Thermal storage and temperature regulation textile material and preparation method thereof
By combining the heat-storing and temperature-regulating particles with polyamide 6 slices, textile materials that can actively adjust the temperature are prepared, which solves the problem that traditional textile materials cannot provide suitable somatosensory temperature when temperature changes, and achieves excellent heat-storing and temperature-regulating performance.
Patent Information
- Application Number
- CN202510114745.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-24
- Publication Date
- 2025-05-30
- Estimated Expiration
- 2045-01-24
AI Technical Summary
Traditional textile materials are difficult to provide a lasting and suitable somatosensory temperature when facing changes in external temperature, and cannot actively adjust their own temperature, resulting in discomfort in cold or hot environments.
Using a combination of polyamide 6 slices and heat-regulating particles, a textile material with heat-regulating properties is prepared by mixing the heat-regulating particles with polyamide 6 slices and then processing them through an extruder and a spinneret.
This textile material can absorb or release latent heat through the phase change process of heat storage and temperature regulating particles, actively adjust the temperature, provide a comfortable wearing experience, and adapt to ambient temperature changes.
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Figure BDA0005257569170000121
Abstract
Description
Technical Field
[0001] The present invention relates to the field of textile materials, and particularly relates to a heat storage and temperature regulating textile material and a preparation method thereof. Background Art
[0002] With the improvement of living standards, people's requirements for the functionality of textiles are increasing day by day. In daily wearing and using scenarios, people often face discomfort caused by changes in environmental temperature. When traditional textile materials face changes in external temperature, they mainly rely on their own heat insulation or heat dissipation performance to cope, and cannot actively adjust their own temperature, making it difficult to provide a lasting and suitable body feeling temperature. For example, in a cold environment, the heat preservation effect of ordinary clothes is limited, and the body heat is easily dissipated, making people feel cold; while in a hot environment, clothes are difficult to effectively dissipate heat, resulting in stuffy discomfort. Therefore, it is of great practical significance to develop a heat storage and temperature regulating textile material. Summary of the Invention
[0003] In order to overcome the above technical problems, the purpose of the present invention is to provide a heat storage and temperature regulating textile material and a preparation method thereof, which solves the problem that traditional textile materials are difficult to provide a lasting and suitable body feeling temperature when facing changes in external temperature.
[0004] The purpose of the present invention can be achieved by the following technical solutions:
[0005] A heat storage and temperature regulating textile material, comprising the following components in parts by weight:
[0006] 100 parts of polyamide 6 chips, 1.2 - 5.8 parts of heat storage and temperature regulating particles;
[0007] Among them, the heat storage and temperature regulating particles are prepared by the following steps:
[0008] Step s1: Add cetyltrimethylammonium bromide, triethanolamine, and deionized water to a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, introduce nitrogen protection, and stir and react at a temperature of 25 - 30 °C and a stirring rate of 300 - 400 r / min for 20 - 30 min. Then add zinc nitrate hexahydrate and continue to stir and react for 20 - 30 min. Then add tetraethyl orthosilicate and cyclohexane in sequence and continue to stir and react at a temperature of 60 - 65 °C for 6 - 8 h. Then raise the temperature to 95 - 100 °C and continue to stir and react for 3 - 5 h. After the reaction is completed, cool the reaction product to room temperature, then centrifuge, wash the precipitate with anhydrous ethanol and distilled water 3 - 5 times in sequence, then place it in a vacuum drying oven and dry it at a temperature of 80 - 85 °C for 2 - 3 h. Then place it in a muffle furnace and calcine it at a temperature of 450 - 460 °C for 3 - 4 h, and then cool it with the furnace to obtain a silicon-zinc composite;
[0009] Step s2: Add absolute ethanol and deionized water into a three-necked flask equipped with a stirrer, a thermometer and a gas pipe. Introduce nitrogen for protection. Stir and react for 20 - 30 min under the conditions of a temperature of 25 - 30 °C and a stirring rate of 300 - 400 r / min. Then adjust the pH to 9 - 9.5 with ammonia water. After that, add the zinc silicate complex and γ-methacryloxypropyltrimethoxysilane and continue to stir and react for 2 - 3 h. After the reaction is completed, centrifuge the reaction product, place the precipitate in a vacuum drying oven, and dry it for 1 - 1.5 h under the condition of a temperature of 80 - 85 °C to obtain the modified zinc silicate complex;
