Dyeing process of real silk fabric

By mixing the madder dye with safflower dye, dissolved in ethanol solution and ultrasonic treatment, the problems of uneven dyeing of silk fabrics and protein denaturation are solved, and efficient and uniform dyeing effect is achieved.

CN119593231APending Publication Date: 2025-03-11WUJIANG SANGSHANG SILK CO LTD
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Patent Information

Application Number
CN202411731955.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-29
Publication Date
2025-03-11

AI Technical Summary

Technical Problem

In the prior art, when using madder dye to dye silk fabrics, the content of dye in the dye solution is low, resulting in uneven dyeing and insufficient dyeing rate. At the same time, high-temperature dyeing will damage the structure of the silk fabric.

Method used

The madder dye is mixed with safflower dye, dissolved in ethanol solution to form a dye solution, and ultrasonic treatment is carried out under low temperature conditions, and pre-media treatment and color fixation treatment are carried out in combination with the mottled liquid and the acid color fixation liquid.

Benefits of technology

It improves the solubility and dispersion of dyes, ensures uniform distribution and high dyeing rate, and reduces the probability of protein denaturation of silk fabrics during dyeing.

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Abstract

The invention discloses a real silk fabric dyeing process, which comprises: dye preparation: dissolving a madder dye and a safflower dye in an ethanol solution to prepare a dye liquid, and carrying out ultrasonic treatment on the dye liquid at a temperature of 40-50 DEG C; real silk pretreatment: washing real silk with clear water; carrying out pre-mordanting treatment on the cleaned real silk by utilizing mordanting liquid under the condition of 40-50 DEG C; real silk dyeing: heating the dye liquor by 2 DEG C every 3-5 minutes, keeping the dye liquor in a constant-temperature state when the temperature is 65-70 DEG C, and dyeing for 1.5-2 hours under a sealed condition; carrying out real silk post-treatment; and S3, carrying out color fixation on the real silk dyed in the step S3 by using an acidic color fixation solution, then cleaning, and drying at 50-60 DEG C to obtain the real silk fabric with the color between orange and red. The problem that in the prior art, due to the fact that the content of madder dye in dye liquor is not high, when real silk fabric needs to be subjected to high-temperature dyeing, protein fibers forming real silk are denatured is solved.
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Description

Technical Field

[0001] The invention relates to the field of textile technology, in particular to a dyeing process for real silk fabrics. Background Art

[0002] Silk fabrics are popular for their unique luster, soft feel and good breathability. As consumers pay more attention to the quality of textiles, silk fabrics with various appearance colors dyed by different dyeing processes have gradually appeared in the eyes of consumers. Using plant dyes to dye silk is already a common process. Rubia cordifolia L. is a plant of the Rubiaceae family. Its root has the effects of cooling blood and removing blood stasis. It is a common medicinal material. At the same time, Rubia cordifolia is also one of the earliest red natural dyes used by humans and one of the most commonly used fabric dyes.

[0003] Silk fabric is a protein fiber fabric, and the process of dyeing silk with madder dye is also widely used. However, the main component of madder dye is alizarin, which belongs to the anthraquinone compound and is usually difficult to dissolve in water. The content of madder dye in the dye solution is usually low. In order to solve the water solubility problem of madder and make madder dye better for dyeing, the existing technical means usually use a high-temperature dyeing process for dyeing. However, the protein fibers that make up the silk fabric will increase the probability of denaturation as the temperature rises, which may destroy the structure of the silk fabric during the dyeing process. Therefore, it is necessary to optimize the dyeing process of silk fabric to solve the problems of uneven silk dyeing and insufficient dye uptake that may be caused by the low content of madder dye in the dye solution, while ensuring that the silk fabric can be fully and evenly dyed at low temperature to reduce the probability of protein fiber denaturation. Summary of the invention

[0004] The invention overcomes the shortcomings of the prior art and provides a dyeing process for silk fabrics.

