Processing method of aniline intermediate production wastewater

A treatment method and technology for producing wastewater, which can be used in water/sewage multi-stage treatment, water/sludge/sewage treatment, chemical instruments and methods, etc., and can solve problems such as affecting the quality of salt crystals and blocking pipes.

Active Publication Date: 2015-07-29
ZHEJIANG LONGSHENG GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing methods for treating wastewater containing ammonium chloride and sodium chloride mostly use evaporation and crystallization, such as patents CN1224694A, CN101544437A, etc., but in the actual evaporation and crystallization process, tar is produced or organic matter is enriched, which will block the Pipelines and affecting the crystallization quality of the salt

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  • Processing method of aniline intermediate production wastewater
  • Processing method of aniline intermediate production wastewater

Examples

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Effect test

Embodiment 1

[0055] The waste water is m-acetamido-N, N-diethylaniline synthesis wastewater (m-amino acetanilide and ethyl chloride undergo an alkylation reaction in the presence of ammonia water to produce waste water containing ammonium chloride), and the microfilter is equipped with a 50-micron filter The macroporous resin packed in the resin columns in the adsorption towers A~D is DA201-C resin, and the volume of the resin column is 4m 3 , waste water with 12m 3 The adsorption tower reaches saturation in 10 hours at a flow rate of / h, and the desorbent is 90% methanol. 3 / h flow rate washing or desorption for 1 hour, the specific steps are as follows:

[0056] 1) Collect the wastewater into the raw water pool, adjust the pH to 6.8-7.0, filter through the microfilter, and pump it into the resin adsorption device with three ABC towers in series (4 towers and 3 in series, D tower for standby) for adsorption operation;

[0057] 2) After the A adsorption tower is saturated, the feed is st...

Embodiment 2

[0066] 2-methoxy-5-acetamido-N, N-diallylaniline synthetic wastewater (2-methoxy-5-acetamidoaniline and allyl chloride undergo alkylation reaction in the presence of ammonia water will produce chlorinated Ammonium waste water) is operated by the method described in embodiment 1, and difference is: waste water is adjusted pH5.0 with hydrochloric acid earlier, and waste water is with 10m 3 / h flow rate adsorption for 10 hours, desorbent is 10% hydrochloric acid, water and desorbent are 6m 3 / h flow rate washing or desorption for 1 hour, the analysis solution in the analysis solution recovery tank is used for the synthesis of subsequent dyes; when the three-effect evaporation is set, the first effect temperature is 90°C, the first effect vacuum degree is -40KPa, and the second effect temperature is 80 ℃, second effect vacuum degree -60KPa, third effect temperature 65℃, third effect vacuum degree -85KPa. The obtained ammonium chloride had a yield of 99.5% and a purity of 99.3%. ...

Embodiment 3

[0068] 2-cyano-4-nitroaniline synthesis waste water (2-cyano-4-nitrochlorinated benzene and liquid ammonia ammonolysis reaction can produce waste water containing ammonium chloride) by the method described in Example 1, The difference is: waste water is 16m 3 / h flow rate adsorption for 10 hours, the desorbent is 95% methanol, and the water and desorbent are 8m 3 / h flow rate washing or desorption for 1 hour; when three-effect evaporation, set the first effect temperature to 98°C, the first effect vacuum degree to -36KPa, the second effect temperature to 75°C, the second effect vacuum degree to -62KPa, and the third effect temperature to 68 ℃, third effect vacuum -88KPa. The obtained ammonium chloride has a yield of 99.6%, a purity of 99.1%, and a recovery of 2-cyano-4-nitroaniline of 64%.

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Abstract

A processing method of aniline intermediate production wastewater comprises the following steps: (1) mother liquor wastewater containing sodium chloride or ammonium chloride during the production process of an aniline intermediate firstly undergoes physical filtration to remove impurities; (2) after filtration, the mother liquor wastewater enters an N-staged series resin adsorption device, wherein N is a natural number being greater than or equal to 2; the N-staged series resin adsorption device is an N+1 towers N-staged series resin adsorption device formed by series connection of N+1 adsorption towers filled with resin columns; one of the adsorption towers is a standby tower; the whole resin adsorption device ceaselessly carries out wastewater adsorption and resin desorption regeneration; (3) after the mother liquor wastewater undergoes adsorption by the resin adsorption device, physical filtration is carried out to remove impurities; (4) the filtered mother liquor wastewater enters a multiple-effect evaporation device to undergo condensation crystallization, an ammonium chloride or sodium chloride solid is finally separated, and the mother liquor returns to the multiple-effect evaporation device to continuously undergo condensation crystallization; and (5) a desorption solution obtained from the step (2) is reused. The processing method provided by the invention is a genuine continuous clear production technology.

Description

(1) Technical field [0001] The invention relates to a method for treating wastewater from the production of aniline intermediates, in particular to a method for treating wastewater containing ammonium chloride or sodium chloride in the production of aniline intermediates. (2) Background technology [0002] Aniline intermediates (including aniline and substituted aniline) have an active amino port, which can be used to synthesize a variety of disperse dye intermediates through amino modification reactions with a variety of substrates, and then prepare a variety of disperse dyes, such as 3-(N , N-diethyl)-4-methoxyacetanilide is an important intermediate for the synthesis of disperse blue 291. -Methoxyacetanilide is used as raw material, bromoethane is used as alkylating agent, and amino substitution reaction is carried out in the presence of acid-binding agent, but the raw material bromoethane is expensive and belongs to hazardous chemicals. For this, the new The process pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01C1/16C01D3/14
Inventor 祝培明倪松涛韩伟金鑫伟余青结蒋应海
Owner ZHEJIANG LONGSHENG GROUP
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