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Preparation method of vat blue dye

A technology for dyes and raw materials, applied in the field of preparation of vat dyes, can solve problems such as difficulty in obtaining pigment-grade vat blue, and achieve the effects of good economic benefits, simplified synthesis procedures and stable performance

Active Publication Date: 2011-10-05
JIANGSU HUAER CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process yield is about 94%, but the yield after refining and purifying hydrosulfite generally only has 88%, and it is difficult to obtain pigment grade vat blue 4 (I) product

Method used

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  • Preparation method of vat blue dye
  • Preparation method of vat blue dye
  • Preparation method of vat blue dye

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 In a 500mL four-necked flask, 120g of water was added into a 10% N,N'-dimethylcyclopropylene urea (IIIa), 0.1g catalyst, 50g of 99.0% purity in 1-aminoanthraquinone ( II), stir and heat up to 95°C, add 150mL 50% potassium hydroxide solution dropwise, oxidize with air, carry out condensation reaction at 100-125°C, add 100mL water to dilute the isolated material after 8 hours of heat preservation reaction, filter the material with suction, and collect the mother liquor , the filter cake was washed with hot water to neutrality, and dried to obtain vat blue 4 (I) 49.2g, yield 98.4%, without further refining and dyeing cotton cloth, bright red light blue can be obtained.

Embodiment 2

[0016] Example 2 In a 500mL four-necked flask, 120g of water was added into a 15% N,N'-dimethylcyclopropylene urea (IIIa), 0.1g catalyst, 50g of 99.0% purity in 1-aminoanthraquinone ( II), stir and heat up to 95°C, add 150mL 50% potassium hydroxide solution dropwise, oxidize with air, carry out condensation reaction at 100-125°C, add 100mL water to dilute the isolated material after 8 hours of heat preservation reaction, filter the material with suction, and collect the mother liquor , the filter cake was washed with hot water to neutrality, and dried to obtain Vat Blue 4 (I) 48.8g, with a yield of 97.6%, without further refining and dyeing cotton cloth to obtain bright red light blue.

Embodiment 3

[0017] Example 3 In a 500mL four-necked flask, 120g of water was added into a 20% N,N'-dimethylcyclopropylene urea (IIIa), 0.1g of catalyst, 50g of 99.0% purity in 1-aminoanthraquinone ( II), stir and heat up to 95°C, add 150mL 50% potassium hydroxide solution dropwise at 95-98°C, oxidize with air, carry out condensation reaction at 100-125°C, add 100mL water to dilute the isolated material after 8 hours of heat preservation reaction, and pump the material Filter, collect mother liquor, filter cake hot water washes to neutrality, dry to obtain vat blue 4 (I) 48.5g, yield 97.0%, can obtain bright red light blue without further refining and dyeing cotton cloth.

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Abstract

The invention relates to a preparation method of a vat dye of a vat blue 4 (I) dye. 1- aminoanthraquinone (II) is used as a raw material, and a hydrous cyclic urea derivative, N, N'-dimethyl propyleneurea (IIIa), is used as a medium; in the presence of a strong base, potassium hydroxide, and a phase-transfer catalyst, condensation is performed using oxygen or air as an oxidant; when the reaction endpoint is reached, filtration, washing and drying are performed to obtain dianthraquinone-N, N'-dihydroazine, that is vat blue 4 (I), with high yield and high purity. After being further refined, the dye can be used as pigment-grade vat blue 4 (I).

Description

Technical field: [0001] The invention relates to a preparation method of vat dyes, more specifically, adopts a new process to synthesize vat blue 4 (I) dyes, and belongs to the technical field of chemical dyes manufacture. Background technique: [0002] Vat blue 4 (I) is the earliest anthraquinone vat dye, which was first prepared by German chemist R. Born in 1901. It is mainly used for cotton fiber dyeing and cotton printing, also used for two-bath overdyeing of cotton and polyester-cotton fabrics, and also used for the manufacture of pigments for inks. Its traditional production process is to use 2-aminoanthraquinone as the raw material, perform condensation and closed-loop in molten potassium hydroxide, sodium hydroxide and anhydrous sodium acetate, dilute with water, reduce it to leuco with hydrosulfite, and separate it from impurities by filtration. Then oxidize the leuco body to obtain the finished product, and the yield is about 56%. The process has problems such as...

Claims

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Application Information

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IPC IPC(8): C09B5/48C09B67/26
Inventor 陈四清汤学斌周多刚
Owner JIANGSU HUAER CHEM
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