A warm-sensing antibacterial warm-keeping fabric and a preparation method thereof

Abstract

The application discloses a temperature-sensing antibacterial warm fabric and a preparation method thereof, and relates to the technical field of fabrics. The low-melting-point isopropyl laurate and ethyl anisate are selected, the low-temperature discoloration of the capsule can be realized, the aroma can be released, the fabric has the temperature-sensing and fragrance effects, the added value of the fabric is improved, and in the microcapsule, the nano-sized porous alumina particles are further added, the nucleating agent is used, the temperature response speed is improved, and the solid solvent phase change is promoted. The fabric is prepared by adopting the double-layer fabric which is mutually bonded and formed, and is attached to the fiber film which bears the temperature-changing material on one side, and the three-layer structure plays different roles, wherein the fiber film located on the outer layer is mainly used for the discoloration and antibacterial action, the middle-layer structure is mainly used for the heat insulation action, and the fabric located on the inner layer is mainly used for the moisture absorption, heat generation, warmth keeping and other actions.

Description

Technical Field

[0001] This invention relates to the field of fabric technology, specifically to a temperature-sensitive antibacterial and warm fabric and its preparation method. Background Technology

[0002] Organic reversible thermochromic materials are functional materials whose color changes when the temperature is above or below a specific temperature. They also have memory function and can be reused repeatedly. Based on the electron gain and loss mechanism, organic reversible thermochromic materials generally consist of a chromophore, a color developer, and a solvent. The chromophore determines the color of the thermochromic material system, the depth of color is mainly determined by the color developer, and the solvent plays a role in regulating the color-changing temperature of the thermochromic system.

[0003] Numerous studies have documented the preparation of organic reversible thermochromic microcapsules, but most are thermochromic or high-temperature thermochromic microcapsules, which closely match the temperature of summer clothing environments. Therefore, they are primarily used in summer fabrics. However, in winter, where temperatures are low, existing thermochromic microcapsules are insufficient to meet the stringent environmental requirements of winter clothing, and thus are rarely used in winter fabrics. Furthermore, existing low-temperature reversible thermochromic microcapsules are mostly found in road coatings. Therefore, this invention innovates on thermochromic microcapsules, enabling their application in winter fabrics, achieving low-temperature reversible color change, and simultaneously imparting a fragrance to the fabric. Summary of the Invention

[0004] The purpose of this invention is to provide a temperature-sensitive antibacterial and warm fabric and its preparation method, so as to solve the problems existing in the prior art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a temperature-sensitive antibacterial and warm fabric, comprising, from the inside out, a skin-friendly inner layer, a heat-insulating middle layer, and an antibacterial temperature-sensitive outer layer. The antibacterial temperature-sensitive outer layer is spun onto the surface of the heat-insulating middle layer by electrospinning. The spinning solution is composed of the following components in parts by weight: 10-30 parts polylactic acid, 5-20 parts temperature-sensitive microcapsules, 5-20 parts Kochia scoparia extract, 50-150 parts dichloromethane, and 2-10 parts nano-titanium dioxide. The temperature-sensitive microcapsules consist of a core material and a wall material encapsulating the core material. The core material includes a colorant, a color developer, a solvent, and porous alumina. The wall material includes monomers, nano-silica, and nano-light-absorbing and heat-generating materials.

[0006] Furthermore, the temperature-sensitive microcapsules are prepared using the following method:

[0007] (1) Disperse 0.1-1.5g of tungsten oxide nanopowder and 0.5-3g of silica nanopowder in 50-150mL of anhydrous ethanol, add 35-100mL of ethanol solution of coupling agent with a concentration of 0.05g / mL dropwise, react for 10-40h in a water bath at 30-40℃, and dry under vacuum at 45-60℃ for 8-12h to obtain the filler;

[0008] (2) 8-12g of monomer, 1-3g of filler and 0.10g of azobisisobutyronitrile are stirred at 80rpm for 30min in a water bath at 65℃. 8-12g of core material compound and 0.5-1g of chain extender are added to obtain a mixture. The mixture is added to 200g of 0.3% polyvinyl alcohol aqueous solution by weight percentage. The mixture is sheared and emulsified for 3min using a high shear emulsifier. Then the temperature is raised to 75℃ and the reaction continues for 3h. The temperature is then raised to 85℃ and the reaction continues for 1h. The product is washed, filtered and dried to obtain the product.