[0005] To achieve the above object, the technical solution adopted by the present invention is: a dyeing process for silk fabrics, characterized in that it comprises the following steps:

[0006] S1. Dissolving madder dye and safflower dye in an ethanol solution to prepare a dye solution, and subjecting the dye solution to ultrasonic treatment at a temperature of 40-50° C.; the madder dye is a solid granular dye extracted from the roots of a plant of the Rubiaceae family and processed therefrom, and the safflower dye is a solid granular dye extracted from a safflower plant and processed therefrom and whose main component is safflower yellow pigment;

[0007] S2, washing the silk with clean water to remove impurities and grease on the surface of the silk, then preparing a mordant solution, and using the mordant solution to pre-treat the washed silk at 40-50°C;

[0008] S3, controlling the dyeing bath ratio of silk to dye solution at 1:45-1:50, then gradually heating the dye solution by 2°C every 3-5 minutes, and maintaining the dye solution at a constant temperature when the temperature is between 65-70°C, immersing the silk treated with pre-medium in S2 in the dye solution for dyeing, and dyeing under sealed conditions for 1.5-2h;

[0009] S4, using an acidic fixing solution to fix the color of the silk dyed in S3, and then washing the fixed silk to remove the floating color on the surface of the silk and drying it.

[0010] In a preferred embodiment of the present invention, the ethanol solution in step S1 is an ethanol aqueous solution with a concentration of 45%-55%.

[0011] In a preferred embodiment of the present invention, the ratio of safflower dye to madder dye is between 2:5 and 5:2.

[0012] In a preferred embodiment of the present invention, in step S1, the specific steps of dissolving the madder dye and safflower dye in an ethanol solution include:

[0013] S11, heating the ethanol solution to 40-50° C., gradually adding alizarin powder to the ethanol solution while stirring until the solid granular alizarin powder is completely dissolved;

[0014] S12, gradually adding safflower yellow pigment powder to the solution obtained in step S11, and continuing heating and stirring until the safflower yellow pigment powder is completely dissolved.

[0015] S13, observing the color change of the dye solution, repeating step S11 or step S12 until the solution shows the desired color, standing for 10-15 minutes, and filtering the dye solution with a microporous filter membrane to obtain the dye solution.

[0016] In a preferred embodiment of the present invention, the mordant in step S2 uses alum as a mordant, the alum accounts for 5-8% of the dry weight of the silk, and the bath ratio of the silk to the mordant is controlled between 1:45-1:50.

[0017] In a preferred embodiment of the present invention, in step S4, the specific method for fixing the color of the silk comprises: immersing the silk in an acidic color fixing solution for 10-15 minutes, wherein the acidic color fixing solution is one of an 8%-10% citric acid color fixing solution or a 5%-8% acetic acid color fixing solution.

[0018] In a preferred embodiment of the present invention, the ultrasonic treatment frequency is 45-60 kHz, and the ultrasonic treatment duration is 20-30 min.

[0019] In a preferred embodiment of the present invention, in step S4, the temperature for drying the silk is controlled at 50-60° C., and the drying time is 30-60 min;

[0020] A preferred embodiment of the present invention provides a dyeing device for silk fabrics, comprising a dye pool, a material guide device located on both sides of the dye pool, a dye temperature control device located in the dye pool, a liquid preparation barrel connected to the dye pool through a first connecting pipe, and a distillation box connected to the dye pool through a second connecting pipe; the dye temperature control device is used to control the temperature of the dye in the dye pool, the liquid preparation barrel is used to prepare the dye, and the distillation box is used to separate ethanol, water, madder dye and safflower dye in the excess dye after dyeing;

[0021] The liquid preparation barrel is provided with an ultrasonic treatment device, a stirring device and a liquid preparation temperature control device; the ultrasonic treatment device is used to perform ultrasonic treatment on the dye solution in the liquid preparation barrel, the stirring device is used to uniformly stir the dye solution in the liquid preparation barrel, and the liquid preparation temperature control device is used to control the temperature of the dye solution in the liquid preparation barrel;

[0022] The distillation box is provided with a dye liquid cavity, which is connected to the distillation cavity of the dye liquid cavity through a third connecting pipe arranged at the upper part of the dye liquid cavity. The distillation cavity is provided with a condenser; the condenser is used to condense the gas evaporated in the dye liquid cavity and flowing into the distillation cavity into liquid.

[0023] In a preferred embodiment of the present invention, the first connecting pipe and the second connecting pipe are both provided with a liquid pump for providing a power source to transfer the dye solution between the liquid preparation barrel, the dye solution pool and the distillation box.

