Underwear fabric with ROS scavenging function and preparation method thereof
By introducing functional layers of materials such as Cu cidopa complex and graphene oxide into the underwear fabric, the problem of free radicals and ROS removal on the skin surface is solved, and anti-aging, moisturizing and antibacterial effects are achieved.
Patent Information
- Application Number
- CN202410918351.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-10
- Publication Date
- 2025-09-02
- Estimated Expiration
- 2044-07-10
AI Technical Summary
The prior art cannot effectively and proactively remove free radicals and reactive oxygen species (ROS) from the skin surface, resulting in problems such as skin aging, dryness, deterioration of skin tone and large pores. The existing methods have limitations and vary greatly in individuals.
The functional layer finishing agent composed of Cu cydopa complex and chitosan, graphene oxide and other materials is designed to design underwear fabrics with low temperature water absorption and swelling and high temperature shrinkage and drainage. Combined with Cu-based polymerization complex, it catalyzes the free radicals and ROS on the skin surface, and has antibacterial properties.
It realizes effective drainage and removal of free radicals and ROS under different temperature conditions, improves the anti-aging and moisturizing effect of the skin, and has excellent antibacterial properties.
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Figure CN118745664B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of textiles, and in particular relates to an underwear fabric with ROS scavenging function and a preparation method thereof. Background Art
[0002] Free radicals and reactive oxygen species (ROS) can cause aging, damage, dissolution, and apoptosis of cell membranes, leading to skin aging, dry skin, poor skin tone, decreased skin elasticity, enlarged pores, and other problems. 1. Skin aging: Free radicals can damage the integrity of cell membranes, causing the skin to lose elasticity, resulting in sagging skin, wrinkles, and dull skin. 2. Dry skin: Free radicals can also cause damage to the skin's stratum corneum, leading to symptoms such as dryness and scaling. 3. Poor skin tone: Free radicals can damage the skin's melanocytes, leading to poor skin tone. 4. Decreased skin elasticity: Free radicals can also damage the skin's collagen, leading to decreased skin elasticity. 5. Enlarged pores: Free radicals can increase the skin's oil secretion, leading to enlarged pores.
[0003] Currently, the problem of free radicals and ROS on the skin's surface can only be addressed through physical methods such as cosmetics, medications, and sunscreens. These methods have limited effectiveness and vary widely from person to person. These solutions are passive and auxiliary, and cannot actively eliminate free radicals and ROS on the skin's surface. This blocks the root cause of the problem and only treats the symptoms rather than the root cause. Summary of the Invention
[0004] In view of this, the purpose of the present invention is to provide an underwear fabric with ROS scavenging function and a preparation method thereof. The functional layer of the fabric can absorb water and swell at low temperatures, and shrink and discharge water at high temperatures. It can drain and diffuse free radicals and ROS on the skin surface into the functional layer, and catalytically scavenged by Cu-based polymer complexes, converting them into inactive or low-activity molecules, thereby reducing their adverse effects on the skin surface, while also having excellent antibacterial properties.
[0005] In order to solve the above technical problems, the present invention provides a method for preparing underwear fabric with ROS scavenging function, comprising the following steps:
[0006] S1. Preparation of a composite Cu-based dopa complex: Carbidopa and CTAB (cetyltrimethylammonium bromide) were sequentially added to water, the pH was adjusted to 10.0-10.5 with sodium hydroxide solution, and the mixture was stirred for 1-2 h. The pH was then adjusted to 5.0-6.0 with hydrochloric acid, and hydrated copper acetate was added. After a hydrothermal reaction, the mixture was concentrated by rotary evaporation at 70-80°C to 1 / 4-1 / 3 of the original volume, and the pH was adjusted to 3.0-4.5 with glacial acetic acid to obtain a composite Cu-based dopa complex solution.