[0010] Step s3: Add carbon nanotubes, concentrated nitric acid and concentrated sulfuric acid into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1 - 2 h under the conditions of a temperature of 50 - 55 °C and a stirring rate of 300 - 400 r / min. Then add deionized water and hydrogen peroxide and continue to stir and react for 3 - 4 h. After the reaction is completed, cool the reaction product to room temperature, then carry out vacuum filtration. Wash the filter cake with distilled water 3 - 5 times, and then place it in a vacuum drying oven and dry it for 4 - 5 h under the condition of a temperature of 60 - 65 °C to obtain activated carbon nanotubes;
[0011] Step s4: Add lauric acid, palmitic acid and n-octadecane into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1 - 2 h under the conditions of a temperature of 70 - 75 °C and a stirring rate of 300 - 400 r / min. Then add the activated carbon nanotubes and continue to stir and react for 2 - 3 h. After the reaction is completed, cool the reaction product to room temperature, and then let it stand for 20 - 30 h to obtain adsorbed carbon nanotubes;
[0012] Step s5: Add the adsorbed carbon nanotubes, the modified zinc silicate complex, azobisisobutyronitrile, methyl methacrylate, butyl acrylate and ethyl acrylate into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1 - 2 h under the conditions of a temperature of 30 - 35 °C and a stirring rate of 300 - 400 r / min to obtain an oil phase. Add sodium dodecylbenzenesulfonate and deionized water into a three-necked flask equipped with a stirrer, a thermometer and a gas pipe. Introduce nitrogen for protection. Stir and react for 1 - 2 h under the conditions of a temperature of 80 - 85 °C and a stirring rate of 600 - 700 r / min to obtain an aqueous phase. Add the oil phase into the aqueous phase while stirring, and then continue to stir and react for 4 - 5 h. After the reaction is completed, cool the reaction product to room temperature, then centrifuge it. Wash the precipitate with absolute ethanol and distilled water 3 - 5 times in sequence, and then place it in a vacuum drying oven and dry it for 2 - 3 h under the condition of a temperature of 60 - 65 °C to obtain the heat storage and temperature regulation particles.
[0013] As a further solution of the present invention: the dosage ratio of cetyltrimethylammonium bromide, triethanolamine, deionized water, zinc nitrate hexahydrate, tetraethyl orthosilicate and cyclohexane in step s1 is 1.1 - 2.5 g: 0.15 - 0.19 g: 50 - 60 mL: 0.7 - 1.1 g: 3.3 - 5.3 g: 15 - 20 mL.
[0014] As a further solution of the present invention: the dosage ratio of absolute ethanol, deionized water, silicon-zinc composite and γ-methacryloxypropyltrimethoxysilane in step s2 is 25 - 30 mL: 25 - 30 mL: 5 g: 0.3 - 1.1 g.
[0015] As a further solution of the present invention: the mass fraction of ammonia water in step s2 is 20 - 25%.
[0016] As a further solution of the present invention: the dosage ratio of carbon nanotubes, concentrated nitric acid, concentrated sulfuric acid, deionized water and hydrogen peroxide in step s3 is 2 g: 10 - 12 mL: 30 - 35 mL: 25 - 30 mL: 5 - 7 mL.
[0017] As a further solution of the present invention: the carbon nanotubes in step s3 are multi-walled carbon nanotubes with an outer diameter of 30 - 60 nm, an inner diameter of 20 - 50 nm and a length of 1 - 10 μm; the mass fraction of the concentrated nitric acid is 65 - 68%; the mass fraction of the concentrated sulfuric acid is 96 - 98%; the mass fraction of the hydrogen peroxide is 30 - 35%.
[0018] As a further solution of the present invention: the dosage ratio of lauric acid, palmitic acid, n-octadecane and adsorbed carbon nanotubes in step s4 is 5 - 6 g: 1.5 - 2.5 g: 3.2 - 4.6 g: 10 g.
[0019] As a further solution of the present invention: the dosage ratio of adsorbed carbon nanotubes, modified silicon-zinc composite, azobisisobutyronitrile, methyl methacrylate, butyl acrylate, ethyl acrylate, sodium dodecylbenzenesulfonate and deionized water in step s5 is 3 g: 0.1 - 0.3 g: 0.05 - 0.09 g: 3.1 - 3.7 g: 0.5 - 0.7 g: 0.5 - 0.7 g: 0.8 - 1 g: 60 - 70 mL.
[0020] As a further solution of the present invention: a preparation method of a heat storage and temperature regulating textile material, comprising the following steps:
[0021] Step 1: Weigh 100 parts of polyamide 6 chips and 1.2 - 5.8 parts of heat storage and temperature regulating particles by weight, and set aside;
[0022] Step 2: Mix the polyamide 6 chips and the heat storage and temperature regulating particles evenly, then melt and extrude them through an extruder, and then extrude them through a spinneret with a pore diameter of 0.4 mm to obtain the heat storage and temperature regulating textile material.