[0024] The present invention solves the defects existing in the background technology and has the following beneficial effects:

[0025] (1) The present invention mixes madder dye and safflower dye, dissolves them in an ethanol solution to form a dye liquor, and utilizes the property of madder dye that can form chemical bonds or physical crosslinks with silk fibers during dyeing, thereby enhancing the interaction between fibers, thereby improving the wrinkle resistance of silk and reducing the splitting phenomenon of silk. At the same time, the solubility of madder dye in water is low. Compared with the prior art, the solubility and dispersibility of madder dye in the dye liquor are improved by utilizing the ethanol solution, the content of madder dye in the dye liquor is increased, the dyeing and dyeing uniformity of the dye are ensured, and at the same time, the safflower dye is combined with the safflower dye to utilize the safflower dye. The carboxyl group of safflower yellow in the material forms hydrogen bonds with the alizarin molecules in madder dye, which further promotes the dispersion and dissolution of alizarin in the low-temperature dye solution, ensuring the dyeing uniformity and dyeing rate of the silk fabric; in addition, the hydroxyl group of safflower dye not only enhances its own water solubility, but also partially destroys the π-π stacking effect between alizarin molecules through hydrogen bonding, which is one of the reasons why alizarin molecules aggregate to form large particles. By reducing this stacking effect, safflower dye helps prevent alizarin molecules from aggregating to form lakes, making them more evenly dispersed in the dye solution combined with ethanol aqueous solution.

[0026] (2) In the process of dye preparation, the present invention also performs ultrasonic treatment on the dye solution, and utilizes ultrasonic wave to further destroy hydrogen bonds between dye molecules, thereby increasing the dispersion of molecules, thereby providing more contact opportunities for safflower dye hydroxyl group and alizarin molecules, increasing the formation of hydrogen bonds, and further improving the solubility and dispersibility of madder dye and safflower dye in low-temperature dye solution. Compared with the prior art, the formation of a large number of hydrogen bonds makes the solubility and dispersibility of the dye in the dye solution higher, and the content of the dye in the dye solution of the same temperature and dosage is higher. Under the condition of the same dyeing rate, the temperature requirement for silk dyeing using madder dye is lower, which greatly reduces the probability of protein denaturation in silk fabrics.

[0027] (3) In the present invention, safflower dye and madder dye are combined, and ethanol aqueous solution is used as a solvent to form a dye solution. Compared with the prior art, the silk fabric dyed with madder dye has the characteristics of high wrinkle resistance and reduced splitting, and it is also ensured that the safflower dye and madder dye can be fully dispersed and dissolved in the ethanol solution at a lower temperature than the prior art, thereby improving the utilization rate of the dye; at the same time, the hydrogen bonds formed between the safflower yellow pigment molecules of the safflower dye and the alizarin molecules of the madder dye are further utilized to further improve the dispersibility of the madder dye and the safflower dye in the low-temperature dye solution. Compared with the prior art, the required temperature for dyeing the silk fabric is lower, which ensures the dyeing effect while greatly reducing the probability of protein denaturation in the silk fabric. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative work.

[0029] Figure 1 is a process step diagram of a preferred embodiment of the present invention;

[0030] Figure 2 It is a schematic diagram of the structure of the dyeing device in the present invention. DETAILED DESCRIPTION

[0031] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0032] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein. Therefore, the protection scope of the present invention is not limited to the specific embodiments disclosed below.

[0033] like Figure 1 As shown, a dyeing process for silk fabrics comprises the following steps:

[0034] S1. Preparation of dye liquor; Two dyes are added to the dye liquor, including madder dye and safflower dye. The madder dye is a solid granular dye extracted from the roots of the madder family plants and processed, which can be purchased from the market. The safflower dye is a solid granular dye extracted from the safflower plant and processed, which can be purchased from the market and whose main component is safflower yellow pigment; the madder dye and safflower dye are dissolved in ethanol solution to prepare dye liquor, and the dye liquor is subjected to ultrasonic treatment at a temperature of 40-50°C. Specifically, the ultrasonic treatment frequency is 45-60kHz, and the ultrasonic treatment duration is 20-30min. Ultrasonic treatment can increase the number of hydrogen bonds formed between madder molecules and safflower yellow pigment molecules in ethanol aqueous solution, thereby greatly increasing the solubility of the dye in the dye liquor, and increasing the content of the dye in the dye liquor, thereby ensuring that the dye liquor contains sufficient dye during dyeing, and the dyeing rate of the dye will not be affected over time, thereby improving the dyeing uniformity of the silk fabric.

