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Anthraquinone type solvent dye and preparation and application thereof

A solvent dye, anthraquinone technology, applied in the field of dyes, can solve problems such as harming the environment, corroding equipment, wasting resources, etc., and achieving the effects of reducing air pollution, low cost and convenient operation

Inactive Publication Date: 2007-10-31
SHENYANG RES INST OF CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resulting by-product industrial waste oil is only burned as fuel, which not only corrodes equipment, endangers the environment, but also wastes resources

Method used

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  • Anthraquinone type solvent dye and preparation and application thereof
  • Anthraquinone type solvent dye and preparation and application thereof
  • Anthraquinone type solvent dye and preparation and application thereof

Examples

Experimental program
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Effect test

example 1

[0039] Example 1: Separation and purification of 2-ethyl-6-sec-butylaniline

[0040]Distillation: Add 600g of industrial waste oil produced in the production of DEA into a 1000ml three-necked flask, add zeolite, and pass nitrogen through the bottom pipe. Distillation conditions: rectification tower diameter 30mm, stainless steel triangular packing, packing height 1100mm, vacuum degree 10mmHg, reflux ratio 5:1. When the liquid phase temperature reaches 137°C, reflux occurs, and the fractions at 141-144°C are collected to obtain 300 g of the main fraction, which is 2-ethyl-6-sec-butylaniline, with a content of 95%.

example 2

[0041] Example 2: Separation and purification of 2-methyl-6-sec-butylaniline

[0042] Distillation: Add 600g of industrial waste oil produced in the production of MEA into a 1000ml three-necked flask, add zeolite, and introduce nitrogen through a bottom pipe. Distillation conditions: rectification tower diameter 30mm, stainless steel triangular packing, packing height 1100mm, vacuum degree 10mmHg, reflux ratio 5:1. When the liquidus temperature reaches 127°C, reflux occurs, and the 130-133°C fractions are collected to obtain 268g of the main fraction, which is 2-methyl-6-sec-butylaniline with a content of 93.5%.

example 3

[0043] Example 3: Synthesis of Compound I

[0044] Add 7.0g 1,4-dihydroxyanthraquinone, 3.0g 1,4-dihydroxyanthraquinone leuco, 1.2g boric acid, 32g 2-ethyl-6-sec-butylaniline in a 100ml four-necked flask, Stir and raise the temperature to 150°C while removing the water brought in by the raw materials and the reaction generated. The reaction is controlled by thin-layer chromatography: when the yellow and orange raw material spots basically disappear, the reaction is considered to have reached the end point, the reaction is stopped, the temperature is reduced to 90°C, potassium hydroxide 5g is added, and air is oxidized until the purple disappears. , Which is the end point of oxidation, the reaction solution was slowly precipitated into 100 ml of hot ethanol, then cooled, filtered, and washed to obtain 16.1 g of compound I with a yield of 69.4%.

[0045] NMR data:

[0046] 1 H NMR(DCCI 3 ,300MHz)δ0.77-0.83(m, 3H, CH 3 ), 1.01-1.17(m, 6H, CH 3 ), 1.48-1.1.54(m, 2H, CH 2 ), 2.44-2.59(...

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PUM

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Abstract

The invention discloses an anthraquinone dissolvent dye and preparation and application in dye technical domain, which is characterized by the following: setting the composite as general formula (I); choosing R1 from hydroxyl group or II; choosing R2 from metyl group or ethyl group; adopting vacuum rectifying craft; extracting 2-ethyl group-6-secondary butyl aniline or 2-metyl group-6-secondary butyl aniline; proceeding condensation reaction with 1, 4-alizarin; preparing the general formula (I) component; decreasing the cost of dye. This dye can be used to color oil, hard plastic rubber and resin, which can get brilliance red light blue and bright violet.

Description

Technical field [0001] The invention belongs to the technical field of dyes, and specifically relates to an anthraquinone solvent dye and its preparation and application. Background technique [0002] The high-end solvent dyes CI Solvent Blue 104 [116-75-6] and CI Solvent Blue 97 [61969-44-6], which were successfully developed and commercialized by Bayer Company in Germany in the early years, have bright, transparent blue and good heat stability. And light fastness, suitable for the coloring of thermoplastics (hard plastics). This type of dye consists of 2,4,6-trimethylaniline, 2,4,6-triethylaniline (or 2,6-diethyl-p-toluidine) and 1,4-dihydroxyanthraquinone respectively. Condensation reaction is obtained. However, due to the high price of 2,4,6-trimethylaniline and 2,4,6-triethylaniline (or 2,6-diethyl-p-toluidine), the price of this type of dye is expensive. Its application has been limited to a certain extent. [0003] On the other hand, we have found that some industrial wast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/32C08K5/18C08J3/20
Inventor 黄海朱红卫崔莉
Owner SHENYANG RES INST OF CHEM IND
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