Washable silk fabric based on eupatorium adenophorum and preparation method of washable silk fabric

Abstract

The invention relates to a washable silk fabric based on eupatorium adenophorum and a preparation method thereof, and belongs to the technical field of dyeing and finishing. The preparation method comprises the following steps: S1, soaking a silk fabric in a crofton weed dye liquor for dyeing to obtain a dyed silk fabric; s2, the dyed silk fabric is soaked in a 1-ethyl-(3-dimethylaminopropyl) carbodiimide / N-hydroxysuccinimide finishing solution to be subjected to activating treatment, and the activated dyed silk fabric is obtained through padder treatment; and S3, dipping the activated dyed silk fabric in a bone glue solution to carry out a cross-linking reaction, and carrying out padder treatment and heat setting to obtain the washable silk fabric based on the ageratina adenophora. The resource utilization of the eupatorium adenophorum is only helped, the ecological after-finishing color fixation of the silk fabric is realized, and the application field of the silk fabric is expanded.

Description

Technical Field

[0001] This invention belongs to the field of dyeing and finishing technology, and in particular relates to a washable silk fabric based on Eupatorium fortunei and its preparation method. Background Technology

[0002] Silk, renowned as the "Queen of Fibers" for its exceptional luster, soft texture, excellent breathability, and unique properties that keep you warm in winter and cool in summer, is a crucial raw material for high-end textiles. However, the traditional processing of silk textiles widely utilizes synthetic dyes and finishing agents. These chemicals not only pose potential health hazards but also generate large amounts of wastewater containing harmful substances, causing severe environmental pollution. With the increasing prevalence of green and environmentally friendly concepts, this traditional processing method no longer meets the sustainable development requirements of "green dyeing and finishing" and "eco-textiles," seriously hindering the transformation and upgrading of my country's textile industry towards mid-to-high-end manufacturing.

[0003] In recent years, the application of natural dyes has gradually attracted attention. Natural dyes are mainly derived from plants, such as fruits, vegetables, flowers, and trees, which contain abundant natural pigments. Using natural dyes eliminates the need for large amounts of auxiliaries like salts and alkalis, thus reducing pollution emissions at the source and offering significant environmental benefits. However, natural dyes face several limitations in practical applications. On the one hand, directly extracting dyes from plants may damage plant resources, contradicting the goal of carbon neutrality. On the other hand, natural dyes have poor dyeing performance, low color fastness, a limited color gamut, and weak binding to protein fibers (such as silk and wool), resulting in poor wash fastness on silk fabrics. This makes it difficult to meet the needs of large-scale industrial production, limiting their widespread application in silk textiles.

[0004] Furthermore, bone glue, as a traditional material, is mainly composed of collagen. Collagen is a chain-like substance with good adhesion, biocompatibility, and biodegradability, and theoretically can be used to improve the performance of silk fabrics. However, unmodified collagen has many defects that make it difficult to meet the requirements of practical applications, which greatly limits its application in the textile field.

[0005] Based on this, the present invention is proposed. Summary of the Invention

[0006] Therefore, the technical problem to be solved by the present invention is to overcome the problems of waste of natural plant extract resources, poor washability of silk fabrics, and potential biotoxicity of some traditional mordants and fixing agents in existing silk fabric dyeing and finishing technologies.

[0007] To address the aforementioned technical problems, this invention provides a washable silk fabric based on *Eupatorium adenophorum* and its preparation method. First, the silk fabric is dyed with *Eupatorium adenophorum* dye solution. Then, 1-ethyl-(3-dimethylaminopropyl)carbodiimide (EDC) and bone glue are used to perform a stereolinking finishing process on the dyed silk fabric, resulting in a washable dyed silk fabric. This not only facilitates the resource utilization of *Eupatorium adenophorum* but also achieves ecological finishing and color fixation of the silk fabric, expanding the application areas of silk fabrics.

[0008] The first objective of this invention is to provide a method for preparing a washable silk fabric based on *Eupatorium adenophorum*, comprising the following steps:

[0009] S1. The silk fabric is immersed in the dyeing solution of Eupatorium fortunei to obtain the dyed silk fabric.