[0035] The main component of madder dye is alizarin molecule, with the chemical formula C 14 H8 O 4 , containing the basic skeleton of anthraquinone. Anthraquinone compounds are usually insoluble in water. According to the principle of like dissolves like, polar molecules tend to dissolve in polar solvents, and non-polar molecules tend to dissolve in non-polar solvents. The alizarin molecule is an organic compound with a certain polarity, and ethanol is also a polar molecule containing hydroxyl groups (-OH). Therefore, according to the principle of like dissolves like, alizarin has a better solubility in ethanol than in water, so madder dye has a higher solubility in ethanol-containing solutions and is more evenly dispersed. Safflower yellow has a higher solubility in water and good dispersibility. The mixed use of safflower dye and madder dye forms hydrogen bonds between the hydroxyl groups of safflower dye and the alizarin molecules. This hydrogen bond The formation helps to bridge the alizarin molecules with water molecules, thereby promoting the dissolution and dispersion of alizarin in low-temperature dye solution, thereby improving the dispersion uniformity of the dye in the entire dye solution and reducing the formation of color lakes. Even under low-temperature conditions where alizarin is not water-soluble, a more uniform and saturated dyeing effect can be achieved through the formation of more hydrogen bonds. In addition, the hydroxyl group of safflower dye not only enhances its own water solubility, but also partially destroys the π-π stacking effect between alizarin molecules through hydrogen bonding, which is one of the reasons why alizarin molecules aggregate to form large particles. By reducing this stacking effect, safflower dye helps prevent alizarin molecules from aggregating to form color lakes, making them more evenly dispersed in the dye solution combined with ethanol and aqueous solution.

[0036] Moreover, safflower dye and madder dye have similar color systems, safflower dye is orange and madder is red. The color of silk dyed by combining the two is between the colors of safflower dye and madder dye. It is easy to adjust the content of a single dye to ensure that the dyeing color system meets the color requirements of the dyeing process.

[0037] The dye liquor is subjected to ultrasonic treatment, and the acoustic flow and micro-jet generated by ultrasonic vibration can strongly stir the dye liquor, increase the contact area between safflower dye particles, madder dye particles and ethanol aqueous solution, thereby improving the dispersion efficiency and solubility of the dye, and further ensuring the uniformity of silk dyeing.

[0038] The invention adopts a combination of safflower dye and madder dye and uses ethanol aqueous solution as solvent, so that the safflower dye is in contact with the madder molecules to form more hydrogen bonds, and the madder dye with low water solubility can be evenly dispersed and dissolved in the dye solution even under low temperature conditions. Compared with the existing technology, the purpose of dyeing silk fabrics at a lower temperature is achieved, thereby reducing the probability of denaturation of protein fibers constituting the silk fabrics during the dyeing process without reducing the dye content in the dye solution to ensure the saturation and uniformity of the dyeing.

[0039] S2. Pretreatment of silk: Wash the silk with clean water to remove impurities and grease on the surface of the silk, then prepare a mordant solution, and use the mordant solution to pre-treat the washed silk at 40-50°C; the mordant solution at 40-50°C can ensure the activity of the mordant molecules in the mordant solution, so that they are evenly dispersed in the mordant solution, thereby increasing the rate at which the mordant solution is dispersed and attached to the silk fabric. Pre-mordant treatment of silk can significantly improve the color fastness of silk fabrics during dyeing and enhance the bonding force between dyes and fibers.

[0040] S3, silk dyeing: control the dyeing bath ratio of silk to dye solution at 1:45-1:50, then gradually heat up the dye solution, heating it up by 2°C every 3-5 minutes, keep the dye solution at a constant temperature when the temperature is between 65-70°C, immerse the silk treated with pre-medium in S2 in the dye solution for dyeing, and dye it under sealed conditions for 1.5-2h; the heating rate of the dye solution will affect the uniformity of the dye dispersion in the dye solution, too high a heating rate causes the dye to dissolve quickly, the dye molecules to move violently, and the concentration in the dye solution is uneven, while too low a heating rate can ensure the uniformity of the dye concentration in the dye solution, but the dyeing efficiency is not high, so controlling the heating rate to heat up by 2°C every 3-5 minutes can ensure the uniformity of the dye dispersion in various parts of the dye solution and ensure efficient dyeing operations.

