1,8-dinitro-3,6-naphthalene disulfonate hydrogenation reduction method

A technology of naphthalene disulfonate and naphthalene disulfonic acid, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of high chroma, high COD, etc., and achieve the effect of high economic value

Active Publication Date: 2013-05-22
ZHEJIANG QICAI ECO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the iron powder-hydrochloric acid method, this method reduces the generation of solid waste, but produces a large amount of dark blue-purple wastewater with high chroma and high COD

Method used

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  • 1,8-dinitro-3,6-naphthalene disulfonate hydrogenation reduction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0016] In 60g of methanol solution, add 40g of 1,8-dinitro-3,6-naphthalene disulfonic acid, and at the same time adjust the pH to 7-10 with ammonia water to convert into ammonium sulfonate, after stabilization, transfer to high-pressure hydrogenation Add 0.1g of ruthenium-silica gel supported catalyst to the kettle, seal and maintain the pressure, replace with nitrogen for 3 times, start to raise the temperature to 70°C, when the temperature is up, start to feed hydrogen, keep the pressure at 1.0MPa, keep the temperature for 5 hours, and turn on the cooling water, cooled down to normal temperature, and after pressure relief, the catalyst was removed by filtration to obtain the acid analysis of the filtrate. Filter and dry the filter cake. The yield of the target main product was 36.25g, the yield was 97.66%, and the purity of the target main product was 98.76%.

Embodiment example 2

[0018] In 80g of aqueous solution, add 20g of 1,8-dinitro-3,6-naphthalene disulfonic acid, and then use 30% liquid caustic soda to adjust the pH value to 7-10 and convert it into sodium sulfonate. Other operations are the same as in the examples 1. Using this embodiment, the yield of the target main product was 18.24 g, the yield was 98.27%, and the purity of the target main product was 99.03%.

Embodiment example 3

[0020] Change catalyst into palladium carbon catalyst 0.02g in case 1, all the other are the same as case 1. Finally, the yield of the target main product was 36.12g, the yield was 97.32%, and the purity of the target main product was 98.47%.

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Abstract

The invention relates to a 1,8-dinitro-3,6-naphthalene disulfonate hydrogenation reduction method belonging to the technical field of hydrogenation reaction of nitro-naphthalene disulfonic acid which contains and is connected to the same carbon skeleton. 1,8-dinitro-3,6-naphthalene disulfonate is reduced into 1,8-diamino-3,6-naphthalene disulfonate through catalytic hydrogenation, and is subjected to acidic hydrolysis to obtain an important intermediate compound H acid in dye industry. The method specifically comprises the following steps: dissolving 1,8-dinitro-3,6-naphthalene disulfonic acid, regulating the pH value to 7-10, and converting into corresponding salt; transferring the solution into a high-pressure hydrogenation kettle, adding a catalyst, heating and maintaining the pressure in a sealed environment, and reacting for 1-20 hours; and cooling to normal temperature, depressurizing, recovering the catalyst, performing acid precipitation on the reaction solution, filtering, and drying the filter cake to obtain 1,8-diamino-3,6-naphthalene disulfonic acid. The technical scheme of the invention has the advantages of no pollution in the preparation process, high product purity and the like.

Description

technical field [0001] The invention relates to a hydrogenation reduction method of 1,8-dinitro-3,6-naphthalene disulfonate, which belongs to the technical field of hydrogenation reaction containing nitronaphthalene disulfonic acid connected to the same carbon frame. Background technique [0002] 1,8-dinitro-3,6-naphthalene disulfonate is hydrogenated and reduced to obtain 1,8-diamino-3,6-naphthalene disulfonate, and the important intermediate H of reactive dyes is prepared by acid monohydrolysis acid. The method for preparing H acid has less pollution, high yield, low cost, and better product quality than the traditional trisulfonic acid method, completely changes the solid waste and wastewater problems produced by the traditional reduction method, and has high economic value. [0003] Traditional reduction methods include iron powder, zinc powder-hydrochloric acid reduction method. In industry, such as: traditional H acid reduction, fluorescent whitening agent DSD acid a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/47C07C303/22
Inventor 李学坤胡启木
Owner ZHEJIANG QICAI ECO TECH CO LTD
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