Real silk softener as well as preparation method and application thereof

Abstract

The invention relates to a real silk softener and a preparation method and application thereof, and belongs to the technical field of green textile processing, the real silk softener comprises the following raw materials by mass: 8-15% of a siloxane compound, 3-5% of polyoxyethylene stearate, 2-3% of hydrolyzed silk protein, 1-2% of glycerol triacetate, 0.2-0.5% of a citric acid-sodium citrate buffer system, 0.5-1% of a nano silica dispersion liquid, and the balance of water. 1% of pentanediol and the balance of ddH2O; the hydrophilic siloxane compound comprises any one of EG / PPG siloxane and hydrophilic block silicone oil. Through a PEG / PPG siloxane or hydrophilic block silicone oil compound system, an ultrathin hydrophilic film is formed on the surface of the fiber, and efficient softness and lasting moisture permeability are synchronously realized; the three technical contradictions of air permeability loss caused by blockage of fiber pores by a traditional softener, potential safety hazards caused by harmful chemical residues and difficulty in synergy of softening effect and fiber protection are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of green textile processing, in particular to a silk softener and a preparation method and application thereof. Background Art

[0002] Silk fabric occupies an important position in the high-end textile field due to its unique softness, glossiness and skin-friendly properties.

[0003] Silk fabrics face multiple technical bottlenecks in industrial processing. During reeling and weaving, the naturally rough microstructure of silk fibers and residual sericin significantly increase the interfiber friction coefficient, leading to frequent static electricity. This in turn causes problems such as tangling and weaving interruptions, significantly reducing production continuity and efficiency. Furthermore, unpretreated silk fabrics have a rough feel, and the irregular surface morphology of the fibers hinders uniform dye penetration and absorption during the dyeing and finishing process, increasing the risk of dyeing defects such as color fringing and spotting, thereby affecting the quality of the finished product. Therefore, silk softeners are often used for pretreatment.

[0004] The performance of silk softeners currently available on the market still has significant limitations: although traditional ingredients such as amino silicone oil and mineral oil can achieve a short-term softening effect, they will clog the fiber pores and destroy the natural breathability and moisture permeability of silk; some products have residual formaldehyde, heavy metals and other harmful chemicals due to defects in the production process. Long-term exposure may cause health risks such as skin sensitivity and respiratory irritation.

[0005] Therefore, there is an urgent need to develop a softener that has high efficiency, lasting hydrophilicity, fiber repair function and is environmentally friendly and safe. This is of great significance to improving the quality of silk products and promoting the sustainable development of the silk industry. Summary of the Invention

[0006] The purpose of the present invention is to provide a silk softener and its preparation method and application, so as to solve the technical problems of traditional softeners causing loss of air permeability due to clogging of fiber pores, safety hazards caused by harmful chemical residues, and difficulty in coordinating softening effect and fiber protection.

[0007] On the one hand, the present invention provides a silk softener, which adopts the following technical solution:

[0008] A silk softener comprising the following raw materials in percentage by mass:

[0009] 8-15% of silicone compound, 3-5% of polyoxyethylene stearate, 2-3% of hydrolyzed silk protein, 1-2% of triacetin, 0.2-0.5% of citric acid-sodium citrate buffer system, 0.5-1% of nano-silica dispersion, 1% of pentylene glycol, and the balance of ddH2O.

[0010] Preferably, the hydrophilic silicone compound includes any one of EG / PPG silicone and hydrophilic block silicone oil.

[0011] Preferably, the molecular weight of the hydrolyzed silk protein is less than 5 kDa;

[0012] After hydrolysis treatment, the recovery rate of silk protein in the hydrolyzed silk is ≥85%;

[0013] The amino acid composition of hydrolyzed silk protein is more than 90% similar to that of natural sericin.

[0014] Preferably, the diameter of the nano-silica particles in the nano-silica dispersion is 20 nm.

[0015] On the other hand, the present invention also provides a method for preparing the above-mentioned silk softener, which adopts the following technical solution:

[0016] A method for preparing a silk softener comprises the following steps:

[0017] S1. Add PEG / PPG siloxane or hydrophilic block silicone oil into a reaction vessel, stir and heat, add polyoxyethylene stearate, and continue stirring until the mixture becomes uniform and transparent to obtain a pre-emulsified silicone oil system for later use;

[0018] S2. Place ddH2O into another reaction container, heat to a high temperature, and sequentially add hydrolyzed silk fibroin and triacetin, stirring until completely dissolved to obtain an aqueous phase system;

[0019] S3, slowly pouring the pre-emulsified silicone oil prepared in step S1 into the aqueous phase system prepared in step S2, turning on the high-speed shearing device until a stable emulsion with uniform particle size and no stratification is formed, then slowly adding the nano-silica dispersion, and continuously stirring until the emulsion is uniformly dispersed, to obtain an emulsion system;

[0020] S4. Cooling the emulsion system obtained in step S3, adding a citric acid-sodium citrate buffer system, adjusting the pH to 5.5-6.5, then adding pentanediol, stirring evenly, filtering, and obtaining a silk softener.