[0041] For natural dyes, too high temperature will cause the decomposition or color change of natural dyes. At the same time, for silk fabrics composed of protein fibers, controlling the temperature at 65-70℃ can minimize the possibility of protein denaturation and ensure that the dye is evenly dissolved and dispersed in the dye solution, thereby ensuring high-efficiency, high-saturation and uniform dyeing without damaging the silk structure.

[0042] S4, post-treatment of silk; using an acidic fixing solution to fix the color of the silk dyed in S3, and then washing the fixed silk, washing away the floating color on the surface of the silk, and drying it at 50-60° C. for 30-60 minutes to obtain a silk fabric with a color between orange and red.

[0043] The cationic groups in the acidic fixing solution can form ionic bonds with the anionic groups in the dye molecules, thereby firmly fixing the dye on the fiber, enhancing the binding force between the dye and the fiber, that is, improving the color fastness of the dyeing.

[0044] Choosing to dry silk fabrics at 50-60℃ can fully evaporate the dye solution after dyeing and fixing, while also preventing the denaturation of protein fibers in the silk fabric and ensuring the structural stability of the silk fabric.

[0045] Specifically, the ethanol solution in step S1 is a 45%-55% ethanol aqueous solution, and the ratio of safflower dye to madder dye is between 2:5 and 5:2; madder dye has good solubility with ethanol, and the use of ethanol solution as the solvent of the dye solution ensures the dissolution of madder dye in the dye solution, which helps to form hydrogen bonds between alizarin molecules and ethanol, while safflower dye has high water solubility, and the use of 45-55% ethanol aqueous solution as the solvent can simultaneously ensure that both dyes have high solubility in the dye solution, increase the content of the dye in the dye solution, thereby ensuring that the dyeing of silk has high color saturation.

[0046] Specifically, in step S1, the specific steps of dissolving madder dye and safflower dye in ethanol solution include: S11, heating the ethanol solution to 40-50° C., gradually adding alizarin powder to the ethanol solution, and stirring at the same time, until the solid granular alizarin powder is completely dissolved;

[0047] S12, gradually adding safflower yellow pigment powder to the solution obtained in step S11, and continuing heating and stirring until the safflower yellow pigment powder is completely dissolved.

[0048] S13, observing the color change of the dye solution, repeating step S11 or step S12 until the solution shows the desired color, standing for 10-15 minutes, and filtering the dye solution with a microporous filter membrane to obtain the dye solution.

[0049] Heating and stirring can improve the uniform dissolution of alizarin powder and safflower yellow pigment powder in the ethanol solution. By repeating steps S11 and S12 to unidirectionally adjust the amount of one of the dye powders, dye solutions of different colors can be adjusted. By standing, the undissolved dye particles in the solution can be precipitated in the solution. By filtering through a microporous filter membrane, these excess dye particles can be separated from the solution, thereby ensuring that the dye is completely dissolved in the dye solution and the dyeing uniformity of the dye solution is ensured.

[0050] Specifically, the mordant in step S2 uses alum as a mordant, alum accounts for 5-8% of the dry weight of silk, and the bath ratio of silk to mordant is controlled between 1:45-1:50. Alum can form chemical bonds with protein fibers in silk fabrics and form complexes with dyes to increase the adhesion of dyes on fibers, thereby improving the dyeing and dyeing fastness of the dyes.

[0051] Specifically, in step S4, the specific method for fixing the color of the silk includes: immersing the silk in an acidic color fixing solution for 10-15 minutes, and the acidic color fixing solution is one of 8%-10% citric acid color fixing solution or 5%-8% acetic acid color fixing solution. Using citric acid color fixing solution or acetic acid color fixing solution to fix the color of the silk can significantly improve the color fastness and uniformity after dyeing and the protective effect on the fiber, ensuring the stability and durability of the dyeing effect.

[0052] Embodiment 1:

[0053] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0054] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 2:5; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0055] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0056] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions;

[0057] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0058] Embodiment 2:

[0059] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0060] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 3:5; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0061] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0062] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions.

[0063] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0064] Embodiment three:

[0065] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0066] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 4:5; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0067] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0068] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions.

[0069] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0070] Embodiment 4:

[0071] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0072] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 5:5; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0073] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0074] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions.

