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Method for preparing active red DF-3BS

A technology of DF-3BS and reactive red, which is applied in the field of preparation of reactive red DF-3BS, can solve problems such as increasing costs, and achieve the effects of reducing raw material costs, excellent color giving power, and avoiding pollution

Active Publication Date: 2008-10-08
泰州市姜堰区东风染料化工厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the existing reactive red DF-3BS synthesis method, waste water is easily generated, especially in the salting-out step, a large amount of chloride needs to be added to the reaction, which not only increases the cost, but also discharges a large amount of sewage into the environment

Method used

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  • Method for preparing active red DF-3BS
  • Method for preparing active red DF-3BS
  • Method for preparing active red DF-3BS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] 1. Ingredients list

[0059] raw material name

Molecular weight

Molecular ratio

100% discount (kg)

Cyanuric chloride

184.5

1.0

149.5

1-naphthylamine-8-hydroxy-3,6-disulfonic acid

341.3

1.0

276.1

M-(βsulfate ethyl sulfone)aniline

281.3

1.03

234.4

2-naphthylamine-1,5-bissulfonic acid

303

0.98

240.2

Sodium Nitrite

69.01

0.98

54.7

Hydrochloric acid

36.5

1.0

29.5

[0060] 2. The synthetic method of reactive red DF-3BS of the present invention is operated as follows:

[0061] A. Dissolution of 1-naphthylamine-8-hydroxy-3,6-disulfonic acid:

[0062] 700L of bottom water, add 276.1kg of 1-naphthylamine-8-hydroxy-3,6-disulfonic acid, add 50kg of sodium dihydrogen phosphate and 75kg of disodium hydrogen phosphate, and beat for 1 hour. Adjust the pH to 6.5 with 10% soda water.

[0063] B. Cyanuric chloride be...

Embodiment 2

[0078] A. Dissolution of 1-naphthylamine-8-hydroxy-3,6-disulfonic acid:

[0079] With 700L of bottom water, put in 1-naphthylamine-8-hydroxy-3,6-disulfonic acid and fold 289.9 kg, add 60 kg of sodium dihydrogen phosphate and 90 kg of disodium hydrogen phosphate, and beat for 1 hour. Adjust the pH to 6.4 with 10% soda ash water.

[0080] B. Cyanuric chloride beating:

[0081] Add 200L of ice water, cool the jacket, and put 142kg of cyanuric chloride industrial product into ice mill for 1 hour.

[0082] C. One time condensation:

[0083] Add the dissolved A step solution to the beaten suspension in about 1.5 hours. After the addition, adjust the pH to 1.9 with soda ash and the temperature at 4°C, and react for 2 hours.

[0084] D. Secondary condensation:

[0085] Add 257.2kg of aniline powder (β-sulfate ethyl sulfone) into the first shrinkage solution of step C, stir for 10 minutes, and evenly raise the temperature to 45°C in about 1 hour, while adjusting the pH=3.7 with 10% soda wa...

Embodiment 3

[0095] A. Dissolution of 1-naphthylamine-8-hydroxy-3,6-disulfonic acid:

[0096] 750L of bottom water, put in 1-naphthylamine-8-hydroxy-3,6-disulfonic acid, break 262.3kg, add 55kg of sodium dihydrogen phosphate and 84kg of disodium hydrogen phosphate, and beat for 1 hour. Adjust the pH to 6.3 with 10% soda ash water.

[0097] B. Cyanuric chloride beating:

[0098] Add 200L of ice water, cool the jacket, and put 157.0kg of cyanuric chloride industrial product into ice mill for 1 hour.

[0099] C. One time condensation:

[0100] Add the dissolved A-step solution to the B-step beating suspension within 1 hour and 20 minutes. After the addition, adjust the pH to 2.0 with soda ash and the temperature at 5° C. and react for 2 hours.

[0101] D. Secondary condensation:

[0102] Put 211.6kg of aniline powder (β-sulfate ethyl sulfone) into the first shrinkage solution of step C, stir for 15 minutes, and evenly raise the temperature to 45°C in 50 minutes, while adjusting the pH=3.9 with 10...

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Abstract

The invention discloses a making method of active red DF-3BS, which comprises the following steps: dissolving 1-naphthylamine-8-hydroxy-3, 6-disulfonic acid in the water; condensing with beaten tricyanide chloride suspension; condensing the reactant with p-(beta sulfate sulfonyl) phenylamine; reacting 2-naphthylamine-1, 5-disulfonic acid with sodium nitrite in the alcaine; obtaining diazo material; adding diazo material in the secondary condensed solution; coupling; removing inorganic salt in the coupling liquid through ionic film; spraying; baking.

Description

Technical field [0001] The invention relates to a method for chemical synthesis of dyes, in particular to a method for preparing reactive red DF-3BS. Background technique [0002] The invention focuses on improving the yield of the product, reducing the cost of the product, and avoiding pollution to the environment and ecology. The DF-3BS synthesized by the invention is a typical green environmental protection dye. [0003] The DF-3BS synthesized by the present invention has the following characteristics: [0004] 1. Excellent reactivity, saving energy consumption; [0005] 2. Excellent cleanliness and good color fastness; [0006] 3. Excellent solubility, level dyeability, and excellent dye depth; [0007] 4. Good stability, excellent pad dyeing and printing performance; [0008] 5. Higher dye uptake and fixation rate, bright color and excellent performance. [0009] In the existing synthetic method of reactive red DF-3BS, waste water is easily generated, especially in the salti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B62/507
Inventor 陈才美李兴喜
Owner 泰州市姜堰区东风染料化工厂