A method of making a smart janus textile with graphene oxide and hydrogel coating with superior thermal regulation

By coating the front and back of the fabric with graphene oxide and hydrogel coatings respectively, the smart Janus textile has overcome the limitations of existing smart clothing in terms of temperature regulation and antibacterial properties, achieving efficient and low-cost bidirectional temperature regulation and antibacterial effects.

CN118007443BActive Publication Date: 2026-08-25YANGZHOU UNIV
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202410355238.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-03-27
Publication Date
2026-08-25
Estimated Expiration
2044-03-27

AI Technical Summary

Technical Problem

Existing smart clothing suffers from limited applicability, complex manufacturing processes, and high costs in terms of temperature regulation and antibacterial properties, and cannot effectively regulate temperature and inhibit bacterial growth in outdoor environments.

Method used

The smart Janus textile, which uses graphene oxide and hydrogel coating, achieves bidirectional temperature regulation and antibacterial function by brushing the graphene oxide coating on the front of the fabric for heating mode, utilizing photothermal conversion performance to raise the temperature, and spraying the hydrogel coating on the back of the fabric for cooling mode.

Benefits of technology

It achieves evaporative cooling in hot environments and solar heating in cold environments, possessing excellent thermal regulation performance, antibacterial properties, low cost, and simple operation.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN118007443B_ABST
    Figure CN118007443B_ABST
Patent Text Reader

Abstract

The application discloses a preparation method of an intelligent Janus textile with an excellent heat-regulating graphene oxide and hydrogel coating, and belongs to the technical field of energy materials. The original fabric is used as a carrier, a graphene oxide coating is brushed on the front of the fabric, the coating belongs to a heating mode, has good light-heat conversion performance, converts solar energy into heat energy, makes the temperature of the fabric rise to achieve a heating effect, and has sterilization performance, so that health problems can be reduced; a hydrogel coating is sprayed on the back of the fabric, the coating belongs to a cooling mode, has good water absorption performance, some water is actively added to the surface of the coating, water is evaporated under sunlight to absorb a large amount of heat, so that the surface temperature of the fabric is reduced to achieve a cooling effect, and 2-(N-(2-(methacryloyloxy)ethyl)-N,N-dimethylamine)ethyl sulfate is added to the cooling layer coating, so that the coating has antibacterial performance and can inhibit the growth of bacteria; the intelligent fabric integrates heating, cooling and antibacterial performance, and the performance value of the intelligent fabric is greatly improved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of energy materials technology, specifically to a method for preparing smart Janus textiles with excellent thermal regulation of graphene oxide and hydrogel coating. Background Technology

[0002] Global warming has led to significantly higher summer temperatures, posing serious threats to human health and property safety, and increasing the demand for comfortable temperatures. Currently, the primary method for addressing this issue remains air conditioning systems to regulate indoor temperatures through active cooling and heating. However, this process consumes substantial amounts of energy and generates greenhouse gas emissions. Furthermore, air conditioning has significant limitations; it is only suitable for indoor use and within buildings, and not for outdoor applications. Therefore, researchers are seeking a convenient and effective solution to this problem.

[0003] Besides active cooling via air conditioning, there is also passive cooling, which does not consume energy. Since the human body is separated from the environment by clothing, temperature can be regulated by changing the clothing, allowing the body to feel cool or warm. In recent years, researchers have developed smart clothing using cooling materials such as porous hydrogels, nanofiber membranes, and functional coatings, achieving reflective and radiative cooling effects. However, these cooling systems have limited applicability, complex manufacturing processes, and high costs. Summary of the Invention

[0004] To address the aforementioned issues, this invention provides a method for preparing smart Janus textiles with excellent thermal regulation of graphene oxide and hydrogel coating.

[0005] The purpose of this invention is to provide a smart Janus textile with excellent thermal regulation through a graphene oxide and hydrogel-coated fabric. Its advantages include integrated cooling, heating, and antibacterial properties. In hot environments, water can be added for evaporative cooling, while in cold environments, it can absorb solar energy and convert it into passive heating. Simultaneously, it inhibits bacterial growth, is low-cost, and simple to operate.

