Method for producing reductive direct black BCN raw dye

A direct dye technology, applied in the field of dyes, can solve the problems of unfavorable environmental protection, high toxicity, strong irritation, etc., and achieve the effects of improving dye shade and application performance, good economic and social benefits, and good health

Active Publication Date: 2014-05-07
江苏嘉利精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] There are following problems in the original process route: (1) synthetic problem of brominated violinanthrone: the traditional technique of BO bromination is carried out in concentrated sulfuric acid, chlorosulfonic acid or nitrobenzene
Because nitrobenzene is highly toxic, carcinogenic and scurvy, it has been gradually eliminated; when concentrated sulfuric acid encounters a large amount of heat, it can cause boiling splashes, and combustibles (such as benzene) and combustibles (such as sugar, cellulose, etc.) Contact will cause violent reaction, and even cause combustion; chlorosulfonic acid is combustion-supporting, highly corrosive and irritating, and needs to be decomposed with a large amount of sulfuric acid at the end of the reaction, resulting in a large amount of sulfuric acid and hydrochloric acid, which is quite unfavorable to environmental protection
(2) Condensation of brominated violanthrone and 1-aminoanthraquinone: the traditional process is completed in nitrobenzene
This reaction is not only toxic, but also energy-intensive
(3) The problem of heavy metal content: the traditional process does not undergo acidification to remove copper, but only boils, and the copper content exceeds the ETAD limit standard

Method used

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  • Method for producing reductive direct black BCN raw dye
  • Method for producing reductive direct black BCN raw dye
  • Method for producing reductive direct black BCN raw dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 210g of water into a 250mL three-necked flask (installed with a thermometer and a reflux condenser, which is filled with frozen brine, with an exhaust pipe and an exhaust gas absorption device attached to remove the generated HBr and other acidic gases), start stirring, and add reduced dark blue BO 15g, beat for 2 hours, add 4.5g of sodium chlorate, 10.5g of bromine, heat up to 70-100°C, and stir at 70-100°C for 5 hours. Recover bromine by distillation, lower the temperature to 50°C, filter, wash until neutral, and dry to obtain violinanthrone bromide. The yield is 130% based on violinthone. The bromine content of the product was detected to be 25.89% (26.1% in theory). The product is dyed cotton in red light navy blue.

Embodiment 2

[0033] Add 350g of water to a 500mL three-necked flask (installed with a thermometer, a reflux condenser, and refrigerated brine into the condenser, with an exhaust pipe and an exhaust gas absorption device attached to remove the generated HBr and other acidic gases), start stirring, and add 25g of BO The filter cake was beaten for 2 hours, 7.5g of sodium chlorate and 17.5g of bromine were added, the temperature was raised to 70-100°C, and the mixture was stirred at 70-100°C for 6 hours. Bromine was recovered by distillation, and the temperature was lowered to 50°C. Filtrate, wash until neutral, and dry to obtain violinanthrone bromide, with a yield of 132% based on violinthrone. The bromine content of the product was detected to be 26.32% (theoretical 26.1%). The product is dyed cotton in red light navy blue.

Embodiment 3

[0035] Using solid phase reaction, add 15g of violinanthrone bromide obtained in Example 1, 13g of 1-aminoanthraquinone, 8g of soda ash, 1g of copper oxide, mix and stir for half an hour, raise the temperature to 120-130°C, dehydrate for 1 hour, continue Raise the temperature to 230-260°C and keep it warm for 5 hours. The temperature was lowered to below 60° C., and the material was discharged to obtain 38 g of crude dye.

[0036] The obtained crude product was added to 600 mL of water, boiled for 1 hour, cooled, filtered, washed until neutral, and dried to obtain 28 g of dry product.

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Abstract

A method for producing reductive direct black BCN raw dye comprises the following steps: a. brominating BO (bromine) in a non-organic solvent and a non-inorganic acid to obtain purple anthrone bromide; b. performing solid phase reaction, and performing condensation reaction on the purple anthrone bromide and 1-amino anthraquinone under the action of a catalyst and an acid binding agent to obtain a crude reductive direct black BCN dye; and c. acidifying the crude reductive direct black BCN dye and removing impurities to obtain the reductive direct black BCN raw dye. The method has the advantages as follows: firstly, in the BO brominating process, any organic solvent or any inorganic acid is not used, only an oxidant is added into water, and the bromination speed is high; secondly, the condensation reaction does not need any solvent and can be finished by heating in a solid phase container, so that the condensation reaction is very safe and environment-friendly; and thirdly, after the crude dye is acidified and copper is removed, the heavy metal content meets an ETAD requirement.

Description

technical field [0001] The invention belongs to the technical field of dyes, and relates to a preparation method of anthraquinone vat dyes, in particular to a production method of reduced direct black BCN. Background technique [0002] With the continuous improvement of people's living standards, the requirements for clothing have also changed from the previous durability to safety, environmental protection, comfort, and beauty; the requirements for dyes are also getting higher and higher. Vat dyes have become the first choice for fashion because they are suitable for dyeing natural cellulose fibers (silk, cotton), and are safe and environmentally friendly. [0003] Black vat dyes are the most important and the most used species of vat dyes, among which the most important black species - vat direct black RB (CASNo.1328-25-2) [0004] [0005] Reduced direct black RB is used for dyeing cotton fibers. It has good level dyeing and affinity, and can be directly dyed black. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B3/30D06P1/24D06P3/62
Inventor 李振奎许崇礼闫德俊项德芝尚庆合窦艳杜辉李剑傅萍王昌敬
Owner 江苏嘉利精细化工有限公司
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