Method for preparing disperse red 60

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...

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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 methanol for isolation. Although the production safety problem and the operating environment have been solved, the loss of ethylene glycol monomethyl ether is high, and the production cost is more prominent.

And in the invention patent of CN 101003691A, 1-amino-2-bromo-4-hydroxyanthraquinone is used as the wet product filter cake as the condensation raw material, and solvent and antioxidant are also added. Although the problem of drying the hydrolyzate is solved, it still solves the problem of Comprehensive recycling of phenol and phenol-soluble disperse red 60 is not possible. At the same time, the water in 1-amino-2-bromo-4-hydroxyanthraquinone still needs to be released during the condensation process, and steam is consumed, which cannot solve the unit consumption of phenol High and yield are not a big problem, the production cost is still high, and the current situation of environmental pollution cannot be changed

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