Temperature-regulating textile material and preparation method thereof

Abstract

The preparation method comprises the following steps: preparing an inorganic / organic composite wall material phase change energy storage microcapsule, carrying out surface modification treatment on the microcapsule, mixing the modified microcapsule with aramid fiber or polyimide, adding a heat conduction reinforcing agent to form a spinning stock solution, and carrying out temperature regulation on the spinning stock solution to obtain the temperature regulation textile material. And after spinning and stretching heat treatment, compounding with a reinforced composite material through a three-dimensional weaving, laminating or blending implanting process. Through the design of the composite wall material, the temperature resistance of the microcapsule exceeds 300 DEG C, and the problem that a traditional organic wall material cannot resist high-temperature spinning is solved; the interface bonding strength and the heat management efficiency are remarkably improved through the synergistic effect of the surface modification and the heat conduction reinforcing agent; the phase change enthalpy of the finally prepared temperature-regulating textile material reaches 10-100 J / g, the temperature-regulating response time is shortened to 2-3 minutes, the tensile strength reaches 260-400 MPa, and the temperature-regulating textile material has excellent temperature-regulating function and mechanical property and can be widely applied to the fields of military protection and civil temperature-control textiles.

Description

Technical Field

[0001] This invention belongs to the field of textile materials technology, specifically, it relates to a temperature-regulating textile material and its preparation method. Background Technology

[0002] With technological advancements and improved living standards, people are increasingly demanding greater comfort and functionality from textile materials. In the military field, soldiers need to maintain combat capabilities in extreme temperature environments; in the civilian sector, consumers are also placing higher demands on the temperature-regulating comfort of clothing. Phase change temperature regulation technology, by utilizing the properties of materials to absorb or release latent heat during phase change processes, provides temperature regulation for the human body and has become a current research hotspot.

[0003] Currently, phase change temperature-regulating fibers mainly employ phase change energy storage microcapsule technology, encapsulating phase change materials within microcapsules and mixing them with spinning solution for spinning. However, existing technologies face the following pressing problems: First, the organic wall materials of traditional phase change microcapsules have poor temperature resistance, typically only ranging from 120 to 200°C, which cannot meet the processing requirements of high-performance polymers (such as aramid and polyimide). The spinning temperatures of these high-performance polymers often reach above 280°C, at which temperature traditional microcapsules decompose and fail. Second, the enthalpy of existing phase change temperature-regulating fibers is generally low, typically only 8–10 J / g, making it difficult to provide significant temperature regulation effects in practical applications. This is mainly due to the limited amount of microcapsules that can be added, as excessive microcapsules can severely affect the spinnability and mechanical properties of fibers. In addition, traditional phase change microcapsules have poor interfacial compatibility with the spinning matrix, which makes them prone to rupture during spinning and leakage of phase change materials. This not only affects the temperature regulation effect but also reduces the mechanical properties of the fibers. Finally, existing technologies are mostly limited to the preparation of single fibers and lack structural composite design with reinforcing composite materials. As a result, the final textile materials do not meet the temperature regulation requirements, and their comprehensive performance, such as mechanical strength and durability, is insufficient, making it difficult to meet the comprehensive performance requirements of special application scenarios.

[0004] Therefore, developing a method for preparing temperature-controlled textile materials that is compatible with high-temperature spinning processes, significantly improves the amount of microcapsules added and the interfacial bonding strength, and achieves effective composite with reinforcing materials has become a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention provides a temperature-regulating textile material and its preparation method.

[0006] To achieve the above objectives, the technical solution provided by the present invention is as follows: A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: Mix the core material and emulsifier, and stir and emulsify at 1500-3500 r / min at 80-120℃ for 1-3 hours until the core material is completely emulsified; then add the initiator and reactant monomer, and stir and reflux at 80-120℃ for 4-6 hours to form organic wall material microcapsules; then add the oxidized inorganic wall material, and heat in a water bath at 80-100℃ for 2-4 hours to carry out the composite reaction; finally cool, filter, wash and dry to obtain inorganic / organic composite wall material phase change energy storage microcapsules; (2) Surface modification treatment of the phase change energy storage microcapsules obtained in step (1): Disperse the microcapsules in ethanol solvent, add 1-5% of silane coupling agent by mass of microcapsules, stir and react at 60-80℃ for 1-2 hours, then wash and dry to obtain surface-modified phase change energy storage microcapsules. (3) Preparation of spinning solution: The surface-modified phase change energy storage microcapsules obtained in step (2) are mixed with a high-performance polymer, and a thermal conductivity enhancer accounting for 0.5-5% of the total mass of the spinning solution is added. The mixture is then mixed with a high-speed shear dispersant to form a uniform and stable spinning solution. The mass percentage of the phase change energy storage microcapsules in the spinning solution is 5-40%. The high-performance polymer is selected from one or two of aramid and polyimide. The thermal conductivity enhancer is selected from at least one of boron nitride, carbon nanotubes, and alumina. (4) Spinning: The spinning solution is spun into temperature-regulating fibers using melt spinning or solution spinning. (5) Perform stretching heat treatment on the temperature-regulating fiber: stretch the fiber at 100~200℃ with a stretch ratio of 1.5~3.0, and then heat treat it at 150~250℃ for 10~30 minutes; (6) Composite: The temperature-regulating fiber is combined with continuous or discontinuous fiber-reinforced composite material through three-dimensional weaving, lamination or blending implantation process to form temperature-regulating textile material.