[0006] This invention is achieved through the following technical solution: A method for preparing a smart Janus textile with a thermally modulated graphene oxide and hydrogel coating, characterized by comprising the following steps: S1: Preparation of 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate: Dimethylaminoethyl methacrylate and 1,3,2-dioxazolthiophene-2,2-dioxide were dissolved in acetonitrile and stirred continuously at 50-60 °C for 24-30 h; the mixture after reaction was cooled to -25 °C, the solid was filtered out and washed with acetonitrile, and then dried under vacuum to obtain 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate; S2: Preparation of a heated and antibacterial fabric: Acryloyloxyethyltrimethylammonium chloride, ethyl acrylate, N,N-methylenebisacrylamide, dimethyl sulfoxide, and TPO-L are mixed evenly in a certain proportion. This solution is then mixed evenly with graphene oxide in a certain proportion. 0.4-0.5 g of this mixture is brushed onto the front side of the fabric at 2000-2500 W / m². 2 Photocuring is performed under light intensity, followed by drying at 40-50 ℃ to obtain a heated and antibacterial fabric. S3: Preparation of a cooling-mode and antibacterial fabric coating solution: Add a certain amount of sodium hydroxide to acrylic acid to form a solution with a neutralization degree of 80%. Then add 2-hydroxyethyl methacrylate, ultrapure water, N,N-methylenebisacrylamide and TPO-L respectively, and shake evenly to obtain a solution. Then mix the solution with 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)ethyl sulfate prepared in step S1 in a certain proportion to obtain a cooling-mode and antibacterial fabric coating solution. S4: Preparation of smart Janus textiles with thermally modulated graphene oxide and hydrogel coatings: Take 0.1-0.3 g of the coating solution obtained in step S3 and spray it onto the reverse side of the fabric prepared in step S2, at 2000-2500 W / m 2 Photocuring is performed under light intensity, followed by drying at 40-50 ℃ to obtain a smart fabric with heat regulation and antibacterial functions.

[0007] In step S1, the mass of dimethylaminoethyl methacrylate is 3.46 g, the mass of 1,3,2-dioxazothiophene-2,2-dioxide is 2.48 g, and the volume of acetonitrile used for dissolution is 30 mL.

[0008] In step S2, the mass percentages of the acryloyloxyethyltrimethylammonium chloride are 5-8 wt%, the mass percentages of ethyl acrylate are 33-35 wt%, the mass percentages of N,N-methylenebisacrylamide are 0.1-0.3 wt%, the mass percentages of dimethyl sulfoxide are 55-58 wt%, and the mass percentages of TPO-L are 0.5-1 wt%. The above substances are mixed in proportion and ultrasonically dissolved evenly. Then, they are mixed with graphene oxide in proportion and ultrasonically vibrated evenly to obtain a mixed solution. The mass percentage of graphene oxide is 5-11 wt%.

[0009] This invention utilizes the excellent photothermal conversion properties of graphene oxide and the antibacterial properties of acryloyloxyethyltrimethylammonium chloride. Graphene oxide is mixed evenly with a precursor solution of acryloyloxyethyltrimethylammonium chloride and ethyl acrylate, then brushed onto the surface of ordinary fabric, cured under light, and then dried to obtain a heated and antibacterial fabric. By utilizing the antibacterial properties of ethyl 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)sulfate, it is mixed evenly with a precursor solution of acrylic acid and hydroxyethyl 2-methacrylate. This solution is then sprayed onto the back of a heated and antibacterial fabric to obtain a smart fabric with dual-mode thermal regulation and antibacterial functions.

[0010] Compared with the prior art, the beneficial effects of the present invention are: This invention prepares a smart Janus textile with excellent thermal regulation through graphene oxide and hydrogel coating. Using the original fabric as a carrier, a graphene oxide coating is brushed onto the front side of the fabric. This coating operates in a heating mode, exhibiting excellent photothermal conversion performance, converting solar energy into heat energy to raise the fabric temperature and achieve a heating effect. It also possesses antibacterial properties, inhibiting bacterial growth and reducing health problems. A hydrogel coating is sprayed onto the reverse side of the fabric. This coating operates in a cooling mode, exhibiting excellent water absorption properties. When water is actively added to its surface, it evaporates under sunlight, absorbing a large amount of heat and lowering the fabric surface temperature to achieve a cooling effect. The cooling layer coating incorporates ethyl 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)sulfate, which has antibacterial properties and inhibits bacterial growth. This smart textile integrates heating, cooling, and antibacterial functions, significantly enhancing its performance value. Attached Figure Description

