Catalytic synthesis method of diphenylamine

Abstract

The invention relates to a catalytic synthesis method of diphenylamine.A synthesis reaction comprises the specific steps of adding a corresponding amount of aniline and phenol into a high pressure reaction kettle according to the mole ratio of 1: 1.25, and after nitrogen displacement is completed, conducting stirring for 1.5 hours at the speed of 40-60 R / min, wherein the temperature of materials is controlled at 60 DEG C or below in the stirring process; adding a corresponding amount of a catalyst Pd / C and accelerant cyclohexylamine into the high pressure reaction kettle in proportion, wherein the catalyst Pd / C accounts for 2% of the total mass of aniline and phenol, and the accelerant cyclohexylamine accounts for 35% of the total mass of aniline and phenol; then conducting a reaction while stirring is conducted, and slowly raising the temperature in the stirring process to the extent that the reaction temperature is 245 DEG C, wherein the reaction pressure is 1.3 mpa, and reaction time is 6 hours; finally cooling the materials to 60 DEG C, conducting pressure-reduced suction filtration, and conducting washing with ethyl alcohol, so that diphenylamine is obtained.The catalytic synthesis method of diphenylamine is simple in process and convenient in operation, and the product obtained through the synthesis reaction is high in yield and good in purity.

Description

technical field

[0001] The invention relates to a catalytic synthesis method of diphenylamine, which belongs to the field of catalytic synthesis of organic matter. Background technique

[0002] Diphenylamine is a white to light gray crystal, volatile, has an aniline-like odor, and is poisonous. Can be used to identify DNA and nitrate. It is used as a stabilizer for dyes and explosives. At present, diphenylamine on the market is generally prepared by a synthetic process. The existing synthesis and preparation process of diphenylamine is complex. In order to better adapt to the industrial production needs of modern chemical industry, we urgently need to design a catalytic synthesis process of diphenylamine with simple process, convenient operation, high product yield and good purity. Contents of the invention

[0003] Aiming at the shortcomings of the above-mentioned prior art, the present invention provides a catalytic synthesis method of diphenylamine, which can effecti...

Examples

Embodiment 1

[0014] (1) Put 100g of aniline and 125g of phenol into the autoclave, and after nitrogen replacement, stir for 1.5h at a stirring speed of 50R / min, and control the material temperature at 55°C during the stirring process;

[0015] (2) Add 4.5g of catalyst Pd / C and 78.75g of accelerator cyclohexylamine to the autoclave in proportion;

[0016] (3) Then carry out the stirring reaction, and slowly heat up to the reaction temperature of 245°C during the stirring process, the reaction pressure of 1.3mpa, and the reaction time of 6h;

[0017] (4) Finally, cool to 60°C, carry out suction filtration under reduced pressure, and wash with ethanol. The selectivity of the reaction is 94%, the conversion rate is 92.8%, and the purity of the obtained product is 99.2%.

Embodiment 2

[0019] (1) Put 200g of aniline and 250g of phenol into the autoclave, and after nitrogen replacement, stir for 1.5h at a stirring speed of 60R / min, and control the material temperature at 53°C during the stirring process;

[0020] (2) Add catalyst Pd / C9g and accelerator cyclohexylamine 157.5g to the autoclave in proportion;

[0021] (3) Then carry out the stirring reaction, and slowly heat up to the reaction temperature of 245°C during the stirring process, the reaction pressure of 1.3mpa, and the reaction time of 6h;

[0022] (4) Finally, cool to 60°C, carry out suction filtration under reduced pressure, and wash with ethanol. The selectivity of the reaction is 93%, the conversion rate is 91.8%, and the purity of the obtained product is 98.5%.

technical field

[0001] The invention relates to a catalytic synthesis method of diphenylamine, which belongs to the field of catalytic synthesis of organic matter. Background technique

[0002] Diphenylamine is a white to light gray crystal, volatile, has an aniline-like odor, and is poisonous. Can be used to identify DNA and nitrate. It is used as a stabilizer for dyes and explosives. At present, diphenylamine on the market is generally prepared by a synthetic process. The existing synthesis and preparation process of diphenylamine is complex. In order to better adapt to the industrial production needs of modern chemical industry, we urgently need to design a catalytic synthesis process of diphenylamine with simple process, convenient operation, high product yield and good purity. Contents of the invention

[0003] Aiming at the shortcomings of the above-mentioned prior art, the present invention provides a catalytic synthesis method of diphenylamine, which can effecti...

Examples

Embodiment 1

[0014] (1) Put 100g of aniline and 125g of phenol into the autoclave, and after nitrogen replacement, stir for 1.5h at a stirring speed of 50R / min, and control the material temperature at 55°C during the stirring process;

[0015] (2) Add 4.5g of catalyst Pd / C and 78.75g of accelerator cyclohexylamine to the autoclave in proportion;

[0016] (3) Then carry out the stirring reaction, and slowly heat up to the reaction temperature of 245°C during the stirring process, the reaction pressure of 1.3mpa, and the reaction time of 6h;

[0017] (4) Finally, cool to 60°C, carry out suction filtration under reduced pressure, and wash with ethanol. The selectivity of the reaction is 94%, the conversion rate is 92.8%, and the purity of the obtained product is 99.2%.

Embodiment 2

[0019] (1) Put 200g of aniline and 250g of phenol into the autoclave, and after nitrogen replacement, stir for 1.5h at a stirring speed of 60R / min, and control the material temperature at 53°C during the stirring process;

[0020] (2) Add catalyst Pd / C9g and accelerator cyclohexylamine 157.5g to the autoclave in proportion;

[0021] (3) Then carry out the stirring reaction, and slowly heat up to the reaction temperature of 245°C during the stirring process, the reaction pressure of 1.3mpa, and the reaction time of 6h;

[0022] (4) Finally, cool to 60°C, carry out suction filtration under reduced pressure, and wash with ethanol. The selectivity of the reaction is 93%, the conversion rate is 91.8%, and the purity of the obtained product is 98.5%.