Preparation method for synthesizing naphthylamine by catalytic hydrogenation

A technology for catalytic hydrogenation and naphthylamine, which is applied in the preparation of organic compounds, preparation of amino compounds, chemical instruments and methods, etc., can solve the problems of less times of catalyst application, high catalyst cost, and low yield, and achieve more application times , simple preparation process and high reaction yield

Inactive Publication Date: 2012-01-04
HUNAN CHEM RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of noble metal-supported catalysts is rarely used in China due to the high cost of catalysts
However, the Raney nickel catalyst itself is easy to catch fire, the yield is not high, and the number of catalyst applications is small, which also has limitations.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] In a 4L beaker, dissolve 380g of sodium hydroxide in 1.5L of distilled water, stir, and cool to 10°C in an ice bath. Under stirring, add 300g of nickel (40%)-copper (10%)-Al (50%) alloy powder into the lye in small quantities in batches, and the speed of addition should be controlled so that the temperature of the solution does not exceed 25°C ( in an ice bath). After all the addition was completed (about 2 hours), the stirring was stopped, the beaker was taken off from the ice bath, and the reaction solution was allowed to rise to room temperature. When the generation of hydrogen gas is slow, it can be heated slowly on a boiling water bath (avoid heating up too fast, in case there are too many bubbles and the reaction solution overflows), until the generation of bubbles slows down again (about 8 to 12 hours, the volume of the solution at this time It should be kept basically constant by adding distilled water). Then stand still, allow the nickel-copper powder to sink...

Embodiment 2

[0012] In a 4L beaker, dissolve 380g of sodium hydroxide in 1.5L of distilled water, stir, and cool to 10°C in an ice bath. Under stirring, add 300g of nickel (45%)-copper (5%)-Al (50%) alloy powder into the lye in small batches, and the speed of addition should be controlled so that the temperature of the solution does not exceed 25°C ( in an ice bath). After all the addition was completed (about 2 hours), the stirring was stopped, the beaker was taken off from the ice bath, and the reaction solution was allowed to rise to room temperature. When the generation of hydrogen gas is slow, it can be heated slowly on a boiling water bath (avoid heating up too fast, in case there are too many bubbles and the reaction solution overflows), until the generation of bubbles slows down again (about 8 to 12 hours, the volume of the solution at this time It should be kept basically constant by adding distilled water). Then stand still, allow the nickel-copper powder to sink, and pour out ...

Embodiment 3

[0014] Add 76g of industrial nitronaphthalene in the 1000ml autoclave, add 300ml of ethanol, and finally add 3.8g of the self-made composite catalyst (containing 80% nickel and 20% copper in the catalyst) that adopts the gained Example 1 of the present invention; the system uses nitrogen and hydrogen After each replacement 3 times, the reaction temperature was controlled at 110°C, and the pressure was stirred at 3.0 MPa. During the reaction, hydrogen was added to 3.0 MPa after the pressure dropped. After 8 hours of reaction, the reaction conversion rate was 99.5%, and the yield was 99.0%.

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PUM

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Abstract

The invention discloses a preparation method for synthesizing naphthylamine by catalytic hydrogenation. The method comprises the following steps: firstly preparing a nickel-copper composite catalyst for synthesizing naphthylamine by catalytic hydrogenation, adding nitronaphthalene, ethanol and the prepared nickel-copper composite catalyst to react for 4-15 hours under the pressure of 3.0-5.0 MPa and the reaction temperature of 80-120 DEG C to obtain the naphthylamine, wherein the reaction conversion rate is not less than 99.0%, and the yield is not less than 99.0%. The invention has easily-obtained materials, high selectivity, high yield and simplicity in operation; the process is environmentally-friendly without generating the three wastes (waster water, waste gas and solid waste); and the catalyst can be recycled for a plurality of times, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method for synthesizing naphthylamine through catalytic hydrogenation. Background technique [0002] Naphthylamine, also known as 1-naphthylamine and α-naphthylamine, is a raw material for the production of important intermediates for dyes, anti-aging agents, and can also be used for the production of pesticides. The traditional production process of naphthalene amine is to use refined naphthalene as raw material, nitrate with mixed acid to obtain 1-nitronaphthalene, and then reduce it with alkali sulfide or iron powder to obtain methylnaphthylamine. Because the reduction of nitronaphthalene with alkali sulfide or iron powder not only has poor product quality (appearance, content) and high labor intensity, but also produces a large amount of difficult-to-treat industrial wastewater, which contains carcinogens and causes serious environmental pollution. Countries and regions have banned the production of naphthyla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/58C07C209/36B01J23/755
CPCY02P20/584
Inventor 陈明臧阳陵恽海顺王燕徐光辉
Owner HUNAN CHEM RES INST
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