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Clean production technique for dye synthesis

A clean production and process technology, applied in the direction of azo dyes, organic dyes, reactive dyes, etc., to achieve the effect of improving utilization rate, completely cleaning production process, and reducing raw material cost

Active Publication Date: 2015-07-15
ZHEJIANG YIDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

No one has proposed a completely clean production process so far, so it is urgent to develop a clean production process for this condensation reaction

Method used

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  • Clean production technique for dye synthesis
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  • Clean production technique for dye synthesis

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: reactive blue 5 chromatic base synthetic techniques

[0017] Step 1: Start stirring, add 58.5g of 2,4-diaminobenzenesulfonic acid to 200g of water in a 500ml three-necked flask, adjust the pH to 8.0 with 2g of soda ash, add 84g of bromic acid, heat up to 70°C with a water bath, and add 50g Baking soda, after stirring for 10 minutes, slowly add 1g of copper powder and 2g of cuprous chloride, keep warm at 70°C for 50 hours, use liquid chromatography to detect the end point, and the bromine ≤ 3.0% is the reaction end point;

[0018]

[0019] Step 2: Add the reacted condensate to 200g of normal temperature water for dilution, then add 50g of sodium chloride for salting out after dilution, and filter to obtain 110g of the condensate used, with a purity (HPLC) of 96% and a molar yield of 89% (calculated as bromic acid), collect waste water;

[0020] Step 3: Pour 370g of waste water (the bromide ion concentration is 4.1% as determined by silver nitrate) into ...

Embodiment 2

[0024] Embodiment 2: Reactive blue 19 chromogen synthetic techniques

[0025] Step 1: Start stirring, add 48g m-(β-hydroxyethylsulfone) aniline to 200g water in a 500ml three-necked flask, adjust the pH to 8.0 with 1g soda ash, then add 84g bromonic acid in a water bath to raise the temperature to 60°C, then Add 50g of baking soda, stir for 10 minutes, then slowly add 1g of copper powder and 2g of cuprous chloride, keep warm at 70°C for 22 hours, use liquid chromatography to detect the end point, and the bromine ≤ 5.0% is the reaction end point;

[0026]

[0027] Step 2: Then directly filter the reacted condensate to obtain 115 g of the condensate used, the purity (HPLC) is 92%, and the molar yield is 91% (calculated as bromic acid), and the waste water is recovered;

[0028] Step 3: Pour 170g of waste water (the bromide ion concentration is 8.3% as determined by silver nitrate) into a dedicated bromine recovery device, inject 10g of 30% hydrogen peroxide, and recover 12.9g...

Embodiment 3

[0032] Embodiment 3: Acid blue 324 synthesis technique

[0033] Step 1: Start stirring, add 50g of m-aminoacetanilide to 200g of water in a 500ml three-necked flask, adjust the pH to 8.0 with 4g of soda ash, then add 84g of bromic acid in a water bath and raise the temperature to 80°C, then add 50g of baking soda, and stir for 10 Minutes later, slowly add 1g of copper powder and 2g of cuprous chloride, keep warm at 70°C for 10 hours, and use liquid chromatography to detect the end point.

[0034]

[0035] Step 2: Then add the reacted condensate to 300g of normal temperature water for dilution, and then add 40g of sodium chloride for salting out after dilution to obtain 103g of the condensate used, with a purity (HPLC) of 96.5% and a molar yield of 88.6% (calculated as bromic acid), and recycle waste water;

[0036] Step 3: Pour 465g of waste water (the bromide ion concentration is 3.32% as determined by silver nitrate) into a dedicated bromine recovery device, inject 7g of...

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Abstract

The invention relates to a clean production technique for dye synthesis. The clean production technique comprises the following steps: obtaining filter liquor after a condensation reaction shown in the following chemical equation is ended; adding an oxidizing agent into the filter liquor to recycle bromine; regulating the pH of the wastewater to 7.0-9.0 after bromine is recycled, then putting the wastewater into a nanofiltration membrane system or a multiple-effect evaporation and concentration system for desalination; ending desalination when the mass percentage of chloride ions in the wastewater is not higher than 5%, and then continuing to concentrate the wastewater until the amino value is not smaller than 10%, wherein the concentrated wastewater is applied to the condensation reaction shown in the chemical equation: in the formula (1), R1, R2, R3, R4 and R5 respectively independently represent -H, -SO3M, -NH2, -NHCOCH3, -SO2CH2CH2OH, -CH3, -OCH3, -CH2CH3 or -OCH2CH3, and M represents hydrogen or alkali metal. The clean production technique disclosed by the invention can be used for solving the wastewater pollution problem caused by condensation reaction, realizing clean production, and improving the raw material utilization rate in dye synthesis and production.

Description

technical field [0001] The invention relates to a clean production process for dye synthesis, in particular to a comprehensive utilization process for waste water after the condensation reaction of bromic acid and aromatic amine in the dye production industry. Background technique [0002] Bromonic acid and aromatic amine are the starting materials, water is the reaction medium, baking soda is the reaction acid-binding agent, copper powder and cuprous chloride are used as the catalyst, the reaction temperature is 60-80°C, and the reaction time is 10-50 hours , after solid-liquid separation such as salting out or direct filtration, the target condensate is obtained. This condensation reaction is a very common reaction type in dye synthesis, such as reactive blue 5, reactive blue 19, reactive blue 49, reactive blue 74, acid blue 25. This reaction is involved in the production process of acid blue 40, acid blue 129, acid blue 145, acid blue 324 and other products. [0003] Thi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B62/505C09B62/80
Inventor 秦杰锋孟胜锋康定潘克存李玲
Owner ZHEJIANG YIDE CHEM