[0023] As a further solution of the present invention: the grade of the polyamide 6 chips is M2400.
[0024] Advantages of the present invention:
[0025] A heat storage and temperature regulating textile material and a preparation method thereof according to the present invention, by mixing the polyamide 6 chips and the heat storage and temperature regulating particles evenly, then melting and extruding them through an extruder, and then extruding them through a spinneret to obtain the heat storage and temperature regulating textile material; this preparation method uses polyamide 6 chips as the main raw material to prepare fiber textile materials. Polyamide 6 has good mechanical strength, wear resistance and chemical stability. By adding heat storage and temperature regulating particles to it, the heat storage and temperature regulating particles can undergo solid-liquid or liquid-solid phase changes, and absorb or release a large amount of latent heat during the phase change process, so as to play a role in regulating temperature. Furthermore, it can endow the textile material with excellent heat storage and temperature regulating performance, enabling it to actively adapt to changes in environmental temperature, providing a comfortable wearing experience for the human body, meeting people's needs for functional textiles, injecting new vitality into the development of the textile industry, having important practical application value and broad market prospects, and meeting diverse market demands.
[0026] In the process of preparing the heat storage and temperature regulating textile material, a heat storage and temperature regulating particle was first prepared. Zinc oxide and silica composite system was prepared by using zinc nitrate hexahydrate as the zinc source and tetraethyl orthosilicate as the silica source to obtain a silicon-zinc composite. Then, the silicon-zinc composite was treated with γ-methacryloxypropyltrimethoxysilane. The siloxane on γ-methacryloxypropyltrimethoxysilane hydrolyzed to form silanol and grafted onto the surface of the silicon-zinc composite particles, and at the same time, an alkenyl group was introduced to obtain a modified silicon-zinc composite. Then, carbon nanotubes were activated with concentrated nitric acid, concentrated sulfuric acid and hydrogen peroxide. A large number of active functional groups were introduced onto its surface while effectively removing the surface impurities to achieve the effect of pore expansion, and activated carbon nanotubes were obtained. Then, lauric acid, palmitic acid and n-octadecane were used as phase change materials. After reasonable proportioning, they were filled into the internal micropores and cavities of the activated carbon nanotubes to obtain adsorbed carbon nanotubes. Then, methyl methacrylate, butyl acrylate and ethyl acrylate were used as polymerization monomers to polymerize outside the adsorbed carbon nanotubes to form a polymer to wrap them. At the same time, the modified silicon-zinc composite also participated in the polymerization reaction by using its alkenyl group to achieve connection in the form of chemical bonds, and heat storage and temperature regulating particles were obtained. The heat storage and temperature regulating particles use lauric acid, palmitic acid and n-octadecane to form a composite phase change material, which has the advantages of low phase change temperature, large phase change latent heat and good thermal stability. After filling it into the carbon nanotubes, it can effectively improve the heat conduction and heat transfer performance of the composite phase change material, and can limit the flow and transfer of the composite phase change material during melting. After being wrapped by the polymer, it can further avoid the leakage of the composite phase change material, making the composite phase change material have excellent thermal cycle stability, and also enabling it to be evenly dispersed in the fiber textile material to ensure the uniformity of the heat storage and temperature regulating effect. Zinc oxide and silica both have excellent far-infrared radiation performance, so that the grafted modified silicon-zinc composite can absorb the short-wave energy in sunlight or the heat emitted by the human body, and act on the human body in the form of far-infrared radiation, so as to achieve the effects of heat storage and warmth preservation, enhancing blood microcirculation and improving metabolism, making the heat storage and temperature regulating textile material have broad application prospects. Detailed implementation mode
[0027] The following will combine the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work belong to the scope of protection of the present invention.