[0021] Preferably, the stirring rate in step S1 is 200-300 r / min, and the mixture is heated to 50-60°C.

[0022] Preferably, the heating temperature in step S2 is 40°C.

[0023] Preferably, the rotation speed of the high-speed shearing device in step S3 is 8000-10000 r / min, and the shearing time is 15 min;

[0024] After adding the nano-silica dispersion, the stirring rate is 300-400 r / min and the stirring time is 30 min.

[0025] Preferably, in step S3, the emulsion system is cooled to 20-30°C.

[0026] On the other hand, the present invention also provides an application of the above-mentioned silk softener, which adopts the following technical solution:

[0027] The invention discloses an application of a silk softener in raw silk, silk textiles and blended products.

[0028] In summary, the present invention has the following beneficial technical effects:

[0029] 1. The silk softener of the present invention adopts hydrophilic silicone compounds as the main softening component, which reduces the friction coefficient and gives the fabric a silky feel; it has both hydrophilicity and hydrophobicity, enhances the stability of the emulsion, significantly improves the softness and antistatic properties of the fabric, and has strong wash resistance, avoiding the waterproof and sweat-inducing problems of traditional silicone oil.

[0030] 2. The PEG / PPG silicone and hydrophilic block silicone oil in the present invention serve as the main softening ingredients. The PEG / PPG silicone forms an ultra-thin lubricating film on the fiber surface, reducing the friction coefficient and giving the fabric a silky feel. It has both hydrophilicity and hydrophobicity, enhancing the stability of the emulsion, significantly improving the softness and antistatic properties of the fabric, and has strong washability, avoiding the waterproof and sweat-sucking problems of traditional silicone oils. The special comb-like structure of the hydrophilic block silicone oil provides long-lasting hydrophilicity, allowing the fabric to absorb moisture and perspiration, enhancing the sliding between fibers, reducing wrinkles, solving the waterproof problem of traditional silicone oils, keeping the fabric dry and comfortable, improving the anti-wrinkle performance, and reducing the need for ironing.

[0031] 3. The polyoxyethylene stearate in the present invention reduces the surface tension of the oil-water interface, stabilizes the pre-emulsification system, synergizes with silicone oil, and reduces fiber entanglement caused by electrostatic adsorption; small molecule proteins with a molecular weight of less than 5kDa penetrate into the fiber, repair damaged structures, form a protective film on the surface, enhance gloss, improve fabric strength and elasticity, impart a silky gloss, improve touch, and are natural ingredients that are safe and skin-friendly; triacetin acts as a plasticizer to dissolve silk protein and adjust the viscosity of the system to ensure uniform dispersion of the ingredients, enhance the permeability of the softener into the fiber, improve the product feel, and reduce the sticky feeling; nano-silica dispersion fills microcracks on the fiber surface, reduces the friction coefficient, and enhances the silky touch; the citric acid-sodium citrate buffer system maintains a weakly acidic environment in the system, ensures the stability of the silicone oil, avoids hydrolysis failure, complies with the skin pH value, reduces irritation, and enhances the activity of silk protein; pentylene glycol acts as a food-grade preservative, is safe to use, inhibits microbial growth, has no irritating odor or chemical toxicity, and meets environmental protection standards.

[0032] 4. After the silk softener prepared by the present invention is used to treat the silk fabric, the swing angle of the silk fabric is increased by 80-88%. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 (A) is a graph showing the centrifugal stability test results of the silk softener prepared in Example 1 of the present invention;

[0034] Figure 1 Middle (B) is a graph showing the centrifugal stability test results of the silk softener prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical solutions and advantages of this application more clear, the following further describes this application in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain this application and are not intended to limit this application.

[0036] Example

[0037] Example 1

[0038] A method for preparing a silk softener comprises the following steps:

[0039] 1) Preparation of pre-emulsified silicone oil system:

[0040] Add 12% PEG / PPG silicone to a reaction vessel equipped with a temperature control device, stir at 250 r / min and heat to 55°C. At the same time, slowly add 4% polyoxyethylene stearate and continue stirring for 25 minutes until the mixture is homogeneous and transparent, forming a stable pre-emulsified silicone oil system.