[0009] The core material compound consists of a colorant, a color developer, a solvent, and porous alumina added sequentially in a water bath at a mass ratio of 1:0.5-4.9:30-50:0.01-0.28, and stirred at 95°C and 300-400 rpm for 10-20 minutes.

[0010] This invention incorporates photothermal materials and silicon dioxide into the wall material, enabling it to absorb light and generate heat. The use of silicon dioxide promotes heat transfer on the film layer, alleviating the lag caused by low thermal conductivity leading to color change in thermochromic materials. Furthermore, its transparency and colorlessness prevent it from obscuring the color of the core material and affecting the color rendering ability of the thermochromic material.

[0011] Furthermore, the solvent is a mixture of isopropyl lauryl acid and ethyl anisinate in a mass ratio of 1–5:4–10.

[0012] Furthermore, the coupling agent is vinyltrimethoxysilane, vinyltriethoxysilane, allyltrimethoxysilane, or allyltriethoxysilane.

[0013] Furthermore, the color-developing agent is at least one selected from crystal violet lactone and 2-phenylamino-6-diethylaminofluorane.

[0014] Furthermore, the color developer is at least one selected from bisphenol A, bisphenol F, 3-diethylamino-7,8-phenylfluorane, and 1,5-dihydroxynaphthalene.

[0015] Furthermore, the porous alumina has a size of 20–60 nm and a pore size of 3–8 nm.

[0016] Furthermore, the voltage of the electrospinning is 10-20kV.

[0017] Furthermore, the monomer is at least one of methyl methacrylate, methacrylic acid, butyl acrylate, and ethyl acrylate.

[0018] Furthermore, the chain extender is at least one of stilbene, N,N-methylenebisacrylamide, divinyl sulfone, and ethylene glycol dimethyl propylene.

[0019] Furthermore, the inner layer has a warp density of 430 threads / 10cm and a weft density of 300 threads / 10cm. The warp yarn is a blended yarn made of moisture-absorbing and heat-generating fibers and cotton fibers, with a thickness of 20-35S / 1. The proportion of moisture-absorbing and heat-generating fibers in the blended yarn is 50-80%, and the proportion of cotton fibers is 50-20%. The moisture-absorbing and heat-generating fibers are cross-linked acrylic fibers. The weft yarn is hollow nylon fiber with a thickness of 20-35S / 1.

[0020] Furthermore, the heat-insulating intermediate layer is made of hollow nylon fibers knitted by a weft knitting circular knitting machine, with a weight of 190-200 g / m². 2 .

[0021] Furthermore, the skin-friendly inner layer and the heat-insulating middle layer are joined together using a double-layer bonding method, employing weft-jointing or top-to-bottom bonding techniques. Through the interlocking of the double-layered structures and the coverage of the fiber membrane, air is not easily dispersed, thus ensuring both superior comfort and excellent warmth retention.

[0022] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0023] (1) The present invention uses a combination of leucocyanide, color developer and solvent as core material to prepare temperature-sensitive microcapsules; the solvent is selected as low melting point isopropyl laurate and ethyl anisinate, which can realize the low temperature color change of the capsule, so that the fabric can also achieve the color change effect in winter. At the same time, ethyl anisinate has a light fragrance and isopropyl laurate has a fragrance-enhancing effect. By controlling the ratio of the two, the microcapsules have the best low melting point and can release fragrance, so that the fabric has both temperature-sensitive and fragrance effects, and enhances the added value of the fabric.

[0024] (2) In the microcapsules, the present invention also adds nano-sized porous alumina particles, which can act as nucleating agents during the process of solvent changing from liquid phase to solid phase. The solid phase uses its surface as the nucleus to promote the nucleation of the solid phase, reduce the supercooling of the solvent, and prevent the low temperature in winter from slowing down the phase change rate of the microcapsules and affecting the temperature-sensitive color change effect of the fabric. On this basis, alumina has a nano-sized porous structure with a high specific surface area, has a good dispersion effect in the solvent, and is transparent, which will not affect the color change. At the same time, alumina itself has a thermal conductivity effect and has a good dispersion effect in the solvent, forming a thermally conductive network that can quickly respond to the external temperature and promote the phase change of the solid solvent.