[0007] S2. Preparation of a functional layer finishing agent: The composite Cu-dopa complex solution prepared in step S1 was cooled to 0-4°C, and CS (chitosan), GO (graphene oxide), NIPAM (N-isopropylacrylamide), BIS (N,N′-methylenebisacrylamide), KPS (potassium persulfate), and TEMED (N,N,N′,N′-tetramethylethylenediamine) were added in sequence and stirred thoroughly to obtain a functional layer finishing agent;
[0008] S3. Fabric finishing: Apply the functional layer finishing agent to the underwear base fabric, 300-500W / m 2 The ultraviolet irradiation is combined with drying at 100-120℃ for shaping, and the finishing process is repeated 3-5 times. The underwear fabric with ROS scavenging function is then washed and dried.
[0009] Preferably, in step S1, the feeding ratio of carbidopa, CTAB, water and hydrated copper acetate is (18.1-22.6) mg: (29.2-36.4) mg: 20 ml: (4.0-5.0) mg.
[0010] Preferably, in step S1, the concentration of the sodium hydroxide solution is 120-200 g / L.
[0011] Preferably, in step S1, the hydrothermal reaction temperature is 120-140° C., and the time is 5-8 h.
[0012] Preferably, in step S2, the feeding ratio of the composite Cu-based dopa complex solution, CS, GO, NIPAM, BIS, KPS and TEMED is 10 ml: (0.05-0.08) g: (50-80) mg: (1.6-2.0) g: (0.05-0.08) g: (0.08-0.10) g: (120-170) μl.
[0013] Preferably, in step S2, the weight average molecular weight of the CS is in the range of 400,000-800,000, and the degree of deacetylation is 85-95%.
[0014] Preferably, in step S2, the average thickness of the GO is 0.55-2.0 nm.
[0015] Preferably, in step S3, the material of the underwear base fabric includes one of silk, cotton and modal.
[0016] Preferably, in step S3, the amount of the functional layer finishing agent is 30-50 g / m 2 Base fabric.
[0017] The present invention also provides an underwear fabric with ROS scavenging function prepared by the above preparation method.
[0018] Beneficial effects:
[0019] 1) This invention utilizes NIPAM to form a network structure through BIS crosslinking. The long chains of chitosan (CS) molecules contain amino, hydroxyl, and undeacylated acetylamino groups, which can hydrogen bond with oxygen and nitrogen in the polymerized PNIPAM, shuttling through the network structure to form a semi-IPN hydrogel, which serves as the functional layer of the underwear fabric. This hydrogel has a phase transition temperature of approximately 33°C. When the temperature is below 33°C, the hydrogel absorbs water and swells. The carbidopa and chitosan in the functional layer enhance the fabric's adhesion to the skin through their hydroxyl and amino structures, directing free radicals and ROS from the skin surface into the semi-IPN hydrogel. After the functional layer has been in close contact with the skin for a period of time, it shrinks dramatically when the temperature rises above 33°C, drawing water out of the network structure and simultaneously detaching the functional layer from the skin. This process, utilizing saturated water vapor on the body surface, directs free radicals and ROS from the surface into the hydrogel, where they are degraded by the Cu-dopa complex within the hydrogel.
[0020] 2) CTAB can not only neutralize the negative charge of carbidopa in alkaline environment, but also work synergistically with Cu to provide excellent antibacterial properties for hydrogels and underwear fabrics.
[0021] 3) GO not only effectively disperses the Cu-based DOPA complex, evenly distributing it throughout the functional layer, but also enhances its efficiency in catalyzing the degradation of ROS and free radicals through the randomly distributed hydroxyl and epoxy groups on the GO surface. Furthermore, GO enhances the strength and wash fastness of the functional layer, making it less susceptible to peeling. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 This is a scanning electron microscope photograph of the underwear fabric prepared in Example 1;
[0023] Figure 2 The reversibility test results of temperature response of various underwear fabrics are shown in Figure 2.
[0024] Figure 3 ROS scavenging performance of various underwear fabrics;
[0025] Figure 4 For the antibacterial properties of various underwear fabrics. DETAILED DESCRIPTION
[0026] In order to further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples. However, it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, rather than for limiting the claims of the present invention.
