New process of amino G acid ammonification production

Abstract

The invention relates to a new process of amino G acid ammonification production, belonging to the field of organic chemistry. In the new process provided by the invention, the finished product of amino G acid is prepared by taking ammonium bicarbonate as an aminolysis agent by the steps such as dosing, low-temperature ammonification and high-temperature high-pressure ammonification; the yield of amino G acid is increased to over 90% from 82% before, and the product purity is improved by 2%. Meanwhile, by adopting the process, the pressure maintained by an ammonification reaction kettle is reduced from 1.2MPa to 0.5MPa, and the process has the characteristics of high safety coefficient and stability.

Description

technical field

[0001] The invention relates to a new ammonification production process of amino G acid, which belongs to the field of organic chemistry. Background technique

[0002] Amino G acid (2-naphthylamine-6,8-disulfonic acid) is an important dye intermediate, industrially using amino G acid can synthesize a variety of dyes, such as CI direct orange 74, CI media yellow 80, CI acid red 47 etc. It can also be used as raw material to synthesize R acid through alkali fusion reaction, or synthesize 2-naphthylamine-3,6,8-trisulfonic acid (K acid) through sulfonation reaction, and further synthesize 2R acid through alkali fusion reaction. At present, the ammoniation of amino G acid is usually synthesized by the pressurized ammoniation reaction of G salt. The ammonia solution agent uses ammonia water, and ammonium bisulfite is used as a catalyst. The pressure of the ammoniation reaction is as high as 1.2MPa, which requires high requirements on the reactor and safety factor....

Examples

Embodiment 1

[0021] In a 5000L stainless steel ammoniation reaction kettle, add 1000L of water, 350 kg of ammonium bicarbonate, and 1600 kg of ammonium 6,8-naphthalene disulfonate (G salt), start stirring and open the jacket to freeze the water in the pot The internal temperature was lowered to 25° C., and the stirring was maintained for 15 minutes, and the stirring speed was controlled at 50 rpm. Open the jacket steam valve, slowly heat up to 60°C, at this time, the pressure in the reactor is 0.3Mpa, maintain the temperature and pressure for 2 hours, and control the stirring speed at 30 rpm. Within 60 minutes, continue to open the jacket steam valve to raise the temperature to 150° C., the pressure in the kettle is 0.5 Mpa, and maintain the temperature and pressure to react for 10 hours. After reacting for 10 hours, take a sample to analyze the ammonia content. If the content is more than 90%, it is qualified; if the ammonia content is less than 90%, it is unqualified. Continue to react u...

Embodiment 2

[0023] In a 5000L stainless steel ammoniation reaction kettle, add 1500L of water, 500 kg of ammonium bicarbonate, and 2000 kg of ammonium 6,8-naphthalene disulfonate (G salt), start stirring and open the jacket to freeze the water in the pot The internal temperature was lowered to below 25° C., and the stirring was maintained for 15 minutes, and the stirring speed was controlled at 60 rpm. Open the jacket steam valve, slowly heat up to 60°C, at this time, the pressure in the reactor is 0.3Mpa, maintain the temperature and pressure for 2 hours, and control the stirring speed at 30 rpm. Within 60 minutes, continue to open the jacket steam valve to raise the temperature to 150° C., the pressure in the kettle is 0.5 Mpa, and maintain the temperature and pressure to react for 10 hours. After reacting for 10 hours, take a sample to analyze the ammonia content. If the content is more than 90%, it is qualified; if the ammonia content is less than 90%, it is unqualified. Continue to r...

Embodiment 3

[0025] In the 5000L stainless steel ammoniation reaction kettle, add 800L of water, add 320 kg of ammonium bicarbonate, add 1300 kg of ammonium 6,8-naphthalene disulfonate (G salt), start stirring and open the jacket to freeze the water to cover the pot The internal temperature was lowered to below 25° C., and the stirring was maintained for 15 minutes, and the stirring speed was controlled at 60 rpm. Open the steam valve of the jacket, slowly heat up to 60°C, at this time, the pressure in the reactor is 0.3Mpa, maintain the temperature and pressure for 2 hours, and control the stirring speed at 30 rpm. Within 60 minutes, continue to open the jacket steam valve to raise the temperature to 150° C., the pressure in the kettle is 0.5 Mpa, and maintain the temperature and pressure to react for 10 hours. After reacting for 10 hours, take a sample to analyze the ammonia content. If the content is more than 90%, it is qualified; if the ammonia content is less than 90%, it is unqualif...

