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Asymmetric metal complex black dye and preparation method thereof

A technology of metal complexing and black dyes, applied in the field of dyes, can solve problems such as weak dyeing, increased production costs, and time-consuming

Active Publication Date: 2018-11-30
上海青石化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the deep black dyeing on polyamide can only be completed by using acid dyes. However, the wet fastness of acid azo dyes is low, and the dyeing is not firm when it is wet at high temperature. The fastness can only be improved by washing once, which not only takes a lot of time, but also produces a lot of waste water, which increases the production cost of the product

Method used

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  • Asymmetric metal complex black dye and preparation method thereof
  • Asymmetric metal complex black dye and preparation method thereof
  • Asymmetric metal complex black dye and preparation method thereof

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preparation example Construction

[0064] Aiming at the defects of the dyes in the prior art, the inventors of the present application obtained the asymmetric metal complex black dye suitable for dyeing hydroxyl-containing or amino-containing fiber materials of the present invention through in-depth research. The preparation method of this dyestuff comprises as follows:

[0065]

[0066] where R 1 , R 2 , R 3 , R 4 each independently hydrogen, nitro, sulfonic acid group, halogen atom or sulfonamide group, R 5 , R 6 Each is independently a halogen atom, a hydroxyl group, an alkoxy group, an aromatic amine or an aliphatic amine.

[0067] In a preferred embodiment of the present invention, step a) is specifically: dissolving the diazo compound shown in formula (3) in ice water under stirring, adjusting the pH=2-4 with alkali; adding 2-naphthol to the water , use sodium hydroxide and sodium carbonate to adjust pH=9-11, stir and dissolve at 50-90°C, then cool down to 30-40°C; add 2-naphthol solution to the ...

Embodiment 1

[0088] a) Preparation of coupling reactant I:

[0089] Add 29.5 parts of 6-nitro-1,2,4-acid oxygen, as shown in formula (3-1), add 150 parts of ice water to mix and beat, stir and cool down to 5°C, adjust with 30% sodium hydroxide solution The pH of the slurry was 2.0 and stirred until fully dissolved.

[0090] Add 14.5 parts of 2-naphthol to 120 parts of water, add 6 parts of 30% sodium hydroxide solution and 4 parts of sodium carbonate, heat in a hot water bath to 50-60 ° C and stir until completely dissolved, then cool the solution to 35°C.

[0091] Under stirring, quickly pour the above 2-naphthol solution into the 6-nitro-1,2,4-acid oxygen body solution for coupling reaction, adjust the pH of the coupling reaction system to 10.0, keep warm at 40°C, and stir for 5 hours. The progress of the reaction was monitored by liquid chromatography. After completion of the reaction, salting out, filtering, washing with water, and drying to obtain the monoazo compound represented b...

Embodiment 2

[0109] a) Preparation of coupling reactant I:

[0110] Add 29.5 parts of 6-nitro-1,2,4-acid oxygen, as shown in formula (3-1), add 150 parts of ice water to mix and beat, stir and cool down to 5°C, adjust with 30% sodium hydroxide solution pH=4.0, stir until completely dissolved.

[0111] Add 14.5 parts of 2-naphthol to 120 parts of water, add 6 parts of 30% sodium hydroxide solution and 4 parts of sodium carbonate, heat in a hot water bath to 70-80 ° C and stir until completely dissolved, then cool the solution to 35°C.

[0112] Under stirring, quickly pour the 2-naphthol solution into the 6-nitro-1,2,4-acid oxygen body solution for coupling, adjust the coupling pH=10.5, keep warm at 40°C and stir for 6 hours, monitor the reaction with liquid chromatography schedule. After completion of the reaction, salting out, filtering, washing with water, and drying to obtain the monoazo compound represented by formula (2-1).

[0113] b) Preparation of 1:1 chromium complex:

[0114]...

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Abstract

The invention relates to an asymmetric metal complex black dye and a preparation method thereof. Specifically, the asymmetric metal complex black dye has a structure represented by the following formula (1). The dye combines the advantages of acid dyes and reactive dyes, and is suitable for printing dyeing of fiber materials containing hydroxyl or amino groups. The dyeing process is simple, stableand reliable, and the dyeing effect is excellent. The material dyed by the dye has good fastness to wet and fastness to daylight.

Description

technical field [0001] The present invention relates to a kind of dye, more specifically, relates to a kind of asymmetric metal complex black dye and its preparation method. Background technique [0002] Since the advent of reactive dyes, due to their excellent wet fastness and level dyeing performance, good color brightness and easy use, their development has been in a leading position. However, with the use of reactive dyes in dyeing, people have put forward higher requirements for the dyeing process and color performance. However, when reactive dyes are used for natural wool fibers and synthetic polyamide fibers, the color performance is insufficient. In particular, black reactive dyes generally have the problems of poor chromatographic breadth and low dyeing reproducibility. Therefore, it is an urgent need for printing and dyeing factories to find a reactive black dye with high dyeing strength, good dyeing fastness and good color expression. [0003] Acid dyes have cer...

Claims

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Application Information

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IPC IPC(8): C09B45/48D06P1/36
CPCC09B45/48D06P1/36
Inventor 尹东赵敏
Owner 上海青石化学有限公司
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