Extraction method of high-stability salix leaf pigment dye

A technology with high stability and extraction method, which is applied in the field of willow leaf pigment dye extraction, can solve the problems of ineffective use of salicylic acid and its derivatives, poor pigment stability and dyeing effect, and achieve high value Utilization, accelerated dissolution, and high stability effects

Inactive Publication Date: 2017-08-04
霍邱县淮美奇工艺品有限公司
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The document "Extraction of Natural Pigment from Willow Leaves and Its Application in Silk Dyeing" extracts willow leaves with sodium hydroxide solution at 80-100°C, and the extract can effectively dye silk, ...
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Abstract

The invention discloses a method for extracting willow leaf pigment dyes with high stability. The alcohol extraction method is used to maximize the extraction of various pigments in willow leaves, which is more efficient than the traditional alkali extraction method. In the process, nano-silica is used as an auxiliary agent to speed up the dissolution of the pigment. At the same time, the amino-protected chitosan compound and the salicylic acid in the pigment undergo an effective esterification reaction to produce salicylated derivatives. , it has very good dyeing-assisting performance, and the pigment stability after chitosan modification is higher, and finally the modified pigment is saponified to make a water-soluble high-stable natural pigment dye, which realizes the high-efficiency of the pigment in willow leaves , Stable extraction, realizing the high-value utilization of willow leaves.

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Example Embodiment

[0019] A method for extracting a highly stable willow leaf pigment dye, comprising the following steps:
[0020] (1) Pick fresh, complete and mature willow leaves, wash them and put them into a grinder, add anhydrous ethanol and nano-silica in turn, and then grind and pulverize them. The slurry is leached twice at 60°C. Lift for 2h to get the extract;
[0021] (2) Filter the extract through an ultrafiltration membrane, collect the filtrate, concentrate and dry the filtrate to obtain pigment powder for use;
[0022] (3) Take chitosan and phthalic anhydride, put them into DMF in turn, heat up to 100°C, stir and reflux for 4 hours under nitrogen atmosphere, pour the reaction product into ice water, and wash the obtained precipitate to neutrality with alcohol After post-drying, the material is ground into fine powder to obtain modified chitosan for use;
[0023] (4) Put the pigment powder and modified chitosan into methylene chloride in turn, stir and react under ice bath conditions for 20min, and vacuum dry the system after the reaction, and recover the solvent;
[0024] (5) Put the material obtained in step (4) into 10 times the amount of ethanol, stir evenly, add sodium hydroxide aqueous solution with a concentration of 10%, adjust the pH value of the system to 10, heat and reflux in a water bath for 1 hour at 50 ° C, and saponify After the reaction, the saponification solution is concentrated under reduced pressure to obtain the willow leaf pigment dye, which can be diluted to the required concentration and pH value during use.
[0025] Wherein the weight ratio of willow leaves and absolute ethanol in step (1) is 1:15.
[0026] Wherein the addition amount of nano-silica in step (1) is 1‰.
[0027] The dosage ratio of chitosan, phthalic anhydride and DMF in step (3) is 1g:3g:20ml.
[0028] The dosage ratio of pigment powder, modified chitosan and dichloromethane in step (4) is 1g:0.01g:10ml.
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the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
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