[0011] Figure 1In the diagram, (a) and (a1) are the macroscopic structure diagram and SEM image of GF(5%) in Embodiment 1 of the present invention; (b) and (b1) are the macroscopic structure diagram and SEM image of GF(7%) in Embodiment 2 of the present invention; (c) and (c1) are the macroscopic structure diagram and SEM image of GF(9%) in Embodiment 3 of the present invention; and (d) and (d1) are the macroscopic structure diagram and SEM image of GF(11%) in Embodiment 4 of the present invention. Figure 2 In the diagrams, (a) and (a1) are macroscopic structural diagrams and SEM images of the unmodified fabric; (b) and (b1) are macroscopic structural diagrams and SEM images of AF(0.1) in Example 5 of the present invention; (c) and (c1) are macroscopic structural diagrams and SEM images of AF(0.2) in Example 6 of the present invention; and (d) and (d1) are macroscopic structural diagrams and SEM images of AF(0.3) in Example 7 of the present invention. Figure 3 (a) shows the Fourier transform infrared spectra of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of this invention; (b) shows the XRD patterns of the fabrics obtained in Examples 1, 2, 3, and 4. Figure 4 (a) and (b) are the reflectance and absorptivity diagrams in the visible and near-infrared regions of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3 and 4 of the present invention, respectively; (c) and (d) are the reflectance and absorptivity diagrams in the visible and near-infrared regions of the unmodified fabric and the fabrics obtained in Examples 5, 6 and 7 of the present invention, respectively. Figure 5 Fourier transform infrared spectrum of 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate (MDES) prepared; Figure 6 (a) shows the heating curves of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of this invention under simulated 0.2 days of sunlight; (b) shows the heating curves of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of this invention under simulated 0.5 days of sunlight; (c) shows the heating curves of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of this invention under simulated 1 day of sunlight; (d) shows the temperature difference between the fabrics obtained in Examples 1, 2, 3, and 4 of this invention and the unmodified fabric after one hour of simulated 0.2 days of sunlight; (e) shows the temperature difference between the fabrics obtained in Examples 1, 2, 3, and 4 of this invention and the unmodified fabric after one hour of simulated 0.5 days of sunlight; (f) shows the temperature difference between the fabrics obtained in Examples 1, 2, 3, and 4 of this invention and the unmodified fabric after one hour of simulated 1 day of sunlight. Figure 7 In example (a), the fabrics obtained in Example 5 of this invention were treated with 0.1 kg m -2and 0.2 kg m -2 (a) Cooling and heating curves under simulated sunlight after water treatment; (b) Fabrics obtained in Example 6 of this invention were treated with 0.1 kgm³ of water. -2 and 0.2 kg m -2 (c) Cooling and heating curves under simulated sunlight after water treatment; (d) Fabrics obtained in Example 7 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 The cooling and heating curves after water treatment under simulated sunlight are shown in (d) and (e) are the fabrics obtained in Examples 5, 6, and 7 of this invention, respectively, after adding 0.1 kg m -2 and 0.2 kg m -2 The temperature difference between the water and the unmodified fabric when cooled under sunlight for one day; Figure 8 In example (a), the fabrics obtained in Example 5 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (a) Cooling and heating curves after water exposure under simulated 0.5 days of sunlight; (b) Fabrics obtained in Example 6 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (c) Cooling and heating curves after water exposure under simulated 0.5 sun illumination; (d) Fabrics obtained in Example 7 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 The cooling and heating curves after water exposure under simulated 0.5 days of sunlight; (d) shows the fabrics obtained in Examples 5, 6, and 7 of this invention after adding 0.1 kg m -2 and 0.2 kg m -2 The temperature difference between the water-cooled fabric and the unmodified fabric when cooled under 0.5 hours of sunlight; Figure 9 In example (a), the fabrics obtained in Example 5 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (a) Cooling and heating curves under simulated 0.2 days of sunlight after water treatment; (b) Fabrics obtained in Example 6 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (c) Cooling and heating curves after water exposure under simulated 0.2 solar rays; (d) Fabrics obtained in Example 7 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 The cooling and heating curves after water exposure under simulated 0.2 solar radiation are shown in Figure 1; (d) shows the fabrics obtained in Examples 5, 6, and 7 of this invention after adding 0.1 kg m³ of water.-2 and 0.2 kg m -2 The temperature difference between the water-cooled fabric and the unmodified fabric when cooled under 0.2 hours of sunlight; Figure 10 In the figures, (a) shows the heating curves of the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight exposure of 0.2, 0.5, and 1 day, respectively; (b) shows the temperature difference between the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight exposure of 0.2 day; (c) shows the temperature difference between the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight exposure of 0.5 day; and (d) shows the temperature difference between the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight exposure of 1 day. Figure 11 In example (a), the fabric obtained in Example 8 of this invention has been treated with 0.2 kg m -2 (a) Cooling and heating curves after water exposure under simulated 0.2 solar rays; (b) Fabric obtained in Example 8 of this invention with 0.2 kg m -2 (c) Cooling and heating curves under simulated 0.5 days of sunlight after water treatment; (d) Fabric obtained in Example 8 of this invention was treated with 0.2 kg m -2 (d) is the cooling and heating curve of the fabric obtained in Example 8 of this invention and the unmodified fabric under simulated sunlight for 0.2, 0.5 and 1 day. Figure 12 In the figure, (a) represents the antibacterial performance test of Staphylococcus aureus on the unmodified fabric, the fabric obtained in Example 4 of the present invention, and the fabric obtained in Example 7 of the present invention using the patch method; and (b) represents the concentration of bacteria after co-culturing the unmodified fabric, the fabric obtained in Example 4 of the present invention, and the fabric obtained in Example 7 of the present invention. Detailed Implementation

[0012] The present invention will be further described below with reference to the accompanying drawings: Example 1

