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Synthetic technology of phenol-free alkali violet

A synthesis process and basic technology are applied in the catalytic oxidation synthesis of phenol-free basic violet dyes, and in the field of phenol-free basic violet synthesis technology, which can solve the problems of high cost, hard oxidizing material, low yield and the like, and reduce the recovery rate. The effect of copper cost, reduced emissions, simple process

Inactive Publication Date: 2011-06-15
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is still in the laboratory stage at present, and the problem of too hard oxide material cannot be solved in the industrialization fashion, which leads to the problem of low yield
This issue is currently unresolved
[0004] The traditional basic violet production process has the problem of producing a large amount of phenol-containing wastewater that is difficult to treat, while the cost of some existing phenol-free processes is too high, which limits its large-scale industrialization

Method used

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  • Synthetic technology of phenol-free alkali violet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Take 160ml of N,N-dimethylaniline aqueous solution (containing about 50g of N,N-dimethylaniline), take 5 grams of AEO-7 and 10 grams of chlorobenzene, 27g of salt, and 30g of copper sulfate crystals into the solution, Vigorously stir at 50-80°C and let in air. At the same time, add acetic acid dropwise to maintain acidity. React for 40-45 hours. The oxidation material is golden and cold and crisp at room temperature, which is the end of the reaction. Add 200ml of chlorobenzene and 100ml of liquid caustic soda and heat up to 100°C, stir for 3 hours, filter, let stand to separate layers, let go of the water layer, treat the organic layer with dilute hydrochloric acid, and pour off the organic phase to obtain 45g of dye. The dye strength is 100 after testing. points, the yield is more than 95%.

Embodiment 2

[0026] Example 2: Take 160ml of N,N-dimethylaniline aqueous solution (containing about 50g of N,N-dimethylaniline), take 4 grams of AEO-12 and 10 grams of chlorobenzene, 27g of salt, and 30g of copper sulfate crystals into the solution, Vigorously stir at 50-80°C and let in air. At the same time, add acetic acid dropwise to keep the acidity. React for 40-45 hours. The oxidation material is golden and crisp at room temperature, which is the end point of the reaction. The treatment method of the oxidation material is the same as in Example 1 to obtain 46g of dye. , the detected dye intensity is 100 points. The yield is above 95%.

Embodiment 3

[0027] Embodiment 3: get 160mlN, N-dimethylaniline aqueous solution (containing N, about N-dimethylaniline 50g), get 5 grams of AN1810 and 10 grams of chlorobenzene, 27g salt, 30g copper sulfate crystals and add solution, at 50 Vigorously stir at ~80°C and feed air. At the same time, add acetic acid dropwise to maintain acidity. React for 40 to 45 hours. The oxidation material is golden and cold and crisp at room temperature, which is the end of the reaction. The detection dye intensity is 100 points. The yield is above 95%.

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Abstract

The invention discloses a process for synthesizing non-phenol basic violet. The process for synthesizing non-phenol basic violet comprises the following steps of mixing N, N-dimethyl aniline compounds with water to form a solution, adopting copper salts as catalyst, using compound nonionic emulsifier to perform emulsification, performing oxidation to a system at the temperature between 50 and 80 DEG C and then using a solvent method to treat oxidized material so as to obtain the high-purity basic violet with low copper content. The process for synthesizing non-phenol basic violet has the advantages of simple process, mild reaction conditions and no discharge of a large amount of wastewater, and has the yield over 95 percent.

Description

technical field [0001] The present invention relates to a kind of synthetic method of dye, specifically, the present invention relates to a kind of catalyzed oxidation synthetic method of phenol-free basic violet dye; More specifically, the present invention is a kind of phenol-free basic violet synthetic process. Background technique [0002] Basic Violet 5BN is usually prepared from N,N-dimethylaniline through two-step condensation and three-step oxidation. Existing industrial technologies all use copper salts such as copper sulfate and copper chloride as oxidants, and oxidize in the presence of a large amount of phenol by passing air into the reaction system. Existing industrial oxidation methods bring a large amount of toxic substances—phenol into dyes and wastewater, which pollutes the environment and reduces the quality of dyes. What is more deadly is that due to the water solubility of phenol, even if phenol is recovered, there is still a part of phenol in the wastew...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B11/18
Inventor 卢克磊林凤章夏清合陈安源
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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