[0028] Example 1:
[0029] This example is a preparation method of a heat storage and temperature regulating textile material, including the following steps:
[0030] Step S1: Add 1.1 g of cetyltrimethylammonium bromide, 0.15 g of triethanolamine, and 50 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas inlet tube. Introduce nitrogen for protection. Stir and react for 20 min under the conditions of a temperature of 25 °C and a stirring rate of 300 r / min. Then add 0.7 g of zinc nitrate hexahydrate and continue to stir and react for 20 min. Subsequently, add 3.3 g of tetraethyl orthosilicate and 15 mL of cyclohexane, and continue to stir and react for 6 h under the condition of heating to 60 °C. Then heat to 95 °C and continue to stir and react for 3 h. After the reaction is completed, cool the reaction product to room temperature, then centrifuge. Wash the precipitate with absolute ethanol and distilled water three times respectively. Then place it in a vacuum drying oven and dry for 2 h under the condition of a temperature of 80 °C. Then place it in a muffle furnace and calcine for 3 h under the condition of a temperature of 450 °C. Then cool with the furnace to obtain a silicon-zinc composite;
[0031] Step S2: Add 25 mL of absolute ethanol and 25 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas inlet tube. Introduce nitrogen for protection. Stir and react for 20 min under the conditions of a temperature of 25 °C and a stirring rate of 300 r / min. Then adjust the pH to 9 with 20% ammonia water. Then add 5 g of the silicon-zinc composite and 0.3 g of γ-methacryloxypropyltrimethoxysilane and continue to stir and react for 2 h. After the reaction is completed, centrifuge the reaction product. Place the precipitate in a vacuum drying oven and dry for 1 h under the condition of a temperature of 80 °C to obtain a modified silicon-zinc composite;
[0032] Step S3: Add 2 g of carbon nanotubes, 10 mL of 65% concentrated nitric acid, and 30 mL of 96% concentrated sulfuric acid into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1 h under the conditions of a temperature of 50 °C and a stirring rate of 300 r / min. Then add 25 mL of deionized water and 5 mL of 30% hydrogen peroxide and continue to stir and react for 3 h. After the reaction is completed, cool the reaction product to room temperature, then vacuum filter. Wash the filter cake with distilled water three times. Then place it in a vacuum drying oven and dry for 4 h under the condition of a temperature of 60 °C to obtain activated carbon nanotubes;
[0033] Step S4: Add 5 g of lauric acid, 1.5 g of palmitic acid, and 3.2 g of n-octadecane into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1 h under the conditions of a temperature of 70 °C and a stirring rate of 300 r / min. Then add 10 g of activated carbon nanotubes and continue to stir and react for 2 h. After the reaction is completed, cool the reaction product to room temperature, then let it stand for 20 h to obtain adsorbed carbon nanotubes;
[0034] Step S5: Add 3 g of adsorbed carbon nanotubes, 0.1 g of modified zinc silicate complex, 0.05 g of azobisisobutyronitrile, 3.1 g of methyl methacrylate, 0.5 g of butyl acrylate, and 0.5 g of ethyl acrylate into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1 h under the conditions of a temperature of 30°C and a stirring rate of 300 r / min to obtain an oil phase. Add 0.8 g of sodium dodecylbenzenesulfonate and 60 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas pipe. Introduce nitrogen for protection and stir and react for 1 h under the conditions of a temperature of 80°C and a stirring rate of 600 r / min to obtain an aqueous phase. Add the oil phase into the aqueous phase while stirring, and then continue to stir and react for 4 h. After the reaction is completed, cool the reaction product to room temperature, then centrifuge. Wash the precipitate with absolute ethanol and distilled water three times in sequence, and then place it in a vacuum drying oven and dry it at a temperature of 60°C for 2 h to obtain heat storage and temperature regulation particles;
[0035] Step S6: Weigh 100 parts of polyamide 6 chips of grade M2400 and 1.2 parts of heat storage and temperature regulation particles by weight and set aside;
[0036] Step S7: Mix the polyamide 6 chips and the heat storage and temperature regulation particles evenly and then melt and extrude them through an extruder, and then extrude them through a spinneret with a pore diameter of 0.4 mm to obtain a heat storage and temperature regulation textile material.
[0037] Example 2:
[0038] This example is a preparation method of a heat storage and temperature regulation textile material, including the following steps:
[0039] Step S1: Add 1.8 g of cetyltrimethylammonium bromide, 0.17 g of triethanolamine, and 55 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas pipe. Introduce nitrogen for protection and stir and react for 25 min under the conditions of a temperature of 28°C and a stirring rate of 350 r / min. Then add 0.9 g of zinc nitrate hexahydrate and continue to stir and react for 25 min. Then add 4.3 g of tetraethyl orthosilicate and 18 mL of cyclohexane in sequence and continue to stir and react for 7 h under the condition of heating to 62°C. Then heat to 98°C and continue to stir and react for 4 h. After the reaction is completed, cool the reaction product to room temperature, then centrifuge. Wash the precipitate with absolute ethanol and distilled water four times in sequence, and then place it in a vacuum drying oven and dry it at a temperature of 82°C for 2.5 h. Then place it in a muffle furnace and calcine it at a temperature of 455°C for 3.5 h, and then cool it with the furnace to obtain a zinc silicate complex;