[0013] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing heat-modified and antibacterial fabrics (GF) include: Under ultrasonic conditions, 9 g of ethyl acrylate, 1.9 g of acryloyloxyethyltrimethylammonium chloride, 15 g of dimethyl sulfoxide, 0.07 g of N,N-methylenebisacrylamide, and 0.22 g of TPO-L (ethyl 2,4,6-trimethylbenzoylphenylphosphonate) were mixed and ultrasonically dissolved until homogeneous. 0.95 g of this solution was then mixed with 0.05 g of graphene oxide and ultrasonically vibrated until homogeneous. 0.4 g of the mixture was brushed onto the fabric surface and heated at 2500 W / m². 2 The fabric was photocured under light intensity and dried at 50 °C to obtain a heated and antibacterial fabric, named GF(5%). Example 2

[0014] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing heat-modified and antibacterial fabrics (GF) include: Under ultrasonic conditions, 9 g of ethyl acrylate, 1.9 g of acryloyloxyethyltrimethylammonium chloride, 15 g of dimethyl sulfoxide, 0.07 g of N,N-methylenebisacrylamide, and 0.22 g of TPO-L were mixed and ultrasonically dissolved until homogeneous. 0.93 g of this solution was then mixed with 0.07 g of graphene oxide and ultrasonically vibrated until homogeneous. 0.4 g of the mixture was brushed onto the fabric surface and heated at 2500 W / m². 2 Photocuring was performed under light intensity, and the product was dried at 50 °C to obtain a heated and antibacterial fabric, which was named GF(7%). Example 3

[0015] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing heat-modified and antibacterial fabrics (GF) include: Under ultrasonic conditions, 9 g of ethyl acrylate, 1.9 g of acryloyloxyethyltrimethylammonium chloride, 15 g of dimethyl sulfoxide, 0.07 g of N,N-methylenebisacrylamide, and 0.22 g of TPO-L were mixed and ultrasonically dissolved until homogeneous. 0.91 g of this solution was then mixed with 0.09 g of graphene oxide and ultrasonically vibrated until homogeneous. 0.4 g of the mixture was brushed onto the fabric surface and heated at 2500 W / m². 2 The fabric was photocured under light intensity and dried at 50 °C to obtain a heated and antibacterial fabric, which was named GF(9%). Example 4

[0016] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing heat-modified and antibacterial fabrics (GF) include: Under ultrasonic conditions, 9 g of ethyl acrylate, 1.9 g of acryloyloxyethyltrimethylammonium chloride, 15 g of dimethyl sulfoxide, 0.07 g of N,N-methylenebisacrylamide, and 0.22 g of TPO-L were mixed and ultrasonically dissolved until homogeneous. 0.89 g of this solution was then mixed with 0.11 g of graphene oxide and ultrasonically vibrated until homogeneous. 0.4 g of the mixture was brushed onto the fabric surface and heated at 2500 W / m². 2 The fabric was photocured under light intensity and dried at 50 °C to obtain a heated and antibacterial fabric, which was named GF(11%). Example 5

[0017] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing cooling-mode and antibacterial fabrics (AF) include: (1) Preparation of ethyl 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)sulfate: 3.46 g of dimethylaminoethyl methacrylate and 2.48 g of 1,3,2-dioxazolthiophene-2,2-dioxide were dissolved in 30 mL of acetonitrile, and the mixture was stirred continuously at 50 °C for 24 h. The resulting mixture was cooled to -25 °C, the solid was filtered off and washed with acetonitrile, and then dried under vacuum to obtain 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate, named MDES.

[0018] (2) Add 10 g of acrylic acid to 14 ml of 8 mol / L solution. -1 In sodium hydroxide, a solution with a neutralization degree of 80% is formed. Then, 0.95 g of hydroxyethyl 2-methacrylate, 2.94 g of ultrapure water, 0.00328 g of N,N-methylenebisacrylamide and 0.01533 g of TPO-L are added to mix the solution and ultrasonically vibrate it until homogeneous.

[0019] (3) Mix the solution prepared in (2) with the MDES prepared in (1) at a ratio of 5:1, and ultrasonically vibrate until homogeneous. Take 0.1 g of the mixture and spray it onto the fabric surface. 2 The fabric obtained by photocuring under light intensity and exhibiting a cooling mode and antibacterial properties was named AF(0.1). Example 6

[0020] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing cooling-mode and antibacterial fabrics (AF) include: (1) Preparation of ethyl 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)sulfate: 3.46 g of dimethylaminoethyl methacrylate and 2.48 g of 1,3,2-dioxazothiophene-2,2-dioxide were dissolved in 30 mL of acetonitrile, and the mixture was stirred continuously at 50 °C for 24 h. The resulting mixture was cooled to -25 °C, the solid was filtered off and washed with acetonitrile, and then dried under vacuum to obtain 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate, named MDES.

[0021] (2) Add 10g of acrylic acid to 14 mL of 8mol / L solution. -1 In sodium hydroxide, a solution with a neutralization degree of 80% is formed. Then, 0.95g of hydroxyethyl 2-methacrylate, 2.94g of ultrapure water, 0.00328g of N,N-methylenebisacrylamide and 0.01533g of TPO-L are added to mix the solution and ultrasonically vibrate it until homogeneous.

