Application of Chinese lacquer original nickel in the preparation of m-phenylene diamine with m-dinitrobenzene liquid phase hydrogenation
A technology of m-dinitrobenzene and m-phenylenediamine, applied in the field of catalyst and its preparation
Inactive Publication Date: 2012-08-29
NANKAI UNIV
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- Description
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- Application Information
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Problems solved by technology
The lacquer original nickel catalyst has the advantages of high activity, good selectivity, high product purity, easy separation, and safe use, but its application in the hydrogenation of m-dinitrobenzene to prepare m-phenylenediamine has not yet been patented.
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 1
[0023] At 45°C, 12.6g of zinc powder and 4ml of water are fully mixed under magnetic stirring, and 10ml of 4.2mol / l NiCl 2 Pour the solution into the suspension of zinc powder, stir quickly until the reaction stops, wash the precipitate with 200ml of deionized water, filter, put the precipitate in 180ml of 20% acetic acid solution and stir for 0.5h, then let it stand at room temperature for 0.5h , fully washed the obtained precipitate to neutrality, and then washed with absolute ethanol, and stored in pro-alcohol to obtain catalyst A.
Embodiment 2
[0025] The same as the preparation process of catalyst A, the addition of zinc powder was changed, and 13.7 g of zinc powder was added to obtain catalyst B.
Embodiment 3
[0027] Same as the preparation process of catalyst A, the addition amount of zinc powder was changed, and 15.1 g of zinc powder was added to obtain catalyst C.
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Abstract
The present invention discloses a method of using the urushibara nickel to catalyze the m-dinitrobenzene liquid phase hydrogenation to prepare the m-phenylenediamine, and the method belongs to the preparing technique of the m-phenylenediamine. The method includes the following steps: adding the nickel salt solution with a definite concentration to the suspension of the zinc dust at a definite temperature, developing the solution with the developing agent with a certain concentration when the reaction has reacted for a certain time, then washing with the deionized water and absolute ethyl alcohol for a plurality of times and the urushibara nickel catalyst. Adding the urushibara nickel catalyst and the m-phenylenediamine and absolute ethyl alcohol or the mixture of the absolute ethyl alcohol and water according to a certain mass ratio to the high-pressure reaction still, the temperature is 60 to 100 DEG C, and the pressure is 1 to 2.5 MPa, the feed stock conversion and product selectivity are all larger than 99% when the reaction has completed. The invention has the advantages of simple technique, simple reaction operation, short reaction time, high product yield and purity and lessenvironmental pollution.
Description
technical field [0001] The invention relates to a catalyst with high catalytic activity for preparing m-phenylenediamine by hydrogenation of m-dinitrobenzene and a preparation method thereof. Background technique [0002] M-phenylenediamine, also known as 1,3-diaminobenzene, is an isomer of aromatic amine compound phenylenediamine. m-Phenylenediamine is an important organic chemical raw material and intermediate, mainly used as a dye intermediate for the manufacture of basic orange, basic brown G, direct tanning G and other dyes, and can also be used for epoxy resin curing agent, cement coagulant, petroleum additive, rubber compounding agent, metal dissolver, and used in hair dye, mordant, color developer, etc. At present, the production of m-phenylenediamine in my country mainly adopts m-dinitrobenzene iron powder reduction method and catalytic hydrogenation method. Although the iron powder reduction method has a simple process and mature technology, it has high productio...
Claims
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IPC IPC(8): B01J23/80B01J23/83C07C211/51C07C209/36
Inventor 李伟刘皓张明慧陶克毅
Owner NANKAI UNIV