[0075] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0076] Embodiment five:

[0077] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0078] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 5:4; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0079] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0080] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions.

[0081] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0082] Embodiment six:

[0083] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0084] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 5:3; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0085] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0086] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions.

[0087] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0088] Embodiment seven:

[0089] This embodiment provides a dyeing process for silk fabrics, comprising the following steps:

[0090] S1, dye solution preparation; madder dye and safflower dye are added to the dye solution, and the ratio of madder dye to safflower dye is 5:2; madder dye and safflower dye are dissolved in 50% ethanol solution to prepare a dye solution, and the dye solution is subjected to ultrasonic treatment at a temperature of 50° C., the ultrasonic treatment frequency is 50 kHz, and the ultrasonic treatment time is 20 min;

[0091] S2, pretreatment of silk: washing the silk with clean water to remove impurities and grease on the surface of the silk, and then preparing a mordant solution, using alum as the mordant solution, controlling the bath ratio of silk to the mordant solution to be 1:50, and the alum content to be 6% of the dry weight of the silk, immersing the silk in the mordant solution, controlling the temperature of the mordant solution to be 50° C., and the immersion time to be 30 minutes, and constantly stirring the mordant solution during the pre-mordant period;

[0092] S3, silk dyeing: put the dye solution prepared in S1 into the dyeing tank, control the dyeing bath ratio of silk to dye solution to be 1:50, then gradually increase the temperature of the dye solution by 2°C every 3 minutes, keep the dye solution at a constant temperature at 70°C, immerse the silk treated with pre-media in S2 in the dye solution for dyeing, and dye for 2 hours under sealed conditions.

[0093] S4, post-treatment of silk; using 8% citric acid fixing solution to fix the silk dyed in S3, then washing the fixed silk, washing off the floating color on the silk surface and drying at 55°C for 45 minutes to obtain a silk fabric with a color between orange and red.

[0094] Experiment 1: Dyeing effect test. Select three positions at least 1m apart on the silk fabric that has completed the dyeing process. Use X-Rite Ci7600 series colorimeter to test and get the K / S values ​​of the three positions. K / S value is a parameter used to describe the color depth of the material, where K represents the absorption coefficient and S represents the scattering coefficient. The difference between the maximum K / S value and the minimum K / S value is taken as the color depth difference (ΔK / S). The average of the three K / S values ​​obtained from the test is taken as the average K / S value. Use X-Rite Model 16Plus Ci series friction color fastness tester to test the color fastness of silk fabric.

[0095] Table 1 Dyeing effect test data of Examples 1 to 7

[0096] Ratio of madder to safflower Color depth difference (ΔK / S) Color fastness Average K / S value 2:5 0.4 4 2.0 3:5 0.3 4 2.2 4:5 0.3 4 2.6 5:5 0.3 4 2.9 5:4 0.3 4 3.2 5:3 0.2 4 3.6 5:2 0.3 4 3.7

[0097] It can be seen from Table 1 that the K / S value increases with the increase of madder dye in the dye ratio, and the color depth difference is the smallest when the ratio of madder dye to safflower dye is 5:3, which means that the silk dyeing has the best dyeing uniformity and a higher color uptake rate at 5:3. In addition, the color fastness rating is 4, which shows that the silk dyed by this dyeing process has good color fastness.

[0098] Experiment 2: Maximum solubility test, take 3 parts of 50% ethanol aqueous solution, each part is 100g, and the temperature is raised to 50℃. Take 3 parts of dye, namely 10g madder dye particles, 10g safflower dye particles and 10g madder dye and 10g safflower dye mixed dye, and dissolve them in ethanol solution to prepare 3 parts of dye solution. Stir evenly during dissolution and undergo ultrasonic treatment until the dye solution has no color change. Then, filter the dye solution with a microporous filter membrane to separate the excess solid dye from the dye solution, and dry and evaporate the liquid attached to the filtered solid dye. Use an electronic balance to measure the weight of the remaining solid dye and calculate the solubility of the dye in the dye solution.

