Synthesis method of dispersive dye diazonium salt

A technology for disperse dyes and synthesis methods, applied in the field of fine chemical synthesis, can solve the problems of reduced effective utilization rate of equipment, increased post-treatment cost, large amount of sulfuric acid for pulping, etc., so as to reduce the generation of waste water and shorten the reaction time of diazotization , the effect of shortened response time

Active Publication Date: 2016-12-07
ZHEJIANG RUNTU INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of beating sulfuric acid required by this preparation method is extremely large, which in turn greatly increases the amount of dilution water in the coupling reaction process, reduces the effec

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 180g of 1,2-dichloroethane into a 500ml four-neck flask, add 34.5g of 2-chloro-4-nitroaniline under stirring, stir and raise the temperature to 45-55°C, and then add dropwise at this temperature Bromine 17.5g, dropwise and keep warm for 1h, add 4g of solid sodium chlorate, add and continue keep warm. Sampling analysis after the end point, the main content is 98.03%, and the raw material is 0.32%;

[0021] After the bromination reaction is completed, lower the temperature to below 25°C, then add 94g of 28% nitrosyl sulfuric acid dropwise at a temperature below 20°C to 25°C, and keep the reaction for 1 to 1.5 hours after the dropwise addition, and the diazotization is completed;

[0022] The above reaction system was left to stand for 2 hours, and then layered to obtain the lower layer of diazonium salt for the synthesis of dyes. The upper organic layer was washed with a small amount of ice water or dilute sulfuric acid, and then allowed to stand and layered again. Th...

Embodiment 2

[0025] Add 90 g of 1,2-dichloroethane obtained by layering in Example 1 into a 250 ml four-neck flask, add 17.25 g of 2-chloro-4-nitroaniline under stirring, and stir to raise the temperature to 45-55°C , and then drop bromine 8.7g at this temperature, drop and complete the heat preservation reaction for 1h, add 2g of solid sodium chlorate, and continue the heat preservation reaction after adding. Sampling analysis after the end point, the main content is 98.21%, and the raw material is 0.32%;

[0026] After the bromination reaction is finished, lower the temperature to below 25°C, then add 47g of 28% nitrosylsulfuric acid dropwise at a temperature below 20°C to 25°C, and keep the reaction for 1 to 1.5 hours after the dropwise addition, and the diazotization is completed;

[0027] The above reaction system was left to stand for 2 hours, and then layered to obtain the lower layer of diazonium salt for the synthesis of dyes. The upper organic layer was washed with a small amount...

Embodiment 3

[0030] Add 120g of 1,2-dichloroethane into a 250ml four-neck flask, add 13.8g of p-nitroaniline under stirring, stir and raise the temperature to 45-55°C, then add 17g of bromine dropwise at this temperature, dropwise After completing the heat preservation reaction for 1 hour, continue to drop 14.5 g of hydrogen peroxide at this temperature, and continue the heat preservation reaction after dropping. Sampling and analysis after the end point, the main content is 98.95%, and monobromide is 0.22%;

[0031] After the bromination reaction is completed, the temperature of the obtained bromination reaction solution is lowered to below 25°C, first dropwise add 15g of sulfuric acid, and then continue to dropwise add 47g of 28% nitrosyl sulfuric acid at a temperature of 15-25°C, after the dropwise addition, keep warm for 1 hour, the diazotization ends;

[0032] The above reaction system was left to stand for 2 hours, and then layered to obtain the lower layer of diazonium salt for the...

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PUM

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Abstract

The invention provides a synthesis method of dispersive dye diazonium salt. In the method, a series compounds, including paranitroaniline, 2,4-dinitroaniline, 2-cyano-4-nitroaniline and the like, are employed as raw materials, which are then subjected to bromination reaction in an organic solvent to respectively prepare solutions or suspension liquids of 2,6-dibromo-4-nitroaniline, 2,4-dinitro-6-bromoaniline, 2-cyano-4-nitro-6-bromoaniline and the like. A certain amount of sulfuric acid is added and then a diazotization reagent is added, or that the diazotization reagent is directly added to perform diazotization; when the diazotization is finished, the reaction products are allowed to stand and are layered to obtain the corresponding diazonium salts and recycled organic solvent which is insoluble in water. Compared with the prior art, the method simplifies a large quantity of process and saves cost. Compared with references in whith bromination is carried out with sulfuric acid as the solvent, the synthesis method greatly reduces the use quantity of the sulfuric acid, thus reducing acidic wastewater emission and saving cost.

Description

technical field [0001] The invention belongs to the technical field of synthesis of fine chemicals, and in particular relates to a synthesis method of diazonium salt of disperse dyes. Background technique [0002] A series of compounds such as 2,6-dibromo-4-nitroaniline, 2,4-dinitro-6-bromoaniline, and 2-cyano-4-nitro-6-bromoaniline are important dye intermediates At present, the commonly used process is carried out in the water phase. After the reaction is completed, the corresponding product is obtained by filtering, washing, and drying; Under the action of diazonium salt. There are disadvantages such as long technological process, high energy consumption and many wastes. [0003] The Chinese patent application whose publication number is CN 101671272 A discloses a kind of synthetic method of 2-cyano-4-nitro-6-bromoaniline diazonium salt. Beating in sulfuric acid with a percentage of 10-98%, adding bromide and oxidizing agent for bromination, and then directly diazotizi...

Claims

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Application Information

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IPC IPC(8): C07C245/20
CPCC07C245/20
Inventor 章文刚丁兴成赵国生
Owner ZHEJIANG RUNTU INST
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