Novel synthesis process of environment-friendly heavy metal vat golden orange G

A low-heavy metal, environment-friendly technology, applied in the field of dyes, can solve the problems of poor environmental performance of heavy metal content, non-conformity with national sustainable development, traditional process pollution, etc., to reduce treatment costs, high product yield, and broad development space Effect

Inactive Publication Date: 2015-01-21
安徽融创化工科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to technical limitations, products produced by traditional processes will be more restricted by the increasingly stringent "green barriers" in the world due to reasons such as heavy metal content exceeding the requirements of ETAD standards and poor environmental performance.
At the same time, due to the serious pollution of traditional crafts, it does not conform to the national sustainable development strategy, and is also very unfavorable to the future development of this product.
At present, there is no new process for reducing golden orange G. The main domestic manufacturers still use T acid as raw material to obtain the original dye through closed-loop chlorination, condensation, copper removal, and closed-loop reaction. During commercial processing, lignin is used as the raw material. Auxiliaries processed into commercial dyes

Method used

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  • Novel synthesis process of environment-friendly heavy metal vat golden orange G
  • Novel synthesis process of environment-friendly heavy metal vat golden orange G

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Chlorination reaction: in parts by weight, adding p-toluoylbenzoic acid 300kg into 100~108% oleum 800L, 200L parts of vitriol oil in 100°C for dehydration at 100°C with an acidity of 300kg was incubated for 1 hour to generate 2 -Methylanthraquinone; then under the action of 1kg of sulfur, chlorine gas was introduced at a temperature of -5°C and a pressure of 0.01MPa for reaction, and after being kept warm for 1 hour, washed and dried to obtain 1-chloro-2-methylanthraquinone;

[0025] (2) Condensation reaction: In parts by weight, add 400kg of 1-chloro-2-methylanthraquinone obtained in step (1) into the condensation pot, heat to 100°C, dehydrate for 1 hour, then add o-dichlorobenzene 30kg, 60kg of N-methylpyrrolidone, heated to 175°C to melt all the materials; slowly add 150kg of copper powder under stirring, then slowly raise the temperature to 170°C, control the pressure at 0.1MPa, keep warm for 11 hours, add 1000L of Chlorobenzene, cooled to 60°C, filtered, and wa...

Embodiment 2

[0028] (1) Chlorination reaction: in parts by weight, adding 550 kg of p-toluoylbenzoic acid into 108% fuming sulfuric acid 1500L and 700L concentrated sulfuric acid is dehydrated at 130° C. for 1.5 hours to generate 2-methyl Anthraquinone; then under the action of 5kg of sulfur, chlorine gas was introduced at a temperature of 20°C and a pressure of 0.05MPa for reaction, and after 1.5 hours of heat preservation, it was washed and dried to obtain 1-chloro-2-methylanthraquinone;

[0029] (2) Condensation reaction: In parts by weight, add 600kg of 1-chloro-2-methylanthraquinone obtained in step (1) into the condensation pot, heat to 106°C, dehydrate for 1.5 hours, then add o-dichlorobenzene 50kg, 100kg of N-methylpyrrolidone, heated to 190°C to melt all the materials; slowly add 300kg of copper powder under stirring, then slowly raise the temperature to 260°C, control the pressure at 0.25MPa, after 12 hours of heat preservation, add 1000L of Chlorobenzene, cooled to 70°C, filtere...

Embodiment 3

[0032] (1) Chlorination reaction: in parts by weight, adding 400 kg of p-toluoylbenzoic acid into 1000 L of oleum and 500 L of concentrated sulfuric acid with an acidity of 105% is dehydrated at 120° C., and is incubated for 1.3 hours to generate 2-methyl Anthraquinone; then, under the action of 3 parts of sulfur, chlorine gas was introduced at a temperature of 0°C and a pressure of 0.03 MPa to react, and after heat preservation for 1.2 hours, it was washed and dried to obtain 1-chloro-2-methylanthraquinone;

[0033](2) Condensation reaction: In parts by weight, add 500 kg of 1-chloro-2-methylanthraquinone obtained in step (1) into the condensation pot, heat to 104°C, dehydrate for 1.2 hours, then add o-dichlorobenzene 40kg, 80kg of N-methylpyrrolidone, heated to 180°C to melt all the materials; slowly add 200kg of copper powder under stirring, then slowly raise the temperature to 180°C, control the pressure at 0.2MPa, keep warm for 11.5 hours, add 1000L of Chlorobenzene, cool...

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Abstract

The invention relates to the technical field of dye, and discloses a novel synthesis process of environment-friendly heavy metal vat golden orange G. A solvent DMF closed loop mode used in a conventional process is adjusted to be a butanol and potassium hydroxide closed loop mode, and in the use process, a closed loop mother liquid is circulated and used indiscriminately, so that the environment-friendly pressure is alleviated, the environment-friendly treatment expense is reduced, and the potential safety hazard is greatly alleviated. The conventional process, namely a copper removal process that a great amount of acids and oxidants are used is adjusted into a separation mode of direct filtration, so that both the production cost is lowered, the security of product production is greatly improved, the environment-friendly pressure is alleviated, the production efficiency is improved, and the product yield is high.

Description

technical field [0001] The invention relates to the technical field of dyes, in particular to a new synthesis process of environment-friendly low heavy metal reduced golden orange G. Background technique [0002] Vat dyes are a class of high-grade dyes with many varieties, complete chromatograms and bright colors. They are mainly used for dyeing and printing of high-grade and functional products of cellulose fibers, and are famous for their excellent dyeing fastness. Since vat dyes do not contain azo groups, and as a pigment-type compound, they have no special biochemical treatment problems, so it is currently impossible to completely replace them with other dyes for industrial fabrics. Therefore, although vat dyes are complicated to manufacture, they still have strong vitality and have a good market development prospect. Due to the particularity of its production, some traditional vat dye production countries in Europe and the United States stopped dye synthesis 20 years a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B3/42D06P1/24D06P3/60D06P3/14D06P3/04
Inventor 王洪卫高鸿宇蒋大为李振徐卉香张文件
Owner 安徽融创化工科技股份有限公司
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