[0027] Example 1
[0028] An underwear fabric with ROS scavenging function and a preparation method thereof, comprising the following steps:
[0029] 1. Preparation of a composite Cu-based dopa complex: 20.0 mg of carbidopa and 33.4 mg of CTAB were added to 20 ml of water, the pH was adjusted to 10.2 with 160 g / L sodium hydroxide solution, and the mixture was stirred for 1.5 h. The pH was then adjusted to 5.5 with hydrochloric acid, and 4.5 mg of hydrated copper acetate was added. The mixture was hydrothermally reacted at 130°C for 7 h, and the mixture was concentrated by rotary evaporation at 75°C to 2 / 7 of the original volume. The pH was then adjusted to 3.4 with glacial acetic acid to obtain a composite Cu-based dopa complex solution.
[0030] 2. Preparation of a functional layer finishing agent: Cool 10 ml of the composite Cu-based dopa complex solution prepared in step 1 to 3°C, and add 0.07 g of CS (weight-average molecular weight 600,000, degree of deacetylation 90%), 65 mg of GO (average thickness 1.0 nm), 1.8 g of NIPAM, 0.06 g of BIS, 0.09 g of KPS, and 150 μl of TEMED in sequence, stirring thoroughly to obtain a functional layer finishing agent.
[0031] 3. Fabric finishing: Apply the functional layer finishing agent at 40g / m 2 Coated on cotton underwear base fabric, 400W / m 2 The ultraviolet irradiation is combined with drying at 110°C for setting, and the finishing process is repeated 4 times. The underwear fabric with ROS scavenging function is then washed and dried.
[0032] Example 2
[0033] An underwear fabric with ROS scavenging function and a preparation method thereof, comprising the following steps:
[0034] 1. Preparation of a composite Cu-based dopa complex: 18.1 mg of carbidopa and 29.2 mg of CTAB were added to 20 ml of water, the pH was adjusted to 10 with 120 g / L sodium hydroxide solution, and the mixture was stirred for 1 hour. The pH was then adjusted to 5 with hydrochloric acid. 4 mg of hydrated copper acetate was then added and the mixture was hydrothermally reacted at 120°C for 8 hours. The mixture was then concentrated by rotary evaporation at 70°C to 1 / 4 of the original volume. The pH was then adjusted to 3 with glacial acetic acid to obtain a composite Cu-based dopa complex solution.
[0035] 2. Preparation of a functional layer finishing agent: Cool 10 ml of the composite Cu-based dopa complex solution prepared in step 1 to 0°C, and add 0.05 g of CS (weight-average molecular weight 400,000, degree of deacetylation 85%), 50 mg of GO (average thickness 0.55 nm), 1.6 g of NIPAM, 0.05 g of BIS, 0.08 g of KPS, and 120 μl of TEMED in sequence, stirring thoroughly to obtain a functional layer finishing agent.
[0036] 3. Fabric finishing: Apply the functional layer finishing agent at 30g / m 2 Coated on silk underwear base fabric, 300W / m 2 The ultraviolet irradiation is combined with drying at 100°C for setting, and the finishing process is repeated three times. The underwear fabric with ROS scavenging function is then washed and dried.
[0037] Example 3
[0038] An underwear fabric with ROS scavenging function and a preparation method thereof, comprising the following steps:
[0039] 1. Preparation of a composite Cu-based dopa complex: 22.6 mg of carbidopa and 36.4 mg of CTAB were added to 20 ml of water, the pH was adjusted to 10.5 with 200 g / L sodium hydroxide solution, and the mixture was stirred for 2 h. The pH was then adjusted to 6 with hydrochloric acid. 5 mg of hydrated copper acetate was then added and the mixture was hydrothermally reacted at 140°C for 5 h. The mixture was then concentrated by rotary evaporation at 80°C to 1 / 3 of the original volume. The pH was then adjusted to 4.5 with glacial acetic acid to obtain a composite Cu-based dopa complex solution.