[0025] (3) The fabric of the present invention is made by bonding two layers of fabric together and attaching a fiber membrane carrying antibacterial temperature-changing material to one side. The three-layer structure plays different roles. The fiber membrane in the outer layer is mainly used for color change and antibacterial function, the middle layer is mainly used for heat insulation function, and the inner layer of fabric is mainly used for moisture absorption, heat generation and warmth retention function. Detailed Implementation

[0026] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0027] Example 1

[0028] A temperature-sensitive antibacterial and warm fabric, consisting of a skin-friendly inner layer, a heat-insulating middle layer, and an antibacterial temperature-sensitive outer layer from the inside out; the skin-friendly inner layer and the heat-insulating middle layer are connected by a double-layer bonding method, using a weft bonding method or an upper-to-lower bonding method.

[0029] The inner layer has a warp density of 430 threads / 10cm and a weft density of 300 threads / 10cm. The warp yarn is a blended yarn made of moisture-absorbing and heat-generating fibers and cotton fibers, with a thickness of 20S / 1. The blended yarn contains 50% moisture-absorbing and heat-generating fibers and 50% cotton fibers, among which the moisture-absorbing and heat-generating fibers are cross-linked acrylic fibers. The weft yarn is made of hollow nylon fibers with a thickness of 20S / 1.

[0030] The heat-insulating interlayer is made of hollow nylon fibers knitted on a circular knitting machine, with a weight of 190 g / m². 2 ;

[0031] The antibacterial temperature-sensitive surface layer is spun onto the surface of the heat-insulating intermediate layer by electrospinning. The spinning solution is made of the following components in parts by weight: 20 parts polylactic acid, 10 parts temperature-sensitive microcapsules, 5 parts Kochia scoparia extract, 55 parts dichloromethane, and 2 parts nano titanium dioxide. The voltage of electrospinning is 18kV.

[0032] The temperature-sensitive microcapsules are prepared using the following method:

[0033] (1) Disperse 0.1g of tungsten oxide nanopowder and 0.5g of silica nanopowder in 50mL of anhydrous ethanol, add 35mL of ethanol solution of vinyltrimethoxysilane with a concentration of 0.05g / mL dropwise, react for 20h in a water bath at 40℃, and dry under vacuum at 50℃ for 10h to obtain the filler.

[0034] (2) 8g of butyl acrylate, 1g of filler and 0.10g of azobisisobutyronitrile were stirred at 80rpm for 30min in a water bath at 65℃. 8g of core material compound and 0.5g of stilbene were added to obtain a mixture. The mixture was added to 200g of 0.3% polyvinyl alcohol aqueous solution and sheared and emulsified using a high shear emulsifier for 3min. Then the temperature was raised to 75℃ and the reaction was continued for 3h. The temperature was then raised to 85℃ and the reaction was continued for 1h. The product was washed, filtered and dried to obtain the product.

[0035] The core material compound consists of crystal violet lactone, bisphenol A, solvent, and porous alumina added sequentially in a water bath at a mass ratio of 1:3:30:0.1 and stirred at 95°C and 400 rpm for 15 min. The solvent is a mixture of isopropyl laurate and ethyl anisinate in a mass ratio of 1:4.

[0036] Example 2

[0037] A temperature-sensitive antibacterial and warm fabric, consisting of a skin-friendly inner layer, a heat-insulating middle layer, and an antibacterial temperature-sensitive outer layer from the inside out; the skin-friendly inner layer and the heat-insulating middle layer are connected by a double-layer bonding method, using a weft bonding method or an upper-to-lower bonding method.

[0038] The inner layer has a warp density of 430 threads / 10cm and a weft density of 300 threads / 10cm. The warp yarn is a blended yarn made of moisture-absorbing and heat-generating fibers and cotton fibers, with a thickness of 25S / 1. The moisture-absorbing and heat-generating fibers account for 75% of the blended yarn, and the cotton fibers account for 25%. The moisture-absorbing and heat-generating fibers are cross-linked acrylic fibers. The weft yarn is hollow nylon fiber with a thickness of 25S / 1.

[0039] The heat-insulating interlayer is made of hollow nylon fibers knitted on a circular knitting machine, with a weight of 190 g / m². 2 ;

[0040] The antibacterial temperature-sensitive surface layer is spun onto the surface of the heat-insulating intermediate layer by electrospinning. The spinning solution is made of the following components in parts by weight: 25 parts polylactic acid, 14 parts temperature-sensitive microcapsules, 12 parts Kochia scoparia extract, 90 parts dichloromethane, and 6 parts nano titanium dioxide. The voltage of electrospinning is 18kV.

