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Application of 1,5-dinitronaphthalene hydrogenation catalyst

A dinitronaphthalene and catalyst technology, applied in the field 1, can solve the problems of high energy consumption, low yield, and three-waste pollution in the electrochemical reduction method, and achieve excellent hydrogenation catalytic performance, high yield, and low catalyst cost Effect

Inactive Publication Date: 2013-08-07
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Iron powder reduction method has mild conditions and simple process, but there are problems of low yield and serious pollution of three wastes
The electrochemical reduction method has the problem of high energy consumption

Method used

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  • Application of 1,5-dinitronaphthalene hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put 10 grams of carbon nanotubes into 100 milliliters of 20% hydrochloric acid for ultrasonic vibration for 1 hour, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 60% to reflux for 12 hours, filter, wash with deionized water, dry in vacuum and set aside. Then 2.9 grams of nickel nitrate was dissolved in 100 milliliters of deionized water, and the above-mentioned carbon nanotubes and 0.1 grams of cobalt acetate were added. Stir and soak for 8 hours and then filter. Dry under vacuum at 100°C for 12 hours. Calcined at 300° C. for 4 hours under the protection of nitrogen, reduced with hydrogen at 350° C. for 4 hours, and lowered the temperature under the protection of nitrogen to obtain the catalyst.

[0032] 45 grams of aniline are added to the reactor, then 9 grams of 1,5-dinitronaphthalene (purity in 98%) and 0.27 grams of the hydrogenation catalyst prepared above are added in the kettle, after replacing t...

Embodiment 2

[0034] Put 10 grams of carbon nanotubes into 100 milliliters of 30% hydrochloric acid for ultrasonic vibration for 1 hour, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 30% to reflux for 12 hours, filter, wash with deionized water, dry in vacuum and set aside. Then 3.7 grams of nickel nitrate was dissolved in 100 milliliters of deionized water, and the above-mentioned carbon nanotubes and 0.1 grams of manganese acetate were added. Stir and soak for 8 hours and then filter. Dry under vacuum at 100°C for 12 hours. Calcined at 450° C. for 4 hours under the protection of nitrogen, reduced by flowing hydrogen at 600° C. for 4.5 hours, and lowered the temperature under the protection of nitrogen to obtain a catalyst.

[0035] 50 grams of Virahol are added to the reactor, then 10 grams of 1,5-dinitronaphthalene (purity is 98%) and 0.3 grams of the hydrogenation catalyst prepared above are added to the kettle, and the ...

Embodiment 3

[0037] Put 10 grams of carbon nanotubes into 100 milliliters of 40% hydrochloric acid for ultrasonic vibration for 1 hour, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 60% to reflux for 12 hours, filter, wash with deionized water, dry in vacuum and set aside. Then 4.9 grams of nickel nitrate was dissolved in 100 milliliters of deionized water, and the above-mentioned carbon nanotubes and 0.1 grams of cobalt acetate were added. Stir and soak for 8 hours and then filter. Dry under vacuum at 100°C for 12 hours. Calcined at 300° C. for 4 hours under the protection of nitrogen, reduced with hydrogen at 350° C. for 5 hours, and lowered the temperature under the protection of nitrogen to obtain the catalyst.

[0038] 50 grams of methyl alcohol are added to the reactor, then 10 grams of 1,5-dinitronaphthalene (purity in 98%) and 0.3 gram of the hydrogenation catalyst prepared above are added in the kettle, after repla...

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Abstract

The invention relates to a preparation method of 1,5-dinitronaphthalene hydrogenation catalyst, and relates to a method for performing 1,5-dinitronaphthalene hydrogenation by using the catalyst. According to the invention, the hydrogenation catalyst with carbon nano tube-loaded group VIII metal and group IVB metal is composed of a carbon nano tube, at least one group VIII metal and at least one metal of iron, manganese and cobalt, wherein the group VIII metal accounts for 3-50% of the total weight of the catalyst, and the at least one metal of iron, manganese and cobalt accounts for 0.1-2% ofthe total weight of the catalyst. The catalyst provided by the invention can be applied to the preparation of 1,5-diaminonaphthalene by1,5-dinitronaphthalene hydrogenation; the catalyst and solvent involved in the invention can be reused, and the cost of the catalyst is low; and no waste residue, waste gas or waste liquid is discharged when the catalyst provided by the invention is applied to thepreparation of 1,5-diaminonaphthalene by1,5-dinitronaphthalene hydrogenation. Thus, the preparation method is a pollution-free clean production process.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, in particular to a preparation method of a 1,5-dinitronaphthalene hydrogenation catalyst, and to a method for preparing 1,5-dinitronaphthalene by hydrogenation of 1,5-dinitronaphthalene using the catalyst. The method of diaminonaphthalene. Background technique [0002] The reduction of nitro compounds can obtain amine compounds, ketoxime compounds and amide compounds with wide applications, and the reduction of 1,5-dinitronaphthalene can obtain 1,5-diaminonaphthalene. 1,5-Diaminonaphthalene is widely used in various fine chemical products such as pigments, dyes, medicines, pesticides, rubber additives, resins, photosensitive materials, etc., especially for the preparation of 1,5-naphthalene diisocyanate, and then the preparation of high-grade polyurethane elastomer. [0003] The preparation methods of 1,5-diaminonaphthalene include naphthalene halide ammonolysis method (US6538158), r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J23/42B01J23/745B01J23/889B01J23/44C07C211/58B01J23/34B01J23/75B01J35/10B01J23/89C07C209/36
Inventor 罗和安刘平乐刘丽娜倪敏游奎一艾秋红
Owner XIANGTAN UNIV