[0040] 2. Preparation of a functional layer finishing agent: Cool 10 ml of the composite Cu-based dopa complex solution prepared in step 1 to 4°C, and add 0.08 g of CS (weight-average molecular weight 800,000, degree of deacetylation 95%), 80 mg of GO (average thickness 2.0 nm), 2 g of NIPAM, 0.08 g of BIS, 0.1 g of KPS, and 170 μl of TEMED in sequence, stirring thoroughly to obtain a functional layer finishing agent.
[0041] 3. Fabric finishing: Apply the functional layer finishing agent at 50g / m 2 Coated on Modal underwear fabric, 500W / m 2 The ultraviolet irradiation is combined with drying at 120°C for setting, and the finishing process is repeated 5 times, and then washed and dried to obtain underwear fabric with ROS scavenging function.
[0042] An underwear fabric and a preparation method thereof, comprising the following steps:
[0043] 1. Preparation of functional layer finishing agent: 10 ml of glacial acetic acid solution (pH 3.4) was cooled to 3°C, and 0.07 g of CS (weight-average molecular weight 600,000, degree of deacetylation 90%), 65 mg of GO (average thickness 1.0 nm), 1.8 g of NIPAM, 0.06 g of BIS, 0.09 g of KPS, and 150 μl of TEMED were added in sequence and stirred thoroughly to obtain the functional layer finishing agent.
[0044] 2. Fabric finishing: Apply the functional layer finishing agent at 40g / m 2 Coated on cotton underwear base fabric, 400W / m 2The fabric is irradiated with ultraviolet light and dried at 110°C for final shaping, and the finishing process is repeated 4 times. The fabric is then washed and dried to obtain the underwear fabric.
[0045] Comparative Example 2 (without CTAB)
[0046] An underwear fabric and a preparation method thereof, comprising the following steps:
[0047] 1. Preparation of a composite Cu-based dopa complex: 20.0 mg of carbidopa was added to 20 ml of water, the pH was adjusted to 10.2 with 160 g / L sodium hydroxide solution, and the mixture was stirred for 1.5 h. The pH was then adjusted to 5.5 with hydrochloric acid, and 4.5 mg of hydrated copper acetate was added. The mixture was hydrothermally reacted at 130°C for 7 h, and then concentrated by rotary evaporation at 75°C to 2 / 7 of the original volume. The pH was then adjusted to 3.4 with glacial acetic acid to obtain a composite Cu-based dopa complex solution.
[0048] 2. Preparation of a functional layer finishing agent: Cool 10 ml of the composite Cu-based dopa complex solution prepared in step 1 to 3°C, and add 0.07 g of CS (weight-average molecular weight 600,000, degree of deacetylation 90%), 65 mg of GO (average thickness 1.0 nm), 1.8 g of NIPAM, 0.06 g of BIS, 0.09 g of KPS, and 150 μl of TEMED in sequence, stirring thoroughly to obtain a functional layer finishing agent.
[0049] 3. Fabric finishing: Apply the functional layer finishing agent at 40g / m 2 Coated on cotton underwear base fabric, 400W / m 2 The fabric is irradiated with ultraviolet light and dried at 110°C for final shaping, and the finishing process is repeated 4 times. The fabric is then washed and dried to obtain the underwear fabric.
[0050] Comparative Example 3 (without GO)
[0051] An underwear fabric and a preparation method thereof, comprising the following steps:
[0052] 1. Preparation of a composite Cu-based dopa complex: 20.0 mg of carbidopa and 33.4 mg of CTAB were added to 20 ml of water, the pH was adjusted to 10.2 with 160 g / L sodium hydroxide solution, and the mixture was stirred for 1.5 h. The pH was then adjusted to 5.5 with hydrochloric acid, and 4.5 mg of hydrated copper acetate was added. The mixture was hydrothermally reacted at 130°C for 7 h, and the mixture was concentrated by rotary evaporation at 75°C to 2 / 7 of the original volume. The pH was then adjusted to 3.4 with glacial acetic acid to obtain a composite Cu-based dopa complex solution.
