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Dispersion red 146 condensation process improvement

A process improvement and disperse red technology, which is applied in the direction of amino-hydroxy anthraquinone dyes, etc., can solve the problems of long condensation reaction time, large product quality fluctuations, unfavorable condensation reaction, etc., and achieve shortened condensation reaction time, energy saving, and economic benefits obvious effect

Inactive Publication Date: 2008-01-30
JIANGSU YABANG DYE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since water is produced during the condensation reaction, a small amount of water will also be brought into the raw materials, which is not conducive to the condensation reaction, resulting in a longer condensation reaction time, which generally takes 6 to 7 hours, and the usual condensation temperature is 150 ~165°C, 1-amino-2-bromo-4-hydroxyanthraquinone and p-hydroxyanisole will be coked at this temperature for a long time, resulting in high tar content in the final product, large fluctuations in product quality, and single The one-step condensation yield is only about 80%, and the production cost is relatively high

Method used

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  • Dispersion red 146 condensation process improvement
  • Dispersion red 146 condensation process improvement
  • Dispersion red 146 condensation process improvement

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add nitrobenzene 1500kg, chlorobenzene 500kg, 1-amino-2-bromo-4-hydroxyanthraquinone wet product filter cake to dry 450kg in the 3000L enamel kettle, heat up azeotropic dehydration, after the distillate separates the water layer, The solvent automatically flows back into the reaction kettle. After the distillate is anhydrous, add 180kg of p-hydroxyanisole, 100kg of acid-binding agent potassium hydroxide, and 50kg of catalyst tetrabutylammonium bromide. After the addition, the temperature is raised to 140~ 145°C, and keep it for 3 hours for condensation at this temperature. After the distillate is collected and separated during the heating and heat preservation process, the solvent is directly used for the next batch of condensation. After the end point is detected, the temperature is lowered to 75-80°C, and then the Transfer the material into a 5000L segregation tank, slowly add 1500kg of methanol dropwise at this temperature for about two hours, then cool down to below ...

Embodiment 2

[0025] Add 1500kg of nitrobenzene, 500kg of xylene, 1-amino-2-bromo-4-hydroxyanthraquinone wet product filter cake to 450kg in a 3000L enamel kettle, heat up and azeotropically dehydrate, and the distillate is separated from the water layer. The solvent automatically flows back into the reaction kettle. After the distillate is anhydrous, add 180kg of p-hydroxyanisole, 100kg of acid-binding agent potassium hydroxide, and 50kg of catalyst tetrabutylammonium bromide. After the addition, the temperature is raised to 140~ 145°C, and keep it for 3 hours for condensation at this temperature. After the distillate is collected and separated during the heating and heat preservation process, the solvent is directly used for the next batch of condensation. After the end point is detected, the temperature is lowered to 75-80°C, and then the Transfer the material into a 5000L segregation tank, slowly add 1500kg of methanol dropwise at this temperature for about two hours, then cool down to b...

Embodiment 3

[0027] Add 1800kg o-dichlorobenzene, 500kg chlorobenzene, 1-amino-2-bromo-4-hydroxyanthraquinone wet filter cake to 450kg in a 3000L enamel kettle, heat up azeotropic dehydration, and separate the distillate into the water layer , the solvent automatically flows back into the reactor, and after the distillate is anhydrous, 180kg of p-hydroxyanisole, 100kg of acid-binding agent potassium hydroxide, and 50kg of catalyst tetrabutylammonium bromide are added, and the temperature is raised to 140 within 3 hours after the addition. ~145°C, and keep it for 4 hours for condensation at this temperature. After the distillate is collected and stratified during the heating and holding process, the solvent is directly used for the next batch of condensation. After the end point is detected, the temperature is lowered to 75-80°C, and then Transfer the material into a 500L segregation kettle, slowly add 1500kg of methanol dropwise at this temperature for about two hours, then lower the temper...

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Abstract

The invention relates to an improved condensation process of disperse red 146. 1-amino-anthraquinone is taken as raw material, 1-amino-2-bromo-4-hydroxyanthraquinone is obtained by bromination and hydrolysis in sulfuric acid solution; the 1-amino-2-bromo-4-hydroxyanthraquinone is condensed with phydroxy phenol in mixed solvent medium, with the existing of acid binding agent and catalyst, and the temperature reduces to 75-80 DEG C after reaching the end point and methanol is dripped with controlling the temperature, and the segregation is done, the temperature is reduced under 50 DEG C after the segregation; the disperse red 146 is produced after standing, filtering and then the filter cake is cleaned by methanol and hot water. The invention is characterized in that: the 1-amino-2-bromo-4-hydroxyanthraquinone used in the condensation is wet cake added with the mixed solvent medium as well as the catalyst. By applying 1-amino-2-bromo-4-hydroxyanthraquinone wet cake directly, drying process is saved and operation is simplified, thereby reducing equipment investment and improving operation environment and reducing labor intensity; besides, the method also improves reaction yield and product quality and the economic benefit is very obvious.

Description

technical field [0001] The invention relates to an improved condensation process of disperse red 146. More specifically, it is the improvement of the condensation process in the existing production method of disperse red 146. Background technique [0002] Disperse Red 146 is also known as Disperse Red SE-BL, Disperse Red E-BS, Disperse Red E-BL, etc., and its chemical name is 1-amino-2-(p-methoxy)phenoxy-4-hydroxyanthraquinone. A dye for polyester and its blended fabrics with excellent performance. The existing production method uses 1-aminoanthraquinone as a raw material to react with bromine in a sulfuric acid medium to obtain 2,4-dibromo-1-aminoanthraquinone, and the reaction product is directly heated and hydrolyzed in sulfuric acid without separation to obtain 1-Amino-2-bromo-4-hydroxyanthraquinone, after isolation, filtration, washing and drying, the product is condensed with p-hydroxyanisole in a nitrobenzene medium, and after reaching the end point, the temperature...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/50
Inventor 吴新民王继昌付亮
Owner JIANGSU YABANG DYE
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