[0010] S2. The dyed silk fabric described in S1 is immersed in 1-ethyl-(3-dimethylaminopropyl)carbodiimide (EDC) / N-hydroxysuccinimide (NHS) finishing solution for activation treatment, and then subjected to padding treatment to obtain activated dyed silk fabric.

[0011] S3. The activated dyed silk fabric described in S2 is immersed in a bone glue solution to carry out a cross-linking reaction, and then subjected to rolling and heat setting to obtain the washable silk fabric based on Agastache rugosa.

[0012] In one embodiment of the present invention, in S1, the preparation of the purple-stemmed eupatorium dye solution specifically includes the following steps: mixing purple-stemmed eupatorium powder and water evenly according to a solid-liquid ratio of 1:(4-6), and then ultrasonically treating it in an ultrasonic cleaner at 65℃-75℃ for 25min-35min, and obtaining the purple-stemmed eupatorium dye solution by centrifugation.

[0013] In one embodiment of the present invention, in S1, the staining process is as follows: the bath ratio is 1:(30-50), the pH is 4-5, the temperature is 75℃-85℃, and the time is 50min-70min.

[0014] In one embodiment of the present invention, in S2, the concentration of the 1-ethyl-(3-dimethylaminopropyl)carbodiimide (EDC) / N-hydroxysuccinimide (NHS) finishing solution is 20 g / L-100 g / L, and the pH is 4.5-5.5; the mass ratio of 1-ethyl-(3-dimethylaminopropyl)carbodiimide to N-hydroxysuccinimide is (2.8-3.2):1; if the concentration is too high, EDC will be adsorbed onto the surface of the silk, reducing the effective cross-linking of the subsequent bone glue, EDC and silk fabric, and causing waste of raw materials; if the concentration is too low, the amount of cross-linking of the bone glue will be reduced.

[0015] In one embodiment of the present invention, in S2, the activation process is as follows: the bath ratio is 1:(30-50), the temperature is 25℃-80℃, and the time is 90min-110min.

[0016] In one embodiment of the present invention, in step S3, the concentration of the bone glue solution is 50 g / L-100 g / L, and the pH is 4.5-5.5.

[0017] In one embodiment of the present invention, in S3, the crosslinking reaction process is as follows: the bath ratio is 1:(30-50), the temperature is 25℃-80℃, and the time is 90min-110min.

[0018] In one embodiment of the present invention, in S3, the heat setting temperature is 110℃-130℃ and the time is 1min-3min.

[0019] In one embodiment of the invention, in S2 and S3, the rolling mill residue after the rolling mill treatment is 95%-105%.

[0020] A second objective of this invention is to provide a washable silk fabric based on *Eupatorium fortunei* prepared by the method described above.

[0021] The mechanism of this invention is as follows: As a natural dye, *Aeonium adenophorum* cannot achieve durable and stable fixation on silk fabrics through direct impregnation and adsorption. This invention improves the adhesion of *Aeonium adenophorum* dye molecules to silk fibers through a two-step cross-linking reaction. When the dyed silk fabric is impregnated in an EDC / NHS finishing solution, the EDC in the solution promotes a more stable silk molecular chain structure. Subsequently, when the EDC-treated dyed silk fabric is impregnated with a glue solution, on the one hand, the glue and EDC undergo a cross-linking reaction to form stable amide bonds; on the other hand, excess glue fills the pores of the silk fibers, making the silk fiber structure more compact. Compared to untreated silk fabrics, the silk fabric of this invention has a higher bonding strength with the glue, and the reaction between EDC and the silk fabric also significantly improves color fastness.

[0022] The technical solution of the present invention has the following advantages compared with the prior art:

[0023] (1) The preparation method described in this invention utilizes the sequential finishing of EDC and bone glue, taking advantage of the fact that both silk fabric and bone glue contain multiple active groups that can participate in the reaction. EDC, as a cross-linking promoter, undergoes a cross-linking reaction with bone glue and silk fabric under certain conditions to form amide bonds, thereby achieving stable cross-linking. The pigment molecules of Adenophora stricta are "fixed" in the three-dimensional network structure of silk and will not fall off due to external forces such as water washing and impact, thus improving the adhesion of pigment molecules to silk.

