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Preparation method of J acid and J acid waste water comprehensive treatment and recycling method

A comprehensive treatment and resource utilization technology, applied in the field of comprehensive treatment and resource utilization of J-acid wastewater, to achieve the effects of high stripping rate, easy regeneration, and high safety factor

Active Publication Date: 2014-07-02
XIANGSHUI HENRYDA TECH CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The treatment method of this liquefied ammonia absorption waste water has not seen any report yet

Method used

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  • Preparation method of J acid and J acid waste water comprehensive treatment and recycling method
  • Preparation method of J acid and J acid waste water comprehensive treatment and recycling method
  • Preparation method of J acid and J acid waste water comprehensive treatment and recycling method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This example provides a kind of production method of J acid, comprises the steps:

[0042] (1) Ammonification: Ammonia solution is prepared, ammonium bisulfite solution is added to the preparation kettle, and then an appropriate amount of ammonia gas is introduced to make ammonia solution. Add the ammoniated solution and sodium 2-hydroxynaphthalenesulfonate into the ammoniated kettle, open the jacket of the reactor and let in steam for heating, control the temperature in the kettle to be around 150°C, and carry out the ammoniation at 0.95MPa at a temperature of 150-155°C. The reaction was carried out and kept for 7 hours to generate 2-naphthylamine-1-sodium sulfonate. After the heat preservation is completed, the steam valve is closed, and the ammoniated solution is transferred to the acidification kettle.

[0043] (2) Acidification: Add a certain amount of dilute sulfuric acid into the acidification kettle, then transfer the ammoniated material into the acidification ...

Embodiment 2

[0051] This example provides a method for the comprehensive treatment and resource utilization of the J-acid waste water that a kind of embodiment 1 produces, specifically as follows:

[0052] (1) Wastewater reuse: 4500 liters of waste water of 30% of the total amount of J acid hydrolyzed waste water is used in the acidification process in the production process of tunic acid;

[0053] (2) Primary extraction: 10,500 liters of wastewater containing 70% of the total amount of J acid hydrolyzed wastewater is fully mixed with the extractant at a ratio of 1:1 to oil and water at normal temperature and pressure. Grade extraction, the extractant is composed of trioctylamine 30wt%, sulfonated kerosene 60% and tributyl phosphate 10%;

[0054] (3) Secondary extraction and back extraction: the extracted water of the primary extraction is fully mixed with the extractant at a ratio of 1:1 to oil and water at normal temperature and pressure for secondary extraction, the extraction phase is ...

Embodiment 3

[0059] This example provides a kind of production method of J acid, and it is basically the same as embodiment 1. The difference is: the ammonification preparation solution used in the ammoniation in the production process of Tuburic acid is prepared with the liquid ammonia absorption wastewater reused in the previous batch reaction, and the acidified water in the production process of Tuburic acid is prepared with the hydrolyzed wastewater reused in the previous batch reaction. ; The part of the hydrolysis preparative liquid used in the J acid hydrolysis process is the filtrate obtained according to the step (5) of Example 2. Compared with Example 1, this method can reduce the water cost of J acid by about 30% and the cost of wastewater treatment by about 40%, and reduce environmental pollution.

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Abstract

The invention relates to a preparation method of J acid and a J acid waste water comprehensive treatment and recycling method. The J acid waste water comprehensive treatment and recycling method is as follows: the following treatment is carried out on hydrolysis waste water: (1) 30-40% of the total quantity of the hydrolysis waste water is used in an acidification reaction for preparing 2-naphthylamine-1-sulphonic acid by utilizing sodium 2-naphthylamine-1-sulphonate; (2) extraction and reextraction are carried out on the residual hydrolysis waste water, so that Na2SO4 and extraction waste liquor are obtained, the extraction waste liquor is used in a hydrolysis working procedure in a J acid production process, an extraction agent adopted during extraction is composed of 10-30wt% of complex agent, 30-70wt% of diluent and 5-20wt% of tributyl phosphate, and the complex agent is trioctylamine, or trialkyl tertiary amine or combination of trioctylamine and trialkyl tertiary amine. By adopting the preparation method of the J acid, the cost of water for the J acid and waste water treatment cost can be greatly reduced, and environmental pollution can be reduced.

Description

technical field [0001] The invention relates to a preparation method of J-acid, in particular to a method for comprehensive treatment and resource utilization of J-acid wastewater. Background technique [0002] J acid (7-amino-4-hydroxy-2-naphthalenesulfonic acid) is an important dye intermediate, which is widely used in the manufacture of direct dyes, acid dyes and reactive dyes. The traditional preparation method of J-acid is: Tuberic acid (2-amino-1-naphthalenesulfonic acid) undergoes disulfonation reaction and trisulfonation reaction in oleum to generate 6-amino-1,3,5-naphthalenetri Sulfonic acid, followed by hydrolysis and desulfonation in sulfuric acid medium to obtain amino J acid (6-amino-1,3-naphthalene disulfonic acid), which is then made into J acid through alkali fusion and acid precipitation. The synthetic route is as follows: [0003] [0004] The "hydrolysis process" of the J acid production process discharges a large amount of strong acid wastewater (pH&l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C07C309/50C07C303/02C01D5/00
Inventor 张正富易元龙蔡运红
Owner XIANGSHUI HENRYDA TECH CHEM
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