Preparation process of anti-yellowing real silk fabric

Abstract

This invention relates to the field of silk fabric technology, and more particularly to a preparation process for an anti-yellowing silk fabric. The preparation process of the aforementioned anti-yellowing silk fabric includes the following steps: soaking the silk fabric in a sodium carbonate aqueous solution and ultrasonically treating for 10-30 minutes, washing with water, air-drying at 30-40°C, and then plasma-treating for 1-2 minutes to obtain a pretreated silk fabric; adding dopamine monomer and silver nitrate to a Tris-HCl buffer solution with a pH of 8-9, adding the pretreated silk fabric to the solution, purging with air and shaking at room temperature for 40-60 minutes, filtering, washing, and air-drying to obtain a loaded silk fabric; adding silk peptides, activated nano-zinc oxide, and a penetrant to an ethanol aqueous solution and stirring until homogeneous; immersing the loaded silk fabric at an immersion bath ratio of 1:40-60 at an immersion temperature of 30-40°C; performing two dips and two nips, each immersion lasting 10-20 minutes, with a nip-out rate of 75-80%; washing with water and air-drying.

Description

Technical Field

[0001] This invention relates to the field of silk fabric technology, and in particular to a preparation process for an anti-yellowing silk fabric. Background Technology

[0002] Silk fabrics are made from natural mulberry silk. With their unique luster, smooth touch, excellent moisture absorption and breathability, and skin-friendly properties, they have become a classic choice for high-end clothing and home furnishings. However, due to the structural characteristics of the natural protein fibers in silk fabrics, silk is easily affected by environmental temperature and humidity, light and microorganisms during processing, daily wear and long-term storage, resulting in yellowing and performance deterioration.

[0003] Yellowing is one of the most prominent signs of aging in silk. Mulberry silk is prone to oxidative degradation under the catalysis of oxygen, ultraviolet light, or metal ions. On the one hand, this produces yellow quinone compounds, causing the fabric to become dull and lose whiteness, severely affecting its appearance. On the other hand, it causes the fibers to become brittle and their tensile strength to decrease, further shortening its lifespan.

[0004] Besides yellowing, while the skin-friendly and highly absorbent properties of silk enhance wearing comfort, they also lead to the growth of microorganisms. In warm and humid conditions, bacteria on the surface of the fabric can easily multiply, which can not only produce odors but also cause health problems such as skin allergies.

[0005] The current market demand for silk products has shifted from simply being aesthetically pleasing to having multiple functions. How to use gentle and efficient modification techniques to achieve both anti-yellowing and antibacterial finishing without damaging the original texture of silk, and to give it long-lasting protective properties, has become a technical challenge that urgently needs to be solved. Summary of the Invention

[0006] The purpose of this invention is to address the shortcomings of existing technologies by proposing a preparation process for anti-yellowing silk fabrics.

[0007] A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak the silk fabric in a sodium carbonate aqueous solution and sonicate for 10-30 minutes, wash with water, air dry at 30-40℃, and then treat with plasma for 1-2 minutes to obtain the pretreated silk fabric. S2. Add dopamine monomer and silver nitrate to Tris-HCl buffer solution with pH 8-9, add pretreated silk fabric to it, purge air and shake at room temperature for 40-60 min, filter, wash and air dry to obtain loaded silk fabric. S3. Add silk peptide, activated nano zinc oxide and penetrant to ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:40-60 and an impregnation temperature of 30-40℃. Perform two dips and two nips, each for 10-20 minutes, with a nip rate of 75-80%. Wash with water and air dry.

[0008] Preferably, in S1, the mass fraction of the sodium carbonate aqueous solution is 0.1-0.5%.

[0009] Preferably, in S1, the ultrasonic frequency is 50-70kHz.

[0010] Preferably, in S1, the plasma treatment gas is oxygen, the treatment power is 100-200W, and the treatment pressure is 20-40Pa.

[0011] Preferably, in S2, the mass ratio of dopamine monomer, silver nitrate, and pretreated silk fabric is 1-3:1-2:10-20.

[0012] Preferably, in S3, the mass ratio of silk peptide, activated nano zinc oxide, and penetrant is 1-3:1-2:1-2.

[0013] Preferably, in S3, the penetrant is sorbitol.

[0014] Preferably, in S3, the activated nano-zinc oxide is obtained by activating the nano-zinc oxide with a silane coupling agent.

[0015] Preferably, the air-drying temperature is 30-40℃.

[0016] An anti-yellowing silk fabric is prepared using the aforementioned anti-yellowing silk fabric preparation process.

