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Resource utilization method of 2,4-diaminobenzenesulfonic acid and waste water produced by 2,4-diaminobenzenesulfonic acid salt

A technology for the production of diaminobenzenesulfonic acid and waste water, which is applied in chemical instruments and methods, organic chemistry, and the preparation of organic compounds. It can solve the problems of unreasonable utilization and waste of resources, and achieve the effect of improving comprehensive utilization.

Active Publication Date: 2017-09-22
ZHEJIANG LONGSHENG GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process solves the problem of treating a large amount of waste sulfuric acid as a sulfonation product, the large amount of organic components contained in the waste acid have not been rationally utilized, resulting in a waste of resources

Method used

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  • Resource utilization method of 2,4-diaminobenzenesulfonic acid and waste water produced by 2,4-diaminobenzenesulfonic acid salt
  • Resource utilization method of 2,4-diaminobenzenesulfonic acid and waste water produced by 2,4-diaminobenzenesulfonic acid salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) The synthesis of 2,4-diaminobenzenesulfonic acid and its salts adopts a conventional process: add 108g of m-phenylenediamine to 378g of 98% sulfuric acid, control the temperature of the addition process within 120°C, and form a uniform salt solution after the addition, and raise the temperature To 150°C, slowly add 271.3g of 50% fuming sulfuric acid for sulfonation, and keep warm for 4h after the addition. After cooling the sulfonated solution to 130°C, slowly add 32.4g of water, keep it warm for 20min, then complete the hydrolysis and cool down to room temperature. Slowly add the cooled hydrolyzate into 550g of ice water, filter at about 15°C, and separate the filter cake and 941g of inter-acid mother liquor A. The filter cake was washed with 200 g of water, and after washing, the meta-acid solid and 343 g of washing liquid B were separated, the meta-acid yield was 74.6%, and the meta-acid purity (HPLC) was 99.5%. Add 32% sodium hydroxide aqueous solution to the m...

Embodiment 2

[0025] (1) according to the method for step (1) described in embodiment 1, synthesizing meta-bis, obtain 941g meta-acid mother liquor A, 343g washing liquid B, 180g neutralize mother liquor C three strands of waste water;

[0026] (2) it is the dilute acid solution that the acidity is 11% that step (1) is mixed with 3900g water preparation acidity mother liquor A, washing solution B, neutralization mother liquor C three waste waters that step (1) obtains, do not add m-phenylenediamine, directly dilute The acid solution was preheated to 240°C and added to the reactor for hydrolysis for 240 minutes; after the reaction, 26g of resorcinol (reduced pure) was obtained by extraction and rectification, the product purity of resorcinol (HPLC) was 99.2%, and the mole of m-phenylenediamine raw material The utilization rate is 97.3%.

Embodiment 3

[0028] (1) according to the method for step (1) described in embodiment 1, synthesizing meta-bis, obtain 941g meta-acid mother liquor A, 343g washing liquid B, 180g neutralize mother liquor C three strands of waste water;

[0029] (2) mixing the meta-acid mother liquor A obtained in step (1) with 3900g water to prepare acidity is a dilute acid solution of 11%, adding 270g of molten m-phenylenediamine to prepare a hydrolysis raw material solution; preheating the prepared hydrolysis raw material solution After reaching 240°C, add the reactor to hydrolyze for 240min to obtain resorcinol hydrolyzate, and obtain 276g of resorcinol (reduced pure) through extraction and rectification. The purity of resorcinol product (HPLC) is 99.7%. The molar utilization rate is 93.7%.

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Abstract

Disclosed is a resource utilization method of 2,4-diaminobenzenesulfonic acid and waste water produced by 2,4-diaminobenzenesulfonic acid salt. The utilization method comprises the step that 1, sulfonation reaction is normally conducted on m-phenylenediamine and sulfuric acid and / or fuming sulfuric acid, and interval acid mother liquid A and an interval acid coarse product which contain the sulfuric acid are obtained; the interval acid coarse product is washed with water, and an inter acid intermediate product and washing liquid B are obtained; the inter acid intermediate product is neutralized by alkali and separated to obtain an interval acid salt product and neutralization mother liquid C; 2, at least one of the interval acid mother liquid A, the washing liquid B and the neutralization mother liquid C is prepared into diluted acid liquid with the acidity of 3-20%, the prepared diluted acid liquid can be directly used as raw material liquid, and resorcinol hydrolysis liquid is obtained through heating hydrolysis; or a certain amount of m-phenylenediamine is supplemented into the prepared diluted acid liquid, mixed liquid is used as the raw material liquid, and the resorcinol hydrolysis liquid is obtained through heating hydrolysis; 3, the esorcinol hydrolysis liquid is extracted and rectified to obtain a resorcinol product. By the adoption of the resource utilization method of 2,4-diaminobenzenesulfonic acid and the waste water produced by the 2,4-diaminobenzenesulfonic acid salt, the emissions of waste acid and waste water produced in the production process of 2,4-diaminobenzenesulfonic acid and the 2,4-diaminobenzenesulfonic acid salt are significantly reduced, and the comprehensive utilization rates of raw materials are increased.

Description

(1) Technical field [0001] The present invention relates to a resource utilization method of 2,4-diaminobenzenesulfonic acid and its salt production wastewater, in particular to a kind of intermediate acid mother liquor, washing liquid and Process for neutralizing mother liquor for production of resorcinol. (2) Background technology [0002] 2,4-Diaminobenzenesulfonic acid, commonly known as m-acid, alias m-phenylenediamine-4-sulfonic acid, is an important chemical raw material, often used as dye intermediates or pharmaceutical intermediates. The traditional meta-acid synthesis process route is to prepare meta-acid by sulfonation of m-phenylenediamine, such as the new synthesis process of document 2,4-diaminobenzenesulfonic acid (Shi Weibin et al., Shanghai Dyestuff, Volume 36 No. 5), CN1900058A , CN102516137A, etc., using m-phenylenediamine as raw material, using sulfuric acid, oleum or SO 3 The gas is used as a sulfonating agent to sulfonate m-phenylenediamine, thereby o...

Claims

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Application Information

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IPC IPC(8): C07C37/05C07C37/68C07C37/72C07C37/74C07C39/08
CPCC07C37/05C07C37/685C07C37/72C07C37/74C07C39/08
Inventor 何旭斌陶建国李建勋张桂香苏建军袁伟杰孟明朱敬鑫
Owner ZHEJIANG LONGSHENG GROUP
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