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Synthetic technology of phenol-free alkali violet

A synthetic process and basic technology, which is applied in the catalytic oxidation synthesis of phenol-free basic violet dye, and in the field of phenol-free basic violet synthesis process, can solve the problems of high cost, hard oxidized material, low yield, etc., and reduce the recovery Copper cost, reduced emissions, simple process effect

Inactive Publication Date: 2009-03-11
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 5g of AEO-7, 10g of chlorobenzene, 27g of salt, and 30g of copper sulfate crystals into the solution. Stir vigorously at 50-80°C and blow in air, while adding acetic acid dropwise to keep acidic, and react for 40-45 hours. The oxidation material is golden and brittle at room temperature as the end of the reaction. Add 200ml of chlorobenzene and 100ml of liquid caustic soda and heat to 100°C, stir for 3 hours, filter, stand for separation, let go of the water layer, treat the organic layer with dilute hydrochloric acid, discard the organic phase, and obtain 45g of dye. The dye strength is determined to be 100. 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 4g of AEO-12, 10g of chlorobenzene, 27g of salt, and 30g of copper sulfate crystals into the solution, Stir vigorously at 50-80°C and blow in air while adding acetic acid dropwise to keep acidic. The reaction is 40-45 hours. The oxidation material is golden and brittle at room temperature, which is the end of the reaction. The oxidation material treatment method is the same as that of Example 1, and 46 g of dye is obtained. , The dye intensity is 100 points after testing. The yield is more than 95%.

Embodiment 3

[0027] Example 3: Take 160ml of N,N-dimethylaniline aqueous solution (containing about 50g of N,N-dimethylaniline), take 5g of AN1810, 10g of chlorobenzene, 27g of salt, and 30g of copper sulfate crystals into the solution. Stir vigorously at ~80°C and blow in air, while adding acetic acid dropwise to keep acidic, react for 40-45 hours. The oxidation material is golden and brittle at room temperature as the end of the reaction. The oxidation material treatment method is the same as that in Example 1, to obtain 43g of dye. The detection dye intensity is 100 points. The yield is more than 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 method for synthesizing dyes. Specifically, the present invention relates to a method for the catalytic oxidation synthesis of phenol-free basic violet dyes; more specifically, the present invention relates to a synthesis process for phenol-free basic violet. Background technique [0002] Basic Violet 5BN is usually prepared from N,N-dimethylaniline as the starting material and 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 in the presence of a large amount of phenol, the oxidation is carried out by blowing air into the reaction system. Existing industrial oxidation methods bring a large amount of toxic substances-phenol to dyes and wastewater, which pollute the environment and reduce the quality of dyes. What’s more deadly is the water solubility of phenol. Even if phenol is recycled, there is still a...

Claims

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Application Information

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Patent Type & Authority Applications(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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