[0017] Compared with existing technologies, the present invention has the following advantages: This invention constructs a multifunctional protective layer on the surface of silk fabrics, which not only significantly improves the anti-yellowing and antibacterial properties, but also fully preserves the original texture of silk.

[0018] This invention uses sodium carbonate solution and ultrasonic cleaning to effectively remove impurities from the fabric surface and improve hydrophilicity. Plasma treatment introduces active groups on the fiber surface, which is more conducive to the stable loading of subsequent functional components and effectively enhances the binding force.

[0019] This invention utilizes dopamine to self-polymerize under alkaline conditions to form a polydopamine film. Its strong adhesion can stabilize and fix silver nanoparticles, which are slowly released to exert a broad-spectrum antibacterial effect, inhibiting the growth of microorganisms and the generation of odors. At the same time, polydopamine can synergistically delay the yellowing caused by the oxidative degradation of silk. Silk peptides, as a natural protein component, have a similar structure to silk fibers, which can repair potential damage and improve skin affinity. Combined with the activation of nano zinc oxide, they assist in antibacterial action.

[0020] The process of this invention is mild and efficient, without the use of strong chemical reagents. While giving silk long-lasting anti-yellowing and antibacterial properties, it maintains the fabric's luster, smooth touch and moisture absorption and breathability, meeting the needs of high-end functional products. Attached Figure Description

[0021] Figure 1 This is a comparison chart showing the yellowing rate of the anti-yellowing silk fabrics obtained in Example 5 and Comparative Examples 1-2 and the untreated silk fabrics under different irradiation levels.

[0022] Figure 2 The graph shows the decrease in antibacterial rate (Staphylococcus aureus, Escherichia coli and Candida albicans) of the anti-yellowing silk fabrics obtained in Example 5 and Comparative Examples 1-2 after 5 washes. Detailed Implementation

[0023] The present invention will now be described in further detail with reference to specific embodiments. The given embodiments are merely illustrative of the invention and not intended to limit its scope. The embodiments provided below can serve as a guide for further improvements by those skilled in the art and do not constitute a limitation on the invention in any way.

[0024] Unless otherwise specified, the experimental methods used in the following examples are conventional methods, performed according to the techniques or conditions described in the literature in this field or according to the product instructions. Unless otherwise specified, the materials and reagents used in the following examples are commercially available.

[0025] The silk fabrics used below are derived from the applicant's pure white silk crepe satin, weighing 147 g / m², with a thickness of 30 momme, and composed of mulberry silk. The dopamine monomers used below are dopamine hydrochloride, purchased from Shanghai Zheyan Biotechnology Co., Ltd. The silk peptides used below are purchased from Shaanxi Cuihe Biotechnology Co., Ltd., obtained by hydrolyzing silk, product model CH6138469. The activated nano-zinc oxide used below is obtained by adding nano-zinc oxide to an ethanol solution of silane coupling agent KH550, stirring for 2 hours, and then drying.

[0026] Example 1 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 10g of silk fabric in 100g of sodium carbonate aqueous solution with a mass fraction of 0.1% and sonicate for 10min at a frequency of 50kHz. Wash twice with deionized water, air dry at 30℃, and then treat with plasma for 1min (the plasma treatment gas is oxygen, the treatment power is 100W, and the treatment pressure is 20Pa) to obtain pretreated silk fabric. S2. Add 1g of dopamine monomer and 1g of silver nitrate to Tris-HCl buffer solution with pH 8-9, add 10g of pretreated silk fabric, purge air and shake at room temperature for 40min, filter, wash, and air dry at 30℃ to obtain loaded silk fabric. S3. Add 1g of silk peptide, 1g of activated nano zinc oxide and 1g of sorbitol to 100g of 30% ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:40 and an impregnation temperature of 30℃. Perform two dips and two nips, each for 10 minutes, with a nip rate of 75%. Wash with water and air dry at 30℃.

[0027] Example 2 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 20g of silk fabric in 150g of sodium carbonate aqueous solution with a mass fraction of 0.5% and sonicate for 30min at a frequency of 70kHz. Wash with deionized water 4 times, air dry at 40℃, and then treat with plasma for 2min (the plasma treatment gas is oxygen, the treatment power is 200W, and the treatment pressure is 40Pa) to obtain the pretreated silk fabric. S2. Add 3g of dopamine monomer and 2g of silver nitrate to Tris-HCl buffer solution with pH 8-9, add 20g of pretreated silk fabric, purge with air and shake at room temperature for 60min, filter, wash, and air dry at 40℃ to obtain loaded silk fabric. S3. Add 3g of silk peptide, 2g of activated nano zinc oxide and 2g of sorbitol to 150g of 40% ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:60 and an impregnation temperature of 40℃. Perform two dips and two nips, each for 20 minutes, with a nip rate of 80%. Wash with water and air dry at 40℃.

