Heat storage and temperature regulating textile material and preparation method thereof
By preparing heat-storage and temperature-regulating particles containing silicon-zinc composites and activated carbon nanotubes and mixing them with polyamide 6 chips, the problem that traditional textile materials cannot actively regulate temperature is solved, active temperature regulation and thermal stability of textile materials are achieved, and a comfortable wearing experience is provided.
Patent Information
- Application Number
- CN202510114745.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-24
- Publication Date
- 2025-09-12
- Estimated Expiration
- 2045-01-24
AI Technical Summary
Traditional textile materials cannot actively regulate temperature, resulting in limited warmth retention in cold environments or poor heat dissipation in hot environments, and are unable to provide a lasting and suitable body temperature.
By mixing polyamide 6 chips with heat storage and temperature regulation particles, silicon zinc composites, activated carbon nanotubes and phase change materials are used to form heat storage and temperature regulation particles during the preparation process, and the temperature is adjusted by absorbing or releasing latent heat through the phase change process.
It realizes active temperature regulation of textile materials, provides a comfortable wearing experience, adapts to changes in ambient temperature, and has good heat storage and temperature regulation performance and thermal stability.
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Figure SMS_1
Abstract
Description
Technical Field
[0001] The invention relates to the field of textile materials, and in particular to a heat-storage temperature-regulating textile material and a preparation method thereof. Background Art
[0002] With the improvement of living standards, people's functional requirements for textiles are increasing. In daily wear and use scenarios, people often face discomfort caused by changes in ambient temperature. Traditional textile materials mainly rely on their own thermal insulation or heat dissipation properties to cope with external temperature changes. They are unable to actively adjust their own temperature and it is difficult to provide a lasting and appropriate body temperature. For example, in a cold environment, ordinary clothing has limited warmth retention effect, and human body heat is easily lost, making people feel cold; in a hot environment, clothing is difficult to dissipate heat effectively, resulting in stuffy discomfort. Therefore, the development of a heat storage and temperature regulating textile material is of great practical significance. 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 appropriate body temperature when facing external temperature changes.
[0004] The purpose of the present invention can be achieved through 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] The heat storage and temperature regulating particles are prepared by the following steps:
[0008] 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 at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 minutes, 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 at a temperature of 60-65° C. for 6-8 hours, then continuing to stir and react at a temperature of 95-100° C. for 3-5 hours, after which the reaction product is cooled to room temperature and then centrifuged, and the precipitate is washed with anhydrous ethanol and distilled water for 3-5 times in sequence, then placed in a vacuum drying oven, dried at a temperature of 80-85° C. for 2-3 hours, then placed in a muffle furnace, calcined at a temperature of 450-460° C. for 3-4 hours, and then cooled with the furnace to obtain a silicon-zinc complex;
[0009] 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 and reacting at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes, then adjusting the pH to 9-9.5 with ammonia water, and then adding the silicon zinc complex and γ-methacryloxypropyltrimethoxysilane and continuing to stir and react 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;
[0010] Step s3: Add carbon nanotubes, concentrated nitric acid, and concentrated sulfuric acid to a three-necked flask equipped with a stirrer and a thermometer, and stir the mixture at a temperature of 50-55°C and a stirring rate of 300-400 r / min for 1-2 hours. Then, add deionized water and hydrogen peroxide and continue stirring for 3-4 hours. After the reaction is completed, cool the reaction product to room temperature and vacuum filter it. 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.
[0011] Step s4: adding lauric acid, palmitic acid and n-octadecane to a three-necked flask equipped with a stirrer and a thermometer, stirring the mixture at a temperature of 70-75°C and a stirring rate of 300-400 r / min for 1-2 hours, then adding activated carbon nanotubes and continuing to stir the mixture for 2-3 hours. After the reaction is completed, the reaction product is cooled to room temperature and then allowed to stand for 20-30 hours to obtain adsorbed carbon nanotubes;
[0012] 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, and stir the mixture 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 guide tube, introduce nitrogen protection, and stir the mixture 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 continue stirring the reaction for 4-5 hours. After the reaction is completed, cool the reaction product to room temperature, then centrifuge it, wash the precipitate with anhydrous ethanol and distilled water for 3-5 times in sequence, and then place it in a vacuum drying oven and dry it at a temperature of 60-65°C for 2-3 hours to obtain heat storage and temperature regulating particles.