technical field

[0001] The invention relates to a new ammonification production process of amino G acid, which belongs to the field of organic chemistry. Background technique

[0002] Amino G acid (2-naphthylamine-6,8-disulfonic acid) is an important dye intermediate, industrially using amino G acid can synthesize a variety of dyes, such as CI direct orange 74, CI media yellow 80, CI acid red 47 etc. It can also be used as raw material to synthesize R acid through alkali fusion reaction, or synthesize 2-naphthylamine-3,6,8-trisulfonic acid (K acid) through sulfonation reaction, and further synthesize 2R acid through alkali fusion reaction. At present, the ammoniation of amino G acid is usually synthesized by the pressurized ammoniation reaction of G salt. The ammonia solution agent uses ammonia water, and ammonium bisulfite is used as a catalyst. The pressure of the ammoniation reaction is as high as 1.2MPa, which requires high requirements on the reactor and safety factor....

Examples

Embodiment 1

[0021] In a 5000L stainless steel ammoniation reaction kettle, add 1000L of water, 350 kg of ammonium bicarbonate, and 1600 kg of ammonium 6,8-naphthalene disulfonate (G salt), start stirring and open the jacket to freeze the water in the pot The internal temperature was lowered to 25° C., and the stirring was maintained for 15 minutes, and the stirring speed was controlled at 50 rpm. Open the jacket steam valve, slowly heat up to 60°C, at this time, the pressure in the reactor is 0.3Mpa, maintain the temperature and pressure for 2 hours, and control the stirring speed at 30 rpm. Within 60 minutes, continue to open the jacket steam valve to raise the temperature to 150° C., the pressure in the kettle is 0.5 Mpa, and maintain the temperature and pressure to react for 10 hours. After reacting for 10 hours, take a sample to analyze the ammonia content. If the content is more than 90%, it is qualified; if the ammonia content is less than 90%, it is unqualified. Continue to react u...

Embodiment 2

[0023] In a 5000L stainless steel ammoniation reaction kettle, add 1500L of water, 500 kg of ammonium bicarbonate, and 2000 kg of ammonium 6,8-naphthalene disulfonate (G salt), start stirring and open the jacket to freeze the water in the pot The internal temperature was lowered to below 25° C., and the stirring was maintained for 15 minutes, and the stirring speed was controlled at 60 rpm. Open the jacket steam valve, slowly heat up to 60°C, at this time, the pressure in the reactor is 0.3Mpa, maintain the temperature and pressure for 2 hours, and control the stirring speed at 30 rpm. Within 60 minutes, continue to open the jacket steam valve to raise the temperature to 150° C., the pressure in the kettle is 0.5 Mpa, and maintain the temperature and pressure to react for 10 hours. After reacting for 10 hours, take a sample to analyze the ammonia content. If the content is more than 90%, it is qualified; if the ammonia content is less than 90%, it is unqualified. Continue to r...

Embodiment 3

[0025] In the 5000L stainless steel ammoniation reaction kettle, add 800L of water, add 320 kg of ammonium bicarbonate, add 1300 kg of ammonium 6,8-naphthalene disulfonate (G salt), start stirring and open the jacket to freeze the water to cover the pot The internal temperature was lowered to below 25° C., and the stirring was maintained for 15 minutes, and the stirring speed was controlled at 60 rpm. Open the steam valve of the jacket, slowly heat up to 60°C, at this time, the pressure in the reactor is 0.3Mpa, maintain the temperature and pressure for 2 hours, and control the stirring speed at 30 rpm. Within 60 minutes, continue to open the jacket steam valve to raise the temperature to 150° C., the pressure in the kettle is 0.5 Mpa, and maintain the temperature and pressure to react for 10 hours. After reacting for 10 hours, take a sample to analyze the ammonia content. If the content is more than 90%, it is qualified; if the ammonia content is less than 90%, it is unqualif...

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