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A kind of treatment method of acid waste water produced in the production process of para-ester

A treatment method, acid wastewater technology, applied in water/sewage treatment, water/sewage multi-stage treatment, heating water/sewage treatment, etc., can solve the problems of poor treatment effect, high treatment cost, waste of resources, etc., and achieve low cost , Protect the ecological environment and realize the effect of recycling

Active Publication Date: 2020-12-15
JIANGSU MINGSHENG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the acidic wastewater produced in the production process of para-ester is generally treated by methods such as alkali neutralization, chemical oxidation or microbial degradation, but the above-mentioned methods have the following defects: the treatment cost is high, and secondary pollution is easy to occur. Poor processing effect, resulting in waste of resources

Method used

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  • A kind of treatment method of acid waste water produced in the production process of para-ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a 500ml four-necked flask, add 300g of para-ester acid waste water (COD=25382ppm, acidity is 36.3%), stir to heat up, depressurize distillation and dehydration, until the dehydration amount reaches more than 150ml (the acidity of waste water is 72.8% at this time). Start to heat up, slowly add 100 g of aniline dropwise, dropwise for 2 hours, and control the temperature to 100-110 °C. After the dropwise addition is complete, continue to heat up to 180 ° C, distill and dehydrate while reacting, and when the reactant in the flask becomes a molten salt state, it is quickly transferred to the kneading dryer that has been heated up in advance, and the temperature is raised to 190 ° C. After the kneading is complete, the material is discharged to obtain Crude product p-aminobenzenesulfonic acid 188g, purity 98.19%, content 96.16%.

[0038] The water from each dehydration step and drying step was collected and combined, and its COD value was measured to be 285 ppm.

Embodiment 2

[0040] In a 500ml four-necked flask, add 400g of para-ester acid waste water (COD=23846ppm, acidity is 28.4%), stir to heat up, depressurize distillation dehydration, until dehydration amount reaches more than 250ml (at this moment, the acidity of waste water is 76.4%). Start to heat up, slowly add 100 g of aniline dropwise, dropwise for 3 hours, and control the temperature to 90-100 °C. After the dropwise addition is complete, continue to heat up to 170 ° C, dehydrate while reacting, and quickly transfer to the kneading dryer that has been heated up in advance when the reactant in the flask is in the state of molten salt, heat up to 180 ° C, and discharge after the kneading is complete to obtain a crude product 191 g of p-aminobenzenesulfonic acid, the purity is 98.06%, and the content is 96.00%.

[0041] The water from each dehydration step and drying step was collected and combined, and its COD value was measured to be 237 ppm.

Embodiment 3

[0043] In a 500ml four-necked flask, add 500g of para-ester acid waste water (COD=27219ppm, acidity is 21.5%), stir to heat up, depressurize distillation and dehydration, until the dehydration amount reaches more than 350ml (the acidity of waste water is 71.3% at this time). Start to heat up, slowly add 100 g of aniline dropwise, dropwise for 2.5 hours, and control the temperature to 110-120 °C. Continue to heat up to 190°C after the dropwise addition is complete, dehydrate while reacting, quickly transfer to the kneading dryer that has been heated up in advance when the reactant in the flask is in the state of molten salt, heat up to 200°C, and discharge after the kneading is complete to obtain a crude product 185 g of p-aminobenzenesulfonic acid, the purity is 98.08%, and the content is 95.77%.

[0044] The water from each dehydration step and drying step was collected and combined, and its COD value was measured to be 243 ppm.

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Abstract

A method for treating acidic waste water generated in a para-ester production process is characterized by comprising the following steps: (1) heating the acidic waste water, and adding aniline in the acidic waste water to obtain reaction liquid; (2) reacting the reaction liquid obtained in the step (1), and distilling to remove water to obtain a coarse product; and (3) refining the coarse product obtained in the step (2) to obtain a fine product which is p-aminobenzene sulfonic acid or salt thereof. The treatment method is simple in technological process, simple to operate and low in cost; and secondary pollutants are not generated. The acidic waste water in the para-ester production process can be treated effectively, meanwhile, the high-purity product which is the p-aminobenzene sulfonic acid or the salt thereof is obtained, and maximization of comprehensive utilization to resources is realized.

Description

technical field [0001] The invention relates to a method for treating acid waste water produced in the production process of para-ester. Background technique [0002] Para-ester is an important reactive dye intermediate, which is used to synthesize EF type, KN type, M / KM type, ME type and other reactive dyes containing vinylsulfone group. The production process of the para-ester is prepared by taking the antipyretic ice (N-acetanilide) as the main raw material and going through the processes of sulfonation, chlorination, reduction, condensation and esterification. In order to complete the reaction conversion, excessive acid needs to be added during the synthesis process, which leads to the production of a large amount of acidic waste water in the production process. Its COD is 5000~30000mg / L and the acidity is 10~35%, which belongs to the organic waste water with high acidity, high COD and refractory degradation. [0003] In the prior art, the acid waste water produced in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F9/10C07C303/44C07C309/46C02F101/30C02F101/34C02F101/38
CPCC02F1/00C02F1/04C02F2101/308C02F2101/34C02F2101/38C02F2101/40C07C303/44C07C309/46
Inventor 阮海兴樊明伟魏艳军彭春嘉郭理想陈伟东
Owner JIANGSU MINGSHENG CHEM