[0013] As a further embodiment of the present invention, the usage ratio of the hexadecyltrimethylammonium bromide, triethanolamine, deionized water, zinc nitrate hexahydrate, ethyl 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 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.
[0015] As a further solution of the present invention: the mass fraction of the ammonia water in step s2 is 20-25%.
[0016] As a further solution of the present invention: in step s3, the carbon nanotubes, concentrated nitric acid, concentrated sulfuric acid, deionized water and hydrogen peroxide are used in a ratio of 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%; and the mass fraction of the hydrogen peroxide is 30-35%.
[0018] As a further solution of the present invention: the usage ratio of the lauric acid, palmitic acid, n-octadecane and activated 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 scheme of the present invention: the usage ratio of the adsorbed carbon nanotubes, modified silicon zinc complex, 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.
[0020] As a further solution of the present invention: a method for preparing a heat storage and temperature regulating textile material comprises the following steps:
[0021] 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;
[0022] 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 pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0023] As a further solution of the present invention: the brand of the polyamide 6 slice is M2400.
[0024] Beneficial effects of the present invention:
[0025] The present invention provides a heat-storage and temperature-regulating textile material and a preparation method thereof. The heat-storage and temperature-regulating textile material is obtained by uniformly mixing polyamide 6 chips and heat-storage and temperature-regulating particles, melting and extruding the mixture through an extruder, and then extruding the mixture through a wire board. The preparation method uses polyamide 6 chips as the main raw material to prepare the fiber textile material. Polyamide 6 has good mechanical strength, wear resistance and chemical stability. By adding heat-storage and temperature-regulating particles thereto, the heat-storage and temperature-regulating particles can undergo solid-liquid or liquid-solid phase change, absorb or release a large amount of latent heat during the phase change process, thereby playing a role in regulating temperature, and further endowing the textile material with excellent heat-storage and temperature-regulating performance, so that the textile material can actively adapt to changes in ambient temperature, provide a comfortable wearing experience for the human body, meet people's demand for functional textiles, inject new vitality into the development of the textile industry, have important practical application value and broad market prospects, and meet diverse market demands.
[0026] In the process of preparing heat-storage and temperature-regulating textile materials, a heat-storage and temperature-regulating particle is first prepared, and a zinc oxide and silicon dioxide composite system is prepared using zinc nitrate hexahydrate as a zinc source and ethyl orthosilicate as a silicon source to obtain a silicon-zinc composite. Then, the silicon-zinc composite is treated with γ-methacryloxypropyltrimethoxysilane, and the siloxane on the γ-methacryloxypropyltrimethoxysilane is hydrolyzed to form silanol and grafted to the particle surface of the silicon-zinc composite. At the same time, alkenyl groups are introduced to obtain a modified silicon-zinc composite. Then, concentrated nitric acid, concentrated sulfuric acid and hydrogen peroxide are used to activate carbon nanotubes, and a large number of active functional groups are introduced on their surface while effectively removing surface impurities to achieve a pore expansion effect, thereby obtaining activated carbon nanotubes. Then, lauric acid, palmitic acid and n-octadecane are used as phase change materials, and after reasonable proportions, they are 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 are used as polymerization monomers to polymerize the outside of the adsorbed carbon nanotubes to form a polymer to wrap it. At the same time, the modified silicon-zinc composite utilizes its alkenyl group to participate in the polymerization reaction to achieve chemical bond connection to obtain heat storage and temperature regulation particles; the heat storage and temperature regulation particles utilize 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 carbon nanotubes, it can effectively improve the thermal conductivity and heat transfer performance of the composite phase change material, and can limit the flow transfer of the composite phase change material when it melts. After being wrapped by the polymer, it can further avoid the leakage of the composite phase change material, so that the composite phase change material has excellent thermal cycle stability and can be evenly dispersed in the fiber textile material to ensure the uniformity of the heat storage and temperature regulation effect. Zinc oxide and silicon dioxide both have excellent far-infrared radiation properties, so that the grafted modified silicon-zinc composite can absorb short-wave energy in sunlight or heat emitted by the human body, and act on the human body in the form of far-infrared radiation, thereby achieving the effects of heat storage and warmth preservation, enhancing blood microcirculation and improving metabolism, making the heat storage and temperature regulation textile material have broad application prospects. DETAILED DESCRIPTION
[0027] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0028] Example 1:
[0029] This embodiment is a method for preparing a heat storage and temperature regulating textile material, comprising the following steps:
[0030] Step S1: 1.1 g of hexadecyltrimethylammonium bromide, 0.15 g of triethanolamine and 50 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen protection was introduced. The mixture was stirred at a temperature of 25 ° C and a stirring rate of 300 r / min for 20 minutes, and then 0.7 g of zinc nitrate hexahydrate was added and the stirring reaction was continued for 20 minutes. Then, 3.3 g of ethyl orthosilicate and 15 mL of cyclohexane were added in sequence and the temperature was raised to 60 ° C and the stirring reaction was continued for 6 hours. Then, the temperature was raised to 95 ° C and the stirring reaction was continued for 3 hours. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with anhydrous ethanol and distilled water three times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 80 ° C for 2 hours. Then, it was placed in a muffle furnace and calcined at a temperature of 450 ° C for 3 hours, and then cooled with the furnace to obtain a silicon zinc complex;
[0031] Step S2: 25 mL of anhydrous ethanol and 25 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 25° C. and a stirring rate of 300 r / min for 20 minutes. Then, the pH was adjusted to 9 with 20% ammonia water. Then, 5 g of silicon-zinc complex and 0.3 g of γ-methacryloyloxypropyltrimethoxysilane were added and the stirring reaction was continued for 2 hours. After the reaction was completed, the reaction product was centrifuged, and the precipitate was placed in a vacuum drying oven and dried at a temperature of 80° C. for 1 hour to obtain a modified silicon-zinc complex;
[0032] Step S3: 2 g of carbon nanotubes, 10 mL of 65% by mass concentrated nitric acid, and 30 mL of 96% by mass concentrated sulfuric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 50° C. and a stirring rate of 300 r / min for 1 h. Then, 25 mL of deionized water and 5 mL of 30% by mass hydrogen peroxide were added and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with distilled water 3 times, and then placed in a vacuum drying oven and dried at 60° C. for 4 h to obtain activated carbon nanotubes;
[0033] Step S4: 5 g of lauric acid, 1.5 g of palmitic acid, and 3.2 g of n-octadecane were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 70° C. and a stirring rate of 300 r / min for 1 h. Then, 10 g of activated carbon nanotubes were added and the stirring reaction was continued for 2 h. After the reaction was completed, the reaction product was cooled to room temperature and then allowed to stand for 20 h to obtain adsorbed carbon nanotubes;
[0034] Step S5: 3 g of adsorbed carbon nanotubes, 0.1 g of modified silicon zinc composite, 0.05 g of azobisisobutyronitrile, 3.1 g of methyl methacrylate, 0.5 g of butyl acrylate and 0.5 g of ethyl acrylate were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 30° C. and a stirring rate of 300 r / min for 1 h to obtain an oil phase. 0.8 g of sodium dodecylbenzenesulfonate and 60 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced. The mixture was stirred for reaction at a temperature of 80° C. and a stirring rate of 600 r / min for 1 h to obtain an aqueous phase. The oil phase was added to the aqueous phase while stirring, and the stirring reaction was continued for 4 h. After the reaction, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed three times with anhydrous ethanol and distilled water in sequence, and then placed in a vacuum drying oven and dried at a temperature of 60° C. for 2 h to obtain heat storage and temperature regulating particles.
[0035] Step S6: Weigh 100 parts of polyamide 6 slices with a brand of M2400 and 1.2 parts of heat storage and temperature regulating particles according to weight, and set aside;
[0036] Step S7: The polyamide 6 slices and the heat storage and temperature regulating particles are evenly mixed and melt-extruded through an extruder, and then extruded through a spinneret with a pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0037] Example 2:
[0038] This embodiment is a method for preparing a heat storage and temperature regulating textile material, comprising the following steps:
[0039] Step S1: 1.8 g of hexadecyltrimethylammonium bromide, 0.17 g of triethanolamine and 55 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen protection was introduced. The mixture was stirred at a temperature of 28 ° C and a stirring rate of 350 r / min for 25 minutes, and then 0.9 g of zinc nitrate hexahydrate was added and the stirring reaction was continued for 25 minutes. Then, 4.3 g of ethyl orthosilicate and 18 mL of cyclohexane were added in sequence and the temperature was raised to 62 ° C and the stirring reaction was continued for 7 hours. Then, the temperature was raised to 98 ° C and the stirring reaction was continued for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with anhydrous ethanol and distilled water 4 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 82 ° C for 2.5 hours. Then, it was placed in a muffle furnace and calcined at a temperature of 455 ° C for 3.5 hours, and then cooled with the furnace to obtain a silicon zinc complex;
[0040] Step S2: 28 mL of anhydrous ethanol and 28 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, and nitrogen protection was introduced. The mixture was stirred at a temperature of 28° C. and a stirring rate of 350 r / min for 25 minutes. The pH was then adjusted to 9 with 22% ammonia water. 5 g of silicon-zinc complex and 0.7 g of γ-methacryloyloxypropyltrimethoxysilane were then added and the mixture was stirred for 2.5 hours. After the reaction was completed, the reaction product was centrifuged, and the precipitate was placed in a vacuum drying oven and dried at 82° C. for 1 hour to obtain a modified silicon-zinc complex.