[0040] Step S2: Add 28 mL of absolute ethanol and 28 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer and a gas pipe. Introduce nitrogen for protection. Stir and react for 25 min under the conditions of a temperature of 28 °C and a stirring rate of 350 r / min. Then adjust the pH to 9 with 22% ammonia water by mass. After that, add 5 g of silicon zinc composite and 0.7 g of γ-methacryloxypropyltrimethoxysilane and continue to stir and react for 2.5 h. After the reaction is completed, centrifuge the reaction product, place the precipitate in a vacuum drying oven, and dry it at a temperature of 82 °C for 1 h to obtain a modified silicon zinc composite;
[0041] Step S3: Add 2 g of carbon nanotubes, 11 mL of 66% concentrated nitric acid by mass and 32 mL of 97% concentrated sulfuric acid by mass into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1.5 h under the conditions of a temperature of 52 °C and a stirring rate of 350 r / min. Then add 28 mL of deionized water and 6 mL of 32% hydrogen peroxide by mass and continue to stir and react for 3.5 h. After the reaction is completed, cool the reaction product to room temperature, then carry out vacuum filtration, wash the filter cake 4 times with distilled water, and then place it in a vacuum drying oven and dry it at a temperature of 62 °C for 4.5 h to obtain activated carbon nanotubes;
[0042] Step S4: Add 5.5 g of lauric acid, 2 g of palmitic acid and 3.9 g of n-octadecane into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1.5 h under the conditions of a temperature of 72 °C and a stirring rate of 350 r / min. Then add 10 g of activated carbon nanotubes and continue to stir and react for 2.5 h. After the reaction is completed, cool the reaction product to room temperature, and then let it stand for 25 h to obtain adsorbed carbon nanotubes;
[0043] Step S5: Add 3 g of adsorbed carbon nanotubes, 0.2 g of modified silicon zinc composite, 0.07 g of azobisisobutyronitrile, 3.4 g of methyl methacrylate, 0.6 g of butyl acrylate and 0.6 g of ethyl acrylate into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 1.5 h under the conditions of a temperature of 32 °C and a stirring rate of 350 r / min to obtain an oil phase. Add 0.9 g of sodium dodecylbenzenesulfonate and 65 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer and a gas pipe. Introduce nitrogen for protection. Stir and react for 1.5 h under the conditions of a temperature of 82 °C and a stirring rate of 650 r / min to obtain an aqueous phase. Add the oil phase into the aqueous phase while stirring, and then continue to stir and react for 4.5 h. After the reaction is completed, cool the reaction product to room temperature, then centrifuge it, wash the precipitate 4 times with absolute ethanol and distilled water in sequence, and then place it in a vacuum drying oven and dry it at a temperature of 62 °C for 2.5 h to obtain heat storage and temperature regulation particles;
[0044] Step S6: Weigh 100 parts of polyamide 6 chips with the grade of M2400 and 3.5 parts of heat storage and temperature regulation particles by weight, and set aside;
[0045] Step S7: Mix the polyamide 6 chips and the heat storage and temperature regulation particles evenly, then melt and extrude them through an extruder, and then extrude them through a spinneret with a pore diameter of 0.4 mm to obtain the heat storage and temperature regulation textile material.
[0046] Example 3:
[0047] This example is a preparation method of a heat storage and temperature regulation textile material, including the following steps:
[0048] Step S1: Add 2.5 g of cetyltrimethylammonium bromide, 0.19 g of triethanolamine, and 60 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, introduce nitrogen for protection, stir and react for 30 min under the conditions of a temperature of 30 °C and a stirring rate of 400 r / min, then add 1.1 g of zinc nitrate hexahydrate and continue to stir and react for 30 min, then sequentially add 5.3 g of tetraethyl orthosilicate and 20 mL of cyclohexane, and continue to stir and react for 8 h under the condition of heating to 65 °C, then continue to stir and react for 5 h under the condition of heating to 100 °C. After the reaction is completed, cool the reaction product to room temperature, then centrifuge, wash the precipitate with anhydrous ethanol and distilled water 5 times in sequence, then place it in a vacuum drying oven, dry it for 3 h under the condition of a temperature of 85 °C, then place it in a muffle furnace, calcine it for 4 h under the condition of a temperature of 460 °C, and then cool it with the furnace to obtain the silicon-zinc composite;
