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Preparation method for disperse red 60

A technology for dispersing red and amino, which is applied in the direction of amino-hydroxyanthraquinone dyes, etc., can solve the problems of long reaction time, dull color, low yield, etc., and achieve the effect of good quality and similar color

Active Publication Date: 2015-03-25
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

The reaction time of this method is long, and the yield is low, and after the dyeing of the obtained disperse red 60 product, the color and luster is dim, bluish phase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation method of Disperse Red 60 of this embodiment is as follows:

[0020] First put 20 grams of potassium carbonate and 180 grams of phenol into the four-necked reaction flask, install the rectification tower, and slowly dehydrate and heat up under normal pressure to 155°C (control the heating rate at 20-25°C / h), to When there is no water in the dehydration device, it can be considered that there is no water in the system, and then 60 grams of 1-amino-2-bromo-4-hydroxyanthraquinone dry product (water content 0.2%) is put into the system, and then the temperature is raised. When the temperature reaches 155°C, keep the temperature, take a sample after 3 hours to measure the end point of the condensation. When the end point is reached, the temperature is reduced to 90°C, and isolating water is added dropwise to precipitate Disperse Red 60, then suction filtration, washing, and drying to obtain 56 g of the product. The rate is 93.3%, and the chromatographic conten...

Embodiment 2

[0022] The preparation method of Disperse Red 60 of this embodiment is as follows:

[0023] Put 20 grams of potassium carbonate and 180 grams of phenol into the four-necked reaction flask, install the rectification tower, and slowly dehydrate and heat up under negative pressure to 155°C (control the heating rate at 20-25°C / h) to When there is no water in the dehydration device, it can be considered that there is no water in the system, and then 60 grams of 1-amino-2-bromo-4-hydroxyanthraquinone dry product (water content 0.2%) is put into the system, and then the temperature is raised. When the temperature reaches 155°C, keep the temperature, take a sample after 2 hours to measure the end point of the condensation. When the end point is reached, the temperature is reduced to 90°C. Segregated water is added dropwise to precipitate Disperse Red 60, and then suction filtration, washing and drying to obtain 56.3 g of the product. The rate is 93.8%, the chromatographic content is 99...

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PUM

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Abstract

The invention relates to a preparation method for disperse red 60. The preparation method comprises the step of conducting reaction on dried 1-amino-2-bromine-4-hydroxy-anthraquinone with phenol under the existence of an acid-binding agent, wherein the moisture content of the dried 1-amino-2-bromine-4-hydroxy-anthraquinone is controlled under 0.2 wt%; the condensation reaction is implemented through the following steps: (1) adding potassium carbonate and phenyl hydroxide in a reaction vessel; mounting a dehydration device; conducting dehydration and temperature increasing to 130-155 DEG C under normal pressure or negative pressure; when no water is dehydrated in the dehydration device, adding the dried 1-amino-2-bromine-4-hydroxy-anthraquinone in a system passing the step (1); maintaining the temperature at 150-158 DEG C for reaction. The yield is up to 93%; the chromatograph content of the obtained disperse red 60 product is above 99.5%; compared the cloth dyed by the disperse red 60 with standard cloth, the clothes are similar in color and luster, and good in quality.

Description

technical field [0001] The invention relates to a preparation method of disperse red 60. Background technique [0002] The existing production method of disperse red 60 is to use 1-aminoanthraquinone as a raw material, and bromine reacts with bromine in a sulfuric acid medium to generate 1-amino-2.4-dibromoanthraquinone, and the reaction product is directly produced without separation. In the presence of urotropine, the temperature is raised for hydrolysis reaction to obtain 1-amino-2 bromo-4-hydroxyanthraquinone, namely the hydrolyzate. Add water to the reaction system for isolation, plate and frame filter press, wash to obtain a hydrolyzate filter cake, and dry to obtain a dry hydrolyzate. Then put the hydrolyzate into the excess phenol medium in the presence of the acid-binding agent potassium carbonate for condensation reaction. After reaching the end point, cool down to 90-95°C, and drop the separated water to make 1-amino-2-phenoxy-4 -Hydroxyanthraquinone is isolated...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/54
Inventor 李根荣徐新连
Owner 苏州市罗森助剂有限公司
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