[0053] 2. Preparation of a functional layer finishing agent: Cool 10 ml of the composite Cu-based dopa complex solution prepared in step 1 to 3°C, then add 0.07 g of CS (weight-average molecular weight 600,000, degree of deacetylation 90%), 1.8 g of NIPAM, 0.06 g of BIS, 0.09 g of KPS, and 150 μl of TEMED in sequence, stirring thoroughly to obtain a functional layer finishing agent.
[0054] 3. Fabric finishing: Apply the functional layer finishing agent at 40g / m 2 Coated on cotton underwear base fabric, 400W / m 2 The fabric is irradiated with ultraviolet light and dried at 110°C for final shaping, and the finishing process is repeated 4 times. The fabric is then washed and dried to obtain the underwear fabric.
[0055] Temperature-responsive reversibility experiment
[0056] The fabrics of Examples 1-3 and Comparative Examples 1-3 were pre-swelled in deionized water at 28°C for equilibrium, and then placed in deionized water at 35°C and 28°C alternately for appropriate periods of time, and their swelling rates were measured. The results are as follows: Figure 2 shown.
[0057] Depend on Figure 2 It can be seen that the underwear fabrics prepared in the examples exhibit excellent temperature response characteristics, absorbing water and swelling at low temperatures, and shrinking and discharging water at higher temperatures. The underwear fabric prepared in Comparative Example 1 does not have a composite Cu-based dopa complex as part of the skeleton support, which has a certain impact on its temperature response characteristics. The underwear fabric prepared in Comparative Example 2 does not contain CTAB and cannot synthesize a composite Cu-based dopa complex, which affects the fabric's temperature response characteristics. The fabric in Comparative Example 3 does not contain GO, and the strength and wash fastness of the functional layer are weakened, which has the greatest impact on the temperature response characteristics.
[0058] ROS scavenging experiment
[0059] The fabrics of Examples 1-3 and Comparative Examples 1-3 were immersed in a hydrogen peroxide solution simulating a ROS environment, and then placed alternately in a water bath at 37°C and 20°C for appropriate periods of time. The hydrogen peroxide content was measured using a hydrogen peroxide detection kit, and the ROS clearance rate was calculated. The results are shown in FIG. Figure 3 shown.
[0060] Depend on Figure 3It can be seen that the underwear fabric prepared in the example has a good ability to remove hydrogen peroxide, while the fabric prepared in the comparative example does not have this property. Hydrogen peroxide is a typical ROS marker, and its removal shows that the underwear fabric prepared in the example has ROS removal ability. The fabric of comparative example 1 does not have a composite Cu-based carbidopa complex and does not have the ability to decompose hydrogen peroxide into water and oxygen. The fabric of comparative example 2 does not have CTAB added, and carbidopa does not have CTAB to neutralize the charge. In an alkaline environment, the intermolecular repulsion is strong, and efficient free radical polymerization cannot be achieved, and a structurally complete composite Cu-based carbidopa complex cannot be obtained, which will also affect the decomposition of hydrogen peroxide. The fabric of comparative example 3 does not contain GO. GO can give the functional layer a certain mechanical strength and corrosion resistance, and has a promoting effect on the activity of the composite Cu-based carbidopa complex. The ROS active scavenging ability without a GO functional layer will be significantly reduced.
[0061] Antibacterial test of underwear fabrics
[0062] GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method" was used to measure the antibacterial rates of the fabrics of Examples 1-3 and Comparative Examples 1-3 against Staphylococcus aureus and Escherichia coli. The results are shown in Figure 4 .
