Method for synthesizing 2,4-dinitro-6-bromoaniline by using bromamine acid product wastewater

A technology of bromo-amino acids and dinitro groups, which is applied in the field of comprehensive utilization of waste water from bromo-amino acid products, can solve the problems of waste water, low equipment requirements, and inability to achieve industrialized treatment.

Pending Publication Date: 2021-05-28
ZHEJIANG YIDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a method for synthesizing 2,4-dinitro-6-bromoaniline by utilizing waste water of bromoacidic products, which has the advantages of simple process, high production efficiency, suitable for industrial production, and low requirements for equipment , to solve the problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment one (acid 129 blue mother liquor water)

[0020] 1. Add 380g of acidic 129 blue mother liquor water into a 1000ML reaction vessel, adjust the pH to 9.5-10.5 with liquid caustic soda with a concentration of 30% by mass percentage, raise the temperature to 50°C, add 2.5g of sodium cyanide, and then raise the temperature to 98-100°C , keep warm at 98-100°C, keep pH 9.5-10.5, react for 4-6 hours until the material is cleared, filter, wash the filter cake with 20g of hot water to synthesize disperse dyes, and 400g of the filtrate is treated as follows:

[0021] 2. Add 25g of sodium hypochlorite with a mass percentage concentration of 10% to the filtrate with a mass of 400g, a temperature of 40-50°C, and a pH of 9.5-10.5, and react for 2-3 hours. After detecting the absence of sodium cyanide, add 2,4-dinitrate Aniline 17.5g, mass percentage concentration 98% sulfuric acid 8g, beating at 40-45°C for 1h; slowly add 1.8g sodium chlorate solution, the temperature is co...

Embodiment 2

[0023] Embodiment two (acid blue 25 mother liquor water)

[0024] 1. Add 400g of acidic 25 blue mother liquor water into a 1000ML reaction vessel, adjust the pH to 9.5-10.5 with liquid caustic soda with a concentration of 30% by mass percentage, raise the temperature to 50°C, add 1.5g of sodium cyanide, and then raise the temperature to 98-100°C , keep warm at 98-100°C, keep pH 9.5-10.5, react for 4-6 hours until the material is cleared, filter, wash the filter cake with 20g of hot water to synthesize disperse dyes, and 400g of the filtrate is treated as follows:

[0025] 2. Add 15g of sodium hypochlorite with a mass percentage concentration of 10% to the filtrate with a mass of 440g, a temperature of 40-50°C, and a pH of 9.5-10.5, and react for 2-3 hours. After detecting that there is no sodium cyanide, add 2,4-dinitrate Aniline 17.5g, mass percent concentration 98% sulfuric acid 9g, beating at 40-45°C for 1 hour; slowly add 1.8g of sodium chlorate solution, the temperature i...

Embodiment 3

[0027] Embodiment three (acid blue 324 mother liquor water)

[0028] 1. Add 440g of acidic 324 blue mother liquor water into a 1000ML reaction vessel, adjust the pH to 9.5-10.5 with liquid caustic soda with a concentration of 30% by mass percentage, raise the temperature to 50°C, add 1.2g of sodium cyanide, and then raise the temperature to 98-100°C , keep warm at 98-100°C, keep pH 9.5-10.5, react for 4-6 hours until the material is cleared, filter, wash the filter cake with 20g of hot water to synthesize disperse dyes, and 400g of the filtrate is treated as follows:

[0029] 2. Add 12g of sodium hypochlorite with a mass percentage concentration of 10% to the filtrate with a mass of 460g, a temperature of 40-50°C, and a pH of 9.5-10.5, and react for 2-3 hours. After detecting that there is no sodium cyanide, add 2,4-dinitrate Aniline 17.5g, mass percent concentration 98% sulfuric acid 9g, beating at 40-45°C for 1 hour; slowly add 1.8g of sodium chlorate solution, the temperatu...

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PUM

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Abstract

The invention relates to the technical field of chemistry and chemical engineering, and discloses a method for synthesizing 2,4-dinitro-6-bromoaniline by using bromamine acid product wastewater. The method comprises the steps of 1, adding sodium cyanide for reaction, synthesizing a disperse dye from byproducts in mother liquor and separated trace main products, filtering, and washing a filter cake with hot water to obtain the disperse dye; 2, adding an oxidizing agent into the filtrate and the washing liquid to oxidize and remove sodium cyanide, then reacting with 2,4-dinitroaniline, pulping in a sulfuric acid medium, dropwise adding sodium chlorate, reacting at the temperature of 35-75 DEG C, filtering the reaction liquid after bromination, washing a filter cake until the pH value is 6-7, and drying to obtain the product 2,4-dinitro-6-bromoaniline; and 3, decolorizing the mother liquor with activated carbon, performing membrane treatment, concentration and separation, recycling low-concentration salt water, and spraying high-concentration salt to be dry to serve as industrial salt (or serving as an active or acid dye assistant for internal digestion of a company). The problems of high COD and high-salt mother liquor wastewater of bromamine acid dye products in the prior art are solved.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a method for comprehensive utilization of waste water from bromic acid products. Background technique [0002] 1. Synthesis method of cyano-containing disperse dyes: one is to replace sulfonic acid groups with sodium cyanide, and the other is cyano-containing diazo components (for example: 2,4-dinitro-6-bromoaniline ) coupling with the coupling component after diazo; [0003] 2. 2,4-Dinitro-6-chloroaniline is an important intermediate of disperse dyes. At present, the commonly used process is to bromate 2,4-dinitroaniline with bromine in hydrochloric acid medium, and then use chlorine gas to or sodium chlorate and other oxidants to replace bromine in the reaction system and further brominate, then filter, wash with water, and dry to obtain solid 2,4-dinitro-6-bromoaniline. [0004] The anthraquinone dye product of bromic acid raw material will produce...

Claims

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Application Information

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IPC IPC(8): C07C209/74C07C211/52
CPCC07C209/74
Inventor 卢林德钱立王磊叶永华上官开泰朱成林
Owner ZHEJIANG YIDE CHEM
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