[0024] (2) The preparation method described in this invention utilizes pigments extracted from *Ageratum aizoon* to dye silk, transforming harmful weeds into high-value resources and mitigating their ecological harm, while also endowing silk with multiple functions. The active components in *Ageratum aizoon*, such as flavonoids, flavonoids, and polyphenols, exhibit good affinity and adsorption capacity for silk, possessing both antibacterial and anti-UV functions. Among these, flavonoids have moderate water solubility, allowing them to firmly bind to silk while easily penetrating and depositing within the fiber. After the glue forms a film, these deposits are effectively fixed and do not easily diffuse outwards, thus improving the durability of the functional finish. Furthermore, EDC, as a crosslinking agent, does not remain within the glue molecules but is transformed into a water-soluble urea derivative with extremely low cytotoxicity through a series of chemical reactions during the crosslinking process. Compared to the extensive use of synthetic dyes, finishing agents, and fixing agents in traditional dyeing and finishing techniques, this method is more environmentally friendly and has significant ecological benefits. Furthermore, the main chain of bone glue is a polypeptide, which is similar to the protein structure of silk, thus it can form good adhesion on the surface and shallow layer of silk. At the same time, the polypeptide chain can also form a strong binding with the flavonoids in Adenophora stricta through hydrogen bonds, thereby further enhancing the stability of Adenophora stricta in silk.

[0025] (3) The purple stem eupatorium pigment in the washable silk fabric of the present invention is a natural dye, which gives the silk fabric a unique color and natural texture. The dyed silk fabric has good ultraviolet protection and antibacterial function, and the natural dye is harmless to human health, which meets the needs of modern consumers for green and environmentally friendly textiles.

[0026] (4) The preparation method described in this invention is simple, the operating conditions are mild, and the required equipment is commonly used in the textile processing field. It is easy to realize industrial production and has good application prospects and economic benefits. Attached Figure Description

[0027] To make the content of this invention easier to understand, the invention will be further described in detail below with reference to specific embodiments and accompanying drawings, wherein:

[0028] Figure 1 The images are SEM images of the silk fabrics prepared in Example 7 and Comparative Example 3 in Test Example 1 of the present invention; wherein, (a) is the SEM image of the silk fabric prepared in Comparative Example 3, and (b) is the SEM image of the silk fabric prepared in Example 7.

[0029] Figure 2 The images shown are SEM images of the silk fabrics prepared in Example 7 and Comparative Example 3 of Test Example 2 of the present invention before and after soaping; wherein, (a) is the SEM image of the silk fabric prepared in Example 7 before soaping, (b) is the SEM image of the silk fabric prepared in Example 7 after soaping, (c) is the SEM image of the silk fabric prepared in Comparative Example 3 before soaping, and (d) is the SEM image of the silk fabric prepared in Comparative Example 3 after soaping. Detailed Implementation

[0030] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, so that those skilled in the art can better understand and implement the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. It should be understood that the specific embodiments are only used to explain the present invention, but the embodiments are not intended to limit the present invention.

[0031] In this invention, unless otherwise stated, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0032] In this invention, unless otherwise stated, the term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0033] In this invention, unless otherwise specified, the experimental methods used in the embodiments of this invention are conventional methods, and the materials and reagents used are commercially available unless otherwise specified.

[0034] In this invention, unless otherwise stated, the preparation of the *Ageratum purpureum* dye solution used in the embodiments of this invention specifically includes the following steps: adding 40g of *Ageratum purpureum* powder to 200mL of water, adjusting the pH value to 7, placing it in an ultrasonic cleaner, ultrasonically treating it at 70℃ for 30min, centrifuging it after the procedure, and taking the supernatant to obtain the *Ageratum purpureum* dye solution.

[0035] In this invention, unless otherwise stated, the mass ratio of EDC to NHS in the EDC / NHS finishing solution used in the embodiments of this invention is 3:1, and the solvent is water.

[0036] In this invention, unless otherwise stated, the bone glue solution used in the embodiments of this invention is bone glue dissolved in water, wherein the bone glue is purchased from Shaanxi Guanchen Biotechnology Co., Ltd.

