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Preparation of CI 222# reactive blue

A technology of CI222 and reactive blue, applied in the direction of reactive dyes, chemical instruments and methods, azo dyes, etc., can solve the problems of dark color of finished dyes, low coupling conversion rate, loss of finished dyes, etc., to achieve easy washing and enhanced conversion rate , maintain the effect of environmental promotion

Inactive Publication Date: 2009-07-15
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved in the present invention is: in one-step condensation, the reaction system in which cyanuric chloride is insoluble in water is a solid-liquid two-phase reaction system, and it is difficult to completely react cyanuric chloride, and a hydrolysis side reaction occurs when cyanuric chloride encounters water , in the acid couple after diazotization, because the pH of the medium is less than 2 and the reaction of adding H acid is slow, the coupling conversion rate is low and monocouples are formed, resulting in dark color and low coloration of the finished dye, so salting out is generally used for refining The method removes side reactants, produces waste water, and has a certain loss of finished dyes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) One-step condensation: add 200Kg of bottom water in the pot, add 600Kg of crushed ice, add 49Kg of 100% cyanuric chloride, then add 0.4Kg of phase transfer catalyst CSC, after stirring for 10 minutes, add 100% para-ester 76.87, Use 10% sodium carbonate solution at 0-5°C to adjust pH=5, and react under this condition for 5 hours to obtain a one-step condensation liquid,

[0031] (2) Two-step condensation: after one-step condensation is completed, add 100% 2,4-diaminobenzenesulfonate sodium 55.21Kg, open the jacket and heat up, adjust pH=6-7 with 10% sodium carbonate solution at the same time, raise the temperature Stop heating at 40-45°C and react at 40-45°C, pH=6-7 for 3 hours to obtain a two-step condensation liquid,

[0032] (3) Diazotization: After the two-step condensation reaction is completed, cool down to 10°C with crushed ice, then add 22.3Kg of 100% hydrochloric acid, and then quickly add 18.5Kg of 100% sodium nitrite to keep the excess of sodium nitrite, t...

Embodiment 2

[0036] (1) One-step condensation: add 200Kg of bottom water in the pot, add 600Kg of crushed ice, add 49Kg of 100% cyanuric chloride, then add phase transfer catalyst CSC 0.4Kg and stir for 10 minutes, then add 100% para-ester 76.87, Adjust the pH to 3 with 10% sodium carbonate solution at 0-5°C, and react under this condition for 4 hours to obtain a one-step condensation liquid;

[0037] (2) Two-step condensation: After the one-step condensation is completed, add 55.21Kg of 100% 2,4-diaminobenzenesulfonate sodium, open the jacket and raise the temperature, and adjust the pH=6-7 with 10% sodium carbonate solution to raise the temperature to 30 Stop heating at -40°C and react at 30-40°C and pH=4-5 for 2 hours to obtain a two-step condensation liquid;

[0038](3) Diazotization: After the two-step condensation reaction is completed, cool down to 10°C with crushed ice, add 100% hydrochloric acid 22.3Kg, and then quickly add 100% sodium nitrite 18.5Kg to keep the excess sodium nitr...

Embodiment 3

[0042] (1) One-step condensation: add 200Kg of bottom water in the pot, add 600Kg of crushed ice, add 49Kg of 100% cyanuric chloride, then add 0.4Kg of phase transfer catalyst CSC, after stirring for 10 minutes, add 76.87Kg of 100% para-position ester , adjust pH=3-5 with 10% sodium carbonate solution at 5-10°C, and react under this condition for 5 hours to obtain a one-step condensation liquid;

[0043] (2) Two-step condensation: After the one-step condensation is completed, add 55.21Kg of 100% 2,4-diaminobenzenesulfonate, open the jacket and raise the temperature, and simultaneously adjust the pH to 6-7 with 10% sodium carbonate solution, and raise the temperature to Stop heating at 30-35°C and react at 30-35°C and pH=6-7 for 3 hours to obtain a two-step condensation liquid;

[0044] (3) Diazotization: After the two-step condensation reaction is completed, cool down to 10°C with crushed ice, then add 22.3Kg of 100% hydrochloric acid, and then quickly add 18.5Kg of 100% sodiu...

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Abstract

The invention provides a method for improving preparation of CI 222# reactive blue. The method changes one-step condensation reaction conditions and acid coupling conditions, so that product transformation ratio is improved by 8%, product quality reaches requirements for qualified products, thus avoiding generating process effluent; specifically, in the method of the invention, phase transfer catalyst is added to shorten ice grinding time in the one-step condensation, therefore, reaction efficiency is greatly improved; pH value of diazo salt is adjusted to 2.0-3.5 before the acid coupling, and after the alkali coupling, dye is blended to be qualified for virgin stock spray drying.

Description

technical field [0001] The invention belongs to the technical field of reactive dyes, in particular to a preparation method of CI 222# reactive blue. Background technique [0002] Reactive dyes have the outstanding characteristics of bright color, excellent application performance, convenient use, and strong applicability. In the past 20 years, due to the constraints of the ecological environment and the economic factors of the three wastes treatment, as well as the production and preparation of reactive dyes, the dyeing rate, fixation rate and dyeing wastewater The requirements are getting higher and higher, so the research and development of reactive dyes has evolved from the past salting-out process to the spray-drying process of the original slurry, but the spray-drying process of the original slurry requires the avoidance of by-products in the synthesis process of the dye. [0003] The molecular formula of CI 222# active blue produced and sold on the market is C 37 h ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B62/513
Inventor 张兴华韩春栋
Owner TIANJIN DEK CHEM
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