[0041] 2) Preparation of aqueous phase:

[0042] In another reaction vessel, add 72.5-82.3% ddH2O, heat to 40°C, add 2.5% hydrolyzed silk protein (molecular weight <5 kDa) and 1.5% triacetin, and stir until completely dissolved to form a uniform aqueous phase system;

[0043] Among them, the molecular weight of hydrolyzed silk protein is <5kDa;

[0044] After hydrolysis treatment, the recovery rate of silk protein in the hydrolyzed silk is ≥85%;

[0045] The amino acid composition of hydrolyzed silk protein is more than 90% similar to that of natural sericin;

[0046] 3) Mixing and emulsification:

[0047] The pre-emulsified silicone oil prepared in step 1) was slowly poured into the aqueous phase system prepared in step 2), and a high-speed shearing device was started to shear at 9000 r / min for 15 minutes until a stable emulsion with uniform particle size and no stratification was formed. 0.75% nano-silica dispersion was slowly added, and stirring was continued at a low speed of 350 r / min for 30 minutes to ensure that the nanoparticles were evenly dispersed and did not agglomerate, thereby obtaining an emulsion system;

[0048] The diameter of the nano-silica particles in the nano-silica dispersion is 20 nm.

[0049] 4) Post-processing:

[0050] The emulsified system prepared in step 3) is cooled to 20-30° C., 0.3% citric acid-sodium citrate buffer system is added to adjust the pH to 5.5-6.5, and 1% pentanediol is added as a preservative. After stirring evenly, impurities are removed by filtering through a 100-mesh filter cloth to obtain a finished silk softener.

[0051] Example 2

[0052] A method for preparing a silk softener comprises the following steps:

[0053] 1) Preparation of pre-emulsified silicone oil system:

[0054] Add 10% hydrophilic block silicone oil to a reaction vessel equipped with a temperature control device, stir at 250 r / min and heat to 55°C. At the same time, slowly add 4% polyoxyethylene stearate and continue stirring for 25 minutes until the mixture is homogeneous and transparent, forming a stable pre-emulsified silicone oil system.

[0055] 2) Preparation of aqueous phase:

[0056] In another reaction vessel, add 75.5-84.3% ddH2O, heat to 40°C, add 2.5% hydrolyzed silk protein and 1.5% triacetin, stir until completely dissolved, and form a uniform aqueous phase system;

[0057] Among them, the molecular weight of hydrolyzed silk protein is <5kDa;

[0058] After hydrolysis treatment, the recovery rate of silk protein in the hydrolyzed silk is ≥85%;

[0059] The amino acid composition of hydrolyzed silk protein is more than 90% similar to that of natural sericin;

[0060] 4) Mixing and emulsification:

[0061] The pre-emulsified silicone oil prepared in step 1) was slowly poured into the aqueous phase system prepared in step 2), and a high-speed shearing device was started to shear at 9000 r / min for 15 minutes until a stable emulsion with uniform particle size and no stratification was formed. 0.75% nano-silica dispersion was slowly added, and stirring was continued at a low speed of 350 r / min for 30 minutes to ensure that the nanoparticles were evenly dispersed and did not agglomerate, thereby obtaining an emulsion system;

[0062] The diameter of the nano-silica particles in the nano-silica dispersion is 20 nm;

[0063] 4) Post-processing:

[0064] The emulsified system prepared in step 3) is cooled to 20-30° C., 0.3% citric acid-sodium citrate buffer system is added to adjust the pH to 5.5-6.5, and 1% pentanediol is added as a preservative. After stirring evenly, impurities are removed by filtering through a 100-mesh filter cloth to obtain a finished silk softener.

[0065] Performance testing

[0066] Test Example 1

[0067] Reference Figure 1 The silk softeners prepared in Example 1 and Example 2 were subjected to centrifugal stability tests under the following conditions: centrifugation at 3000 rpm for 30 min, and the emulsion stratification was observed. Figure 1 It can be seen that the silk softener prepared by Example 1 did not show any stratification, and the silk softener prepared by Example 2 showed less stratification. The silk softener systems prepared by Examples 1 and 2 are stable and can maintain a uniform state during storage and use. The performance of the silk softener is not guaranteed.

[0068] Test Example 2

[0069] According to GB / T18318.3-2009, the Glay method (swing test) was used, and the test was performed using an LFY-208 oscillating fabric softness tester. A 50 g weight was applied, and the silk blanks treated with the working solution prepared with the silk softener prepared in Example 1 and the working solution prepared with the silk softener prepared in Example 2 were recorded, and the swing angle of the silk blanks was recorded.

