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Governing and resource recovering method of 4B acid production waste water

A technology for waste water production and resource recovery, applied in water/sewage treatment, chemical instruments and methods, adsorption water/sewage treatment, etc.

Active Publication Date: 2006-01-25
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The result of literature search shows: before the present invention is completed, only one case adopts the liquid phase extraction method to the report that 4B acid production wastewater is treated, and there is no record of using resin adsorption technology to this wastewater treatment and resource recycling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: 100 mL (about 75 grams) of NDA-99 macroporous adsorption resin was loaded into a jacketed glass adsorption column (Φ32×360 mm). The 4B acid production wastewater was adjusted to pH = 3 with alkali and then filtered. The filtrate passed through the resin bed at a flow rate of 100mL / h at 25±5°C. The treatment capacity was 900mL / batch, and the raw wastewater COD cr 8197mg / L, 4B acid content is 4220mg / L, after resin treatment, the effluent is colorless and transparent, 4B acid content is 32mg / L, COD cr Dropped to 217mg / L.

[0017] Use 100mL of 12% (mass ratio) ammonia water, 100mL of 4% ammonia water and 100mL of water in sequence at a temperature of 35±5°C to pass through the resin bed at a flow rate of 100mL / h for desorption. After desorption is completed, use 80mL of 8% dilute sulfuric acid Acidify the resin for later use. The desorbed high-concentration eluent (150mL) was blown off with air, and water was used as an absorbent to recover ammonia water; after...

Embodiment 2

[0018] Example 2: 100 mL (about 75 grams) of NDA-99 macroporous adsorption resin was loaded into a jacketed glass adsorption column (Φ32×360 mm). The 4B acid production wastewater was adjusted to pH = 3 with alkali and then filtered. The filtrate passed through the resin bed at a flow rate of 150mL / h at 40±5°C. The treatment capacity was 900 mL / batch, and the raw wastewater COD cr 8553mg / L, 4B acid content is 4310mg / L, after resin treatment, the effluent is colorless and transparent, 4B acid content is 42mg / L, COD cr Dropped to 237mg / L.

[0019] Use 100mL of 12% (mass ratio) ammonia water, 100mL of 4% ammonia water and 100mL of water in sequence at a temperature of 45±5°C to pass through the resin bed at a flow rate of 100mL / h for desorption. After desorption is completed, use 80mL of 4% dilute sulfuric acid Acidify the resin for later use. The desorbed high-concentration eluent (150mL) was blown off with air, and water was used as an absorbent to recover ammonia water; afte...

Embodiment 3

[0020] Embodiment 3: Select three 316L stainless steel adsorption towers (Φ600×3500mm) with the same specifications, and fill each tower with 600 kilograms (about 800 L) of NDA-99 macroporous adsorption resin. Adjust the pH of 4B acid production wastewater to 3 with alkali and then filter it. 3 The flow rate of / h is pumped into the adsorption tower, and the adsorption adopts the method of I and II towers in series and downstream adsorption, and the processing capacity is 8m 3 / batch, raw wastewater COD cr 8384mg / L, 4B acid content is 4276mg / L, after resin treatment, the effluent is colorless and transparent, 4B acid content is 39mg / L, COD cr down to 226mg / L.

[0021] will absorb over 8m 3 No. I adsorption tower of waste water carries out desorption. First drain the residual liquid in the adsorption tower, and then use 0.8m 3 12% (mass ratio) ammonia water, 0.8m 3 4% ammonia and 0.8m 3 Water at a temperature of 35±5°C, at 0.8m 3 The flow rate of / h flows through the r...

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PUM

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Abstract

A process for reclaiming the sewage generated during production of 4B acid includes regulating pH value, filtering, adsorbing by macroreticular resin, eluting by diluted ammonia water and water, air blowing, using water as absorbent to recover ammonia water, vacuum distilling for concentrating it, using sulfuric acid to regulate pH=0-3, and filtering to recover coarse 4B acid.

Description

1. Technical field [0001] The invention relates to the treatment of 4B acid production wastewater of benzene series dye intermediates, in particular, a method for enriching, separating and recycling 4B acid in the 4B acid production wastewater by adopting a resin adsorption method. 2. Background technology [0002] 4B acid (4-aminotoluene-3-sulfonic acid) is an important dye intermediate, which is used in the synthesis of various dyes such as Lisol Baohong BK, Reactive Brilliant Red X-7B and Reactive Brilliant Orange K-R. At present, an important production process of 4B acid in China is to use p-toluidine as raw material, first salting with concentrated sulfuric acid, and then baking and transposition at high temperature. To produce one ton of 4B acid products, about 30 tons of brown-red wastewater will be discharged, the pH of the wastewater is 0.8-1.0, and the COD cr Up to 8000-10000mg / L, which mainly contains 4B acid 4000-5000mg / L, p-toluidine 500-800mg / L, and also cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F1/58C02F1/28C02F1/66
Inventor 张全兴孙越王璠周玮王穆君陈金龙鲁俊东
Owner NANJING UNIV
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