[0022] (3) Mix the solution prepared in (2) with the MDES prepared in (1) at a ratio of 5:1, and ultrasonically vibrate until homogeneous. Take 0.2g of the mixture and spray it onto the fabric surface. 2 The fabric obtained by photocuring under light intensity and exhibiting a cooling mode and antibacterial properties was named AF(0.2). Example 7

[0023] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: Methods for preparing cooling-mode and antibacterial fabrics (AF) include: (1) Preparation of ethyl 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)sulfate: 3.46 g of dimethylaminoethyl methacrylate and 2.48 g of 1,3,2-dioxazothiophene-2,2-dioxide were dissolved in 30 mL of acetonitrile, and the mixture was stirred continuously at 50 °C for 24 h. The resulting mixture was cooled to -25 °C, the solid was filtered off and washed with acetonitrile, and then dried under vacuum to obtain 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate, named MDES.

[0024] (2) Add 10 g of acrylic acid to 14 mL of 8 mol L -1In sodium hydroxide, a solution with a neutralization degree of 80% is formed. Then, 0.95 g of hydroxyethyl 2-methacrylate, 2.94 g of ultrapure water, 0.00328 g of N,N-methylenebisacrylamide and 0.01533 g of TPO-L are added to mix the solution and ultrasonically vibrate it until homogeneous.

[0025] (3) Mix the solution prepared in (2) with the MDES prepared in (1) at a ratio of 5:1, and ultrasonically vibrate until homogeneous. Take 0.3 g of the mixture and spray it onto the fabric surface. 2 The fabric obtained by photocuring under light intensity and exhibiting a cooling mode and antibacterial properties was named AF(0.3). Example 8

[0026] A method for preparing a smart Janus textile with excellent thermal regulation of graphene oxide and a hydrogel coating, comprising: (1) A method for preparing a heated and antibacterial fabric (GF) includes: Under ultrasonic conditions, 9 g of ethyl acrylate, 1.9 g of acryloyloxyethyltrimethylammonium chloride, 15 g of dimethyl sulfoxide, 0.07 g of N,N-methylenebisacrylamide, and 0.22 g of TPO-L were mixed and ultrasonically dissolved until homogeneous. 0.89 g of this solution was then mixed with 0.11 g of graphene oxide and ultrasonically vibrated until homogeneous. 0.4 g of the mixture was brushed onto the front side of the fabric and heated at 2500 W / m². 2 Photocuring was performed under light intensity, followed by drying at 50 ℃ to obtain a heated and antibacterial fabric, which was named GF.

[0027] (2) Preparation of ethyl 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)sulfate: 3.46 g of dimethylaminoethyl methacrylate and 2.48 g of 1,3,2-dioxazolthiophene-2,2-dioxide were dissolved in 30 mL of acetonitrile, and the mixture was stirred continuously at 50 °C for 24 h. The resulting mixture was cooled to -25 °C, the solid was filtered off and washed with acetonitrile, and then dried under vacuum to obtain 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate, named MDES.

[0028] (3) The preparation method of the coating solution for cooling and antibacterial fabrics (AF) includes: Add 10 g of acrylic acid to 14 mL of 8 mol / L solution. -1A solution with a neutralization degree of 80% was prepared in sodium hydroxide. Then, 0.95 g of hydroxyethyl 2-methacrylate, 2.94 g of ultrapure water, 0.00328 g of N,N-methylenebisacrylamide, and 0.01533 g of TPO-L were added to the solution, and the mixture was ultrasonically vibrated until homogeneous. The prepared solution was then mixed with the MDES prepared in (2) at a ratio of 5:1 and ultrasonically vibrated until homogeneous.

[0029] (4) The preparation methods of smart fabrics with dual-mode thermal regulation and antibacterial functions include: Take 0.3 g of the solution prepared in step (3) and spray it onto the uncoated side (back side) of the heated and antibacterial fabric (AF) prepared in step (1), at 2500 W / m. 2 Photocuring under light intensity and drying at 50℃ yields a smart fabric with dual-mode thermal regulation and antibacterial functions, named G / AF.

[0030] Figure 1 (a), (b), (c), and (d) are macroscopic structural diagrams of GF (5%) in Example 1, GF (7%) in Example 2, GF (9%) in Example 3, and GF (11%) in Example 4, respectively. It can be seen that the color becomes darker as the concentration of graphene oxide increases. (a1), (b1), (c1), and (d1) are SEM images of the fabrics obtained in Examples 1, 2, 3, and 4, respectively. It can be seen that the fiber structure is retained on the surface, and a clear coating film is visible on the surface.

[0031] Figure 2 (a), (b), (c), and (d) are macroscopic structural diagrams of the original fabric, Example 5 AF (0.1), Example 6 A-F (0.2), and Example 7 AF (0.3), respectively; (a1), (b1), (c1), and (d1) are SEM images of the original fabric, Examples 5, 6, and 7, respectively. It can be seen that the surface of the original fabric is smooth, and the coated fabric fibers exhibit a microparticle structure. The higher the hydrogel content on the fabric, the richer the microparticles on the fabric.

