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Process for preparing disperse red 60

A production method and technology of disperse red, applied in the direction of amino-hydroxyanthraquinone dyes, etc., can solve the problems of shortening the condensation reaction time, lowering the condensation reaction temperature, etc., and achieve the effect of meeting the requirements of clean production, reducing consumption, and no sewage discharge

Inactive Publication Date: 2011-05-18
苏州市罗森助剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can shorten the condensation reaction time, and appropriately reduce the condensation reaction temperature, and reduce the possibility of coking of 1-amino-2-bromo-4-hydroxyanthraquinone and phenol, but this method still needs to add water after the end point of condensation. Disperse Red 60 is precipitated, and since it can only reduce the amount of phenol by 20-30%, it is still unavoidable to pollute the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 60 grams of dry product of 1-amino-2-bromo-4-hydroxyanthraquinone, 100 grams of phenol, 180 grams of nitrobenzene and 20 grams of potassium carbonate to the reaction kettle, and keep it warm for 7 to 9 hours at 155 ° C. After the end point is reached, excess phenol is removed by vacuum distillation. After the phenol is removed, it is cooled to 40°C, filtered with suction, and the mother liquor is reserved for the next batch. The filter cake was boiled with water to recover the solvent nitrobenzene. After the nitrobenzene was recovered, it was suction-filtered, drained, washed with a small amount of water, and dried to obtain 54.5 grams of a dry filter cake, which was Disperse Red 60, and the calculated yield was 89.7%.

Embodiment 2

[0027] Add 60 grams of 1-amino-2-bromo-4-hydroxyanthraquinone dry product, 100 grams of phenol, 180 grams of No. 200 solvent naphtha, and 20 grams of potassium carbonate to the reaction kettle, and keep the temperature at 155°C for 7 to 9 hours. After the measurement end point is reached, the excess phenol is removed by vacuum distillation. After the phenol is removed, it is cooled to 40°C, filtered with suction, and the mother liquor is reserved for the next batch. The filter cake was boiled with water to recover the solvent nitrobenzene. After the recovery of the nitrobenzene, it was suction-filtered, drained, washed with a small amount of water, and dried to obtain 53.8 grams of a dry filter cake, which was Disperse Red 60, and the calculated yield was 89.7%.

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Abstract

The invention relates to a producing method of disperse red 60. The producing method mainly comprises the steps that firstly, 1-anthraquinone is adopted as raw material to make 1-amino-2-bromine-4-hydroxyanthraquinone dry product; secondly, the 1-amino-2-bromine-4-hydroxyanthraquinone dry product reacts with phenol to perform condensation reaction under the existence of acid binding agent to generate 1-amino-2-phenoxy -4-hydroxyanthraquinone, in the second step, the condensation reaction is performed in inert solvent with a high boiling point, the mass ratio of the inert solvent with a high boiling point, the phenol and the 1-amino-2-bromine-4-hydroxyanthraquinone dry product is 2.5 to 3.5 : 1.7 to 1.05 : 1, the inert solvent with a high boiling point is organic solvent which is insolublein water and has a higher boiling point than that of the phenol, when the condensation reaction reaches the end, the phenol is removed through pressure reduction and distillation, 1-amino-2-phenoxy -4-hydroxyanthraquinone is separated through cooling, and the disperse red 60 is obtained through filtering. The producing method is simple, no wastewater is discharged, and the producing method can meet the requirement for clean production.

Description

technical field [0001] The invention relates to a production method of disperse red 60. Background technique [0002] The chemical name of Disperse Red 60 is 1-amino-2-phenoxy-4-hydroxyanthraquinone. The existing production method of disperse red 60 is to use 1-aminoanthraquinone as a raw material, react with bromine in a sulfuric acid medium to obtain 2,4-dibromo-1-aminoanthraquinone, and the reaction product is not separated directly in the Heat up hydrolysis in sulfuric acid to obtain 1-amino-2-bromo-4-hydroxyanthraquinone. After isolation, filtration, washing and drying, the product is condensed in a phenol medium. Add water at this temperature, then add liquid caustic soda dropwise, and finally lower the temperature to 50-52°C, filter, wash, and dry to obtain 1-amino-2-phenoxy-4-hydroxyanthraquinone, namely Disperse Red 60. However, since water will be produced during the condensation reaction in the phenol medium, and a small amount of water will also be brought into...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B1/50
Inventor 李根荣徐新连潘泉根
Owner 苏州市罗森助剂有限公司
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