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Method for preparing m-phenylenediamine through hydrogenating m-dinitrobenzene

A technology of m-dinitrobenzene and m-phenylenediamine is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of difficult catalyst separation and poor reaction selectivity.

Active Publication Date: 2018-01-05
NANJING UNIV
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Problems solved by technology

[0004] At present, the reaction of catalytic hydrogenation to synthesize m-phenylenediamine is mostly carried out in mud flow reactor or trickle bed reactor, but they have the problems of difficult catalyst separation and poor reaction selectivity.

Method used

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Experimental program
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Embodiment 1

[0014] Under vigorous stirring, 100ml was dissolved with 14.9g Ni(NO 3 ) 2 ·6H 2 O, 11.1g Mg(NO 3 ) 2 ·6H 2 O and 1.8gAl(NO 3 ) 3 9H 2 The aqueous solution of O and 100ml contain 11.9g Na 2 CO 3 The aqueous solution is added dropwise in the beaker that fills 100ml distilled water simultaneously, generates green precipitation, filters, washes and dries at 393K, obtains the supported nickel catalyst precursor, and the mass percent composition of nickel wherein is about 60%.

[0015] The above-mentioned supported nickel catalyst precursor was pressed into tablets, crushed and sieved. Take 1.4g of 20-40 mesh particles and dilute them to 3ml with 20-40 mesh quartz sand, fill them in a fixed-bed reactor, treat them in 40ml / min flowing hydrogen at 723K for 2h, then lower the temperature to 443K, and use 2% triphenyl Phosphine (PPh 3 ) in n-heptane solution for phosphating for 24 hours, then heated up to 573K and continued to feed hydrogen for 3 hours to obtain supported Ni...

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Abstract

The invention provides a method for preparing m-phenylenediamine through carrying out catalytic hydrogenation on m-dinitrobenzene in a fixed bed reactor with a supported Ni2P as a catalyst. The methodhas the advantages of simple process, mild reactions and high yield, and the conversion rate of the m-dinitrobenzene and the selectivity of the m-phenylenediamine respectively reach 100%.

Description

technical field [0001] The invention relates to a method for preparing m-phenylenediamine by hydrogenating m-dinitrobenzene, which belongs to the technical field of catalytic hydrogenation. technical background [0002] M-phenylenediamine is an important chemical raw material, mainly used as dye intermediates and pharmaceutical intermediates, and also used as mordant, hair dye, color developer, rubber compounding agent, epoxy resin curing agent, petroleum additive, cement coagulation accelerator Synthesis of materials such as solvents and metal dissolvers. M-phenylenediamine can also be synthesized with phthaloyl chloride to produce high-temperature-resistant aromatic polyamide resin and flame-retardant fiber, which are used in special fields such as national defense and aerospace. [0003] The industrial production of m-phenylenediamine mainly adopts m-dinitrobenzene iron powder reduction method and catalytic hydrogenation method. Although the iron powder reduction method...

Claims

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Application Information

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IPC IPC(8): C07C209/36C07C211/51B01J27/185
Inventor 沈俭一陈慧王俊恩傅玉川
Owner NANJING UNIV
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