[0032] Figure 3 (a) shows the Fourier transform infrared spectra of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of this invention; (b) shows the XRD patterns of Examples 1, 2, 3, and 4. It can be seen from the figures that the GF fabric was successfully synthesized.

[0033] Figure 4(a) and (b) are the reflectance and absorptivity diagrams in the visible and near-infrared regions of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3 and 4 of the present invention, respectively; (c) and (d) are the reflectance and absorptivity diagrams in the visible and near-infrared regions of the unmodified fabric and the fabrics obtained in Examples 5, 6 and 7 of the present invention, respectively.

[0034] Figure 5 Fourier transform infrared spectra of 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate (MDES) were obtained. The figure shows that 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate was successfully synthesized.

[0035] Figure 6 (a) shows the temperature rise curves of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of the present invention under simulated 0.2 solar intensity; (b) shows the temperature rise curves of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of the present invention under simulated 0.5 solar intensity; (c) shows the temperature rise curves of the unmodified fabric and the fabrics obtained in Examples 1, 2, 3, and 4 of the present invention under simulated 1 solar intensity; (d) shows the temperature difference between the fabrics obtained in Examples 1, 2, 3, and 4 of the present invention and the unmodified fabric after one hour of illumination under simulated 0.2 solar intensity; (e) shows the temperature difference between the fabrics obtained in Examples 1, 2, 3, and 4 of the present invention and the unmodified fabric after one hour of illumination under simulated 0.5 solar intensity; (f) shows the temperature difference between the fabrics obtained in Examples 1, 2, 3, and 4 of the present invention and the unmodified fabric after one hour of illumination under simulated 1 solar intensity.

[0036] Figure 7 In example (a), the fabrics obtained in Example 5 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (a) Cooling and heating curves of the fabric obtained in Example 6 of this invention after being exposed to simulated sunlight intensity; (b) The fabric obtained after being exposed to simulated sunlight intensity intensity after being exposed to simulated sunlight intensity intensity after being exposed to simulated sunlight intensity intensity. -2 and 0.2 kg m -2 (c) Cooling and heating curves of the fabric obtained in Example 7 of this invention after being exposed to simulated sunlight intensity; -2 and 0.2 kg m -2 The cooling and heating curves after water treatment under simulated sunlight intensity are shown in Figure 5; (d) shows the fabrics obtained in Examples 5, 6, and 7 of this invention after adding 0.1 kg m³ of water. -2 and 0.2 kg m -2 The temperature difference between the water-cooled fabric and the unmodified fabric when cooled under strong sunlight.

[0037] Figure 8 In example (a), the fabrics obtained in Example 5 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (a) Cooling and heating curves of the fabric obtained in Example 6 of this invention after being exposed to water under simulated sunlight intensity of 0.5; (b) Adding 0.1 kg m -2 and 0.2 kg m -2 (c) Cooling and heating curves of the fabric obtained in Example 7 of this invention after being exposed to water under simulated sunlight intensity of 0.5; -2 and 0.2 kg m -2 The cooling and heating curves after water treatment under simulated 0.5 solar intensity are shown in Figure 1; (d) shows the cooling and heating curves of the fabrics obtained in Examples 5, 6, and 7 of this invention after adding 0.1 kg m³ of water. -2 and 0.2 kg m -2 The temperature difference between the water-cooled fabric and the unmodified fabric when cooled under 0.5 times sunlight intensity.

[0038] Figure 9 In example (a), the fabrics obtained in Example 5 of this invention were treated with 0.1 kg m -2 and 0.2 kg m -2 (a) Cooling and heating curves of the fabric obtained in Example 6 of this invention after being exposed to simulated sunlight intensity of 0.2; (b) The fabric obtained after being exposed to simulated sunlight intensity of 0.1 kg m -2 and 0.2 kg m -2 (c) Cooling and heating curves of the fabric obtained in Example 7 of this invention after being exposed to water under simulated sunlight intensity of 0.2; -2 and 0.2 kg m -2 The cooling and heating curves after water treatment under simulated sunlight intensity of 0.2 are shown in Figure 1; (d) shows the cooling and heating curves of the fabrics obtained in Examples 5, 6, and 7 of this invention after adding 0.1 kg m³ of water. -2 and 0.2 kg m -2 The temperature difference between the water-cooled fabric and the unmodified fabric when cooled under 0.2 times sunlight intensity.

[0039] Figure 10 In the figure, (a) is the heating curve of the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight intensity of 0.2, 0.5 and 1, respectively; (b) is the temperature difference between the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight intensity of 0.2; (c) is the temperature difference between the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight intensity of 0.5; and (d) is the temperature difference between the fabric obtained in Example 8 of the present invention and the unmodified fabric under simulated sunlight intensity of 1.

