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A method for removing cyanide and copper in the production process of cyanide dye

A dye and filter cake technology, applied in the direction of organic dyes, etc., can solve the problems of incomplete oxidation of cuprous ions, low qualified rate of dye color and light, unfavorable subsequent treatment of wastewater, etc., to improve product economy, simple copper removal process, Easy-to-control effects

Active Publication Date: 2017-06-13
ZHEJIANG LONGSHENG CHEM RES +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Under acidic conditions, sodium chlorate has strong oxidizing properties, safe and convenient operation, and a high degree of automation, but the treatment effect is greatly affected by pH, and chloride ions are highly corrosive, and have adverse effects on the subsequent treatment of wastewater.
[0008] The above-mentioned removal of cyanide and copper from the cyanide dye filter cake is carried out in different reaction kettles. During the process, the materials need to be transferred, the operation is cumbersome, and it will also lead to the loss of materials; at the same time, the oxidation of cuprous ions is not complete, and the copper removal effect Unsatisfactory, further copper removal is required for two or more times, and the pass rate of dye shade after cyanide and copper removal is not high

Method used

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  • A method for removing cyanide and copper in the production process of cyanide dye
  • A method for removing cyanide and copper in the production process of cyanide dye
  • A method for removing cyanide and copper in the production process of cyanide dye

Examples

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Effect test

Embodiment 1

[0037] Add 100g of cyanide dye CI Disperse Blue 366 [the following formula (Ⅰ-1)] crude filter cake and 200g tap water into a 500mL flask and stir for 1h, then add 20g of 20% sodium bromate solution and 10g of 50% dilute sulfuric acid. , Warm up to 45℃, keep for 4h; add 80g of 25% ammonia aqueous solution after the end of the incubation, continue to keep for 8h, filter and wash to neutral, and then add 200g of auxiliary MF for conventional commercial post-treatment (that is, pre-dispersed Then enter the sand mill or grinder for homogenization and drying to obtain the finished dye), take a sample, and test the copper content in the dye according to the method described in GB 20814-2006 to be 146ppm, which meets the limit of less than 250ppm in the finished dye Requirements, the dye shade and intensity after treatment are qualified.

[0038]

Embodiment 2

[0040] Add 100g of the cyanide dye CI Disperse Blue 366 crude filter cake and 200g of tap water into a 500mL flask and stir for 1h, add 20g of 10% sodium bromate solution and 10g of 30% dilute sulfuric acid, heat up to 45℃, keep for 4h; After the incubation, 80 g of 20% ammonia aqueous solution was added, and after the incubation was continued for 8 hours, it was filtered and washed to neutrality. The treated dye filter cake is added with 200g dispersant MF for conventional commercialization, that is, it is pre-dispersed and then entered into a sand mill or grinder for further homogenization and dried to obtain finished dyes, according to GB 20814-2006 Methods Sampling and testing the copper ion content in the finished dyestuff is 165ppm, which meets the limit requirement of the copper content in the finished dyestuff below 250ppm, and the shade and intensity of the dye cake after treatment are all qualified.

Embodiment 3

[0042] Add 100g of cyanide dye CI Disperse Blue 165 [the following formula (Ⅰ-2)] crude filter cake and 200g tap water into a 500mL flask. After stirring for 1h, add 20g of 20% sodium bromate solution and 10g of 50% dilute sulfuric acid. , The temperature was raised to 45°C, and the temperature was kept for 4 hours; after the completion of the temperature keeping, 80 g of 25% ammonia aqueous solution was added, and after keeping the temperature for 8 hours, it was filtered and washed to neutrality. The treated dye filter cake is added with 200g dispersant MF for conventional commercialization, that is, it is pre-dispersed and then entered into a sand mill or grinder for further homogenization and dried to obtain finished dyes, according to GB 20814-2006 Methods Sampling and testing the copper ion content in the finished dyestuff is 124ppm, which meets the limit requirement of the copper content in the finished dyestuff below 250ppm, and the shade and intensity of the dye cake af...

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Abstract

A method for removing cyanide and copper from cyanide dyes, comprising the steps of: (1) adding crude cyanide dye filter cakes in a reaction vessel, adding water to beat the filter cakes, beating completely, adding sodium bromate solution and stirring evenly, slowly Add sulfuric acid solution dropwise to form an acidic environment, and stir to react; (2) After the reaction in step (1), add ammonia solution or other complexing agents to the reaction pot, and stir to remove copper; The cake is washed with water to obtain a cyanide dye filter cake after removing cyanide and copper. The invention has mild reaction conditions, is easy to control, has high cyanide and copper removal efficiency, and the dye quality after cyanide and copper removal is good.

Description

[0001] (1) Technical field [0002] The invention relates to a method for removing cyanide and copper from a cyanide dye filter cake, and belongs to the technical field of dye production. [0003] (2) Background technology [0004] Cyanide dyes refer to a class of dyes with cyano groups in the dye structure. This type of dye has the characteristics of high tinting power, bright shade, large molar extinction coefficient, and good fastness, whether it is used in a single variety or mixed It has excellent performance when used. The cyanation reaction of the dye is to react a halogen-containing intermediate with cuprous cyanide or cuprous halide plus sodium cyanide in a polar inert organic solvent. After the cyanidation reaction is completed, the filter cake obtained by filtering will retain unreacted inorganic cyanide and introduced cuprous ions, which will affect the quality and application of the dye. The Chinese standard "Limits and determination of 10 heavy metal elements in dye pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B67/54C09B67/36
Inventor 何旭斌姜兴中荆钰陶建国张桂香孟明朱敬鑫
Owner ZHEJIANG LONGSHENG CHEM RES
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