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A kind of preparation method of vat yellow 3rt

A technology of reactor and magnesium chloride, applied in the field of preparation of vat yellow 3RT, can solve the problems of heavy pollution, low product yield, poor environmental protection performance, etc., achieve product yield and purity improvement, safe and convenient operation, and reduce production cost Effect

Active Publication Date: 2020-01-07
安徽融创化工科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the cost of this traditional process is high, the product yield is low, and the pollution is heavy. At the same time, the environmental protection performance of the product is poor, which does not conform to the national sustainable development strategy. In the face of the increasingly stringent "green barriers" of the international community The greater constraints received are very unfavorable to the future development of the product

Method used

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  • A kind of preparation method of vat yellow 3rt
  • A kind of preparation method of vat yellow 3rt

Examples

Experimental program
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Effect test

Embodiment 1

[0022] A preparation method of vat yellow 3RT, comprising the steps of:

[0023] (1) Ring-closing reaction: Add 200 parts of o-dichlorobenzene to reactor A, add 64 parts of trianthraquinone imine under stirring, heat the oil bath to 120°C, add 20 parts of magnesium chloride in 4 batches, and add 20 parts of magnesium chloride in adjacent batches. After that, 8 parts of titanium tetrachloride were slowly added dropwise at one time. When the solution turned black, the reaction was continued for 4 hours, the reaction was stopped, and the magnesium chloride was recovered by filtration; Wash with o-dichlorobenzene for 3 times, and then wash with ethanol for 5 times, then use an oil pump to evacuate and dry in vacuum at 95°C, then wash with water, and dry to obtain a dark reddish-brown solid with a yield of 92.5%;

[0024] (2) Oxidation reaction: Weigh 40 parts of the dark reddish-brown solid obtained in step (1) and grind it into 180-mesh powder, add it to reactor B, then add 160 p...

Embodiment 2

[0026] A preparation method of vat yellow 3RT, comprising the steps of:

[0027] (1) Ring-closing reaction: Add 240 parts of o-dichlorobenzene to reactor A, add 70 parts of trianthraquinone imine under stirring, heat the oil bath to 130°C, add 15 parts of magnesium chloride in 3 batches, and add 15 parts of magnesium chloride in adjacent batches. The interval between them is 8 minutes; after that, 6 parts of titanium tetrachloride are slowly added dropwise at one time. When the solution turns black, continue to react for 6 hours, stop the reaction, and recover magnesium chloride by filtration; Wash with o-dichlorobenzene for 3 times, and then wash with ethanol for 4 times, then use an oil pump to evacuate and dry in vacuum at 92°C, then wash with water, and dry to obtain a dark reddish-brown solid with a yield of 91.5%;

[0028] (2) Oxidation reaction: Weigh 32 parts of the dark reddish-brown solid obtained in step (1) and grind it into 150-mesh powder, add it to reactor B, th...

Embodiment 3

[0030] A preparation method of vat yellow 3RT, comprising the steps of:

[0031] (1) Ring-closing reaction: Add 200 parts of o-dichlorobenzene to reactor A, add 55 parts of trianthraquinone imine with stirring, heat the oil bath to 115°C, add 25 parts of magnesium chloride in 4 batches, and add 25 parts of magnesium chloride in adjacent batches. After that, 10 parts of titanium tetrachloride was slowly dropped in at one time, and when the solution turned black, the reaction was continued for 5 hours, the reaction was stopped, and the magnesium chloride was recovered by filtration; after the reaction system was lowered to room temperature, suction filtration was used first Wash with o-dichlorobenzene twice, then wash with ethanol for 4 times, and then use an oil pump to evacuate and dry in vacuum at 95°C, then wash with water, and dry to obtain a dark reddish-brown solid with a yield of 91%;

[0032] (2) Oxidation reaction: Weigh 45 parts of the dark reddish-brown solid obtaine...

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Abstract

The invention provides a preparation method of vat yellow 3RT, which comprises the following steps: (1) ring-closure reaction: adding o-dichlorobenzene and trianthraquinone imine into a reactor A, heating in an oil bath to 115 to 130 DEG C, adding magnesium chloride in batches, dropwise adding titanium tetrachloride in one time, continuously reacting for 4 to 6 hours after the solution is changedinto black, stopping reaction, filtering, cooling, suction filtering, washing, vacuum drying at high temperature, washing and drying to obtain dark red brown solid; (2) oxidation reaction: grinding the dark red brown solid into powder, adding the powder into a reactor B, adding water, heating to 40 to 45 DEG C, adding potassium hydroxide, sodium acetate, urea and potassium permanganate, heating ina water bath to 50 to 55 DEG C, reacting; cooling to room temperature, suction filtering, washing to be neutral to obtain the vat yellow 3RT. The vat yellow 3RT prepared by the invention has high yield and good quality. The preparation method can effectively reduce the production cost, has lower reaction temperature than the traditional reaction and is safer and more convenient during operation.

Description

technical field [0001] The invention relates to the technical field of dye preparation, in particular to a preparation method of vat yellow 3RT. Background technique [0002] Vat dyes, formerly known as vat dyes, are insoluble in water, and are reduced in alkaline solution by sodium dithionite (sodium hydrosulfite) to dye fibers. Its light fastness and washing fastness are particularly outstanding, and it can be used for dyeing and printing of cotton, linen, viscose, vinylon and other fibers. [0003] The molecular structure of vat dyes does not contain water-soluble groups such as sulfonic acid groups and carboxylic acid groups, so it is insoluble in water and cannot be directly dyed; its molecular conjugated double bond system contains at least two carbonyl groups, and it can be combined with Sodium hydrochloride interacts, and the carbonyl group is reduced and transformed into a hydroxyl group, becoming a water-soluble compound—leuco. The leuco has affinity to the fiber...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B5/28
CPCC09B5/28
Inventor 王洪卫徐卉香孙茂义蒋大为郭元张文件高鸿宇
Owner 安徽融创化工科技股份有限公司