Circulation applying process for mother liquor waste water of coupling reaction

A technology of coupling reaction and waste water recycling, applied in azo dyes, monoazo dyes, organic dyes, etc., can solve problems such as environmental hazards, achieve the effect of improving yield, obvious economic benefits, and solving problems of treatment and discharge

Inactive Publication Date: 2013-01-30
汤宝祥
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disposing of this waste water very economically is a challenge and discharging it is harmful to the environment

Method used

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  • Circulation applying process for mother liquor waste water of coupling reaction
  • Circulation applying process for mother liquor waste water of coupling reaction
  • Circulation applying process for mother liquor waste water of coupling reaction

Examples

Experimental program
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Effect test

example 1

[0014] Example 1: Synthesis of Acid Mordant Brown RH (C.I.Mordant.Brown33):

[0015] (1) Prepare five parts of a 40ml volume containing 0.02172mol p-nitro-o-aminophenol sodium diazonium salt suspension, and set aside;

[0016] (2) 5.6800 g of sodium 2,4 diaminobenzenesulfonate (80.25%), dissolved in 80 ml of water, mixed with a portion of the above-mentioned diazonium salt, adjusted to PH with soda ash, heated and maintained at 50°C, and coupled Salt out after reaching the end point, filter out the acid medium brown RH dye filter cake and dry;

[0017] (3) Replace 80ml of water in step (2) with 80ml of coupling mother liquor, and keep other conditions unchanged, repeat the above coupling reaction, and the experimental results are listed in Table (1).

[0018] Table (1) Experimental results of acid medium brown RH

[0019] Experiment sequence

example 2

[0020] Example 2: Synthesis of Disperse Orange F-3R (C.I.Dis.Orange25):

[0021] (1) Prepare four parts of a suspension containing 0.020mol p-nitroaniline diazonium salt with a volume of 15ml, and set aside;

[0022] (2) 3.5340 grams of N-ethyl-N-cyanoethylaniline (98.5%), 30ml of water, 1.85ml of concentrated HCL, after beating for 1.5 hours, cool in an ice bath to a temperature below 10°C, and keep the subsequent reaction at this temperature Within the range, drop a portion of the p-nitroaniline diazonium salt suspension prepared in step (1), adjust the acidity and alkalinity with soda ash, keep the pH around 3.5, filter after the coupling reaction is completed, and obtain the dispersed orange F-3R 14.3 grams of wet filter cake, 30 ml of mother liquor, and the Disperse Orange F-3R wet filter cake was further washed to neutrality and then dried;

[0023] (3) Replace 30ml of water in step (2) with 60ml of coupling mother liquor, and keep other conditions unchanged, repeat the...

example 3

[0026] Example three: the synthesis of acid orange II (C.I.Acid.Orange7):

[0027] (1) Prepare five parts of 32ml suspension containing 0.0200mol diazonium sulfanilate, and set aside;

[0028] (2) Prepare five parts of β-naphthol solution for subsequent use: 2.9087 (99.8%) gram of β-naphthol, 2.6mlNaOH (35%), 7.5ml water, stirring and dissolving into solution;

[0029] (3) Take 40ml of water, add β-naphthol solution and p-aminobenzenesulfonic acid diazonium salt suspension alternately under stirring, keep the temperature below 10°C in an ice bath, add soda ash to keep the pH between 8.5-9.0, After the β-naphthol solution and the diazonium salt suspension of p-aminobenzenesulfonic acid are all dripped, continue the reaction until the coupling end point, salt out and filter out the acid orange II dye filter cake;

[0030] (4) Replace 40ml of water in step (3) with 75ml coupling mother liquor, other conditions are unchanged, repeat above-mentioned coupling reaction, experimental...

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Abstract

The invention relates to a circulation applying process for mother liquor waste water of a coupling reaction. A diazonium salt solution or a suspension is subjected to the coupling reaction with dissolved or beat coupling components, during a reaction process, a reaction temperature is controlled through cooling, liquidity is regulated through adding water, the PH is kept to be in a suitable range through adding acid or alkali, after the coupling is ended, the mother liquor is subjected to salting out and filter pressing to extract dye filter cake, most of the mother liquor waste water returns to a previous coupling reaction process for recycling, the mother liquor waste water further returns to a coupling component dissolving or beating process for recycling on the premise that the mother liquor waste water has proper dissolubility or is suitable for beating, and residual mother liquor waste water is discharged after conventional treatment. According to the process, consumption of auxiliary raw materials such as acid, alkali and salt is reduced, the dye yield is improved partially, waste water discharge volume is reduced, and the dual purposes of environment protection and economic performance improvement are achieved simultaneously.

Description

Technical field: [0001] The patent of the present invention relates to a waste water discharge reduction process, in particular to a coupling reaction mother liquid waste water recycling process. Background technique: [0002] The diazo coupling reaction is the most important basic reaction for the synthesis of dyes and coatings. Based on this, a series of mature processes for the synthesis of dyes and coatings have been developed. For example, the synthesis process of Weak Acid Yellow S (C.I.Acid Yellow65): [0003] (1) will 2 / -(p-aminoanilino)-5 / - After 6.02 grams of nitrobenzenesulfonic acid (92%), 0.875 grams of NaOH (96%), and 60 ml of water were stirred and dissolved, 6 ml of HCL (35%) was added, and an appropriate amount of ice was added to cool down to 5-10°C, and then reacted Always maintain the temperature in this range, drop by NaN0 2 (99%) 1.4219 gram and the solution that 5 milliliters of water are made into, continue to stir and insulate until the diazon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B29/085C09B29/15C09B62/085
Inventor 汤宝祥
Owner 汤宝祥
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