[0041] The temperature-sensitive microcapsules are prepared using the following method:

[0042] (1) Disperse 0.8g of tungsten oxide nanopowder and 2.0g of silica nanopowder in 80mL of anhydrous ethanol, add 75mL of ethanol solution of allyltrimethoxysilane with a concentration of 0.05g / mL dropwise, react for 25h in a water bath at 40℃, and dry under vacuum at 50℃ for 10h to obtain the filler.

[0043] (2) 10g of ethyl acrylate, 2g of filler and 0.10g of azobisisobutyronitrile were stirred at 80rpm for 30min in a water bath at 65℃. 10g of core material compound and 0.5g of N,N-methylenebisacrylamide were added to obtain a mixture. The mixture was added to 200g of 0.3% polyvinyl alcohol aqueous solution and sheared and emulsified using a high shear emulsifier for 3min. Then the temperature was raised to 75℃ and the reaction was continued for 3h. The temperature was then raised to 85℃ and the reaction was continued for 1h. The product was washed, filtered and dried to obtain the product.

[0044] The core material compound consists of crystal violet lactone, bisphenol A, solvent, and porous alumina added sequentially in a water bath at a mass ratio of 1:3.8:40:0.14 and stirred at 95°C and 400 rpm for 15 min. The solvent is a mixture of isopropyl laurate and ethyl anisinate in a mass ratio of 3:7.

[0045] Example 3

[0046] A temperature-sensitive antibacterial and warm fabric, consisting of a skin-friendly inner layer, a heat-insulating middle layer, and an antibacterial temperature-sensitive outer layer from the inside out; the skin-friendly inner layer and the heat-insulating middle layer are connected by a double-layer bonding method, using a weft bonding method or an upper-to-lower bonding method.

[0047] The inner layer has a warp density of 430 threads / 10cm and a weft density of 300 threads / 10cm. The warp yarn is a blended yarn made of moisture-absorbing and heat-generating fibers and cotton fibers, with a thickness of 35S / 1. The moisture-absorbing and heat-generating fibers account for 80% and cotton fibers account for 20% of the blended yarn, of which the moisture-absorbing and heat-generating fibers are cross-linked acrylic fibers. The weft yarn is hollow nylon fiber with a thickness of 35S / 1.

[0048] The heat-insulating interlayer is made of hollow nylon fibers knitted on a circular knitting machine, with a weight of 190 g / m². 2 ;

[0049] The antibacterial temperature-sensitive surface layer is spun onto the surface of the heat-insulating intermediate layer by electrospinning. The spinning solution is made of the following components in parts by weight: 30 parts polylactic acid, 20 parts temperature-sensitive microcapsules, 20 parts Kochia scoparia extract, 150 parts dichloromethane, and 10 parts nano titanium dioxide. The voltage of electrospinning is 18kV.

[0050] The temperature-sensitive microcapsules are prepared using the following method:

[0051] (1) Disperse 1.5g of tungsten oxide nanopowder and 3g of silica nanopowder in 150mL of anhydrous ethanol, add 100mL of ethanol solution of allyltriethoxysilane with a concentration of 0.05g / mL dropwise, react for 35h in a water bath at 40℃, and dry under vacuum at 50℃ for 10h to obtain the filler.

[0052] (2) 8g of methyl methacrylate, 4g of butyl acrylate, 3g of filler, and 0.10g of azobisisobutyronitrile were stirred at 80rpm for 30min in a water bath at 65℃. 12g of core material compound and 0.5g of dimethyl propylene glycol were added to obtain a mixture. The mixture was added to 200g of a 0.3% polyvinyl alcohol aqueous solution and sheared and emulsified using a high-shear emulsifier for 3min. Then the temperature was raised to 75℃ and the reaction was continued for 3h. The temperature was then raised to 85℃ and the reaction was continued for 1h. The product was washed, filtered, and dried to obtain the product.

[0053] The core material compound consists of crystal violet lactone, bisphenol A, solvent, and porous alumina added sequentially in a water bath at a mass ratio of 1:4.9:45:0.28 and stirred at 95°C and 400 rpm for 15 min. The solvent is a mixture of isopropyl laurate and ethyl anisinate in a mass ratio of 5:10.

[0054] The temperature-sensitive antibacterial and thermal insulation fabric of this invention achieves reversible color change at 0℃ with a color change time of ≤40s; the antibacterial rate of Staphylococcus aureus is ≥95%, and the antibacterial rate of Escherichia coli is ≥95%; the thermal insulation performance is tested in accordance with the provisions of GB / T11048-1989 "Test Methods for Thermal Insulation Performance of Textiles". The thermal insulation rate of the temperature-sensitive antibacterial and thermal insulation fabrics prepared in Examples 1 to 3 is above 30%, which shows good thermal insulation performance.

