Anthraquinone-based dichloro-s-triazine reactive disperse dye and preparation method thereof
A dichloro-s-triazine type, reactive disperse dye technology, applied in the direction of reactive dyes, organic dyes, azo dyes, etc., can solve the problems of increasing reactive disperse dye types, unable to meet natural fibers, incomplete chromatography, etc., and achieve low cost , The effect of strong applicability and high reaction efficiency
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Embodiment 1
[0032] This embodiment provides anthraquinone-based dichloro-triazine type reactive disperse dye II a And preparation method thereof, concrete steps are as follows:
[0033] (1) Add 0.002mol 1-chloroanthraquinone, 0.002mol N-(2-aminoethyl) aniline, 0.002mol potassium hydroxide and 0.2mmol copper powder in sequence in a 100mL three-necked flask, and blow nitrogen into the three-necked flask , and then dropwise added 5mL of N,N-dimethylformamide, and reacted at 100°C for 10h.
[0034] (2) After the reaction, the reaction solution obtained in step (1) was cooled, then extracted with dichloromethane as an extractant, concentrated, and dried in vacuo to obtain a reddish-brown solid powder. The solid powder was purified by column chromatography, and the eluent was a mixture of dichloromethane and petroleum ether (volume ratio of 1: 2) to obtain the dye precursor I a The purified product, the separation yield is 50%;
[0035] (3) 0.001mol dye precursor I a The purified product an...
Embodiment 2
[0039] This embodiment provides a dichloro-s-triazine-type anthraquinone structure reactive disperse dye II b And preparation method thereof, concrete steps are similar to embodiment 1. The difference is that:
[0040] Replace N-(2-aminoethyl)aniline in step (1) with N-(2-aminoethyl)-3-methylaniline; potassium hydroxide, copper powder and N,N-dimethylformaldehyde The dosages of amides were 0.004mol, 0.1mmol and 10mL respectively, and the reaction temperature was 90°C. Wherein the synthesis method of N-(2-aminoethyl)-3-methylaniline is: in a nitrogen atmosphere, 0.030mol m-toluidine and 0.010mol 2-bromoethylamine hydrobromide are successively added to a 100mL three-necked flask 15 mL of toluene was added dropwise, refluxed for 20 h, suction filtered after cooling, and the filter residue was purified by column chromatography, the eluent was acetone, and the separation yield was 80%.
[0041] When carrying out column chromatography purification in step (2), eluent is the mixtu...
Embodiment 3
[0046] This embodiment provides a dichloro-s-triazine-type anthraquinone structure reactive disperse dye II c And preparation method thereof, concrete steps are similar to embodiment 2. The difference is that:
[0047] N-(2-aminoethyl)-3-methylaniline in step (1) is replaced with N-(2-aminoethyl)-3-methoxyaniline, and its synthetic method is: in nitrogen atmosphere , 0.025mol 3-methoxyaniline and 0.010mol 2-bromoethylamine hydrobromide were successively added to a 100mL three-neck flask, and 20mL of toluene was added dropwise, refluxed for 20h, cooled and filtered, and the filter residue was subjected to column Purified by chromatography, the eluent is acetone, and the separation yield is 79%.
[0048] When carrying out column chromatography purification in step (2), eluent is the mixture (volume ratio is 1: 1) of dichloromethane and sherwood oil, makes dye precursor I c The purified product, the isolated yield is 48%.
[0049] Dye precursor I in step (3) b Change to Dye ...
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