A plant dye for silk fabric and preparation method thereof

By using plant dyes with ingredients such as turmeric dyes, cork dyes, antibacterial liquids and quaternized chitosan, the problem of insufficient antibacterial and flame retardant effects of silk fabrics is solved, and good antibacterial and fire-retardant properties are achieved.

CN119119761BActive Publication Date: 2025-05-02NAPO TONGYIXIN SILK TECH IND CO LTD
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Patent Information

Application Number
CN202411250068.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-06
Publication Date
2025-05-02
Estimated Expiration
2044-09-06

AI Technical Summary

Technical Problem

The antibacterial and flame retardant effects of existing silk fabrics are insufficient, especially when placed for a long time, they are susceptible to bacterial erosion and are flammable.

Method used

Using a plant dye, including turmeric dye, cork dye, antibacterial liquid, quaternized chitosan and water, the antibacterial liquid and quaternized chitosan are prepared by specific reaction steps, and the plant dye combining these ingredients is used for the dyeing of silk fabrics.

Benefits of technology

It achieves good antibacterial and flame retardant effects of silk fabrics, which can effectively prevent bacterial erosion and fire spread.

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Abstract

The present invention relates to the technical field of dyes, and discloses a plant dye for silk fabrics and a preparation method thereof. The present invention is provided by adding turmeric dye, phellodendron dye, antibacterial liquid, quaternized chitosan and water into a stirrer, stirring at room temperature, and obtaining the plant dye for silk fabrics after the end. The antibacterial liquid and quaternized chitosan contain a large amount of quaternary ammonium salt groups, which play a good antibacterial role. The cardanol in the antibacterial liquid itself has a certain antibacterial effect, and synergistically antibacterial with the quaternary ammonium salt. The sulfur element contained in the antibacterial liquid can promote the dehydration of the polymer substrate into carbon during the heating process. This carbon layer can effectively isolate the contact between oxygen in the air and the polymer substrate, thereby achieving a flame retardant effect; the boron element can form a glassy coating covering the polymer when heated, and the coating can effectively isolate oxygen and heat, thereby protecting the internal polymer from further combustion, thereby achieving a flame retardant effect.
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Description

Technical Field

[0001] The invention relates to the technical field of dyes, in particular to a plant dye for silk fabrics and a preparation method thereof. Background Art

[0002] At present, the dyes used by textile printing and dyeing enterprises are basically chemical dyes. Silk fiber is a natural protein fiber, which is known as the "Queen of Fiber". It has good health, comfort and nobility, and is widely used in clothing and decorative materials. However, during long-term storage, bacteria will erode it, affecting the quality of the product; it will be flammable when encountering fire, causing damage to clothing, so how to avoid this phenomenon is the key to solving the problem. For example, patent CN108385406A discloses a pure natural antibacterial silk fabric and its preparation method. The prepared pure natural antibacterial silk fabric has bright color, soft skin-friendly, good wearing performance, and has good antibacterial effect on Staphylococcus aureus, Escherichia coli, and Candida albicans, but its flame retardant effect has not been improved. Summary of the invention

[0003] 1. Technical issues to be resolved

[0004] In view of the deficiencies of the prior art, the present invention provides a plant dye for silk fabrics and a preparation method thereof, which has good antibacterial and flame retardant effects.

[0005] (II) Technical solution

[0006] To achieve the above object, the present invention provides the following technical solution: a plant dye for silk fabrics, comprising the following components by weight: 20-35 parts by weight of turmeric dye, 30-40 parts by weight of phellodendron dye, 3-6 parts by weight of antibacterial liquid, 4-8 parts by weight of quaternized chitosan, and 80-120 parts by weight of water;

[0007] Chitosan is added into an ethanol solvent for dissolution, heated in a water bath at 70-85° C., and then 2,3-epoxypropyltrimethylammonium chloride is added under constant pressure for a reaction of 6-10 hours. After the reaction, the mixture is washed with anhydrous ethanol, dried, dialyzed, and concentrated to obtain quaternized chitosan.