[0063] Depend on Figure 4 It can be seen that the underwear fabric prepared in the examples has good antibacterial properties, while the fabric prepared in the comparative examples has poor antibacterial ability. The reason is that the fabric in comparative example 1 does not have the composite Cu-based dopa complex and CTAB, and does not have the synergistic bactericidal effect of Cu and CTAB, so the antibacterial ability is poor. The fabric in comparative example 2 does not have CTAB added, which hinders the synthesis of the composite Cu-based dopa complex. 2+ The fabric was ultimately washed and free of CTAB, resulting in an antibacterial effect similar to that of Comparative Example 1. The fabric of Comparative Example 3 lacked GO. GO effectively dispersed the Cu-based dopa complex while also improving the strength and wash fastness of the functional layer. Without GO, the antibacterial substances were easily eroded along with the functional layer, reducing the antibacterial efficacy.
[0064] The present invention provides a method and concept for producing underwear fabric with ROS scavenging capabilities. While there are numerous methods and approaches for implementing this technical solution, the aforementioned are merely preferred embodiments of the present invention. It should be noted that those skilled in the art may make improvements and modifications without departing from the principles of the present invention, and such improvements and modifications are also within the scope of protection of the present invention. Any components not specified in this embodiment may be implemented using existing technologies.
Claims
1. A method for preparing underwear fabric with ROS scavenging function, characterized in that: The steps include: S1. Preparation of a composite Cu-based dopa complex: Carbidopa and CTAB were sequentially added to water, the pH was adjusted to 10.0-10.5 with sodium hydroxide solution, and the mixture was stirred for 1-2 h. The pH was then adjusted to 5.0-6.0 with hydrochloric acid, and hydrated copper acetate was added. After a hydrothermal reaction, the mixture was concentrated by rotary evaporation at 70-80°C to 1 / 4-1 / 3 of the original volume, and the pH was adjusted to 3.0-4.5 with glacial acetic acid to obtain a composite Cu-based dopa complex solution. S2. Preparation of a functional layer finishing agent: The composite Cu-based dopa complex solution prepared in step S1 was cooled to 0-4 ° C, and CS, GO, NIPAM, BIS, KPS and TEMED were added sequentially and stirred to obtain a functional layer finishing agent; S3. Fabric finishing: Apply the functional layer finishing agent to the underwear base fabric, 300-500W / m 2 The ultraviolet irradiation is combined with drying at 100-120℃ for shaping, and the finishing process is repeated 3-5 times. The underwear fabric with ROS scavenging function is then washed and dried.
2. The preparation method according to claim 1, characterized in that In step S1, the feeding ratio of carbidopa, CTAB, water and hydrated copper acetate is (18.1-22.6) mg: (29.2-36.4) mg: 20 ml: (4.0-5.0) mg.
3. The preparation method according to claim 1, characterized in that In step S1, the concentration of the sodium hydroxide solution is 120-200 g / L.
4. The preparation method according to claim 1, characterized in that In step S1, the hydrothermal reaction temperature is 120-140° C. and the time is 5-8 hours.
5. The preparation method according to claim 1, characterized in that In step S2, the feeding ratio of the composite Cu-based dopa complex solution, CS, GO, NIPAM, BIS, KPS and TEMED is 10 ml: (0.05-0.08) g: (50-80) mg: (1.6-2.0) g: (0.05-0.08) g: (0.08-0.10) g: (120-170) μl.
6. The preparation method according to claim 1, characterized in that In step S2, the weight average molecular weight of the CS is in the range of 400,000 to 800,000, and the degree of deacetylation is 85-95%.
7. The preparation method according to claim 1, characterized in that In step S2, the average thickness of the GO is 0.55-2.0 nm.
8. The preparation method according to claim 1, characterized in that In step S3, the material of the underwear base fabric includes one of silk, cotton and modal.
9. The preparation method according to claim 1, characterized in that In step S3, the amount of the functional layer finishing agent is 30-50 g / m 2 Underwear base fabric.
10. Underwear fabric with ROS scavenging function prepared according to the preparation method according to any one of claims 1 to 9.
Citation Information
Patent Citations
Antibacterial finishing agent for silk fabrics and preparation method of antibacterial finishing agent
CN112575581A
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CN115948913A