[0037] Example 1

[0038] The washable silk fabric based on *Eupatorium adenophorum* and its preparation method in this embodiment specifically include the following steps:

[0039] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0040] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 20g / L at a liquor ratio of 1:40. Shake at 25℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0041] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 50g / L at a bath ratio of 1:40. Shake the solution at 25℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0042] Example 2

[0043] The process is basically the same as in Example 1, except for the concentration of the EDC / NHS finishing solution, and specifically includes the following steps:

[0044] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0045] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 100g / L at a liquor ratio of 1:40. Shake at 25℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0046] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 50g / L at a bath ratio of 1:40. Shake the solution at 25℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0047] Example 3

[0048] The process is basically the same as in Example 1, except for the concentration of the EDC / NHS finishing solution and the treatment temperature in the EDC / NHS finishing solution. Specifically, it includes the following steps:

[0049] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0050] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 100g / L at a liquor ratio of 1:40. Shake at 80℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0051] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 50g / L at a bath ratio of 1:40. Shake the solution at 25℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0052] Example 4

[0053] The process is basically the same as in Example 1, except for the concentration of the EDC / NHS finishing solution and the treatment temperature in the EDC / NHS finishing solution. Specifically, it includes the following steps:

[0054] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0055] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 100g / L at a liquor ratio of 1:40. Shake at 40℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0056] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 50g / L at a bath ratio of 1:40. Shake the solution at 25℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0057] Example 5

[0058] The process is basically the same as in Example 1, except for the concentration of the EDC / NHS finishing solution, the treatment temperature in the EDC / NHS finishing solution, and the concentration of the bone glue solution. Specifically, it includes the following steps:

[0059] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0060] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 100g / L at a liquor ratio of 1:40. Shake at 40℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0061] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 100g / L at a bath ratio of 1:40. Shake the solution at 25℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0062] Example 6

[0063] The procedure is basically the same as in Example 1, except for the concentration of the EDC / NHS finishing solution, the treatment temperature in the EDC / NHS finishing solution, the concentration of the bone glue solution, and the treatment temperature in the bone glue solution. Specifically, it includes the following steps:

[0064] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0065] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 100g / L at a liquor ratio of 1:40. Shake at 40℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0066] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 100g / L at a bath ratio of 1:40. Shake the solution at 80℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0067] Example 7

[0068] The procedure is basically the same as in Example 1, except for the concentration of the EDC / NHS finishing solution, the treatment temperature in the EDC / NHS finishing solution, the concentration of the bone glue solution, and the treatment temperature in the bone glue solution. Specifically, it includes the following steps:

[0069] S1. Immerse 1g of silk fabric in the purple stem eupatorium dye liquor at a liquor ratio of 1:40 for dyeing. Adjust the pH value to 4.2, raise the temperature to 80℃, keep warm for 60min, and air dry at room temperature to obtain the dyed silk fabric.

[0070] S2. Immerse 1g of dyed silk fabric in EDC / NHS finishing solution with pH value of 5 and concentration of 100g / L at a liquor ratio of 1:40. Shake at 40℃ for 100min. After the treatment, perform a padding process with a padding rate of 100% to obtain activated dyed silk fabric.

[0071] S3. Immerse 1g of activated dyed silk fabric in a bone glue solution with a pH of 5 and a concentration of 100g / L at a bath ratio of 1:40. Shake the solution at 40℃ for 100min. After the treatment, perform a roll-up process with a roll-up rate of 100%. Heat set the solution at 120℃ for 2min to obtain a washable silk fabric based on Eupatorium fortunei.

[0072] Comparative Example 1

[0073] The method is basically the same as in Example 7, except that the purple stem eupatorium dye solution is replaced with curcumin dye solution.

[0074] Comparative Example 2

[0075] The method is basically the same as in Example 7, except that the purple stem eupatorium dye solution is replaced with radish red dye solution.

[0076] Comparative Example 3

[0077] The process is basically the same as in Example 7, except that EDC / NHS finishing solution is not used.

[0078] Comparative Example 4

[0079] The process is basically the same as in Example 7, except that the EDC / NHS finishing solution is replaced with glutaraldehyde finishing solution.

[0080] Comparative Example 5

[0081] It is basically the same as Example 7, except that bone glue solution is not used for finishing.

[0082] Comparative Example 6

[0083] The method is basically the same as in Example 7, except that the bone glue solution is replaced with a starch solution.