[0028] Example 3 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 12g of silk fabric in 130g of sodium carbonate aqueous solution with a mass fraction of 0.2% and sonicate for 25min at a frequency of 55kHz. Wash with deionized water three times, air dry at 37℃, and then treat with plasma for 1.5min (the plasma treatment gas is oxygen, the treatment power is 120W, and the treatment pressure is 35Pa) to obtain the pretreated silk fabric. S2. Add 1.5g of dopamine monomer and 1.8g of silver nitrate to Tris-HCl buffer solution with pH 9, add 12g of pretreated silk fabric, purge with air and shake at room temperature for 55min, filter, wash, and air dry at 33℃ to obtain loaded silk fabric. S3. Add 2.5g of silk peptide, 1.2g of activated nano zinc oxide and 1.8g of sorbitol to 110g of 37% ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:45 and an impregnation temperature of 37℃. Perform two dips and two nips, each dip lasting 12 minutes, with a nip rate of 79%. Wash with water and air dry at 33℃.

[0029] Example 4 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 18g of silk fabric in 110g of sodium carbonate aqueous solution with a mass fraction of 0.4% and sonicate for 15min at a frequency of 65kHz. Wash three times with deionized water, air dry at 33℃, and then treat with plasma for 1.5min (the plasma treatment gas is oxygen, the treatment power is 180W, and the treatment pressure is 25Pa) to obtain the pretreated silk fabric. S2. Add 2.5g of dopamine monomer and 1.2g of silver nitrate to Tris-HCl buffer solution with pH 9, add 18g of pretreated silk fabric, purge with air and shake at room temperature for 45min, filter, wash, and air dry at 37℃ to obtain loaded silk fabric. S3. Add 1.5g of silk peptide, 1.8g of activated nano zinc oxide and 1.2g of sorbitol to 130g of 33% ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:55 and an impregnation temperature of 33℃. Perform two dips and two nips, each dip lasting 18 minutes, with a nip-out rate of 76%. Wash with water and air dry at 37℃.

[0030] Example 5 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 15g of silk fabric in 120g of 0.3% sodium carbonate aqueous solution and sonicate for 20min at a frequency of 60kHz. Wash three times with deionized water, air dry at 35℃, and then treat with plasma for 1.5min (the plasma treatment gas is oxygen, the treatment power is 150W, and the treatment pressure is 30Pa) to obtain the pretreated silk fabric. S2. Add 2g of dopamine monomer and 1.5g of silver nitrate to Tris-HCl buffer solution with pH 9, add 15g of pretreated silk fabric, purge with air and shake at room temperature for 50min, filter, wash, and air dry at 35℃ to obtain loaded silk fabric. S3. Add 2g of silk peptide, 1.5g of activated nano zinc oxide and 1.5g of sorbitol to 120g of 35% ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:50 and an impregnation temperature of 35℃. Perform two dips and two nips, each dip lasting 15 minutes, with a nip rate of 78%. Wash with water and air dry at 35℃.

[0031] Comparative Example 1 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 15g of silk fabric in 120g of sodium carbonate aqueous solution with a mass fraction of 0.3% and sonicate for 20min at a sonic frequency of 60kHz. Wash with deionized water 3 times and air dry at 35℃ to obtain pretreated silk fabric. S2. Add 2g of dopamine monomer and 1.5g of silver nitrate to Tris-HCl buffer solution with pH 9, add 15g of pretreated silk fabric, purge with air and shake at room temperature for 50min, filter, wash, and air dry at 35℃ to obtain loaded silk fabric. S3. Add 2g of silk peptide, 1.5g of activated nano zinc oxide and 1.5g of sorbitol to 120g of 35% ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:50 and an impregnation temperature of 35℃. Perform two dips and two nips, each dip lasting 15 minutes, with a nip rate of 78%. Wash with water and air dry at 35℃.