[0041] Step S3: 2 g of carbon nanotubes, 11 mL of 66% concentrated nitric acid, and 32 mL of 97% concentrated sulfuric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 52° C. and a stirring rate of 350 r / min for 1.5 h. Subsequently, 28 mL of deionized water and 6 mL of 32% hydrogen peroxide were added and the stirring reaction was continued for 3.5 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with distilled water four times and then placed in a vacuum drying oven and dried at 62° C. for 4.5 h to obtain activated carbon nanotubes;
[0042] Step S4: 5.5 g of lauric acid, 2 g of palmitic acid, and 3.9 g of n-octadecane were added to a three-necked flask equipped with a stirrer and a thermometer, and the mixture was stirred at 72° C. and a stirring rate of 350 r / min for 1.5 h. Subsequently, 10 g of activated carbon nanotubes were added and the stirring reaction was continued for 2.5 h. After the reaction was completed, the reaction product was cooled to room temperature and then allowed to stand for 25 h to obtain adsorbed carbon nanotubes;
[0043] Step S5: 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 were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for 1.5 h at a temperature of 32 ° C and a stirring rate of 350 r / min to obtain an oil phase, 0.9 g of sodium dodecylbenzenesulfonate and 65 mL of deionized water were added to a three-necked flask equipped with a stirrer and a thermometer. and a three-necked flask with an air guide tube, nitrogen was introduced for protection, and the reaction was stirred for 1.5 hours at a temperature of 82°C and a stirring rate of 650r / min to obtain an aqueous phase. The oil phase was added to the aqueous phase while stirring, and the stirring reaction was continued for 4.5 hours. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with anhydrous ethanol and distilled water four times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 62°C for 2.5 hours to obtain thermal storage and temperature regulating particles;
[0044] Step S6: Weigh 100 parts of polyamide 6 slices with a brand of M2400 and 3.5 parts of heat storage and temperature regulating particles according to weight, and set aside;
[0045] Step S7: The polyamide 6 slices and the heat storage and temperature regulating particles are evenly mixed and melt-extruded through an extruder, and then extruded through a spinneret with a pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0046] Example 3:
[0047] This embodiment is a method for preparing a heat storage and temperature regulating textile material, comprising the following steps:
[0048] Step S1: 2.5 g of hexadecyltrimethylammonium bromide, 0.19 g of triethanolamine and 60 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen protection was introduced. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 minutes, and then 1.1 g of zinc nitrate hexahydrate was added and the stirring reaction was continued for 30 minutes. Then, 5.3 g of ethyl orthosilicate and 20 mL of cyclohexane were added in sequence and the temperature was raised to 65 ° C and the stirring reaction was continued for 8 hours. Then, the temperature was raised to 100 ° C and the stirring reaction was continued for 5 hours. After the reaction, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with anhydrous ethanol and distilled water 5 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 85 ° C for 3 hours. Then, it was placed in a muffle furnace and calcined at a temperature of 460 ° C for 4 hours, and then cooled with the furnace to obtain a silicon zinc complex;
[0049] Step S2: 30 mL of anhydrous ethanol and 30 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. Then, the pH was adjusted to 9.5 with 25% ammonia water. Then, 5 g of silicon-zinc complex and 1.1 g of γ-methacryloyloxypropyltrimethoxysilane were added and the stirring reaction was continued for 3 hours. After the reaction was completed, the reaction product was centrifuged, and the precipitate was placed in a vacuum drying oven and dried at a temperature of 85° C. for 1.5 hours to obtain a modified silicon-zinc complex;
[0050] Step S3: 2 g of carbon nanotubes, 12 mL of 68% concentrated nitric acid, and 35 mL of 98% concentrated sulfuric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 55° C. and a stirring rate of 400 r / min for 2 h. Subsequently, 30 mL of deionized water and 7 mL of 35% hydrogen peroxide were added and the stirring reaction was continued for 4 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with distilled water 5 times, and then placed in a vacuum drying oven and dried at 65° C. for 5 h to obtain activated carbon nanotubes;
[0051] Step S4: 6 g of lauric acid, 2.5 g of palmitic acid, and 4.6 g of n-octadecane were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 75° C. and a stirring rate of 400 r / min for 2 h. Then, 10 g of activated carbon nanotubes were added and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature and then allowed to stand for 30 h to obtain adsorbed carbon nanotubes;
