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2,4-diamino benzenesulfonic acid and its salt synthesizing method

A technology of diaminobenzene sulfonate and diaminobenzene sulfonic acid, applied in 2 fields, can solve problems such as environmental pollution and rising production costs

Inactive Publication Date: 2007-03-28
SHANGHAI WORLD PROSPECT INT TRADE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of preparation 2, the method for 4-diaminobenzenesulfonic acid, this method can overcome in the prior art because needs to use a large amount of sulfuric acid (or oleum) and cause environmental pollution and production cost rise question
[0007] The inventor of the present invention finds after in-depth research, by carrying out solid phase reaction with specific amount of sulfuric acid or oleum and m-phenylenediamine in specific temperature to prepare 2,4-diaminobenzenesulfonic acid, can effectively solve In the prior art, the problems of environmental pollution and production cost increase caused by the use of a large amount of sulfuric acid can obtain higher reaction yield and product quality at the same time

Method used

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  • 2,4-diamino benzenesulfonic acid and its salt synthesizing method

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preparation example Construction

[0031] In the preparation method of the present invention, the sulfonation reaction is carried out in the temperature range of 160-250°C, preferably in the temperature range of 165-220°C, more preferably in the temperature range of 170-220°C, especially preferably at 175 It is carried out in the temperature range of ~220°C.

[0032] Amount of reactant

[0033] "Sulfuric acid" used in the present invention refers to sulfuric acid of any concentration or oleum of any concentration diluted to sulfuric acid of any concentration through water. For example, the sulfuric acid used in the present invention can be sulfuric acid with a concentration of 0.1-100% or any concentration of oleum diluted with water to 0.1-100% sulfuric acid. Sulfuric acid is more preferably sulfuric acid with a content of 60-100%, more preferably sulfuric acid with a content of 85-100%, particularly preferably sulfuric acid with a content of 90-100%.

[0034] The fuming sulfuric acid used in the preparation...

Embodiment 1

[0045] In reactor, add 100 milliliters of 98% sulfuric acid (184 grams) (corresponding to 100 percent sulfuric acid of 180 grams or 1.84 moles of 100 percent sulfuric acid) and 100 grams of 100% m-phenylenediamine (corresponding to 0.926 moles), after mixing, Raise the temperature to 181°C, react at 181-185°C for 4 hours, cool, add 400 ml of water, and purify by decolorization to obtain 168.8 g of 2,4-diaminobenzenesulfonic acid. The appearance of the obtained product is white crystal, the chromatographic content is 99% (as determined by HPLC), the chemical content is 98% (as determined by diazo titration), and the product yield is 95% (calculated as m-phenylenediamine).

Embodiment 2

[0047] Add 260 grams of 100% sulfuric acid and 100 grams of 100% m-phenylenediamine into the reactor, mix evenly, heat up to 210 ° C, react at 210-215 ° C for 4 hours, cool, add 400 ml of water, and purify through decolorization to obtain 159.9 grams of 2,4-diaminobenzenesulfonic acid. The appearance of the obtained product is white crystal, the chromatographic content is 99% (as determined by HPLC), the chemical content is 98% (as determined by diazo titration), and the product yield is 90% (calculated as m-phenylenediamine).

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Abstract

The invention discloses a 2, 4-diamino benzenesulfonic acid preparing method, comprising the step of: making m-phenylene diamine and vitriol or oleum react at 160-250 deg.C to make it. And the invention also discloses a 2, 4-diamino besilate preparing method, comprising the steps of: as above making 2, 4-diamino benzenesulfonic acid; then making salification reaction to make the needed 2, 4-diamino besilate. And the invention can effectively solve the problems of environmental pollution and increase of production costs, and besides, obtain higher reaction yield and quality of product.

Description

technical field [0001] The invention relates to a synthesis method of 2,4-diaminobenzenesulfonic acid and its salts. Background technique [0002] 2,4-diaminobenzenesulfonic acid, also known as m-phenylenediamine-4-sulfonic acid, has the following structural formula: [0003] [0004] 2,4-diaminobenzenesulfonic acid and its salts (especially the sodium salt) are mainly used as important intermediates for the synthesis of dyes, and their derivatives are widely used in our production and life. [0005] In the prior art, using m-phenylenediamine as a raw material to prepare 2, the method for 4-diaminobenzenesulfonic acid (such as Japanese Patent Publication No. 57-48961, Japanese Patent Publication No. 4-13657) is a liquid phase method, namely Use a large amount of sulfuric acid (or oleum) as a solvent, and then use oleum or SO 3 The gas is used as a sulfonating agent to sulfonate the m-phenylenediamine to obtain the product 2,4-diaminobenzenesulfonic acid. The disadvanta...

Claims

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Application Information

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IPC IPC(8): C07C309/46C07C303/06
Inventor 唐会林许晓峻
Owner SHANGHAI WORLD PROSPECT INT TRADE
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