[0049] Step S2: Add 30 mL of anhydrous ethanol and 30 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, introduce nitrogen for protection, stir and react for 30 min under the conditions of a temperature of 30 °C and a stirring rate of 400 r / min, then adjust the pH to 9.5 with 25% ammonia water by mass fraction, then add 5 g of the silicon-zinc composite and 1.1 g of γ-methacryloxypropyltrimethoxysilane, and continue to stir and react for 3 h. After the reaction is completed, centrifuge the reaction product, and place the precipitate in a vacuum drying oven, dry it for 1.5 h under the condition of a temperature of 85 °C to obtain the modified silicon-zinc composite;
[0050] Step S3: Add 2 g of carbon nanotubes, 12 mL of concentrated nitric acid with a mass fraction of 68%, and 35 mL of concentrated sulfuric acid with a mass fraction of 98% into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 2 h under the conditions of a temperature of 55 °C and a stirring rate of 400 r / min. Then add 30 mL of deionized water and 7 mL of hydrogen peroxide with a mass fraction of 35% and continue to stir and react for 4 h. After the reaction is completed, cool the reaction product to room temperature, then perform vacuum filtration. Wash the filter cake 5 times with distilled water, and then place it in a vacuum drying oven and dry it at a temperature of 65 °C for 5 h to obtain activated carbon nanotubes;
[0051] Step S4: Add 6 g of lauric acid, 2.5 g of palmitic acid, and 4.6 g of n-octadecane into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 2 h under the conditions of a temperature of 75 °C and a stirring rate of 400 r / min. Then add 10 g of activated carbon nanotubes and continue to stir and react for 3 h. After the reaction is completed, cool the reaction product to room temperature, and then let it stand for 30 h to obtain adsorbed carbon nanotubes;
[0052] Step S5: Add 3 g of adsorbed carbon nanotubes, 0.3 g of modified zinc silicate composite, 0.09 g of azobisisobutyronitrile, 3.7 g of methyl methacrylate, 0.7 g of butyl acrylate, and 0.7 g of ethyl acrylate into a three-necked flask equipped with a stirrer and a thermometer. Stir and react for 2 h at a temperature of 35 °C and a stirring rate of 400 r / min to obtain an oil phase. Add 1 g of sodium dodecylbenzenesulfonate and 70 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, introduce nitrogen for protection, and stir and react for 2 h at a temperature of 85 °C and a stirring rate of 700 r / min to obtain an aqueous phase. Add the oil phase to the aqueous phase while stirring, and then continue to stir and react for 5 h. After the reaction is completed, cool the reaction product to room temperature, and then centrifuge. Wash the precipitate 5 times with anhydrous ethanol and distilled water respectively, and then place it in a vacuum drying oven and dry it at a temperature of 65 °C for 3 h to obtain heat storage and temperature regulation particles;
[0053] Step S6: Weigh 100 parts of polyamide 6 chips of grade M2400 and 5.8 parts of heat storage and temperature regulation particles by weight for standby;
[0054] Step S7: Mix the polyamide 6 chips and the heat storage and temperature regulation particles evenly, then melt and extrude them through an extruder, and then extrude them through a spinneret with a pore diameter of 0.4 mm to obtain a heat storage and temperature regulation textile material.
[0055] Comparative Example 1:
[0056] This comparative example is a preparation method of a heat storage and temperature regulation textile material, including the following steps:
[0057] The polyamide 6 chips are melt-extruded through an extruder and then extruded through a spinneret with a pore size of 0.4 mm to obtain the heat storage and temperature regulation textile material.
[0058] Comparative Example 2:
[0059] This comparative example is a preparation method of a heat storage and temperature regulation textile material, including the following steps:
[0060] Step S1: Add 2 g of carbon nanotubes, 12 mL of concentrated nitric acid with a mass fraction of 68%, and 35 mL of concentrated sulfuric acid with a mass fraction of 98% into a three-necked flask equipped with a stirrer and a thermometer. Stir and react at a temperature of 55 °C and a stirring rate of 400 r / min for 2 h. Then add 30 mL of deionized water and 7 mL of hydrogen peroxide with a mass fraction of 35% and continue to stir and react for 4 h. After the reaction is completed, cool the reaction product to room temperature, then perform vacuum filtration. Wash the filter cake 5 times with distilled water, and then place it in a vacuum drying oven and dry it at a temperature of 65 °C for 5 h to obtain activated carbon nanotubes;
[0061] Step S2: Add 6 g of lauric acid, 2.5 g of palmitic acid, and 4.6 g of n-octadecane into a three-necked flask equipped with a stirrer and a thermometer. Stir and react at a temperature of 75 °C and a stirring rate of 400 r / min for 2 h. Then add 10 g of activated carbon nanotubes and continue to stir and react for 3 h. After the reaction is completed, cool the reaction product to room temperature, and then let it stand for 30 h to obtain adsorbed carbon nanotubes;
[0062] Step S3: Weigh 100 parts of polyamide 6 chips of grade M2400 and 5.8 parts of adsorbed carbon nanotubes by weight and set aside;
[0063] Step S4: Mix the polyamide 6 chips and the adsorbed carbon nanotubes evenly and then melt-extrude them through an extruder, and then extrude them through a spinneret with a pore size of 0.4 mm to obtain the heat storage and temperature regulation textile material.