[0084] Comparative Example 7

[0085] It is basically the same as Example 7, except that only dyeing is performed, and no color fixing and finishing are performed.

[0086] Test Example 1

[0087] The silk fabrics prepared in Example 7 and Comparative Example 3 were characterized using a desktop scanning electron microscope (SEM) TM 3030 (Hitachi, USA). The results are as follows: Figure 1 As shown. From Figure 1It can be seen that the silk fabric of Example 7 forms a thicker film with a certain degree of toughness, significantly reduces cracks, and appears as a flexible material that easily adheres to the silk fibers; the silk fabric of Comparative Example 3 forms a more brittle film with an obvious cracked structure, containing a large number of discontinuous cracks, and easily falls off the silk fibers.

[0088] Test Example 2

[0089] Referring to the standard GB / T 3921-2008 "Textiles - Tests for Color Fastness to Soap Washing", the silk fabrics prepared in Example 7 and Comparative Example 3 were soap washed once. The silk fabrics before and after soap washing were characterized using a desktop scanning electron microscope. The results are as follows: Figure 2 As shown. From Figure 2 It can be seen that before soaping, the silk fabrics prepared in Example 7 and Comparative Example 3 had obvious color-fixing films. After soaping, the color-fixing film on the silk fabric prepared in Example 7 showed good adhesion stability, with only slight peeling, and the overall structure of the film remained intact. However, the color-fixing film on the silk fabric prepared in Comparative Example 3 almost completely disappeared after soaping, and no obvious film residue was observed. This is because EDC, as a crosslinking agent, has a strong electrophilicity in its carbodiimide group (-N=C=N-), which reacts with the carboxyl groups (-COOH) on the surface of the dyed silk fabric, activating the carboxyl groups and forming an O-acylisourea active intermediate. Subsequently, when the dyed silk fabric treated with EDC is immersed in a glue solution, the O-acylisourea active intermediate undergoes a nucleophilic substitution reaction with the amino groups in the glue molecules to form amide bonds, thereby achieving stable crosslinking.

[0090] Test Example 3

[0091] The silk fabrics prepared in Examples 1-7 and Comparative Examples 1-7 were soaped once. The color depth K / S values ​​of the silk fabrics before and after soaping were tested and evaluated using a spectrophotometer (HunterLab). The decrease rate ΔK / S of the K / S value after soaping was calculated. The results are shown in Table 1.

[0092] Table 1

[0093]

[0094]

[0095] As can be seen from Table 1, the ΔK / S ratio of the silk fabrics prepared in the examples is less than 16% after soaping, indicating that the EDC / NHS-bone glue two-step crosslinking system can construct a dense three-dimensional network on the surface of silk, firmly "anchoring" the pigment of Agastache rugosa, and greatly inhibiting the pigment loss caused by washing.

[0096] Comparing Example 1 and Comparative Example 1, it can be seen that the ΔK / S of Example 1 is much lower than that of Comparative Example 1 (57.9%). This is because curcumin is highly hydrophobic and poorly water-soluble, making it difficult to penetrate evenly into the silk; its molecular weight is small and it only contains a diketone structure, lacking active sites for covalent cross-linking with the EDC-gelatin system. The pigment can only be adsorbed by weak van der Waals forces, and therefore it is very easy to fall off during the soaping process.

[0097] Comparing Example 1 and Comparative Example 2, it can be seen that the ΔK / S of Example 1 is significantly lower than that of Comparative Example 2 (72.7%). This is because although radish red pigment has good water solubility, it has a small molecular weight and high charge density, which makes it easy to form unstable electrostatic adsorption on the fiber surface. During soaping, it is released from the fiber, causing the color to lighten.

[0098] Comparing Example 1 and Comparative Example 3, it can be seen that the ΔK / S of Example 1 is much lower than that of Comparative Example 3 (80.7%). This is because, without EDC activation, the carboxyl groups on the surface of the silk are not converted into highly active O-acyl isourea intermediates, and the bone glue cannot form stable amide bonds with them, resulting only in physical deposition. Therefore, the entire film layer is detached during soaping, and a large amount of pigment is lost as a result.

[0099] Comparing Example 1 and Comparative Example 4, it can be seen that the ΔK / S of Example 1 is significantly lower than that of Comparative Example 4 (75.2%). This is because glutaraldehyde, as a hydroxyl crosslinking agent, can crosslink with silk and bone glue, but the reaction is unstable, and the residual aldehyde group is cytotoxic.