[0007] Furthermore, the phase change energy storage microcapsules have a particle size of 500~3000 nm. Controlling the particle size of the phase change energy storage microcapsules within this range helps maintain good flowability during spinning, avoids spinneret clogging, and ensures that the microcapsules have a high core material ratio and phase change enthalpy, which is beneficial for the final fiber to obtain significant temperature regulation capability.

[0008] Furthermore, the phase change energy storage microcapsules constitute 10-30% by mass in the spinning solution. This range achieves an optimal balance between ensuring significant phase change temperature regulation (high enthalpy) in the fiber and maintaining good spinnability and mechanical properties.

[0009] Furthermore, in the wall material of the phase change energy storage microcapsule, the mass ratio of inorganic wall material to organic wall material is (0.1~2):1. Controlling the mass ratio of inorganic to organic wall material within this range allows for the full utilization of the synergistic effect between the rigidity and heat resistance of inorganic materials and the toughness and sealing properties of organic materials, thereby producing composite microcapsules with high wall strength, good density, and excellent temperature resistance. Furthermore, the core material is selected from one or more of paraffin wax, soybean wax, polyethylene glycol, aliphatic hydrocarbons, fatty acids, and fatty alcohols; the organic wall material is selected from one of polyurethane, polymethyl methacrylate, phenolic resin, and polystyrene; and the inorganic wall material is selected from at least one of graphene, carbon nanotubes, and silicon carbide. By limiting the specific types of the core material, organic wall material, and inorganic wall material, the compatibility and reactivity between the components are ensured, which is beneficial for forming high-performance phase change energy storage microcapsules with stable structure and good sealing performance.

[0010] Furthermore, the phase change enthalpy of the phase change energy storage microcapsules is 150~250 J / g. This phase change enthalpy is the material basis for endowing the final textile material with high energy storage density and is the core guarantee for achieving efficient temperature regulation.

[0011] This invention also provides a temperature-regulating textile material prepared by the above method. The temperature-regulating textile material comprises temperature-regulating fibers and a continuous or discontinuous fiber-reinforced composite material. The temperature-regulating fibers contain surface-modified phase change energy storage microcapsules and a thermal conductivity enhancer. Furthermore, the temperature-regulating fibers are formed from at least one high-performance polymer, selected from one or two of aramid and polyimide. This material ultimately exhibits the characteristics of a functional textile material with high phase change enthalpy, excellent temperature resistance, good mechanical properties, and a composite structure.

[0012] Furthermore, the phase change energy storage microcapsules have a particle size of 500~3000 nm. This size facilitates the uniform distribution of microcapsules within the fiber, reduces stress concentration points, and thus minimizes the negative impact on the mechanical properties of the fiber while exerting a temperature regulation function.

[0013] Furthermore, the phase change energy storage microcapsules constitute 5-35% of the mass of the temperature-regulating fiber. This range is directly related to the temperature regulation capability of the final product, ensuring that the textile material can provide a significant phase change enthalpy of 10-60 J / g, meeting the temperature regulation range requirements in practical applications.

[0014] Furthermore, the phase transition enthalpy of the temperature-regulating textile material is 10~100 J / g. This value is significantly higher than that of common products on the market (8~10 J / g), demonstrating the significant progress of this invention in improving the temperature-regulating function of textiles, and providing the human body with more durable and effective temperature buffering and comfort protection.

[0015] Compared with the prior art, the present invention has the following beneficial effects: I. This invention effectively solves the bottleneck of temperature resistance and broadens the application range of materials. By constructing a composite wall material combining inorganic materials such as graphene and carbon nanotubes with organic polymers, the inherent high thermal stability of inorganic components enables phase change microcapsules to withstand processing environments above 280°C. This effectively solves the problem of insufficient temperature resistance (usually below 200°C) of traditional organic wall materials, allowing microcapsules to be successfully combined with high-performance polymers such as aramid and polyimide that require high-temperature processing, thus broadening the range of matrix materials that can be selected for temperature-regulating fibers.

