Method for preparing salt-free 2-amino-1,5-naphthalenedisulfonic acid

A technology for salt sulfonating Tuburic acid and Tuburic acid, applied in chemical instruments and methods, preparation of sulfonic acid, preparation of organic compounds, etc., can solve the problems of general product quality, immature process, environmental pollution, etc., and achieve economical Significant benefits and social benefits, low labor intensity, and the effect of reducing pollution

Inactive Publication Date: 2013-11-13
山西翔宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most domestic manufacturers produce salt-sulfonated turezic acid, but there are few manufacturers producing salt-free sulfonated turezic acid, and the technology is not mature. The environment causes a lot of pollution

Method used

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  • Method for preparing salt-free 2-amino-1,5-naphthalenedisulfonic acid
  • Method for preparing salt-free 2-amino-1,5-naphthalenedisulfonic acid
  • Method for preparing salt-free 2-amino-1,5-naphthalenedisulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 5

[0070] Embodiment 5-acid out process:

[0071] Add 500 grams of refined acid-containing filtrate to a five-necked flask equipped with a sickle stirrer, 2 feeding ports, a condenser and a thermal resistance. Feed port is sealed with cork, start stirring, add 100 grams of demineralized water, after stirring for 10 minutes, sampling analysis, the acidity value of containing acid filtrate is 500g / L, then, the inner coil pipe of flask is cooled by chilled water, and temperature is controlled at 25 At about ℃, slowly add 200 grams of refined sulfonation solution. After the addition, continue to stir and react for 3 hours to form an acid precipitation feed solution. Stop stirring and the acid precipitation ends.

[0072] The so-called acid precipitation feed liquid refers to the mixed feed liquid formed by salt-free sulfonated turezied acid crystal particles, water, sulfuric acid and trace amount of turezied acid.

[0073] The entire reaction device was installed in a fume hood to p...

Embodiment 6

[0076] Embodiment 6-acid out process:

[0077] Add 500 grams of refined acid-containing filtrate to a five-necked flask equipped with a sickle stirrer, 2 feeding ports, a condenser and a thermal resistance. The feeding port is sealed with a soft plug, and the stirring is started, and 400 grams of soft water are added, and after stirring for 10 minutes, sampling analysis shows that the acidity value of the acid-containing filtrate is 450g / L. At about ℃, slowly add 300 grams of refined sulfonation solution. After the addition, continue to stir and react for 2.5 hours to form an acid precipitation feed solution. Stop stirring and the acid precipitation is over.

[0078] The so-called acid precipitation feed liquid refers to the mixed feed liquid formed by salt-free sulfonated turezied acid crystal particles, water, sulfuric acid and trace amount of turezied acid.

[0079] The entire reaction device was installed in a fume hood to prevent trace SO 3 The gas escapes and hurts peo...

Embodiment 7

[0082] Embodiment 7-acid out process:

[0083] Add 600 grams of refined acid-containing filtrate to a five-necked flask equipped with a sickle stirrer, 2 feeding ports, a condenser and a thermal resistance. The feeding port is sealed with a soft plug, and stirring is started, and 200 grams of reclaimed acid solution is added. After stirring for 10 minutes, sampling analysis shows that the acidity value of the acid-containing filtrate is 550g / L. At about 30°C, slowly add 300 grams of refined sulfonation solution. After the addition, continue to stir and react for 2 hours to form an acid precipitation feed solution. Stop stirring and the acid precipitation ends.

[0084] The so-called acid precipitation feed liquid refers to the mixed feed liquid formed by salt-free sulfonated turezied acid crystal particles, water, sulfuric acid and trace amount of turezied acid.

[0085] The entire reaction device was installed in a fume hood to prevent trace SO 3 The gas escapes and hurts p...

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Abstract

The invention discloses a method for preparing salt-free 2-amino-1,5-naphthalenedisulfonic acid, which comprises the following steps: (1) performing a sulfonation reaction; (2) refining sulfonation solution; (3) performing acid eduction; (4) decreasing and maintaining temperature; (5) centrifuging; (6) refining acid filtrate; and (7) recovering sulphuric acid tail gas and SO3 gas. Based on the technical scheme of the invention, the method for preparing salt-free 2-amino-1,5-naphthalenedisulfonic acid is suitable for industrial production, requires low sulfonation reaction temperature and mild reaction conditions, causes fewer byproducts, realizes high conversion rate and high selectivity, lowers labor intensity, allows the acid filtrate and harmful gas to be recycled and relieves environment pollution.

Description

technical field [0001] The invention belongs to the field of preparation methods of chemical raw materials, and in particular relates to a method for preparing salt-free sulfonated torezic acid, which uses fuming sulfuric acid and torezic acid as raw materials, and adopts the operation process of circulating acid-containing filtrate, continuously Preparation of salt-free sulfonated turezic acid. Background technique [0002] Salt-free sulfonated tunic acid can be used as an intermediate in the synthesis of reactive dyes, photosensitive materials and organic dyes. Reactive dyes, photosensitive materials and organic dyes are widely used in the textile industry, plate making industry, and dye industry, and the application fields are further expanding. Therefore, the demand for salt-free sulfonated turezic acid as an intermediate is also constantly increasing. Large, with broad market prospects and development space. [0003] At present, most domestic manufacturers produce sal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/47C07C303/06C07C303/44
Inventor 李丰年
Owner 山西翔宇化工有限公司
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