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Clean preparation method of 1, 8-dinitro-3, 6-naphthalenedisulfonic acid

A technology of naphthalene disulfonic acid and dinitro, which is applied in 1 field, can solve the problems of large nitrification wastewater and discharge, and achieve high yield and simple and practical treatment process

Active Publication Date: 2013-02-20
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a clean preparation method of 1,8-dinitro-3,6-naphthalene disulfonic acid, to solve the problem of massive discharge of nitrification wastewater

Method used

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  • Clean preparation method of 1, 8-dinitro-3, 6-naphthalenedisulfonic acid
  • Clean preparation method of 1, 8-dinitro-3, 6-naphthalenedisulfonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Dissolve 1008 grams of 2,7-naphthalene disulfonic acid in 3L of industrial sulfuric acid with a mass fraction of 93%, keep the temperature at 0-5°C, add 630 grams of 98% fuming nitric acid dropwise within 2 hours, and keep the reaction for 2 hours until nitration The reaction is complete. 4600ml of water was added dropwise to the reactant, and then the temperature was raised to 95-100° C., and the air was continuously fed under stirring, and the temperature was lowered after keeping the temperature for 3 hours. Filtration at room temperature yielded 1976 g of light yellow 1,8-dinitro-3,6-naphthalene disulfonic acid filter cake with a purity of 98.83%, a solid content of 60.87%, and a yield of 90.91%. Obtain 6.87L of reddish-brown nitration mother liquor, COD value 47000mg / L, for subsequent treatment.

Embodiment 2

[0024] Take 1 L of the nitration mother liquor obtained in Example 1, stir rapidly at room temperature (360r / min, the same below), add 0.5 g of the previously prepared flocculant, and reduce the stirring speed after ten minutes (60r / min, the same below). After 1 hour, it was filtered, and the color of the mother liquor changed from reddish brown to light yellow. The COD value is 2200mg / L.

Embodiment 3

[0026] Add 0.1 g of the above-prepared flocculant to 1 L of nitration mother liquor with rapid stirring at 10°C, and reduce the stirring speed after ten minutes. Filter after 2 hours, the filtrate is light yellow, and the COD value is 3700mg / L.

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Abstract

The invention provides a clean preparation method of 1, 8-dinitro-3, 6-naphthalenedisulfonic acid. A reaction formula is shown in the description. The method includes: taking 2, 7-naphthalenedisulfonic acid as a reaction raw material, adopting sulfuric acid as a solvent, and adding fuming nitric acid with a content of 98% dropwisely to prepare 1, 8-dinitro-3, 6-naphthalenedisulfonic acid; and after the end of the reaction, adding water to conduct dilution and isolating the product, subjecting the remaining nitrification mother solution to flocculation treatment so as to remove impurities, and then carrying out pressure reduction concentrating to recover the sulfuric acid as the solvent for next reaction. The method provided in the invention has the advantages of short technological process, simple operation, good quality product, and no wastewater discharge, thus being suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to a clean preparation method of 1,8-dinitro-3,6-naphthalene disulfonic acid. Background technique [0002] The main application value of 1,8-dinitro-3,6-naphthalene disulfonic acid is the synthesis of H acid. The traditional production process of H acid is made by heating 1-naphthylamine-3,6,8-trisulfonic acid with alkali, followed by acid precipitation. In the 1980s, Japanese patents JP8451253 and JP4210954 reported a kind of 2,7-naphthalene disulfonic acid as raw material to prepare intermediate 1,8-dinitro-3,6-naphthalene disulfonic acid, and further reduce , A new process for hydrolyzing and synthesizing H acid. In recent years, Chinese patent CN101717355 also reported a method for synthesizing H acid from refined naphthalene as a starting material through intermediate 1,8-dinitro-3,6-naphthalene disulfonic acid. Compared with the traditional process, the yield of the above-men...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/40C07C303/22
Inventor 马瑛刘东孟明扬高嘉新杨文东王玉灿刘志敏孟伯德李锋
Owner 中国中化股份有限公司
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