[0008] Preferably, the preparation method of the antibacterial liquid is:

[0009] (1) Adding boric acid to ether solvent, stirring and dispersing, then adding 4-methyl-5-thiazoleethanol, reacting at 105-120°C for 8-13h, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0010] (2) Add chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, stir to dissolve, react at 60-85°C for 10-12 hours, and then perform rotary distillation, wash with ethanol, filter, and dry to obtain quaternary boric acid;

[0011] (3) Adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, stirring and dispersing, and reflux reacting at 50-80° C. for 14-18 hours. After completion, cooling to room temperature, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0012] (4) Add the intermediate and quaternized boric acid to N,N-dimethylformamide solvent, raise the temperature to 75-90°C, then continue to add triethylamine catalyst, stir and react for 6-10 hours, and after the reaction, rotary distill to remove the solvent, wash with petroleum ether, and dry to obtain an antibacterial liquid.

[0013] Preferably, the mass ratio of boric acid to 4-methyl-5-thiazoleethanol in (1) is 1:1.2-1.4.

[0014] Preferably, the mass ratio of chloroacetyl chloride to boric acid-modified thiazole in (2) is 1:0.9-1.3.

[0015] Preferably, the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst in (3) is 1.2-1.5:1:0.01-0.02.

[0016] Preferably, the mass ratio of the intermediate, quaternary ammonium boric acid and triethylamine catalyst in (4) is 1:1.4-1.7:0.02-0.04.

[0017] Preferably, the preparation method of the plant dye for silk fabric is: adding turmeric dye, phellodendron dye, antibacterial liquid, quaternized chitosan and water into a stirrer, stirring at room temperature for 12-20 minutes, and obtaining the plant dye for silk fabric after the stirring.

[0018] 3. Beneficial technical effects

[0019] The invention adds turmeric dye, phellodendron dye, antibacterial liquid, quaternized chitosan and water into a stirrer, and stirs at room temperature to obtain the plant dye for silk fabrics.

[0020] Boric acid is reacted with the hydroxyl group in 4-methyl-5-thiazoleethanol to obtain boric acid-modified thiazole, the chlorine group in chloroacetyl chloride is reacted with the tertiary amine group in boric acid-modified thiazole to generate a quaternary ammonium salt group, and an acyl chloride group is introduced to obtain quaternary boric acid; the phenol group in cardanol and the chlorine group in 2-chloro-4,6-diamine-1,3,5-triazine are subjected to a substitution reaction to introduce a large number of amino groups to obtain an intermediate, the amino group in the intermediate and the acyl chloride in the quaternary boric acid are subjected to an amidation reaction to generate an amide group to obtain an antibacterial liquid; the amino group in chitosan and the epoxy group in 2,3-epoxypropyltrimethylammonium chloride are subjected to a ring-opening reaction to generate a hydroxyl group to obtain quaternary chitosan.

[0021] The antibacterial liquid and quaternized chitosan contain a large number of quaternary ammonium salt groups, which play a good antibacterial role. The cardanol in the antibacterial liquid itself has a certain antibacterial effect, and synergistically fights against bacteria with the quaternary ammonium salt. The sulfur element contained in the antibacterial liquid can promote the dehydration of the polymer substrate into carbon during the heating process. This carbon layer can effectively isolate the oxygen in the air from the contact with the polymer substrate, prevent the spread of flames, and achieve a flame retardant effect; the boron element can form a glass-like coating covering the polymer when heated. The coating can effectively isolate oxygen and heat, thereby protecting the internal polymer from further combustion, thereby achieving a flame retardant effect; the chitosan in the quaternized chitosan itself has flame retardant and antibacterial effects. DETAILED DESCRIPTION Example 1

[0022] (1) Adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, wherein the mass ratio of boric acid to 4-methyl-5-thiazoleethanol is 1:1.2, reacting at 105°C for 8 hours, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0023] (2) adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, wherein the mass ratio of chloroacetyl chloride to boric acid-modified thiazole is 1:0.9, stirring to dissolve, reacting at 60° C. for 10 h, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary ammonium boric acid;

[0024] (3) Adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, wherein the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst is 1.2:1:0.01, stirring and dispersing, reflux reaction at 50°C for 14 hours, cooling to room temperature after completion, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0025] (4) adding the intermediate and quaternary ammonium boric acid to N,N-dimethylformamide solvent, heating to 75°C, and then continuing to add triethylamine catalyst, wherein the mass ratio of the intermediate, quaternary ammonium boric acid, and triethylamine catalyst is 1:1.4:0.02, stirring and reacting for 6 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid;