[0100] Comparing Example 1 and Comparative Example 5, it can be seen that the ΔK / S of Example 1 is much lower than that of Comparative Example 5 (78.0%). This is because, without the film-forming and filling effect of bone glue, the intermediate generated by EDC activation only reacts with silk and cannot form a film structure with color-fixing effect on the fiber surface, which is easily peeled off during washing.

[0101] Comparing Example 1 and Comparative Example 6, it can be seen that the ΔK / S of Example 1 is significantly lower than that of Comparative Example 6 (81.0%). This is because starch contains only hydroxyl groups, which cannot accept EDC-activated carboxyl groups, nor can they form covalent bonds with collagen, and can only be physically coated; during soaping, the starch film swells and ruptures, and the pigment is rapidly lost.

[0102] Comparing Example 1 and Comparative Example 7, it can be seen that the ΔK / S of Example 1 is much lower than that of Comparative Example 7 (86.2%). This is because when only dyeing is performed without any color fixation treatment, the pigment of Agastache rugosa is adsorbed only by hydrogen bonds and van der Waals forces, lacking chemical bonding and film-forming protection. It is then largely removed after a single soaping wash, resulting in the worst fastness.

[0103] In summary, this invention uses Eupatorium fortunei dye to dye silk fabrics, and then uses EDC and bone glue to perform a two-step immersion finishing process on the dyed silk fabrics, resulting in silk fabrics with excellent wash resistance. This solves the problems of waste of natural plant extract resources, poor wash resistance of silk fibers, and potential biotoxicity of some traditional mordants and fixing agents in traditional dyeing and finishing technologies, and has extremely broad application prospects.

[0104] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for preparing a washable silk fabric based on *Eupatorium adenophorum*, characterized in that, Includes the following steps: S1. The silk fabric is immersed in the dyeing solution of Eupatorium fortunei to obtain the dyed silk fabric. S2. The dyed silk fabric described in S1 is immersed in a 1-ethyl-(3-dimethylaminopropyl)carbodiimide / N-hydroxysuccinimide finishing solution for activation treatment, and then subjected to a rolling process to obtain the activated dyed silk fabric. S3. The activated dyed silk fabric described in S2 is immersed in a bone glue solution to carry out a cross-linking reaction, and then subjected to rolling and heat setting to obtain the washable silk fabric based on Agastache rugosa.

2. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S1, the preparation of the purple-stemmed eupatorium dye solution specifically includes the following steps: mixing purple-stemmed eupatorium powder and water evenly according to a solid-liquid ratio of 1:(4-6), and then ultrasonically treating it in an ultrasonic cleaner at 65℃-75℃ for 25min-35min, and obtaining the purple-stemmed eupatorium dye solution by centrifugation.

3. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S1, the dyeing process is as follows: bath ratio of 1:(30-50), pH of 4-5, temperature of 75℃-85℃, and time of 50min-70min.

4. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S2, the concentration of the 1-ethyl-(3-dimethylaminopropyl)carbodiimide / N-hydroxysuccinimide finishing solution is 20 g / L-100 g / L, and the pH is 4.5-5.5; the mass ratio of 1-ethyl-(3-dimethylaminopropyl)carbodiimide to N-hydroxysuccinimide is (2.8-3.2):

1.

5. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S2, the activation process is as follows: the bath ratio is 1:(30-50), the temperature is 25℃-80℃, and the time is 90min-110min.

6. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S3, the concentration of the bone glue solution is 50 g / L-100 g / L, and the pH is 4.5-5.

5.

7. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S3, the crosslinking reaction process is as follows: the bath ratio is 1:(30-50), the temperature is 25℃-80℃, and the time is 90min-110min.

8. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S3, the heat setting temperature is 110℃-130℃, and the time is 1min-3min.

9. The method for preparing washable silk fabric based on *Eupatorium adenophorum* according to claim 1, characterized in that, In S2 and S3, the rolling mill residue after the rolling mill process is 95%-105%.

10. A washable silk fabric based on *Eupatorium fortunei* prepared by the method according to any one of claims 1-9.

Images