[0099] Table 2 Maximum solubility test data

[0100] Ethanol solution / g Madder dye / g Safflower dye / g Dye after filtration / g Solubility 100 10 0 8.902 1.098% 100 0 10 7.884 2.116% 100 10 10 14.721 5.279%

[0101] It can be seen from Table 2 that the solubility of the dye obtained by mixing madder dye and safflower dye and dissolving them together in ethanol solution is significantly greater than the solubility of a single dye in ethanol solution. The reason is that more hydrogen bonds will be formed between the madder dye molecules in the madder dye and the safflower yellow pigment molecules in the safflower dye under the action of ultrasound, thereby increasing the solubility of the madder dye and the safflower dye in the ethanol solution, so that the dye solution obtained by mixing the two dyes has a higher content of dye at a lower temperature, thereby ensuring that under the same dyeing temperature conditions, the dye solution prepared by this process has a higher content of madder dye and safflower dye than the prior art under the same temperature conditions, and when the temperature during the dyeing of silk fabrics is reduced, the dissolution of sufficient dyes in the dye solution can be ensured, thereby reducing the possibility of denaturation of protein fibers constituting the silk fabrics.

[0102] like Figure 2 As shown, a dyeing device for silk fabrics comprises a dyeing liquid pool, a material guiding device located at both sides of the dyeing liquid pool, a dyeing liquid temperature control device located in the dyeing liquid pool, a liquid preparation barrel connected to the dyeing liquid pool through a first connecting pipe, and a distillation box connected to the dyeing liquid pool through a second connecting pipe; the dyeing liquid temperature control device is used to control the temperature of the dyeing liquid in the dyeing liquid pool, the liquid preparation barrel is used to prepare the dyeing liquid, and the distillation box is used to separate ethanol, water, madder dye and safflower dye from the excess dyeing liquid after dyeing;

[0103] The liquid preparation barrel is provided with an ultrasonic treatment device, a stirring device and a liquid preparation temperature control device; the ultrasonic treatment device is used to perform ultrasonic treatment on the dye solution in the liquid preparation barrel, the stirring device is used to evenly stir the dye solution in the liquid preparation barrel, and the liquid preparation temperature control device is used to control the temperature of the dye solution in the liquid preparation barrel;

[0104] A dye liquid cavity is arranged in the distillation box, and the dye liquid cavity is connected to the distillation cavity through a third connecting pipe arranged at the upper part of the dye liquid cavity. A condenser is arranged in the distillation cavity; the condenser is used to condense the gas evaporated in the dye liquid cavity and flowing into the distillation cavity into liquid.

[0105] Furthermore, the first connecting pipe and the second connecting pipe are both provided with a liquid pump for providing a power source to transfer the dye solution between the liquid preparation barrel, the dye solution pool and the distillation box.

[0106] The operation steps of the dyeing device for silk fabrics proposed above are as follows:

[0107] A1. Add madder dye, safflower dye and ethanol solution to the liquid preparation barrel, raise the temperature to 40-50° C. using the liquid preparation temperature control device and start the stirring device for stirring during the addition process;

[0108] A2. Place the silk in the material guide mechanism, use the liquid pump in the first connecting pipe to suck the prepared dye solution in the liquid preparation barrel into the dye solution pool, then seal the dye solution pool, use the dye solution temperature control device to heat the dye solution to 65-70° C., and dye for 1.5-2 hours;

[0109] A3. After dyeing is completed and the silk is taken out, the liquid extraction pump in the second connecting pipe is started to suck the excess dye liquid into the dye liquid chamber of the distillation box, and the distillation box is heated to 80°C. At this time, the ethanol liquid reaches the boiling point to form gas, and the ethanol gas evaporates into the distillation chamber along the third connecting pipe. The gaseous ethanol is condensed and collected by a condenser, and then the distillation box is heated to 100°C to separate the dye from the water and collect the excess dye retained in the dye liquid chamber.

[0110] The above is based on the ideal embodiment of the present invention. Through the above description, relevant personnel can make various changes and modifications without departing from the technical concept of the present invention. The technical scope of the present invention is not limited to the content in the specification, and the technical scope must be determined according to the scope of the claims.