[0064] Comparative Example 3:
[0065] This comparative example is a preparation method of a heat storage and temperature regulation textile material, including the following steps:
[0066] Step S1: Add 2.5 g of cetyltrimethylammonium bromide, 0.19 g of triethanolamine, and 60 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas pipe. Introduce nitrogen for protection. Stir and react for 30 min under the conditions of a temperature of 30 °C and a stirring rate of 400 r / min. Then add 1.1 g of zinc nitrate hexahydrate and continue to stir and react for 30 min. Then successively add 5.3 g of tetraethyl orthosilicate and 20 mL of cyclohexane, and continue to stir and react for 8 h under the condition of heating to 65 °C. Then continue to stir and react for 5 h under the condition of heating to 100 °C. After the reaction is completed, cool the reaction product to room temperature, then centrifuge, wash the precipitate with absolute ethanol and distilled water 5 times respectively, then place it in a vacuum drying oven and dry for 3 h under the condition of a temperature of 85 °C. Then place it in a muffle furnace and calcine for 4 h under the condition of a temperature of 460 °C, and then cool with the furnace to obtain a silicon-zinc composite;
[0067] Step S2: Add 30 mL of absolute ethanol and 30 mL of deionized water into a three-necked flask equipped with a stirrer, a thermometer, and a gas pipe. Introduce nitrogen for protection. Stir and react for 30 min under the conditions of a temperature of 30 °C and a stirring rate of 400 r / min. Then adjust the pH to 9.5 with 25% ammonia water by mass fraction. Then add 5 g of the silicon-zinc composite and 1.1 g of γ-methacryloxypropyltrimethoxysilane and continue to stir and react for 3 h. After the reaction is completed, centrifuge the reaction product, and place the precipitate in a vacuum drying oven and dry for 1.5 h under the condition of a temperature of 85 °C to obtain a modified silicon-zinc composite;
[0068] Step S3: Weigh 100 parts of polyamide 6 chips of grade M2400 and 5.8 parts of the modified silicon-zinc composite by weight, and set aside;
[0069] Step S4: Mix the polyamide 6 chips and the modified silicon-zinc composite evenly, then melt and extrude them through an extruder, and then extrude them through a spinneret with a pore diameter of 0.4 mm to obtain a heat storage and temperature regulation textile material.
[0070] Perform performance tests on the heat storage and temperature regulation textile materials of Examples 1-3 and Comparative Examples 1-3. The test results are as follows:
[0071]
[0072] Referring to the data in the above table, according to the comparison between Examples 1-3 and Comparative Examples 1-3, it can be known that the heat storage and temperature regulation textile material of the present application has excellent heat storage and temperature regulation performance.
[0073] In the description of this specification, the descriptions referring to the terms "one embodiment", "example", "specific example", etc. mean that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in a suitable manner in any one or more embodiments or examples.
[0074] The above content is only an example and illustration of the present invention. Those skilled in the art to which this technology belongs can make various modifications or supplements to the described specific embodiments or use similar ways to replace them. As long as they do not deviate from the invention or exceed the scope defined by this application, they should all fall within the protection scope of the present invention.
Claims
1. A heat storage and temperature regulating textile material, characterized in that: It includes the following components by weight: 100 parts of polyamide 6 slices, 1.2-5.8 parts of heat storage and temperature regulating particles; The heat storage and temperature regulating particles are prepared by the following steps: Step s1: adding hexadecyltrimethylammonium bromide, triethanolamine and deionized water to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, introducing nitrogen protection, stirring and reacting for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400r / min, then adding zinc nitrate hexahydrate and continuing to stir and react for 20-30 minutes, then adding tetraethyl orthosilicate and cyclohexane in sequence and continuing to stir and react for 6-8 hours at a temperature of 60-65°C, then continuing to stir and react for 3-5 hours at a temperature of 95-100°C, after the reaction is completed, cooling the reaction product to room temperature, then centrifuging, washing the precipitate with anhydrous ethanol and distilled water in sequence for 3-5 times, then placing it in a vacuum drying oven, drying it at a temperature of 80-85°C for 2-3 hours, then placing it in a muffle furnace, calcining it at a temperature of 450-460°C for 3-4 hours, then cooling it with the furnace to obtain a silicon-zinc composite; Step s2: adding anhydrous ethanol and deionized water to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, introducing nitrogen protection, stirring the reaction for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400r / min, then adjusting the