[0055] Comparative Example 1

[0056] The difference between Comparative Example 1 and Example 1 is that methyl lauryl ester was used as a solvent in the preparation of temperature-sensitive microcapsules, while the other components and preparation methods were the same as in Example 1.

[0057] Comparative Example 2

[0058] The difference between Comparative Example 2 and Example 1 is that porous alumina is not added in the preparation of temperature-sensitive microcapsules, while the other components and preparation methods are the same as in Example 1.

[0059] Comparative Example 3

[0060] The difference between Comparative Example 3 and Example 1 is that conventional form of alumina was added in the preparation of temperature-sensitive microcapsules, while the other components and preparation methods are the same as in Example 1.

[0061] Comparative Example 4

[0062] The difference between Comparative Example 4 and Example 1 is that carbon-based materials are used instead of porous alumina in the preparation of temperature-sensitive microcapsules, while the other components and preparation methods are the same as in Example 1.

[0063] Comparative Example 5

[0064] The difference between Comparative Example 5 and Example 1 is that tungsten oxide nanopowder is not added in the preparation of temperature-sensitive microcapsules, while the other components and preparation methods are the same as in Example 1.

[0065] Comparative Example 6

[0066] The difference between Comparative Example 6 and Example 1 is that silica nanopowder is not added in the preparation of temperature-sensitive microcapsules, while the other components and preparation methods are the same as in Example 1.

[0067] The test results of temperature-sensitive fabrics in Comparative Examples 1 to 6 and Example 1 are listed in Table 1.

[0068] Table 1

[0069]

[0070] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.

Claims

1. A temperature-sensitive antibacterial and thermal insulation fabric, comprising, from the inside out, a skin-friendly inner layer, a heat-insulating middle layer, and an antibacterial temperature-sensitive outer layer; wherein the skin-friendly inner layer and the heat-insulating middle layer are connected together by a double-layer bonding method, using a weft-bonding or top-to-bottom bonding method. The inner layer has a warp density of 430 threads / 10cm and a weft density of 300 threads / 10cm. The warp yarn is a blended yarn made of moisture-absorbing and heat-generating fibers and cotton fibers, with a thickness of 25S / 1. The moisture-absorbing and heat-generating fibers account for 75% of the blended yarn, and the cotton fibers account for 25%. The moisture-absorbing and heat-generating fibers are cross-linked acrylic fibers. The weft yarn is hollow nylon fiber with a thickness of 25S / 1. The heat-insulating interlayer is made of hollow nylon fibers knitted on a circular knitting machine, with a weight of 190 g / m². 2 ; The antibacterial temperature-sensitive surface layer is spun onto the surface of the heat-insulating intermediate layer by electrospinning, wherein... The spinning solution is made of the following components in parts by weight: 25 parts polylactic acid, 14 parts temperature-sensitive microcapsules, 12 parts Kochia scoparia extract, 90 parts dichloromethane, and 6 parts nano titanium dioxide; the electrospinning voltage is 18kV. The preparation method of the temperature-sensitive microcapsules includes the following steps: (1) Disperse 0.8g of tungsten oxide nanopowder and 2.0g of silica nanopowder in 80mL of anhydrous ethanol, add 75mL of ethanol solution of allyltrimethoxysilane with a concentration of 0.05g / mL dropwise, react for 25h in a water bath at 40℃, and dry under vacuum at 50℃ for 10h to obtain the filler. (2) 10g of ethyl acrylate, 2g of filler and 0.10g of azobisisobutyronitrile were stirred at 80rpm for 30min in a water bath at 65℃. 10g of core material compound and 0.5g of N,N-methylenebisacrylamide were added to obtain a mixture. The mixture was added to 200g of 0.3% polyvinyl alcohol aqueous solution and sheared and emulsified using a high shear emulsifier for 3min. Then the temperature was raised to 75℃ and the reaction was continued for 3h. The temperature was then raised to 85℃ and the reaction was continued for 1h. The product was washed, filtered and dried to obtain the product. The core material compound consists of crystal violet lactone, bisphenol A, solvent, and porous alumina added sequentially in a water bath at a mass ratio of 1:3.8:40:0.14 and stirred at 95°C and 400 rpm for 15 min. The solvent is a mixture of isopropyl laurate and ethyl anisinate in a mass ratio of 3:7.

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