CN104646030A - Preparation method of catalyst for synthesis of 2,2,6,6-tetramethyl-4-piperylhydrazine - Google Patents

Abstract

The invention discloses a preparation method of a catalyst for synthesis of 2,2,6,6-tetramethyl-4-piperylhydrazine. The method includes the following steps: 1, adding sodium hydroxide and distilled water to a beaker equipped with a thermometer and a frame type glass blender, preparing a solution, reducing the temperature to 50 DEG C, adding a Ni-Al alloy powder, and leaching under 50 DEG C for 50min; and 2, removing an upper layer solution, washing the precipitate with distilled water to a neutral state, then washing with ethanol, washing with anhydrous ethanol, and finally, preserving the prepared skeleton nickel catalyst in a grinding bottle with anhydrous ethanol. The skeleton nickel catalyst prepared by the preparation method provided by the invention realizes high yield and high purity of the obtained product in the catalysis of hydroamination synthesis of 2,2,6,6-tetramethyl-4-piperylhydrazine.

Description

For the synthesis of the preparation method of the catalyst of 2,2,6,6-tetramethyl-4-piperidinamine

 

Technical field

The present invention relates to a kind of preparation method of catalyst, be specifically related to a kind of preparation method for the synthesis of the catalyst of 2,2,6,6-tetramethyl-4-piperidinamine.

 

Background technology

2,2,6,6-tetramethyl-4-piperidinamine is a kind of important intermediate, be used for synthesizing the hindered amine light stabilizer of a series of excellent performance, synthetic method conventional in the world mainly contains Study on Catalytic Amination of Alcohols method and electrochemical reducing etc., electrochemical reducing synthesis 2,2,6,6-tetramethyl-4-piperidinamine has process and is easy to control, easily realizes that serialization, byproduct of reaction are few, product is easy to advantages such as being separated, reaction condition is gentle, but energy consumption is high, equipment investment large, is difficult to realize suitability for industrialized production.

 

Summary of the invention

The object of the invention is to, provide a kind of preparation method for the synthesis of the catalyst of 2,2,6,6-tetramethyl-4-piperidinamine, gained skeletal nickel catalyst, catalytic hydrogenation amination synthesis 2,2,6,6-tetramethyl-4-piperidinamine, product yield is high, and products obtained therefrom purity is high.

The preparation method of the described catalyst for the synthesis of 2,2,6,6-tetramethyl-4-piperidinamine, it comprises the following steps:

One, in the beaker that thermometer and frame glassed agitator are housed, add NaOH and distilled water, be mixed with solution, be cooled to 50 DEG C, add Ni-Al alloyed powder, at 50 DEG C, soak 50min;

Two, shifting out upper solution, is neutral by distilled water washing precipitate to washing lotion, then with ethanol washing, then uses absolute ethanol washing, is finally kept at by obtained skeletal nickel catalyst and is filled with in the port grinding bottle of absolute ethyl alcohol.

The preparation method of the catalyst for the synthesis of 2,2,6,6-tetramethyl-4-piperidinamine provided by the invention, its beneficial effect is, gained skeletal nickel catalyst, catalytic hydrogenation amination synthesis 2,2,6,6-tetramethyl-4-piperidinamine, product yield is high, and products obtained therefrom purity is high.

 

Detailed description of the invention

Below in conjunction with an embodiment, the preparation method of the catalyst for the synthesis of 2,2,6,6-tetramethyl-4-piperidinamine provided by the invention is described in detail.

 

Embodiment

One, in the beaker that thermometer and frame glassed agitator are housed, add NaOH and distilled water, be mixed with solution, be cooled to 50 DEG C, add Ni-Al alloyed powder, at 50 DEG C, soak 50min;

Two, shifting out upper solution, is neutral by distilled water washing precipitate to washing lotion, then with ethanol washing, then uses absolute ethanol washing, is finally kept at by obtained skeletal nickel catalyst and is filled with in the port grinding bottle of absolute ethyl alcohol.

Claims (1)

1. one kind for the synthesis of the preparation method of the catalyst of 2,2,6,6-tetramethyl-4-piperidinamine, it is characterized in that: it comprises the following steps:

One, in the beaker that thermometer and frame glassed agitator are housed, add NaOH and distilled water, be mixed with solution, be cooled to 50 DEG C, add Ni-Al alloyed powder, at 50 DEG C, soak 50min;

Two, shifting out upper solution, is neutral by distilled water washing precipitate to washing lotion, then with ethanol washing, then uses absolute ethanol washing, is finally kept at by obtained skeletal nickel catalyst and is filled with in the port grinding bottle of absolute ethyl alcohol.