[0026] (5) adding chitosan into an ethanol solvent to dissolve it, heating it in a water bath at 70°C, then adding 2,3-epoxypropyltrimethylammonium chloride under constant pressure, reacting for 6 hours, washing with anhydrous ethanol after the reaction, drying, dialyzing, and concentrating to obtain quaternized chitosan;

[0027] (6) 20 parts by weight of turmeric dye, 30 parts by weight of phellodendron dye, 3 parts by weight of antibacterial liquid, 4 parts by weight of quaternized chitosan, and 80 parts by weight of water are added into a blender and stirred at room temperature for 12 minutes to obtain a plant dye for silk fabric. Example 2

[0028] (1) Adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, wherein the mass ratio of boric acid to 4-methyl-5-thiazoleethanol is 1:1.4, reacting at 120°C for 13 hours, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0029] (2) adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, wherein the mass ratio of chloroacetyl chloride to boric acid-modified thiazole is 1:1.3, stirring to dissolve, reacting at 85°C for 12 hours, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary ammonium boric acid;

[0030] (3) adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, wherein the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst is 1.5:1:0.02, stirring and dispersing, and reflux reaction at 80°C for 18 hours. After completion, cooling to room temperature, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0031] (4) adding the intermediate and quaternary ammonium boric acid to N,N-dimethylformamide solvent, heating to 90°C, and then continuing to add triethylamine catalyst, wherein the mass ratio of the intermediate, quaternary ammonium boric acid, and triethylamine catalyst is 1:1.7:0.04, stirring and reacting for 10 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid;

[0032] (5) adding chitosan into an ethanol solvent to dissolve it, heating it in a water bath at 85°C, then adding 2,3-epoxypropyltrimethylammonium chloride under constant pressure, reacting it for 10 hours, washing it with anhydrous ethanol after the reaction, drying it, dialyzing it, and concentrating it to obtain quaternized chitosan;

[0033] (6) 35 parts by weight of turmeric dye, 40 parts by weight of phellodendron dye, 6 parts by weight of antibacterial liquid, 8 parts by weight of quaternized chitosan, and 120 parts by weight of water are added into a blender and stirred at room temperature for 20 minutes to obtain a plant dye for silk fabrics. Example 3

[0034] (1) Adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, wherein the mass ratio of boric acid to 4-methyl-5-thiazoleethanol is 1:1.3, reacting at 112°C for 10.5h, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0035] (2) Adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, wherein the mass ratio of chloroacetyl chloride to boric acid-modified thiazole is 1:1.1, stirring to dissolve, reacting at 72.5°C for 11 hours, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary ammonium boric acid;

[0036] (3) Adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, wherein the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst is 1.35:1:0.015, stirring and dispersing, reflux reaction at 65°C for 16 hours, cooling to room temperature after completion, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0037] (4) adding the intermediate and quaternary ammonium boric acid to N,N-dimethylformamide solvent, heating to 82.5°C, and then continuing to add triethylamine catalyst, wherein the mass ratio of the intermediate, quaternary ammonium boric acid, and triethylamine catalyst is 1:1.55:0.03, stirring and reacting for 8 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid;

[0038] (5) adding chitosan into an ethanol solvent to dissolve it, heating it in a water bath at 77°C, then adding 2,3-epoxypropyltrimethylammonium chloride under constant pressure, reacting for 8 hours, washing with anhydrous ethanol after the reaction, drying, dialyzing, and concentrating to obtain quaternized chitosan;

[0039] (6) 27.5 parts by weight of turmeric dye, 35 parts by weight of phellodendron dye, 4.5 parts by weight of antibacterial liquid, 6 parts by weight of quaternized chitosan, and 100 parts by weight of water were added into a blender and stirred at room temperature for 16 minutes to obtain a plant dye for silk fabric. Example 4

[0040] (1) Adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, wherein the mass ratio of boric acid to 4-methyl-5-thiazoleethanol is 1:1.2, reacting at 105°C for 8 hours, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0041] (2) adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, wherein the mass ratio of chloroacetyl chloride to boric acid-modified thiazole is 1:0.9, stirring to dissolve, reacting at 60° C. for 10 h, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary ammonium boric acid;

