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Clean production process for dye intermediate sulfonated para-ester

A technology of clean production and para-ester, which is applied in the field of clean production process of dye intermediate sulfonated para-ester, can solve the problems of inability to remove residual salt of waste acid and low adsorption efficiency, achieve mild reaction conditions and reduce waste of resources , the effect of simple operation

Active Publication Date: 2015-12-09
JIANGSU YUANZHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This treatment method only uses activated carbon to adsorb organic matter, and the adsorption efficiency is low; moreover, the residual salt in the waste acid cannot be removed, and the subsequent reaction will be adversely affected when it is reused.

Method used

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  • Clean production process for dye intermediate sulfonated para-ester
  • Clean production process for dye intermediate sulfonated para-ester
  • Clean production process for dye intermediate sulfonated para-ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Sulfonation: Add 420 g of fuming sulfuric acid to a 500 ml four-neck flask equipped with a thermometer and a stirring device, add 184 g of p-β-hydroxyethylsulfone acetanilide below 45 °C, and heat up to 133 °C in 1 hour , and insulated at 133-135°C for 4 hours.

[0045] (2) Hydrolysis: cool down the sulfonated compound to 82-85°C, add 28g of water at 82-85°C, raise the temperature to 105-110°C and keep it warm for 5 hours;

[0046](3) Dilution: Cool the hydrolyzate to below 30°C, slowly put the material into a 2000ml beaker prepared with 150g of bottom water and 700g of ice for dilution, and control the dilution temperature below 25°C;

[0047] (4) Salt-out crystallization: the temperature of the diluent is controlled at 25°C, and 110 g of potassium sulfate is added to precipitate the sulfonated para-ester;

[0048] (5) Filtration: The salting-out material is filtered to obtain 212.8 g of light pink solid sulfonated para-ester, with an HPLC purity of 95.2% and an a...

Embodiment 2

[0060] Keeping other conditions unchanged in Example 1, the filter cake I obtained in the previous batch was added to step (2) for hydrolysis, and after salting out, crystallization and filtration, 219.5 g of light pink solid sulfonated para-ester was obtained, and the HPLC purity was 95.4%, the amino value is 70.7%. On the premise of product quality assurance, the yield increased by 2.9%.

Embodiment 3

[0062] (1) Sulfonation: Add 420 g of fuming sulfuric acid to a 500 ml four-necked flask equipped with a thermometer and stirring, add 184 g of p-β-hydroxyethylsulfone acetanilide below 45 ° C, and heat up to 133 ° C in 1 hour. And keep it warm at 133-135°C for 4 hours.

[0063] (2) Hydrolysis: cool down the sulfonate to 82-85°C, add 28g of water at 82-85°C, then add the filter cake I recovered in the previous batch, heat up to 105-110°C and keep it warm for 5 hours;

[0064] (3) Dilution: Cool the hydrolyzate to below 30°C, slowly put the material into a 2000ml beaker prepared with 150g of bottom water and 700g of ice for dilution, and control the dilution temperature below 25°C;

[0065] (4) Salt-out crystallization: the temperature of the diluent is controlled at 20°C, and 100 g of potassium sulfate is added to precipitate the sulfonated para-ester;

[0066] (5) Filtration: the salting-out material is filtered to obtain 220.1 g of light pink solid sulfonated para-ester, the...

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Abstract

The invention discloses a clean production process for a dye intermediate sulfonated para-ester. The process comprises the following steps: (1) sulfonation: carrying out a reaction on p-beta-ethoxyl sulfonyl acetanilide and sulfuric acid to obtain a sulfonated body; (2) hydrolyzation: carrying out hydrolysis reaction on the sulfonated body and water to obtain a hydrolysate; (3) dilution: adding water into the hydrolysate to dilute the hydrolysate to obtain a diluted liquid; (4) salting-out crystallization: adding potassium sulfate into the diluted liquid for salting-out crystallization and filtering the liquid to obtain sulfonated para-ester and mother liquor wastewater; and (5) resource recycling of the mother liquor wastewater: cooling and cold-separating the mother liquor wastewater and filtering the mother liquor wastewater to obtain a filtrate I and a filter cake I, adding an adsorbent into the filtrate I for adsorption, filtering the filtrate to obtain a filtrate II, and then concentrating the filtrate II, carrying out cooling crystallization and separation on the concentrated filtrate II to obtain diluted sulfuric acid and solid potassium sulfate. According to the clean production process, useful intermediate product, potassium sulfate and sulfuric acid in the wastewater are effectively recovered by adding the potassium sulfate for salting-out crystallization, and meanwhile, COD of the wastewater is reduced.

Description

technical field [0001] The invention belongs to the field of dye production, and in particular relates to a clean production process for dye intermediate sulfonated para-ester. Background technique [0002] Sulfonated para-ester, also known as 4-β-hydroxyethylsulfone sulfate aniline-2-sulfonic acid, CAS No. 42986-22-1, is an important intermediate of KN dyes. [0003] The synthesis process of sulfonated para-ester mainly uses para-ester as raw material, after sulfonation with oleum, hydrolysis to remove bis-sulfonated para-ester, dilution with ice water, salting out with potassium chloride, and filtration to obtain the final Products, there is no report on salting out with potassium sulfate. [0004] In the production process, a large amount of orange-red mother liquor wastewater will be produced, in which the content of sulfuric acid is 25-30% (based on the quality of wastewater), and the content of organic matter (mainly disulfonated para-ester and sulfonated para-ester) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/36C07C315/04C01B17/90C01D5/16
Inventor 陈田木陈宝兴王海明杨洋
Owner JIANGSU YUANZHENG CHEM
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