Method for preparing disperse red 60

A technology of disperse red and weight percentage, applied in the direction of amino-hydroxyanthraquinone dyes, etc., can solve the problems of inability to change environmental pollution, low yield, consumption of steam, etc., achieve obvious economic and environmental benefits, and reduce the loss of phenol , the effect of reducing the operation process

Active Publication Date: 2008-05-21
浙江长征化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phenol is usually recovered from the filtered condensation mother liquor in water by vacuum distillation, but the distillation residue obtained after recovery still contains phenol, disperse red 60, potassium bromide, etc., the product yield is low, and the consumption of phenol is large. Complex, high energy consumption, single-step condensation yield is only about 85-88%, high production cost, and great environmental pollution
There is also the addition of methanol for separation after the condensation reaction is over. Although the product quality has improved, the yield is still low because the condensation reaction itself has not been improved, and the unit consumption of phenol is still high. At the same time, the boiling point of methanol is too low and it is flammable. Explosive and dangerous goods, serious safety hazards during use
There is also the use of ethylene glycol monomethyl ether instead of metha

Method used

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  • Method for preparing disperse red 60
  • Method for preparing disperse red 60
  • Method for preparing disperse red 60

Examples

Experimental program
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Effect test

Example Embodiment

[0021] Example 1: The 4M 3 Condensation mother liquor water was pumped into a 6300L enamel kettle, stirring was turned on, and 60kg of 98% sulfuric acid and 50kg of sodium sulfate were slowly added. After the addition, stir for half an hour, and then separate into layers. The upper layer is a solution containing phenol and disperse red 60 dissolved in phenol, and the lower layer is a potassium bromide solution. The upper layer solution is added with alkali to adjust the pH to 6-9, which is the mother liquor water after treatment. In a 5000L enamel reactor, add 700kg of the above-prepared treated mother liquor water, 300kg of phenol, 500kg of 1-amino-2-bromo-4-hydroxyanthraquinone dry product and 180kg of acid binding agent potassium carbonate, and the addition ends in 2 hours. Raise the temperature to 148-150℃, and keep the temperature for 5-6 hours. After the detection reaches the end, the temperature is reduced to 90-105℃. At this temperature, 1000kg of 3-5% light alkali water i...

Example Embodiment

[0022] Example 2: The 4M 3 The condensed mother liquor water was pumped into a 6300L enamel kettle, stirring was turned on, and 250 kg of 50% waste sulfuric acid and 90 kg of sodium chloride were slowly added. The following process steps were the same as in Example 1. In a 5000L enamel reactor, add 600kg of the above-prepared treated mother liquor water, 400kg of phenol, 500kg of 1-amino-2-bromo-4-hydroxyanthraquinone dry product, and 180kg of acid binding agent potassium carbonate. The following process steps are the same. example 1. That is, 513 kg of Disperse Red 60% off and dried, the yield is 98.6%, and the content is 99.7%. The unit consumption of phenol per ton of Disperse Red 60 is 477kg.

Example Embodiment

[0023] Example 3: The 4M 3 The condensed mother liquor water was pumped into a 6300L enamel kettle, the stirring was turned on, and 240 kg of 25% sulfuric acid and 200 kg of sodium sulfate were slowly added. The following process steps are the same as in Example 1. In a 5000L enamel reactor, add 900kg of the above-prepared treated mother liquor water, 200kg of phenol, 500kg of 1-amino-2-bromo-4-hydroxyanthraquinone dry product, and 180kg of acid binding agent potassium carbonate. The following process steps are the same. example 1. That is, 518 kg of Disperse Red 60% off and dried, the yield is 99.5%, and the content is 99.2%. The unit consumption of phenol per ton of Disperse Red 60 is 410kg.

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Abstract

A method for preparing disperse red 60, which belongs to the technical field of manufacturing chemical dyes and chemicals, and uses 1-aminoanthraquinone as a raw material to obtain 1-amino-2-bromo-4-hydroxyanthracene through bromination and hydrolysis in a sulfuric acid medium Quinone, characterized in that 1-amino-2-bromo-4-hydroxyanthraquinone undergoes condensation reaction in the presence of treated mother liquor water, phenol, and acid-binding agent to obtain Disperse Red 60; said treated mother liquor water is 1-amino- After the condensation reaction of 2-bromo-4-hydroxyanthraquinone, the condensation mother liquid water obtained by filtering is adjusted to acidity by adding acid, and acidified by adding sulfate or hydrochloride, and standing for more than half an hour, the upper layer is containing phenol and The solution of disperse red 60 dissolved in phenol, after adding alkali to adjust the pH to 6-9, is the treated mother liquor water, and the addition amount is 20% by weight of 1-amino-2-bromo-4-hydroxyanthraquinone ~200%. The invention can effectively reduce the unit consumption of phenol, increase product yield, reduce production cost and reduce environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of disperse red 60, which belongs to the technical field of manufacturing chemical dyes and chemicals. 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 mainly to use 1-aminoanthraquinone as a raw material, and react with bromine in a sulfuric acid medium to prepare Obtain 2,4-dibromo-1-aminoanthraquinone, and then directly heat up hydrolysis in sulfuric acid to obtain 1-amino-2-bromo-4-hydroxyanthraquinone, and the product is isolated, filtered, washed, and dried in pure phenol In the medium, condense under the condition of an acid-binding agent. After reaching the end point of condensation, cool down to 95-100°C, add light alkaline water, and finally cool down to 50-60°C, filter, wash with water, and dry. The obtained filter cake is dispersed Red 60. However, the filtered condensation mothe...

Claims

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Application Information

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IPC IPC(8): C09B1/50
Inventor 金永辉阮国涛赵锋莫琰杜伟丰
Owner 浙江长征化工有限公司
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