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Preparation method and application of porous microspheres and reduction method of nitro compound

A technology of nitro compounds and porous microspheres, applied in the field of fine chemistry, can solve the problems of difficulty in applying fixed bed reactors, insufficient strength of alumina microspheres, large amount of solvent volatilization and not environmental protection, etc., and achieves low cost and surface holes. Multiple, high-strength effects

Pending Publication Date: 2021-11-19
珠海派锐尔新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is a commonly used method for the preparation of alumina microspheres at this stage, and the molding efficiency is low due to multiple process steps, and the large amount of solvent volatilization is not environmentally friendly.
The prepared alumina microspheres are not strong enough to be used in fixed bed reactors

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1A

[0051] Preparation of porous alumina microspheres:

[0052] Add 30 grams of polyethylene, 60 grams of alumina micropowder, add 3 grams of polyethylene glycol, mix well and grind them, heat press them into microspheres in a mold at 180°C, and then sinter the microspheres at 500°C to form alumina porous microspheres. The prepared porous microspheres were immersed in 0.2 mol / L nickel nitrate solution for 4 hours, then dried, then reduced with formaldehyde aqueous solution, and dried to obtain an alumina-supported Ni catalyst.

[0053] Fixed bed catalytic hydrogenation reduction process:

[0054] Add the supported Ni catalyst prepared above in the fixed bed reactor, the solvent is DMF, the mass ratio of DMF and 4,4-dinitrodiphenyl ether is 5:1, the hydrogen pressure is 3MPa, and the reaction temperature is 120°C. The liquid space velocity is 0.03L / h. After the reaction is completed, the pressure is reduced to separate the hydrogen. The diaminodiphenyl ether and the DMF solvent a...

Embodiment 1B

[0056] Use activity after 300 hours of circulation:

[0057] Continue to react in the above-mentioned fixed bed reactor for 300 hours, the solvent is DMF, the mass ratio of DMF and 4,4-dinitrodiphenyl ether is 5:1, the hydrogen pressure is 3MPa, the reaction temperature is 120°C, and the reaction liquid is empty. The speed is 0.2L / h. After the reaction is completed, the pressure is reduced first, and the hydrogen is separated. The diaminodiphenyl ether and the DMF solvent are separated by a continuous rectification process, and the DMF and high-purity diaminodiphenyl ether are separated, and the diaminodiphenyl ether is analyzed by gas chromatography. The purity of phenyl ether is 99.9%, and the conversion rate of 4,4-dinitrodiphenyl ether is 99.5%.

[0058] Summary: The alumina porous microsphere Ni catalyst obtained by the preparation method of the porous microsphere of the present invention has high strength, can be used for long-term and repeated catalytic use, and fully m...

Embodiment 2A

[0060] Add 1 gram of aliphatic amine solidifying agent in epoxy resin 50 grams / titanium dioxide micropowder 50 grams (weight ratio is 1:1), mix uniformly, solidify in mold, form the microsphere of epoxy resin / titanium dioxide, microsphere is in It is sintered and solidified at a high temperature of 600°C to obtain porous microspheres of titanium dioxide. The above-mentioned microspheres were immersed in a solution of 1 mol / L chloroplatinic acid for 2 hours, and reduced with hydrazine hydrate to obtain a platinum-loaded titanium dioxide catalyst with a platinum content of 2%.

[0061] Add the supported platinum catalyst prepared above into the fixed bed reactor, the solvent is DMF, the mass ratio of DMF and 4,4-dinitrodiphenyl ether is 2:1, the hydrogen pressure is 5MPa, and the reaction temperature is 100°C. The liquid space velocity is 0.1L / h. After the reaction is completed, the pressure is reduced first to separate the hydrogen. The diaminodiphenyl ether and DMF solvent are...

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PUM

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Abstract

The invention discloses a preparation method of porous microspheres for a supported catalyst. The porous microspheres are obtained by sintering after hot press molding of an inorganic material and resin. The microspheres are inorganic nano porous microspheres, are firm and have many holes, and can adsorb a large amount of catalyst. The invention also discloses an application of the porous microspheres loaded with the catalyst to catalytic hydrogenation reaction of a fixed bed reactor, and an application of the porous microspheres loaded with the catalyst to nitro reduction reaction of nitro-containing compounds, especially to reduction of dinitro-containing compounds and multi-nitro-containing compounds, the obtained amino compounds are high in purity and high in conversion rate, the durability of the catalyst is strong, and the catalyst can be recycled for multiple times for a long time.

Description

technical field [0001] The invention relates to the technical field of fine chemistry, in particular to a preparation method and application of porous microspheres and a reduction method of nitro compounds. Background technique [0002] Common amino compounds such as 4,4 diaminodiphenyl ether (ODA) are important organic chemical products, mainly used in the synthesis of high-performance polyimides. Early industrial production usually used iron powder catalytic reduction, but the yield was low, the cost was high, and a large amount of iron sludge and wastewater that were difficult to handle would be produced, causing serious environmental pollution. At present, catalytic hydrogenation reduction is mostly used in industrial production, but most of them still use reactor-type intermittent catalytic hydrogenation reduction. Such as patent 201110330139.9. The batch process operation is complex and the production cost is high. [0003] The fixed-bed hydrogenation process is sim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/42B01J23/44B01J32/00B01J35/08B01J35/10C07C217/90C07C213/02C07C209/36C07C211/51
CPCB01J23/755B01J23/42B01J23/44C07C213/02C07C209/36B01J35/60B01J35/51C07C217/90C07C211/51Y02P20/584
Inventor 饶先花王贤文黄华鹏胡三友杨思思
Owner 珠海派锐尔新材料有限公司