[0042] (3) adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, wherein the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst is 1.5:1:0.02, stirring and dispersing, and reflux reaction at 80°C for 18 hours. After completion, cooling to room temperature, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0043] (4) adding the intermediate and quaternary ammonium boric acid to N,N-dimethylformamide solvent, heating to 90°C, and then continuing to add triethylamine catalyst, wherein the mass ratio of the intermediate, quaternary ammonium boric acid, and triethylamine catalyst is 1:1.7:0.04, stirring and reacting for 10 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid;

[0044] (5) adding chitosan into an ethanol solvent to dissolve it, heating it in a water bath at 77°C, then adding 2,3-epoxypropyltrimethylammonium chloride under constant pressure, reacting for 8 hours, washing with anhydrous ethanol after the reaction, drying, dialyzing, and concentrating to obtain quaternized chitosan;

[0045] (6) 27.5 parts by weight of turmeric dye, 35 parts by weight of phellodendron dye, 4.5 parts by weight of antibacterial liquid, 6 parts by weight of quaternized chitosan, and 100 parts by weight of water were added into a blender and stirred at room temperature for 16 minutes to obtain a plant dye for silk fabric. Example 5

[0046] (1) Adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, wherein the mass ratio of boric acid to 4-methyl-5-thiazoleethanol is 1:1.4, reacting at 120°C for 13 hours, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0047] (2) adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, wherein the mass ratio of chloroacetyl chloride to boric acid-modified thiazole is 1:1.3, stirring to dissolve, reacting at 85°C for 12 hours, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary ammonium boric acid;

[0048] (3) Adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, wherein the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst is 1.35:1:0.015, stirring and dispersing, reflux reaction at 65°C for 16 hours, cooling to room temperature after completion, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0049] (4) adding the intermediate and quaternary ammonium boric acid to N,N-dimethylformamide solvent, heating to 82.5°C, and then continuing to add triethylamine catalyst, wherein the mass ratio of the intermediate, quaternary ammonium boric acid, and triethylamine catalyst is 1:1.55:0.03, stirring and reacting for 8 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid;

[0050] (5) adding chitosan into an ethanol solvent to dissolve it, heating it in a water bath at 70°C, then adding 2,3-epoxypropyltrimethylammonium chloride under constant pressure, reacting for 6 hours, washing with anhydrous ethanol after the reaction, drying, dialyzing, and concentrating to obtain quaternized chitosan;

[0051] (6) 20 parts by weight of turmeric dye, 30 parts by weight of phellodendron dye, 3 parts by weight of antibacterial liquid, 4 parts by weight of quaternized chitosan, and 80 parts by weight of water are added into a blender and stirred at room temperature for 12 minutes to obtain a plant dye for silk fabric.

[0052] Comparative Example 1

[0053] (1) adding chitosan into an ethanol solvent to dissolve it, heating it in a water bath at 70°C, then adding 2,3-epoxypropyltrimethylammonium chloride under constant pressure, reacting for 6 hours, washing with anhydrous ethanol after the reaction, drying, dialyzing, and concentrating to obtain quaternized chitosan;

[0054] (2) 20 parts by weight of turmeric dye, 30 parts by weight of phellodendron dye, 4 parts by weight of quaternized chitosan, and 80 parts by weight of water are added into a stirrer and stirred at room temperature for 12 minutes to obtain a plant dye for silk fabrics.

[0055] Comparative Example 2

[0056] (1) Adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, wherein the mass ratio of boric acid to 4-methyl-5-thiazoleethanol is 1:1.4, reacting at 120°C for 13 hours, and after the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole;

[0057] (2) adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, wherein the mass ratio of chloroacetyl chloride to boric acid-modified thiazole is 1:1.3, stirring to dissolve, reacting at 85°C for 12 hours, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary ammonium boric acid;

[0058] (3) Adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, wherein the mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst is 1.35:1:0.015, stirring and dispersing, reflux reaction at 65°C for 16 hours, cooling to room temperature after completion, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate;

[0059] (4) adding the intermediate and quaternary ammonium boric acid to N,N-dimethylformamide solvent, heating to 82.5°C, and then continuing to add triethylamine catalyst, wherein the mass ratio of the intermediate, quaternary ammonium boric acid, and triethylamine catalyst is 1:1.55:0.03, stirring and reacting for 8 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid;

[0060] (5) 20 parts by weight of turmeric dye, 30 parts by weight of phellodendron dye, 3 parts by weight of antibacterial liquid, and 80 parts by weight of water are added into a blender and stirred at room temperature for 12 minutes to obtain a plant dye for silk fabrics.