[0052] Step S5: 3 g of adsorbed carbon nanotubes, 0.3 g of modified silicon zinc 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 were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 35° C. and a stirring rate of 400 r / min for 2 h to obtain an oil phase. 1 g of sodium dodecylbenzenesulfonate and 70 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced. The mixture was stirred for reaction at a temperature of 85° C. and a stirring rate of 700 r / min for 2 h to obtain an aqueous phase. The oil phase was added to the aqueous phase while stirring, and the stirring reaction was continued for 5 h. After the reaction, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed 5 times with anhydrous ethanol and distilled water in sequence, and then placed in a vacuum drying oven and dried at a temperature of 65° C. for 3 h to obtain heat storage and temperature regulating particles.
[0053] Step S6: Weigh 100 parts of polyamide 6 slices with a brand of M2400 and 5.8 parts of heat storage and temperature regulating particles according to weight, and set aside;
[0054] Step S7: The polyamide 6 slices and the heat storage and temperature regulating particles are evenly mixed and melt-extruded through an extruder, and then extruded through a spinneret with a pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0055] Comparative Example 1:
[0056] This comparative example is a method for preparing a heat storage and temperature regulating textile material, comprising the following steps:
[0057] The polyamide 6 slices were melt-extruded through an extruder and then extruded through a spinneret with a pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0058] Comparative Example 2:
[0059] This comparative example is a method for preparing a heat storage and temperature regulating textile material, comprising the following steps:
[0060] Step S1: 2 g of carbon nanotubes, 12 mL of 68% concentrated nitric acid, and 35 mL of 98% concentrated sulfuric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 55° C. and 400 r / min for 2 h. Then, 30 mL of deionized water and 7 mL of 35% hydrogen peroxide were added and the stirring was continued for 4 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with distilled water 5 times, and then placed in a vacuum drying oven and dried at 65° C. for 5 h to obtain activated carbon nanotubes;
[0061] Step S2: 6 g of lauric acid, 2.5 g of palmitic acid, and 4.6 g of n-octadecane were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 75° C. and a stirring rate of 400 r / min for 2 h. Then, 10 g of activated carbon nanotubes were added and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature and then allowed to stand for 30 h to obtain adsorbed carbon nanotubes;
[0062] Step S3: Weigh 100 parts of polyamide 6 slices with a brand of M2400 and 5.8 parts of adsorbed carbon nanotubes according to weight and set aside;
[0063] Step S4: The polyamide 6 slices and the adsorbed carbon nanotubes are mixed evenly, melt-extruded through an extruder, and then extruded through a spinneret with a pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0064] Comparative Example 3:
[0065] This comparative example is a method for preparing a heat storage and temperature regulating textile material, comprising the following steps:
[0066] Step S1: 2.5 g of hexadecyltrimethylammonium bromide, 0.19 g of triethanolamine and 60 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen protection was introduced. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 minutes, and then 1.1 g of zinc nitrate hexahydrate was added and the stirring reaction was continued for 30 minutes. Then, 5.3 g of ethyl orthosilicate and 20 mL of cyclohexane were added in sequence and the temperature was raised to 65 ° C and the stirring reaction was continued for 8 hours. Then, the temperature was raised to 100 ° C and the stirring reaction was continued for 5 hours. After the reaction, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with anhydrous ethanol and distilled water 5 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 85 ° C for 3 hours. Then, it was placed in a muffle furnace and calcined at a temperature of 460 ° C for 4 hours, and then cooled with the furnace to obtain a silicon zinc complex;
[0067] Step S2: 30 mL of anhydrous ethanol and 30 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. Then, the pH was adjusted to 9.5 with 25% ammonia water. Then, 5 g of silicon-zinc complex and 1.1 g of γ-methacryloyloxypropyltrimethoxysilane were added and the stirring reaction was continued for 3 hours. After the reaction was completed, the reaction product was centrifuged, and the precipitate was placed in a vacuum drying oven and dried at a temperature of 85° C. for 1.5 hours to obtain a modified silicon-zinc complex;
[0068] Step S3: Weigh 100 parts of polyamide 6 slices with a brand of M2400 and 5.8 parts of modified silicon-zinc composite according to weight and set aside;
[0069] Step S4: The polyamide 6 slices and the modified silicon-zinc composite are uniformly mixed and melt-extruded through an extruder, and then extruded through a spinneret with a pore size of 0.4 mm to obtain a heat storage and temperature regulating textile material.
