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Process for preparing 2,4-diamino benzenesulfonic acid and sodium salt thereof

A technology of sodium diaminobenzenesulfonate and diaminobenzenesulfonic acid, applied in 2 fields

Inactive Publication Date: 2012-01-11
青岛奥盖克化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This method is simple in process and easy to increase the output. The disadvantage is that the amount of waste acid is large, and each ton of product produces about 7 tons of 50% to 55% waste acid

Method used

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  • Process for preparing 2,4-diamino benzenesulfonic acid and sodium salt thereof
  • Process for preparing 2,4-diamino benzenesulfonic acid and sodium salt thereof
  • Process for preparing 2,4-diamino benzenesulfonic acid and sodium salt thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: in 1000ml autoclave, add water 500ml, 2,4-sodium dinitrobenzene sulfonate 176.5g (content 85%), palladium carbon catalyst 5g, airtight autoclave, first vacuumize to-0.095MPa, Refill nitrogen gas at 1MPa. Repeat 3~5 times, and finally vacuumize the system, heat the reaction solution to 50°C, start to pass hydrogen, the pressure is 1~1.6MPa, control the reaction temperature at 50~100°C, until the reaction kettle The hydrogen pressure was no longer reduced, the temperature was lowered, and the autoclave was opened after venting, the palladium carbon was removed by filtration, decolorized with 10 g of activated carbon, concentrated to one-third of the original volume, and 115 g of sodium 2,4-diaminobenzenesulfonate crystallized after cooling. Content 82.6%, yield 81.42%.

Embodiment 2

[0019] Embodiment 2: in 1000ml autoclave, add water 500ml, 2,4-dinitrobenzene sodium sulfonate 176.5g (content 85%), palladium carbon catalyst 2g, airtight autoclave, first vacuumize to-0.095MPa, Refill nitrogen gas at 1MPa. Repeat 3~5 times, and finally vacuumize the system, heat the reaction solution to 50°C, start to pass hydrogen, the pressure is 1~1.6MPa, control the reaction temperature at 50~100°C, until the reaction kettle The hydrogen pressure is no longer reduced, the temperature is lowered, the autoclave is opened after venting, the palladium carbon is removed by filtration, the mother liquor filtered in Example 1 is poured, 10 g of activated carbon is added for decolorization, the solution is concentrated to one-third of the original volume, and crystallization occurs after cooling. 133g of sodium 2,4-diaminobenzenesulfonate. Content 82.3%, yield 93.82%.

Embodiment 3

[0020] Example 3: The feeding reaction and post-treatment are the same as in Example 2. After concentrating to one-third of the original volume, adjust the pH to about 2 with 30% hydrochloric acid, and cool down to crystallize 2,4-diaminobenzenesulfonic acid. After suction filtration Weighs 106g. Content 92.4%, yield 94.18%.

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PUM

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Abstract

The invention discloses a preparation technology of 2, 4-diaminobenzene sulphonic acid and sodium salts thereof, which adopts 2, 4-dinitrobenzene sulfonate sodium as raw material, uses palladium-charcoal or nickel aluminum alloy as a catalyst, and uses water or a lower alcohol as a solvent. 2, 4-diaminobenzene sulfonate sodium solution is produced through hydrogenation; the catalyst is removed through filtration; the colour removal is performed through active carbon; 2, 4-diaminobenzene sulfonate sodium is separated by crystallization after part of the solvent is removed, or hydrochloric acidis utilized to adjust the pH value to be 2 so as to separate out 2, 4-diaminobenzene sulphonic acid by crystallization after part of the solvent is removed. The preparation technology reduces the manufacture cost, no wastewater is discharged during the whole manufacturing process, the problem of waste acid discharge does not exist, and the environmental requirements are better satisfied.

Description

Technical field: [0001] The invention relates to a preparation process of 2,4-diaminobenzenesulfonic acid and its sodium salt, belonging to the field of compound preparation. technical background: [0002] Sodium 2,4-diaminobenzenesulfonate is widely used in the production of reactive dyes and acid dyes because it contains three active groups and is used as a bridging group in dye synthesis. [0003] There are two traditional production methods of 2,4-diaminobenzenesulfonate sodium: [0004] 1. 2,4-Dinitrobenzene sulfonate sodium iron powder reduction method: [0005] [0006] 1.8-2 tons of iron powder is used for each ton of products, but due to the continuous rise in the price of iron powder, poor production environment, and major environmental protection problems, it has been gradually eliminated. [0007] 2. M-phenylenediamine sulfuric acid sulfonation method: [0008] [0009] This method has a simple process and is easy to increase the output. The disadvantag...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/46C07C303/22
Inventor 王在军石艳
Owner 青岛奥盖克化工股份有限公司