[0061] Performance Testing:

[0062] The silk fabric is immersed in the plant dye and dyed at 80° C. for 50 minutes to obtain the dyed silk fabric.

[0063] Use an oxygen index meter to test the limiting oxygen index of silk fabrics, and use a horizontal and vertical combustion instrument to test the combustion level of materials.

[0064] Table 1: Flame retardancy test

[0065]

[0066] It can be seen from Table 1 that Examples 1-5 of the present invention have better flame retardant effects than Comparative Examples 1-2.

[0067] The antibacterial properties of the plant dyes of Examples 1-5 and Comparative Examples 1-2 were measured according to the method of GB / T 20944.3-2008. The test results are shown in Table 2.

[0068] Table 2: Antimicrobial Test

[0069]

[0070] It can be seen from Table 2 that Examples 1-5 of the present invention have better antibacterial effects than Comparative Examples 1-2.

[0071] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A plant dye for silk fabrics, characterized in that: The invention comprises the following components by weight: 20-35 parts by weight of turmeric dye, 30-40 parts by weight of phellodendron dye, 3-6 parts by weight of antibacterial liquid, 4-8 parts by weight of quaternized chitosan, and 80-120 parts by weight of water; The chitosan is added into an ethanol solvent for dissolution, heated in a water bath at 70-85° C., and then 2,3-epoxypropyltrimethylammonium chloride is added under constant pressure for reaction for 6-10 hours. After the reaction, the chitosan is washed with anhydrous ethanol, dried, dialyzed, and concentrated to obtain quaternized chitosan. The preparation method of the antibacterial liquid is: (1) adding boric acid to an ether solvent, stirring and dispersing, and then adding 4-methyl-5-thiazoleethanol thereto, reacting at 105-120° C. for 8-13 hours. After the reaction is completed, distilling under reduced pressure, filtering and drying to obtain boric acid-modified thiazole; (2) adding chloroacetyl chloride and boric acid-modified thiazole to N,N-dimethylformamide solvent, stirring to dissolve, reacting at 60-85° C. for 10-12 hours, and then rotary distilling, washing with ethanol, filtering, and drying to obtain quaternary boric acid; (3) adding cardanol and 2-chloro-4,6-diamine-1,3,5-triazine to an acetone solvent, and then adding potassium carbonate catalyst thereto, stirring and dispersing, and reflux reacting at 50-80° C. for 14-18 hours. After completion, cooling to room temperature, filtering, washing with deionized water, extracting with ethyl acetate, and drying the organic phase to obtain an intermediate; (4) adding the intermediate and quaternized boric acid to N,N-dimethylformamide solvent, heating to 75-90° C., then continuing to add triethylamine catalyst, stirring and reacting for 6-10 hours, and after the reaction, rotary distilling to remove the solvent, washing with petroleum ether, and drying to obtain an antibacterial liquid; The mass ratio of boric acid to 4-methyl-5-thiazoleethanol in (1) is 1:1.2-1.4; The mass ratio of chloroacetyl chloride to boric acid-modified thiazole in (2) is 1:0.9-1.3; The mass ratio of cardanol, 2-chloro-4,6-diamine-1,3,5-triazine and potassium carbonate catalyst in (3) is 1.2-1.5:1:0.01-0.02; The mass ratio of the intermediate, quaternary ammonium boric acid and triethylamine catalyst in (4) is 1:1.4-1.7:0.02-0.

04.

2. A method for preparing a plant dye for silk fabrics as claimed in claim 1, characterized in that: The preparation method of the plant dye for silk fabrics comprises the following steps: adding turmeric dye, phellodendron dye, antibacterial liquid, quaternized chitosan and water into a stirrer, stirring for 12-20 minutes at room temperature, and obtaining the plant dye for silk fabrics.

Citation Information

Patent Citations

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    CN108385406A

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