[0070] The heat storage and temperature regulating textile materials of Examples 1-3 and Comparative Examples 1-3 were subjected to performance tests, and the test results are shown below:
[0071]
[0072] Referring to the data in the above table, based on the comparison between Examples 1-3 and Comparative Examples 1-3, it can be seen that the heat storage and temperature regulation textile material of the present application has excellent heat storage and temperature regulation performance.
[0073] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
[0074] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in similar ways. As long as they do not deviate from the invention or exceed the scope defined in this application, they should all fall within the scope of protection of the present invention.
Claims
1. A heat storage and temperature regulating textile material, characterized in that: It comprises the following components in parts by weight: 100 parts of polyamide 6 chips, 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 at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 minutes, 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 at a temperature of 60-65° C. for 6-8 hours, then continuing to stir and react at a temperature of 95-100° C. for 3-5 hours, after which the reaction product is cooled to room temperature and then centrifuged, and the precipitate is washed with anhydrous ethanol and distilled water for 3-5 times in sequence, then placed in a vacuum drying oven, dried at a temperature of 80-85° C. for 2-3 hours, then placed in a muffle furnace, calcined at a temperature of 450-460° C. for 3-4 hours, and then cooled with the furnace to obtain a silicon-zinc complex; 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 and reacting at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes, then adjusting the pH to 9-9.5 with ammonia water, and then adding the silicon zinc complex and γ-methacryloxypropyltrimethoxysilane and continuing to stir and react 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 to a three-necked flask equipped with a stirrer and a thermometer, and stir the mixture at a temperature of 50-55°C and a stirring rate of 300-400 r / min for 1-2 hours. Then, add deionized water and hydrogen peroxide and continue stirring for 3-4 hours. After the reaction is completed, cool the reaction product to room temperature and vacuum filter it. 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 to a three-necked flask equipped with a stirrer and a thermometer, stirring the mixture at a temperature of 70-75°C and a stirring rate of 300-400 r / min for 1-2 hours, then adding activated carbon nanotubes and continuing to stir the mixture for 2-3 hours. After the reaction is completed, the reaction product is cooled to room temperature and then allowed to stand 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, and stir the mixture 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 guide tube, introduce nitrogen protection, and stir the mixture 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 continue stirring the reaction for 4-5 hours. After the reaction is completed, cool the reaction product to room temperature, then centrifuge it, wash the precipitate with anhydrous ethanol and distilled water for 3-5 times in sequence, and then place it in a vacuum drying oven and dry it 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, ethyl 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: In step s3, the usage ratio of the carbon nanotubes, concentrated nitric acid, concentrated sulfuric acid, deionized water and hydrogen peroxide is 2 g: 10-12 mL: 30-35 mL: 25-30 mL: 5-7 mL.
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 activated carbon nanotubes in step s4 is 5-6 g: 1.5-2.5 g: 3.2-4.6 g: 10 g.
8. The heat storage and temperature regulating textile material according to claim 1, characterized in that: The usage ratio of the adsorbed carbon nanotubes, modified silicon zinc complex, 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 the heat storage and temperature regulating textile material according to any one of claims 1 to 8, 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 pore size 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
Patent Citations
Organic phase change microcapsule material as well as preparation method and application thereof
CN116688889A