Novel method for post-processing vat yellow GCN

A new method and crude technology, applied in the field of dyes, can solve problems such as inability to completely control

Inactive Publication Date: 2014-02-19
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

The waste acid contains organic substances such as naphthalenesulfonic acid and be

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 17.5 grams of vat yellow GCN crude product (intensity compared with the standard is 90.27%; brightness difference (DC) is 3.38) into 175 grams of tetrachloroethylene, stir and heat to 120 ° C, reflux for 6 hours, cool to room temperature and filter. The filter cake was washed three times with 33 grams of tetrachlorethylene, and sucked dry. Add 99 grams of water to the above-mentioned naphthalene-free filter cake for beating, add 34 grams of 30% hydrochloric acid and 0.45 grams of sodium chlorate, slowly heat to 80 ° C under stirring, and keep warm for 2 hours. Filter while it is hot, wash the filter cake until neutral drying, and obtain 10 grams of pretreated reduced yellow GCN dry product. Add 185 grams of concentrated sulfuric acid solution with a concentration of 50% by weight to the above-mentioned dry product, stir and heat up to 150°C for 2 hours, then take a sample, observe with a microscope, if the crystal becomes transparent, the end point of the crystal tr...

Embodiment 2

[0021] Take 10 grams of the above pretreated vat yellow GCN dry product, add 205 grams of sulfuric acid concentrated solution with a concentration of 50% by weight, stir and heat up to 140 ° C for 3 hours, then take a sample, observe with a microscope, if the crystal becomes transparent, it means the end point of crystal transformation To, down to room temperature, add 77 grams of water to isolate the material, the material is suction filtered, and the mother liquor is collected. Subsequent operations were the same as above to obtain 9.8 grams of reduced yellow GCN dry product. Compared with the standard, the intensity is 216.87%, and the brightness difference (DC) is 0.61.

Embodiment 3

[0023] Take 10 grams of the above-mentioned pretreated vat yellow GCN dry product, add 225 grams of sulfuric acid concentrated solution with a concentration of 50% by weight, stir and heat up to 130 ° C for 4 hours, then take a sample, observe with a microscope, if the crystal becomes transparent, it means the end point of crystal transformation To, down to room temperature, add 57 grams of water to isolate the material, the material is suction filtered, and the mother liquor is collected. Subsequent operations were the same as above to obtain 9.5 grams of reduced yellow GCN dry product. Compared with the standard, the strength is 204.85%, and the brightness difference (DC) is 0.68.

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PUM

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Abstract

The invention provides a novel method for post-processing vat yellow GCN to greatly reduce the amount of waste acid. A crude product of vat yellow GCN is added into a solvent tetrachloroethylene, stirred, heated to 120 DEG C, subjected to a backflow reaction for 6 hours, cooled to the room temperature and then filtered, and the residue naphthaline in a filter cake is cleaned in multiple times by using rationed tetrachloroethylene; the filter cake in which the naphthaline is removed is added into a hydrochloric acid solution to remove copper, stirred, added with sodium chlorate, heated to 70-90 DEG C, thermally insulated for 2 hours, filtered while being hot, washed to neutral state and dried, the pre-processed vat yellow GCN dry product is added into a sulfuric acid concentrated solution, stirred, heated to 130-150 DEG C and reacted for 2-4 hours, a sample is taken and observed by using a microscope, if a crystal becomes transparent, then the crystal transformation is completed, the mixture is cooled to the room temperature, added with water to separate the material and filtered in a suction manner, the filter cake is washed with water to the neutral state, reacts in a sodium hypochlorite solution again at 70-80 DEG C for 2 hours and filtered, and the filter cake is washed to the neutral state and dried to obtain the vat yellow GCN dry product.

Description

technical field [0001] The invention belongs to the technical field of dyes, and in particular relates to a new post-treatment method for vat yellow GCN (vat.yellow2; CAS: 129-09). Background technique [0002] Vat Yellow GCN is a yellow dye with good levelness and particularly bright color. In the patent data, there are several synthetic routes. The prior art is based on the method of German IG Farben Dyestuff Industry Co., Ltd. (I.G., Frankfurt am Main, Germany). For relevant documents, see BIOS987, 59; FIAT1313, 2, 61; GB322184. That is, in molten naphthalene, copper chloride is used as a catalyst and a mixture of 2,6-diaminoanthraquinone, trichlorotoluene and sulfur is co-heated at 180-224 ° C to obtain a crude product of vat yellow GCN. The crude product was purified by treatment with concentrated sulfuric acid and alkaline sodium hypochlorite. The crude product of vat yellow GCN is reacted in 98% sulfuric acid at 80°C for 2 hours, diluted in clean water, the acidity...

Claims

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Application Information

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IPC IPC(8): C09B67/28C09B67/54
Inventor 何可立丁国跃
Owner 上海华元实业有限公司
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