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Recovery method of glycolic acid in phenoxy carboxylic acid industrial wastewater

The technology of a phenoxycarboxylic acid and a recovery method is applied in the field of treatment of phenoxycarboxylic acid production wastewater, which can solve problems such as non-compliance with national requirements, waste of resources, etc., and achieve good economic benefits, reduce emissions, and reduce costs. Effect

Active Publication Date: 2013-07-10
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the reaction is similar, the components in the phenoxycarboxylic acid production wastewater are basically the same, generally including 5% glycolic acid, 20% NaCl, 3% phenol, and 2% phenoxycarboxylic acid. The treatment of this part of wastewater has always been production 2, The problem of 4-D products and phenoxyacetic acid products is that the glycolic acid in the wastewater increases the organic content of the wastewater and increases the COD. Direct discharge does not meet the national requirements and wastes resources. In view of the low corrosion of glycolic acid cleaning equipment, With the advantages of high efficiency and low cost, the recycling and reuse of glycolic acid in wastewater is a method that is both environmentally friendly and conducive to the reuse of resources, which meets the requirements of national policies

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 2,4-D production wastewater (first grade wastewater) contains 5.2% glycolic acid, 1.8% phenol, 2.3% 2,4-D acid, 19.5% NaCl, pH=2.0, take 1000g of wastewater, add complex extraction agent three normal Octylamine 13%, tributyl phosphate 6%, diesel oil 81% 300g, mixed with a static mixer at a temperature of 35°C and statically layered, extracted phenol and 2,4-D acid in wastewater, detected The content of phenol and 2,4-D acid in the wastewater is 0.08%, and then the wastewater is transferred to a multi-effect evaporation system, and evaporated at 75°C to obtain 200g of concentrated wastewater mother liquor, which consists of 38.40% glycolic acid and 13.6% sodium chloride , water 45.0%, other impurities 3%. Add hydrochloric acid to the mother liquor to adjust pH=1, dehydrate under vacuum degree -0.095MPa between 60°C and 95°C to continuously precipitate sodium chloride, stop distillation when the temperature reaches 95°C, and separate the precipitated sodium chloride, 96 ...

Embodiment 2

[0026] 2M and 4C chlorine production wastewater (first grade wastewater) contains 5.7% glycolic acid, 1.1% phenol, 1.8% acid, 21.2% NaCl, pH = 1.6, add complex extractant tri-n-octylamine 15%, n-butyl Alcohol 7%, kerosene 78%, according to the extraction agent: waste water=1:5.0v / v, use a static mixer to mix and static layer at a temperature of 35°C, extract phenol and 2-methyl-4-chloric acid in the waste water, 0.06% of the phenol and acid content in the extracted waste water was detected, and then the waste water was transferred to the MVR evaporation system for evaporation treatment to obtain a waste water mother liquor, which was composed of 31.2% glycolic acid, 16.3% sodium chloride, 49.5% water, and 3% other impurities . Take 200g of the mother liquor, add hydrochloric acid to adjust pH = 2, dehydrate at a vacuum degree of -0.098MPa between 60 and 95°C to continuously precipitate sodium chloride, stop distillation when the temperature reaches 95°C, and carry out the prec...

Embodiment 3

[0028] 2,4-D production wastewater contains 5.3% glycolic acid, 1.5% phenol, 2.1% 2,4-D acid, 22.1% NaCl, pH=2.0, add complex extraction agent trin-octylamine 13%, phosphoric acid to the wastewater 6% tributyl ester, 81% diesel oil, according to the extraction agent: waste water = 1:3.0v / v (volume ratio), use a static mixer to mix and statically layer at a temperature of 35°C, and extract phenol and 2,4-D acid, 0.08% of phenol and 2,4-D acid content in the wastewater after detection and extraction, and then transfer the wastewater to the MVR evaporation system for evaporation treatment to obtain the wastewater mother liquor, which consists of 24.60% glycolic acid, chlorinated Sodium 18.40%, water 54.0%, other impurities 3%. Take 200g of the mother liquor, add sulfuric acid to adjust the pH=2.5, and dehydrate at -0.098Mpa in vacuum between 60 and 95°C to continuously precipitate sodium chloride. After the temperature reaches 95°C, stop the distillation and separate the precipit...

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Abstract

The invention discloses a recovery method of glycolic acid in phenoxy carboxylic acid industrial wastewater. The recovery method comprises the following steps of: extracting the wastewater to remove most of the organic substances in the wastewater, and treating the extracted wastewater in the next step; evaporating and concentrating the wastewater to remove most of the inorganic salt in the wastewater; adjusting the pH value of the desalted wastewater to 1-4, carrying out reduced pressure distillation to remove most of the water in the wastewater, separating out salt from the wastewater in the distillation process, and filtering to remove the salt in the wastewater, thus obtaining more than 70% of henoxy carboxylic acid solution. The recovery method has the advantages of being simple in operation and low in cost, separating out the glycolic acid with high quality from the wastewater, solving the difficulty in treatment of phenoxy carboxylic acid industrial wastewater, being in line with national policy requirements, realizing resource utilization, obtaining good economic benefits, reducing product cost and achieving the clean production requirements.

Description

technical field [0001] The invention relates to a treatment method for phenoxycarboxylic acid production wastewater, in particular to a treatment method for phenoxycarboxylic acid production wastewater and a method for recovering by-product glycolic acid therefrom. Background technique [0002] Glycolic acid (2-hydroxyethanoic acid), also known as glycolic acid, glycolic acid, structural formula HOCH 2 COOH, molecular formula C 2 H4O 3 , molecular weight 76.05. Glycolic acid is a colorless, odorless, translucent crystalline solid belonging to the monoclinic prism system. Soluble in water, methanol, acetone, acetic acid, ethyl acetate and other organic solvents, slightly soluble in ether, almost insoluble in hydrocarbon solvents. As a new type of fine chemical intermediate, glycolic acid is mainly used in the fields of cleaning agents, insecticides, new biodegradable materials and daily chemicals, and its application range is very wide. In recent years, glycolic acid has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/06C07C51/42
Inventor 孙国庆侯永生李宗清李志清高技峰胡义山贺恩静许园园吕鹏孙伟王浩良王宁宁袁海明张国锋崔杰尧
Owner SHANDONG WEIFANG RAINBOW CHEM
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