Modified synthesis technique for disperse red 92

A synthesis process, disperse red technology, applied in the direction of amino-hydroxy anthraquinone dyes, etc., can solve the problems of high production cost, difficult recovery, low recovery rate, etc., and achieve the guarantee of condensation speed and yield, yield and quality Affected, the effect of increasing the reaction yield

Active Publication Date: 2008-02-20
JIANGSU YABANG DYE
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AI Technical Summary

Problems solved by technology

[0011] This method reaction speed is fast, and product quality is excellent, but used raw material gamma-methoxypropylamine (or gamma-ethoxypropylamine) is expensive, and this raw material is easily soluble in water, so it is difficult to recover after separation, and the rate of recovery is extremely low and High energy consumption and high production costs

Method used

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  • Modified synthesis technique for disperse red 92
  • Modified synthesis technique for disperse red 92
  • Modified synthesis technique for disperse red 92

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 500kg of chlorosulfonic acid into a 1000L enamel kettle, control the temperature at 25-35°C for about 2-3 hours and slowly add 150kg of dry product of Disperse Red 60, after the addition is completed, keep it warm at this temperature for 1-2 hours, and then in 2 Slowly add 100kg of thionyl chloride dropwise for ~3 hours. After the dropwise addition, keep it warm at 25-35°C for 7 hours. After the reaction, transfer the material to the isolation kettle, and slowly add ice water dropwise in the isolation kettle for 1-2 hours. 2500kg, continue to stir for one hour and then filter, wash the filter cake with cold water until neutral;

[0027] Add 1500kg of clear water into a 3000L enamel kettle, put in the above-mentioned intermediate filter cake, stir evenly, add 50kg of sodium carbonate and 110kg of γ-ethoxypropylamine, keep it at 35-40°C for 6 hours, and filter after detecting the end point. The cake was washed with hot water at 70-80°C to neutrality, and then discharg...

Embodiment 2

[0029] The amount of chlorosulfonic acid in Example 1 is increased from 500kg to 700kg, and other feeding ratios and operating methods are unchanged to obtain Disperse Red 92 filter cake product 225kg, with a total yield of 97.5% and a content of 99.6%.

Embodiment 3

[0031] Chlorosulfonic acid consumption is increased to 700kg by 500kg among the embodiment 1, sulfur oxychloride is reduced to 80kg by 100kg simultaneously, other feeding ratio and operating method are constant, obtain disperse red 92 filter cake product 218kg, total yield is 94.5%, the content is 99.7%.

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Abstract

The invention relates to an improved disperse red 92 synthesis technique. The invention takes disperse red 60 as raw material and chlorosulfonic acid as sulfonation reagent and after sulfonation, ionyl chloride is added for chlorosulfonation and the two steps are completed in one bath; icy water is added for segregation and filtration; the filter cake is washed by cold water; then in the water the filtrated mixture is reacted with condensing agent of Gamma-methoxy propylamine or Gamma-ethoxy propylamine with the function of catalysis to obtain the final product. The technique makes use of ionyl chloride as chlorosulfonation reagent, which improves reaction activity, reduces reaction temperature and coking during reaction process, improves product quality and dramatically improves reaction yield; by adopting water to replace Gamma-methoxy propylamine or Gamma-ethoxy propylamine in the prior art as reaction medium during condensing process, the invention greatly saves production cost and has significant economic benefit.

Description

technical field [0001] The invention relates to a method for improving the synthesis process of disperse red 92, more specifically, the improvement of the chlorosulfonation process and condensation process in the existing production method of disperse red 92. Background technique [0002] Disperse Red 92 (C.I.Disperse Red 92) is also known as Disperse Red FBL, Disperse Red S-BCF, Disperse Brilliant Red BEL, Disperse Blue Light Red FBL, etc. The original production method is to use Disperse Red 60 as raw material, and a large amount of excess chlorosulfur The acid reacts at a higher reaction temperature to generate 1-amino-4-hydroxy-2-(p-sulfonyl chloride)phenoxyanthraquinone. After the reaction, slowly add ice water and isolate at low temperature. The precipitated intermediate is filtered Fully wash the remaining acid in the filter cake with cold water, and then condense with γ-methoxypropylamine (or γ-ethoxypropylamine) to obtain the product. [0003] In this technology, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/52C09B1/54
Inventor 黄斌尹云李少文季政
Owner JIANGSU YABANG DYE
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