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Synthetic method of gardenia blue dye with double-chromophoric structures
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A synthetic method, the technology of gardenia blue, applied in the direction of dyeing, natural dyes, azo dyes, etc., can solve the problems of poor affinity and color fastness of gardenia blue pigment, so as to improve the affinity and color fastness, The effect of good structural symmetry and large molecular weight
Active Publication Date: 2020-02-21
WUHAN TEXTILE UNIV
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[0004] The purpose of the present invention is to provide a kind of synthetic method of gardenia blue dye with double-color structure in order to overcome the problem of poor affinity and color fastness of gardenia blue pigment on textiles existing in the prior art
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[0023] A first aspect of the present invention provides a method for synthesizing a gardenia blue dye with a dual chromophoric structure, the method comprising the following steps:
[0025] (2) extracting the solution obtained in step (1) and collecting the aqueous layer solution, then adjusting the pH value, standing, centrifuging and drying successively to obtain the initial product;
[0026] (3) The initial product obtained in step (2) is reacted in an alkaline solution, and then concentrated and freeze-dried in sequence.
[0027] In the method of the present invention, the genipin is the product of geniposide hydrolyzed by β-glucosidase, and the structural formula is shown in formula I.
[0028]
[0029] In the method of the present invention, in step (1), the molar ratio of the lysine to the genipin can be 1:(1-3). Specifically, for example, it can be 1:1, 1:2 or 1:3.
[0030] In the method of th...
Embodiment 1
[0048] Lysine was added to the buffer solution with pH=7, and then the dissolved genipin was slowly added dropwise, wherein the molar ratio of genipin and lysine was 1:1, the reaction temperature was 60° C., and the reaction was stirred for 6 hours. After the reaction, extract with ethyl acetate, collect the aqueous layer solution, adjust the pH value of the solution to 4, stand at 0 °C for 24 h, centrifuge 5 times, and dry to obtain a solid initial product, which is pH=12. The caustic soda solution was reacted for 6 h, concentrated, and freeze-dried to obtain double-chromophoric structure gardenia blue dye A1.
Embodiment 2
[0050]Lysine was added to the buffer solution with pH=8, and the dissolved genipin was slowly added dropwise, wherein the molar ratio of genipin and lysine was 2:1, the reaction temperature was 80° C., and the reaction was stirred for 32 hours. After the reaction, extract with ethyl acetate, collect the aqueous layer solution, adjust the pH value of the solution to 3, stand at 0 °C for 36 h, centrifuge 6 times, and dry to obtain a solid initial product, which is pH=11 The caustic soda solution was reacted for 16h, concentrated, and freeze-dried to obtain double-chromophoric structure gardenia blue dye A2.
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Abstract
The invention relates to the field of dye synthesis, in particular to a synthesis method of a gardeniablue dye with double-chromophoric structures. The method comprises the following steps: (1) mixing lysine and genipin in a buffer solution for reaction; (2) extracting a solution obtained in the step (1), collecting a water layer solution, and then sequentially carrying out pH value adjustment, standing, centrifugation and drying to obtain a primary product; and (3) carrying out reaction on the primary product obtained in the step (2) in an alkaline solution, and then sequentially carrying out concentration and freeze drying. The gardeniablue dye with the double-chromophoric structures synthesized by the method disclosed by the invention has two same chromophoric structures, the structural symmetry is increased, the molecular weight is increased, and the affinity and the color fastness of the gardeniablue dye with the double-chromophoric structures and fibers can be further improved.
Description
technical field [0001] The invention relates to the field of dye synthesis, in particular to a method for synthesizing a gardenia blue dye with a dual chromophoric structure. Background technique [0002] Natural pigments have attracted more and more attention due to their green, healthy and safe characteristics. Blue pigments are relatively rare in nature, and gardenia blue is one of them. Its natural origin, good human compatibility and high safety are widely used in the food processing industry. [0003] At present, the preparation of gardenia blue pigment mainly adopts microbial fermentation and two-step synthesis. The microbial fermentation method completes hydrolysis and synthesis in one step, but has problems such as low product quality and waste of raw materials; the two-step method first uses gardeniside as a raw material, and under the action of β-glucosidase, hydrolysis is converted into genipin, Genipin and amino acids undergo a series of polymerization and rea...
Claims
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