[0040] Figure 11 In example (a), the fabric obtained in Example 8 of this invention has been treated with 0.2 kg m -2 (a) Cooling and temperature rise curve of the fabric obtained in Example 8 of this invention after water treatment under simulated 0.2 solar intensity; (b) Adding 0.2 kg m -2 (c) The cooling and temperature rise curve of the fabric obtained in Example 8 of this invention after being soaked in water under simulated 0.5 solar intensity; -2 (d) is the temperature difference between the fabric obtained in Example 8 of this invention and the unmodified fabric when cooled under simulated sunlight intensity of 0.2, 0.5, and 1.

[0041] Figure 12 In the figures, (a) represents the unmodified fabric, the fabric obtained in Example 4 of the present invention, and Example 7 of the present invention, and the antibacterial performance of Staphylococcus aureus was tested using the patch method; (b) represents the concentration of bacteria after the unmodified fabric, the fabric obtained in Example 4 of the present invention, and Example 7 of the present invention were cultured using the co-culture method.

[0042] Test Results 1. GF heating performance test To investigate the heating performance of GF(5%), GF(7%), GF(9%), and GF(11%) of this invention, xenon lamps were used to simulate 0.2, 0.5, and 1 sun, respectively. The environmental conditions were 35% humidity and 30°C. GF(5%), GF(7%), GF(9%), and GF(11%) were each irradiated for one hour, and their surface temperature changes were recorded using an infrared thermal imager. Figure 6 (a, b, and c) show that the sample surface temperature increases in all cases. Figure 6 (d, e, and f) show that GF(11%) has the best heating effect, with temperatures 16.5 ℃, 28.4 ℃, and 44.9 ℃ higher than the original fabric under 0.2, 0.5, and 1 suns, respectively.

[0043] 2. AF Cooling Performance Test To investigate the cooling performance of AF(0.1), AF(0.2), and AF(0.3) of this invention, xenon lamps were used to simulate 0.2, 0.5, and 1 sun, respectively. The environmental conditions were: humidity 35% and temperature 30°C. 0.1 kgm³ of heat was added to AF(0.1), AF(0.2), and AF(0.3) respectively. -2 0.2kg m -2 After being submerged in water, each sample was exposed to light for one hour, and the surface temperature changes were recorded using an infrared thermal imager.

[0044] from Figure 7(a, b, and c) show that after adding water, the temperatures of AF(0.1), AF(0.2), and AF(0.3) were significantly lower than the original fabric temperature under one day of sunlight. AF(0.3) was further treated with 0.1 kg m -2 0.2kg m -2 After 15 minutes of exposure to sunlight, the temperature of the fabric was 6.9°C and 7.7°C lower than the original fabric, respectively. Further cooling experiments were conducted under 0.5 and 0.2 solar exposures. Figure 8 (a,b,c) and Figure 9 (a, b, c) shows that AF(0.1), AF(0.2), and AF(0.3) with added water heated up slowly, and each added 0.1 kg m -2 0.2 kg m -2 After 15 minutes of exposure to 0.5 suns, the water-based AF (0.1) fabric was 8.1 °C and 11.3 °C lower in temperature than the original fabric, respectively. This was achieved by adding 0.1 kg m... -2 0.2kg m -2 After being exposed to 0.2 suns for 15 minutes, the water-based AF(0.3) fabric was 3.7°C and 5.1°C lower in temperature than the original fabric, respectively. Therefore, AF(0.3) was selected.

[0045] 3. G / AF heating performance test To study the heating performance of the G / AF of this invention, xenon lamps were used to simulate 0.2, 0.5, and 1 sun, under environmental conditions of 35% humidity and 30°C. The G / AF was exposed to the light for one hour each time, and its surface temperature changes were recorded using an infrared thermal imager. Figure 10 As shown in (a). After one hour of illumination, from Figure 10 (b) Figure 10 (c) and Figure 10 As shown in (d), the temperature of the G / AF fabric is 15.4 ℃, 22.7 ℃ and 43.7 ℃ higher than that of the original fabric, respectively, demonstrating the excellent heating performance of the G / AF fabric.

[0046] 4. G / AF Cooling Performance Test To investigate the cooling performance of the G / AF of this invention, xenon lamps were used to simulate 0.2, 0.5, and 1 suns. The environmental conditions were: humidity 35% and temperature 30 °C. A 0.2 kg m³ / h ionization charge was applied to the G / AF. -2 After being submerged in water, each sample was exposed to light for one hour, and the surface temperature changes were recorded using an infrared thermal imager. Figure 11 As shown in (a), 11 (b), and 11 (c). Under 0.2 and 0.5 solar irradiation, G / AF was replenished every 20 minutes; under 1 solar irradiation, G / AF was replenished every 10 minutes. From Figure 11(d) It can be seen that after 15 minutes of light exposure, the temperature of G / AF is 7.1 ℃ lower than that of the original fabric.

