Preparation method of o-aminobenzenesulfonic acid
A technology of anthranilic acid and nitrobenzenesulfonic acid, which is applied to the preparation of sulfonic acid, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of low production efficiency, low safety, and high energy consumption
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Embodiment 1
[0096] A kind of preparation method of o-aminobenzenesulfonic acid, take o-nitrobenzenesulfonic acid as raw material, adopt Pd / Al 2 o 3 Catalyst, continuous catalytic hydrogenation reaction is carried out in the reactor, after the catalyst is separated and recovered, the reducing solution is desolvated and purified to obtain the target product anthranilic acid.
[0097] Specific steps include:
[0098] (1) Put 5000kg of 50% methanol aqueous solution and 1250kg of o-nitrobenzenesulfonic acid into the chemical material tank, follow-up feeding is carried out according to this ratio, stir evenly, pump into the first-level hydrogenation reactor, and add Pd / Al 2 o 3 Catalyst 125kg, the particle size of the catalyst is 10nm, pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump it into the first-stage hydrogenation tank at a flow rate of 6000L / h The raw ma...
Embodiment 2
[0102] (1) Put 5000kg of 50% methanol aqueous solution and 1250kg of o-nitrobenzenesulfonic acid into the chemical material tank, follow up the feeding according to the ratio, stir evenly, pump into the primary hydrogenation reactor, and add Pd / Al 2 o 3 125kg of catalyst, the particle size of the catalyst is 500μm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 80-90°C, and pump it into the first-stage hydrogenation tank at a flow rate of 5000L / h The raw material solution of o-nitrobenzenesulfonic acid is passed into H 2 , control the hydrogen pressure in the system to 3.0MPa, and add Pd / Al to the primary hydrogenation reactor every 3h 2 o 3 Catalyst 2.5 kg, after the material in the primary hydrogenation tank gradually increases, it flows into the secondary hydrogenation tank through the overflow port, the material stays in the hydrogenation tank for about 2-3h...
Embodiment 3
[0106] (1) Put 12500kg of 50% methanol aqueous solution and 1250kg of o-nitrobenzenesulfonic acid into the chemical material tank, and the subsequent feeding is stirred evenly according to the ratio. Al 2 o 3 Catalyst 125kg, the particle size of the catalyst is 10nm; pass through the nitrogen replacement system three times, then pass through the hydrogen replacement system three times, start stirring, raise the temperature to 90-100°C, and pump it into the primary hydrogenation tank at a flow rate of 6000L / h The raw material solution of o-nitrobenzenesulfonic acid is passed into H 2 , control the hydrogen pressure in the system to 3.0MPa, and add Pd / Al to the primary hydrogenation reactor every 3h 2 o 3 Catalyst 2.5kg, after the material in the primary hydrogenation tank gradually increases, it flows into the secondary hydrogenation tank through the overflow port. acid residue ≤ 0.2%), overflow to the settling tank through the secondary hydrogenation tank.
[0107] (2) Af...
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