After-treatment clean process for purifying vat blue 66 dye

A dye and cleaning technology, applied in the direction of organic dyes, inorganic chemistry, sulfur compounds, etc., can solve problems that cannot be completely treated, and achieve the effect of reducing the amount of waste acid

Inactive Publication Date: 2015-02-11
上海华元实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above purification, about 12 tons of sulfuric acid with a concentration of about 95% is consumed per ton of vat blue 66 crude product, and about 25 tons of 45% waste acid is produced, which contains unreacted raw materials, impurities of unknown structure and a small amount of products, which cannot be completely cured at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] 10 grams of the crude product of Vat Blue 66 (through a 300-mesh sieve), add 132 grams of sulfuric acid concentrate (concentration 75% by weight) under stirring, heat up to 90°C, keep warm for 4 hours, cool to 50°C, stir for 6 hours and filter, filter cake Wash with 60 grams of concentrated sulfuric acid of 75% by weight or 75% by weight of sulfuric acid, add 300 grams of water to the filter cake for beating, heat up to 80°C, stir for 0.5 hours, filter, and the filtrate is to be diluted; the filter cake is washed to neutral, Dry at 90°C to obtain 8.5 g of vat blue 66 dye bright blue powder. Compared with the standard, the intensity is 107.13%; the brightness difference (DC) is 0.64.

[0010] Dilute the above-mentioned filtrate with water under stirring to a concentration of 25-30% by weight, filter, add a decolorizer to the filtrate, heat up to 90°C, keep warm for 1-2 hours, filter, and distill the filtrate to collect fractions at 170-180°C to obtain a concentration of ...

Embodiment 2

[0012] 10 grams of vat blue 66 crude product (crossing 300 mesh sieve), add 140 grams of sulfuric acid concentrate (concentration 70% by weight) under stirring, be warming up to 70 ℃, keep warm for 6 hours, cool to 50 ℃, stir for 8 hours, filter, filter The cake is washed with 60 grams of sulfuric acid concentrate of 70% by weight or 70% by weight of sulfuric acid, and the filter cake is beaten with 300 grams of water, heated to 80°C, stirred for 1 hour, filtered, and the filtrate is to be diluted; the filter cake is washed to neutral, Dry at 90°C to obtain 8.4 g of vat blue 66 dye bright blue powder. Compared with the standard, the strength is 101.5%; the brightness difference (DC) is 0.28.

[0013] Dilute the above-mentioned filtrate with water under stirring to a concentration of 25-30% by weight, filter, add a decolorizer to the filtrate, heat up to 90°C, keep warm for 1-2 hours, filter, and distill the filtrate to collect fractions at 170-180°C to obtain a concentration o...

Embodiment 3

[0015] 10 grams of reduction blue 66 crude product (crossing 300 mesh sieves), add 135 grams of sulfuric acid concentrate (concentration 73% by weight) under stirring, be warming up to 80 ℃, keep warm for 4 hours, cool to 50 ℃, stir for 8 hours, filter, filter The cake is washed with 60 grams of sulfuric acid concentrated solution with a concentration of 73% by weight or sulfuric acid with a concentration of 73% by weight, and the filter cake is beaten with 300 grams of water, heated to 80°C, stirred for 1 hour, filtered, and the filtrate is to be diluted; the filter cake is washed with water until neutral , and dried at 90°C to obtain 8.6 g of vat blue 66 dye bright blue powder. Compared with the standard, the strength is 106.1%; the brightness difference (DC) is 0.54.

[0016] Dilute the above-mentioned filtrate with water under stirring to a concentration of 25-30% by weight, filter, add a decolorizer to the filtrate, heat up to 90°C, keep warm for 1-2 hours, filter, and di...

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PUM

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Abstract

The invention relates to an after-treatment clean process for purifying vat blue 66 dye. The clean process comprises the steps: levigating a vat blue 66 crude product, filtering the levigated vat blue 66 by adopting a 300-mesh sieve, adding he filtered vat blue 66 in a sulfuric acid concentrated solution, wherein the weight ratio of the vat blue 66 crude product and the sulfuric acid concentrated solution is 1: (13-15), and the concentration of the sulfuric acid concentrated solution is 70 to 75 percent by weight; heating the mixed solution to 70 to 90 DEG C, stirring and insulating the mixed solution for 4 to 6 hours, when the vat blue 66 crude product is stirred and insulated in the sulfuric acid concentrated solution, the color of the mixed solution is turned from dark blue to olivine, cooling the mixed solution to the temperature of 50 DEG C after the mixed solution is thermally insulated, stirring the mixed solution for 4 to 8 hours, filtering the mixed solution, washing filter cake by utilizing the70% to 75% sulfuric acid concentrated solution or the sulfuric acid solution which is identical in the concentration, adding water to the filter cake, pulping the filter cake, heating the pulp to the temperature of 80 DEG C, preserving the pump for 0.5 to 1 hour, and drying the filter cake at the temperature of 90 DEG C to obtain a vat blue 66 dye dry product. The sulfuric acid concentrated solution with the concentration of 70 to 75 percent is obtained by after-processing the sulfuric acid concentrated mother solution obtained by purifying the vat blue 66. The invention provides the after-treatment clean production process of the vat blue 66.

Description

technical field [0001] The invention relates to a post-treatment cleaning process for purifying vat blue 66 dye, and belongs to the technical field of dye production. Background technique [0002] Vat blue 66 (CAS: 32220-82-9) is a high-quality blue vat dye, and its purification method has been reported in literature, see CN1737063. That is, the crude product of Vat Blue 66 is completely dissolved in concentrated sulfuric acid, diluted with water, and the acidity is controlled at 40% to 50% by weight, then cooled, crystallized, and dried to obtain high-purity Vat Blue 66 dye. In the above purification, about 12 tons of sulfuric acid with a concentration of about 95% is consumed per ton of vat blue 66 crude product, and about 25 tons of 45% waste acid is produced, which contains unreacted raw materials, impurities of unknown structure and a small amount of products, which cannot be completely cured at present. Contents of the invention [0003] The purpose of the present ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/10C09B67/54C01B17/88C01B17/90
Inventor 丁国跃何可立
Owner 上海华元实业有限公司
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