[0047] 5. Antibacterial performance test of GF and AF (1) Inoculate 1% Staphylococcus warwick (Gram-positive bacteria) into LB liquid medium and incubate for 24 h. Then add 100 μL of bacterial solution to LB semi-solid medium, mix well, and pour into a petri dish containing LB solid medium. Place the original fabric GF and AF (both with a diameter of 1 cm) in the center of the petri dish and incubate for 24 h. Observe the size of the inhibition zone.

[0048] (2) Gram-positive Staphylococcus warneri was inoculated into 1% LB liquid medium. Subsequently, 10 mL of medium was taken from each tube, and 0.5 g of the original fabric or GF / AF was added respectively. Three groups were set up for each fabric type. The bacterial concentration was evaluated after incubation for 24 h.

[0049] from Figure 12 As shown in Figure a, the culture dish containing the original fabric showed no inhibition zone, indicating that it had no antibacterial properties. The culture dish containing the GF fabric showed a clear inhibition zone around the fabric, indicating its ability to inhibit the growth of *Staphylococcus vannamei*. The culture dish containing the AF fabric showed a significantly larger inhibition zone around the fabric, demonstrating a significantly stronger antibacterial effect. Therefore, it can be concluded that the G / AF fabric possesses antibacterial properties.

[0050] In summary, these are merely preferred embodiments of the present invention and are not intended to limit the scope of the invention. All equivalent variations and modifications made in accordance with the shape, structure, features and spirit described in the claims of the present invention should be included within the scope of the claims of the present invention.

Claims

1. A method for preparing a smart Janus textile with a thermally modulated graphene oxide and hydrogel coating, characterized in that: The steps include the following: S1: Preparation of 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate: Dimethylaminoethyl methacrylate and 1,3,2-dioxazolthiophene-2,2-dioxide were dissolved in acetonitrile and stirred continuously at 50-60 °C for 24-30 h; the mixture after reaction was cooled to -25 °C, the solid was filtered out and washed with acetonitrile, and then dried under vacuum to obtain 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine) ethyl sulfate; S2: Preparation of a heated and antibacterial fabric: Acryloyloxyethyltrimethylammonium chloride, ethyl acrylate, N,N-methylenebisacrylamide, dimethyl sulfoxide, and TPO-L are mixed evenly in a certain proportion. This solution is then mixed evenly with graphene oxide in a certain proportion. 0.4-0.5 g of this mixture is brushed onto the front side of the fabric at 2000-2500 W / m². 2 Photocuring is performed under light intensity, followed by drying at 40-50 ℃ to obtain a heated and antibacterial fabric. S3: Preparation of a cooling-mode and antibacterial fabric coating solution: A certain amount of sodium hydroxide is added to acrylic acid to form a solution with a neutralization degree of 80%. Then, 2-hydroxyethyl methacrylate, ultrapure water, N,N-methylenebisacrylamide and TPO-L are added separately and shaken to obtain a solution. The solution is then mixed with 2-(N-(2-(methacryloxy)ethyl)-N,N-dimethylamine)ethyl sulfate prepared in step S1 in a certain proportion to obtain a cooling-mode and antibacterial fabric coating solution. S4: Preparation of smart Janus textiles with thermally modulated graphene oxide and hydrogel coatings: Spray 0.1-0.3 g of the coating solution obtained in step S3 onto the reverse side of the fabric prepared in step S2, at 2000-2500 W / m 2 Photocuring is performed under light intensity, followed by drying at 40-50 ℃ to obtain a smart fabric with heat regulation and antibacterial functions.

2. The method for preparing a smart Janus textile with a thermally modulated graphene oxide and hydrogel coating according to claim 1, characterized in that: In step S1, the mass of dimethylaminoethyl methacrylate is 3.46 g, the mass of 1,3,2-dioxazolthiophene-2,2-dioxide is 2.48 g, and the volume of acetonitrile used for dissolution is 30 mL.

3. The method for preparing a smart Janus textile with a thermally modulated graphene oxide and hydrogel coating according to claim 1, characterized in that: In step S2, the mass percentages of the acryloyloxyethyltrimethylammonium chloride are 5-8 wt%, the mass percentages of ethyl acrylate are 33-35 wt%, the mass percentages of N,N-methylenebisacrylamide are 0.1-0.3 wt%, the mass percentages of dimethyl sulfoxide are 55-58 wt%, and the mass percentages of TPO-L are 0.5-1 wt%. The above substances are mixed in proportion and ultrasonically dissolved evenly. Then, they are mixed with graphene oxide in proportion and ultrasonically vibrated evenly to obtain a mixed solution. The mass percentage of graphene oxide is 5-11 wt%.

Citation Information

Patent Citations

  • External-hot and internal-cold type Janus antibacterial material with photoresponsiveness and preparation method of external-hot and internal-cold type Janus antibacterial material

    CN115110308A

  • Fabric with radiation cooling and photoelectric-thermal conversion functions and preparation method thereof

    CN115787294A