pH to 9-9.5 with ammonia water, and then adding silicon zinc complex and γ-methacryloxypropyltrimethoxysilane to continue stirring the reaction for 2-3 hours. After the reaction is completed, the reaction product is centrifuged, and the precipitate is placed in a vacuum drying oven and dried at a temperature of 80-85°C for 1-1.5 hours to obtain a modified silicon zinc complex; Step s3: Add carbon nanotubes, concentrated nitric acid and concentrated sulfuric acid into a three-necked flask equipped with a stirrer and a thermometer, stir and react for 1-2 hours at a temperature of 50-55°C and a stirring rate of 300-400r / min, then add deionized water and hydrogen peroxide and continue stirring and reacting for 3-4 hours. After the reaction is completed, cool the reaction product to room temperature, then vacuum filter, wash the filter cake with distilled water for 3-5 times, and then place it in a vacuum drying oven and dry it at a temperature of 60-65°C for 4-5 hours to obtain activated carbon nanotubes; Step s4: adding lauric acid, palmitic acid and n-octadecane into a three-necked flask equipped with a stirrer and a thermometer, stirring the reaction for 1-2 hours at a temperature of 70-75°C and a stirring rate of 300-400 r / min, then adding activated carbon nanotubes and continuing to stir the reaction for 2-3 hours, and after the reaction is completed, cooling the reaction product to room temperature, and then standing it for 20-30 hours to obtain adsorbed carbon nanotubes; Step s5: Add the adsorbed carbon nanotubes, modified silicon zinc complex, azobisisobutyronitrile, methyl methacrylate, butyl acrylate and ethyl acrylate into a three-necked flask equipped with a stirrer and a thermometer, stir and react for 1-2 hours at a temperature of 30-35°C and a stirring rate of 300-400r / min to obtain an oil phase, add sodium dodecylbenzenesulfonate and deionized water into a three-necked flask equipped with a stirrer, a thermometer and an air duct, introduce nitrogen protection, stir and react for 1-2 hours at a temperature of 80-85°C and a stirring rate of 600-700r / min to obtain an aqueous phase, add the oil phase to the aqueous phase while stirring, and then continue to stir and react for 4-5 hours. After the reaction is completed, the reaction product is cooled to room temperature and then centrifuged. The precipitate is washed with anhydrous ethanol and distilled water for 3-5 times in turn, and then placed in a vacuum drying oven and dried at a temperature of 60-65°C for 2-3 hours to obtain heat storage and temperature regulating particles.
2. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The usage ratio of the hexadecyltrimethylammonium bromide, triethanolamine, deionized water, zinc nitrate hexahydrate, tetraethyl orthosilicate and cyclohexane in step s1 is 1.1-2.5 g: 0.15-0.19 g: 50-60 mL: 0.7-1.1 g: 3.3-5.3 g: 15-20 mL.
3. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The usage ratio of the anhydrous ethanol, deionized water, silicon-zinc complex and γ-methacryloxypropyltrimethoxysilane in step s2 is 25-30 mL: 25-30 mL: 5 g: 0.3-1.1 g.
4. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The mass fraction of the ammonia water in step s2 is 20-25%.
5. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The usage ratio of the carbon nanotubes, concentrated nitric acid, concentrated sulfuric acid, deionized water and hydrogen peroxide in step s3 is 2g:10-12mL:30-35mL:25-30mL:5-7mL.
6. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The carbon nanotubes in step s3 are multi-walled carbon nanotubes with an outer diameter of 30-60 nm, an inner diameter of 20-50 nm, and a length of 1-10 μm; the mass fraction of the concentrated nitric acid is 65-68%; the mass fraction of the concentrated sulfuric acid is 96-98%; and the mass fraction of the hydrogen peroxide is 30-35%.
7. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The usage ratio of the lauric acid, palmitic acid, n-octadecane and adsorbed carbon nanotubes in step s4 is 5-6g:1.5-2.5g:3.2-4.6g:10g.
8. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The dosage ratio of the adsorbed carbon nanotubes, modified silicon-zinc composite, azobisisobutyronitrile, methyl methacrylate, butyl acrylate, ethyl acrylate, sodium dodecylbenzenesulfonate and deionized water in step s5 is 3g: 0.1-0.3g: 0.05-0.09g: 3.1-3.7g: 0.5-0.7g: 0.5-0.7g: 0.8-1g: 60-70mL.
9. A method for preparing a heat storage and temperature regulating textile material, characterized in that: The following steps are involved: Step 1: Weigh 100 parts of polyamide 6 slices and 1.2-5.8 parts of heat storage and temperature regulating particles according to weight, and set aside; Step 2: The polyamide 6 slices and the heat storage and temperature regulating particles are evenly mixed and melted through an extruder, and then extruded through a spinneret with a hole diameter of 0.4 mm to obtain a heat storage and temperature regulating textile material.
10. The method for preparing a heat storage and temperature regulating textile material according to claim 9, characterized in that: The grade of the polyamide 6 slice is M2400.
Citation Information
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