stir for half an hour after the color of the system turned black and gas was no longer released. Stand still until all the black powder in the system sinks to the bottom of the bottle, suck out the upper liquid, first wash repeatedly with deionized water to maintain the pH value of the obtained product at about 7, then add 50ml of methanol washing solution for washing, and put it in a vacuum drying oven after washing Dry at room temperature for 12 hours to obtain magnetic nanoparticles.

[0031] Weigh 50 g of deionized water, add 5 mmol of cobalt sulfate, stir and dissolve for 5 min to obtain cobalt sulfate solution, add 0.01 mol of nano-magnetic particles prepared above, and pass N 2 Protected,...

Embodiment 2

[0034] Add 270ml of deionized water and 60g of ferric sulfate into a 500ml three-necked flask and stir to form a homogeneous solution. Add 0.3M KO 2 Slowly add to the solution, stir vigorously, and pass through N 2 Protected, reacted at a temperature of 343K for 2h, and continued to stir for half an hour after the color of the system turned black and gas was no longer released. Stand still until all the black powder in the system sinks to the bottom of the bottle, suck out the upper liquid, first wash repeatedly with deionized water to maintain the pH value of the obtained product at about 7, then add 50ml of methanol washing solution for washing, and put it in a vacuum drying oven after washing Dry at room temperature for 10 h to obtain magnetic nanoparticles.

[0035] Weigh 50g of deionized water, add 5mmol cobalt chloride, stir and dissolve for 5min to obtain a cobalt chloride solution, add 0.01mol of the above-prepared nano-magnetic particles, and pass N 2 Protected, ult...

Embodiment 3

[0038] Add 270ml of deionized water and 60g of ferric sulfate into a 500ml three-necked flask and stir to form a homogeneous solution. Add 0.2M KO 2 Slowly add to the solution, stir vigorously, and pass through N 2 Protected, reacted at a temperature of 343K for 2h, and continued to stir for half an hour after the color of the system turned black and gas was no longer released. Stand still until all the black powder in the system sinks to the bottom of the bottle, suck out the upper liquid, first wash repeatedly with deionized water to maintain the pH value of the obtained product at about 7, then add 50ml of methanol washing solution for washing, and put it in a vacuum drying oven after washing Dry at room temperature for 10 h to obtain magnetic nanoparticles.

[0039] Weigh 50g of deionized water, add 5mmol of cobalt nitrate, stir and dissolve for 5min to obtain a cobalt nitrate solution, add 0.01mol of the above-prepared nano-magnetic particles, and pass N 2 Protected, ul...

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Abstract

The invention relates to a parachloronitrobenzene hydrogenation reduction catalyst capable of being magnetically recycled and a preparation method. Prepared Fe3O4 nanometer magnetic particles and water-soluble cobalt salt are added into water; ultrasonic full mixing is performed under the protection of inert gas, a reducing agent is added, and a target product is obtained after full reaction under ultrasound. Relevant salts such as iron and cobalt which are rich in nature are adopted as a matrix, raw materials are easy to obtain, and the cost is low. The prepared catalyst can be recycled through an external magnetic field due to the fact that the catalyst contains the Fe3O4 nanometer magnetic particles. The grain size of the prepared catalyst is 5-30 nm, so that the specific surface area can be 100-180 m<2>/g, and thus extremely huge promoting effects can be achieved on reagent adsorption and dispersion in the catalytic reaction process, and finally the conversion rate and selectivity reach 100%. The preparation method is simple, low in energy consumption, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a magnetically recoverable p-chloronitrobenzene hydrogenation reduction catalyst and a preparation method. Background technique [0002] Aromatic amines are important intermediates in drug synthesis, pesticides, dyes, herbicides, polymers, etc. Chloroaniline is a typical aromatic amine. A large part of the source of chloroaniline comes from the nitro reduction of p-chloronitrobenzene. The selective reduction of p-chloronitrobenzene to p-chloroaniline is a very important organic reaction no matter in industry or academia. So far, there are many preparation methods, such as iron powder reduction, electrochemical reduction, CO / H 2 O reduction method, photocatalytic reduction, hydrazine hydrate reduction, catalytic hydrogenation reduction, NaBH 4 Restoration, etc. In the above-mentioned preparation method, for the iron powder reduction method, the traditional method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75C07C209/36C07C211/52
CPCY02P20/584B01J23/75B01J35/0013B01J35/0033C07C209/365
Inventor 张其坤杨兵马晓晔石敬民郑国静徐华清匡芮王赤峰陈雪雪张程程
Owner SHANDONG NORMAL UNIV
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