[0070] The same silk stock was divided into two groups. The swing angles of the two groups of silk stock were first measured before treatment with a silk softener. One group of silk stock was immersed in a working solution containing the silk softener prepared in Example 1 at a concentration of 5% and a bath ratio of 1:30. The treatment was continued at 45°C for 1 hour, followed by washing and drying. The swing angles of the silk stock were then measured. The other group of silk stock was immersed in a working solution containing the silk softener prepared in Example 2 at a concentration of 5% and a bath ratio of 1:30. The treatment was continued at 45°C for 1 hour, followed by washing and drying. The swing angles of the silk stock were then measured. The test results are shown in Table 1.

[0071] Table 1 Test results of silk blank swing angle

[0072]

[0073] From the test results in Table 1, it can be seen that the silk softener prepared in Example 1 can increase the swing angle of the silk blank by 80%, significantly improve the softness, and have good antistatic performance; the silk softener prepared in Example 2 performs better in improving softness, with the swing angle increased by 88%, the softness increased by 88%, and the feel smoother.

[0074] Test Example 3

[0075] Silk blanks treated with the working solution of the silk softener prepared in Example 1 and the working solution of the silk softener prepared in Example 2 were placed in a constant temperature oven at 70°C and aged for 48 hours. The yellowing degree of the untreated silk blanks was compared. The test results are shown in Table 2.

[0076] Table 2 Test results of yellowing degree of silk blank

[0077]

[0078] From the test results in Table 2, it can be seen that after aging in a constant temperature oven at 70°C for 48 hours, the silk blank treated with the silk softener prepared in Example 1 has a yellowing ΔE=0.9, with no obvious color change, and both softness and color stability are taken into account; the silk blank treated with the silk softener prepared in Example 2 has a yellowing ΔE=0.85, which is close to the natural color and has outstanding stability at high temperatures.

[0079] The above are all preferred embodiments of the present invention, and are not intended to limit the scope of protection of the present invention. Therefore, any equivalent changes made based on the structure, shape, and principle of the present invention should be included in the scope of protection of the present invention.

Claims

1. A silk softener, characterized in that: The following raw materials are included in mass percentage: 8-15% silicone compound, 3-5% polyoxyethylene stearate, 2-3% hydrolyzed silk protein, 1-2% triacetin, 0.2-0.5% citric acid-sodium citrate buffer system, 0.5-1% nano-silica dispersion, 1% pentylene glycol, and the balance ddH2O.

2. A silk softener according to claim 1, characterized in that: The hydrophilic silicone compound includes any one of EG / PPG silicone and hydrophilic block silicone oil.

3. A silk softener according to claim 1, characterized in that: The molecular weight of the hydrolyzed silk protein is less than 5 kDa; After hydrolysis treatment, the recovery rate of silk protein in hydrolyzed silk is ≥85%; The amino acid composition of hydrolyzed silk protein is more than 90% similar to that of natural sericin.

4. A silk softener according to claim 1, characterized in that: The diameter of the nano-silicon dioxide particles in the nano-silicon dioxide dispersion is 20 nm.

5. A method for preparing the silk softener according to any one of claims 1 to 4, characterized in that: The method comprises the following preparation steps: S1. Add PEG / PPG siloxane or hydrophilic block silicone oil into a reaction vessel, stir and heat, add polyoxyethylene stearate, and continue stirring until the mixture becomes uniform and transparent to obtain a pre-emulsified silicone oil system for later use; S2. Place ddH2O into another reaction container, heat to a high temperature, and sequentially add hydrolyzed silk fibroin and triacetin, stirring until completely dissolved to obtain an aqueous phase system; S3, slowly pouring the pre-emulsified silicone oil prepared in step S1 into the aqueous phase system prepared in step S2, turning on the high-speed shearing device until a stable emulsion with uniform particle size and no stratification is formed, then slowly adding the nano-silica dispersion, and continuously stirring until the emulsion is uniformly dispersed, to obtain an emulsion system; S4. Cooling the emulsion system obtained in step S3, adding a citric acid-sodium citrate buffer system, adjusting the pH to 5.5-6.5, then adding pentanediol, stirring evenly, filtering, and obtaining a silk softener.

6. The method for preparing the silk softener according to claim 5, wherein: The stirring rate in step S1 is 200-300 r / min, and the mixture is heated to 50-60°C.

7. The method for preparing the silk softener according to claim 5, wherein: The heating temperature in step S2 is 40°C.

8. The method for preparing the silk softener according to claim 5, wherein: In step S3, the rotation speed of the high-speed shearing equipment is 8000-10000 r / min, and the shearing time is 15 min; After adding the nano-silica dispersion, the stirring rate is 300-400 r / min and the stirring time is 30 min.

9. The method for preparing the silk softener according to claim 5, wherein: In step S3, the emulsion system is cooled to 20-30°C.

10. Use of the silk softener according to any one of claims 1 to 4 in raw silk, silk textiles and blended products.

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