[0032] Comparative Example 2 A process for preparing an anti-yellowing silk fabric includes the following steps: S1. Soak 15g of silk fabric in 120g of 0.3% sodium carbonate aqueous solution and sonicate for 20min at a frequency of 60kHz. Wash three times with deionized water, air dry at 35℃, and then treat with plasma for 1.5min (the plasma treatment gas is oxygen, the treatment power is 150W, and the treatment pressure is 30Pa) to obtain the pretreated silk fabric. S2. Add 2g of silk peptide, 1.5g of activated nano zinc oxide, 1.5g of silver nitrate and 1.5g of sorbitol to 120g of 35% ethanol aqueous solution and stir well. Immerse the pretreated silk fabric in the immersion bath at a ratio of 1:50 and an immersion temperature of 35℃. Perform two immersions and two nips, each immersion for 15 minutes, with a nip rate of 78%. Wash with water and air dry at 35℃.

[0033] Referring to GB / T 8427-2019 "Textiles - Tests for color fastness - Color fastness to artificial light: Xenon arc", xenon arc lamps with wavelengths of 50, 100, and 150 kJ / m were used at different irradiance levels. 2The anti-yellowing silk fabrics obtained in Example 5 and Comparative Examples 1-2, as well as untreated silk fabrics, were treated, and the yellowing rate was calculated.

[0034] Yellowing rate = (original whiteness - whiteness after illumination) ÷ original whiteness × 100%.

[0035] like Figure 1 As shown, the yellowing rate of the anti-yellowing silk fabrics obtained in Example 5 and Comparative Examples 1-2 was significantly lower than that of untreated silk fabrics under different irradiation levels; while the yellowing rate of the anti-yellowing silk fabric obtained in Example 5 was the lowest, significantly better than the other groups of silk fabrics.

[0036] Referring to GB / T 20944.3-2008 "Evaluation of antimicrobial properties of textiles - Part 3: Oscillation method", the anti-yellowing silk fabrics obtained in Example 5 and Comparative Examples 1-2 were evaluated for their antibacterial rates against Staphylococcus aureus, Escherichia coli, and Candida albicans in unwashed and 5-wash conditions. The rate of decrease in antibacterial rate after 5 washes was calculated.

[0037] Antibacterial rate decrease rate = (antibacterial rate without washing - antibacterial rate after 5 washes) ÷ antibacterial rate without washing × 100%.

[0038] like Figure 2 As shown, the anti-yellowing silk fabric obtained in Example 5 had the lowest antibacterial rate decrease after 5 washes, which was significantly better than the other silk fabrics.

[0039] The present invention has been described in detail above. Those skilled in the art will recognize that the invention can be practiced in a wide range of ways with equivalent parameters, concentrations, and conditions without departing from its spirit and scope, and without requiring unnecessary experiments. While specific embodiments have been provided, it should be understood that further modifications can be made to the invention. In summary, according to the principles of the invention, this application is intended to include any changes, uses, or improvements to the invention, including changes made using conventional techniques known in the art that depart from the scope disclosed herein.

Claims

1. A preparation process for an anti-yellowing silk fabric, characterized in that, Includes the following steps: S1. Soak the silk fabric in a sodium carbonate aqueous solution and sonicate for 10-30 minutes, wash with water, air dry at 30-40℃, and then treat with plasma for 1-2 minutes to obtain the pretreated silk fabric. S2. Add dopamine monomer and silver nitrate to Tris-HCl buffer solution with pH 8-9, add pretreated silk fabric to it, purge air and shake at room temperature for 40-60 min, filter, wash and air dry to obtain loaded silk fabric. S3. Add silk peptide, activated nano zinc oxide and penetrant to ethanol aqueous solution and stir evenly. Impregnate the loaded silk fabric with an impregnation bath ratio of 1:40-60 and an impregnation temperature of 30-40℃. Perform two dips and two nips, each for 10-20 minutes, with a nip rate of 75-80%. Wash with water and air dry.

2. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S1, the mass fraction of sodium carbonate aqueous solution is 0.1-0.5%.

3. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S1, the ultrasonic frequency is 50-70kHz.

4. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S1, the plasma treatment gas is oxygen, the treatment power is 100-200W, and the treatment pressure is 20-40Pa.

5. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S2, the mass ratio of dopamine monomer, silver nitrate, and pretreated silk fabric is 1-3:1-2:10-20.

6. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S3, the mass ratio of silk peptide, activated nano zinc oxide, and penetrant is 1-3:1-2:1-2.

7. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S3, the penetrant is sorbitol.

8. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, In S3, activated nano-zinc oxide is obtained by activating nano-zinc oxide with a silane coupling agent.

9. The preparation process of the anti-yellowing silk fabric according to claim 1, characterized in that, The air-drying temperature is 30-40℃.

10. A type of anti-yellowing silk fabric, characterized in that, It is prepared using the preparation process of the anti-yellowing silk fabric according to any one of claims 1-9.

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