Claims

1. A dyeing process for silk fabrics, characterized in that: The following steps are involved: S1. Dissolving madder dye and safflower dye in an ethanol solution to prepare a dye solution, and subjecting the dye solution to ultrasonic treatment at a temperature of 40-50° C.; the madder dye is a solid granular dye extracted from the roots of a plant of the Rubiaceae family and processed therefrom, and the safflower dye is a solid granular dye extracted from a safflower plant and processed therefrom and whose main component is safflower yellow pigment; S2, washing the silk with clean water to remove impurities and grease on the surface of the silk, then preparing a mordant solution, and using the mordant solution to pre-treat the washed silk at 40-50°C; S3, controlling the dyeing bath ratio of silk to dye solution at 1:45-1:50, then gradually heating the dye solution by 2°C every 3-5 minutes, and maintaining the dye solution at a constant temperature when the temperature is between 65-70°C, immersing the silk treated with pre-medium in S2 in the dye solution for dyeing, and dyeing under sealed conditions for 1.5-2h; S4, using an acidic fixing solution to fix the color of the silk dyed in S3, and then washing the fixed silk to remove the floating color on the surface of the silk and drying it.

2. The dyeing process of a silk fabric according to claim 1, characterized in that: The ethanol solution in step S1 is an ethanol aqueous solution with a concentration of 45%-55%.

3. The dyeing process of a silk fabric according to claim 1, characterized in that: The ratio of the safflower dye to the madder dye is between 2:5 and 5:

2.

4. The dyeing process of a silk fabric according to claim 2, characterized in that: In step S1, the specific steps of dissolving the madder dye and safflower dye in an ethanol solution include: S11, heating the ethanol solution to 40-50° C., gradually adding alizarin powder to the ethanol solution while stirring until the solid granular alizarin powder is completely dissolved; S12, gradually adding safflower yellow pigment powder to the solution obtained in step S11, and continuing heating and stirring until the safflower yellow pigment powder is completely dissolved. S13, observing the color change of the dye solution, repeating step S11 or step S12 until the solution shows the desired color, standing for 10-15 minutes, and filtering the dye solution with a microporous filter membrane to obtain the dye solution.

5. The dyeing process of a silk fabric according to claim 1, characterized in that: The mordant liquid in step S2 uses alum as a mordant, the alum accounts for 5-8% of the dry weight of the silk, and the bath ratio of the silk to the mordant liquid is controlled between 1:45-1:

50.

6. The dyeing process of a silk fabric according to claim 1, characterized in that: In step S4, the specific method of fixing the color of the silk comprises: immersing the silk in an acidic color fixing solution for 10-15 minutes, wherein the acidic color fixing solution is one of an 8%-10% citric acid color fixing solution or a 5%-8% acetic acid color fixing solution.

7. The dyeing process of a silk fabric according to claim 1, characterized in that: The ultrasonic treatment frequency is 45-60kHz, and the ultrasonic treatment duration is 20-30min.

8. The dyeing process of a silk fabric according to claim 1, characterized in that: In step S4, the temperature for drying the silk is controlled at 50-60° C., and the drying time is 30-60 minutes.

9. A silk fabric dyeing device, applicable to the silk fabric dyeing process according to any one of claims 1 to 6, characterized in that: It comprises a dye liquid pool, a material guide device located at both sides of the dye liquid pool, a dye liquid temperature control device located in the dye liquid pool, a liquid preparation barrel connected to the dye liquid pool through a first connecting pipe, and a distillation box connected to the dye liquid pool through a second connecting pipe; the dye liquid temperature control device is used to control the temperature of the dye liquid in the dye liquid pool, the liquid preparation barrel is used to prepare the dye liquid, and the distillation box is used to separate ethanol, water, madder dye and safflower dye from the excess dye liquid after dyeing; The liquid preparation barrel is provided with an ultrasonic treatment device, a stirring device and a liquid preparation temperature control device; the ultrasonic treatment device is used to perform ultrasonic treatment on the dye solution in the liquid preparation barrel, the stirring device is used to uniformly stir the dye solution in the liquid preparation barrel, and the liquid preparation temperature control device is used to control the temperature of the dye solution in the liquid preparation barrel; The distillation box is provided with a dye liquid cavity, which is connected to the distillation cavity of the dye liquid cavity through a third connecting pipe arranged at the upper part of the dye liquid cavity. The distillation cavity is provided with a condenser; the condenser is used to condense the gas evaporated in the dye liquid cavity and flowing into the distillation cavity into liquid.

10. The silk fabric dyeing device according to claim 7, characterized in that: The first connecting pipe and the second connecting pipe are both provided with a liquid pump for providing a power source to transfer the dye solution between the liquid preparation barrel, the dye solution pool and the distillation box.