[0016] II. This invention employs a synergistic approach of surface modification and specific thermal conductivity enhancers to synergistically improve material compatibility and thermal management efficiency. Surface modification enhances the interfacial bonding between microcapsules and the polymer matrix through silane coupling agents, reducing the risk of microcapsule rupture at high addition levels and helping to maintain the mechanical properties of the fiber. Simultaneously, the introduction of thermally conductive agents such as boron nitride and carbon nanotubes promotes heat transfer within the fiber, contributing to improved response speed and uniformity of the phase change process, thus supporting the achievement of higher energy storage density (phase change enthalpy).

[0017] Third, this invention achieves an integrated combination of temperature regulation function and structural performance. Through composite processes such as three-dimensional weaving and lamination, temperature-regulating fibers are combined with fiber reinforcement materials. This design enables the final textile material to not only possess phase change temperature regulation function, but also integrate the advantages of mechanical strength and durability of the reinforcement materials, thereby meeting the application scenarios with comprehensive requirements for thermal comfort and mechanical performance, and enhancing the practical value of the product. Detailed Implementation

[0018] The specific embodiments are described in detail below, but it should be understood that the scope of protection of this invention is not limited to the specific embodiments. Unless otherwise specified, the raw materials and reagents used in the examples are commercially available. This invention has been verified through numerous experiments, and its objectives can be achieved within the stated parameter range. Those skilled in the art can adjust the process parameters within the scope of the claims according to the specific raw materials and equipment available.

[0019] Example 1 A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 30 kg of paraffin core material (Changyingtong RK-58) and 120 kg of Tween 60 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2500 r / min for 2 hours at 100°C until the core material was completely emulsified. 5 kg of potassium persulfate initiator and 50 kg of methyl methacrylate monomer were added and stirred and refluxed at 100°C for 5 hours to form organic wall material microcapsules. 15 kg of graphene inorganic wall material oxidized by Hummer method was added and heated in a water bath at 90°C for 3 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 200 kg of ethanol solvent, 1 kg of KH-550 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 70 °C for 1.5 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: 20 kg of surface-modified phase change energy storage microcapsules were mixed with 80 kg of polyimide resin (DuPont Vespel® SP-1), and 2 kg of boron nitride thermal conductivity enhancer was added. The mixture was stirred for 1 hour at 3000 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 19.6%. The calculation method was: 20 kg microcapsules / (20 kg microcapsules + 80 kg polyimide resin + 2 kg boron nitride) × 100%. (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 320°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 150°C with a stretch ratio of 2.0, and then heat treat it at 200°C for 20 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and T300 grade carbon fiber plain weave fabric are used to reinforce the composite material (area density 200g / m²). 2 Through a combination of three-dimensional weaving techniques, the final temperature-regulating textile material is formed.

[0020] Example 2 A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 20 kg of soybean wax core material (simel-52) and 80 kg of polyvinyl alcohol emulsifier (NOVELUTION-S90K) were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 1500 r / min for 3 hours at 80°C until the core material was completely emulsified. 3 kg of benzoyl peroxide initiator and 30 kg of styrene monomer were added and stirred and refluxed at 80°C for 6 hours to form organic wall material microcapsules. 2 kg of carbon nanotube inorganic wall material oxidized by the Hummer method was added and heated in a water bath at 80°C for 4 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 150 kg of ethanol solvent, 1 kg of KH-570 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 60 °C for 2 hours; the mixture was filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules. (3) Preparation of spinning solution: 15 kg of surface-modified phase change energy storage microcapsules were mixed with 95 kg of aramid resin (DuPont Kevlar®), and 0.5 kg of carbon nanotube thermal conductivity enhancer was added. The mixture was stirred for 1.5 hours at 2000 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 13.6%. The calculation method was: 15 kg microcapsules / (15 kg microcapsules + 95 kg aramid resin + 0.5 kg carbon nanotubes) × 100%). (4) Spinning process: Solution spinning is used to spin fibers, with N,N-dimethylacetamide as the solvent, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 100℃ with a stretch ratio of 1.5, and then heat treat it at 150℃ for 30 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and E-glass fiber plain weave fabric are used to reinforce the composite material (area density 300 g / m²). 2 Through lamination, the final temperature-regulating textile material is formed.

[0021] Example 3 A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 50 kg of polyethylene glycol core material (PEG-6000) and 150 kg of Tween 20 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 3500 r / min for 1 hour at 95°C until the core material was completely emulsified. 10 kg of azobisisobutyronitrile initiator and 80 kg of methyl methacrylate monomer were added and stirred and refluxed at 95°C for 4 hours to form organic wall material microcapsules. 100 kg of silicon carbide inorganic wall material oxidized by Hummer method was added and heated in a water bath at 100°C for 2 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 300 kg of ethanol solvent, 5 kg of KH-550 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 80 °C for 1 hour; the mixture was filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: 40 kg of surface-modified phase change energy storage microcapsules were mixed with 60 kg of aramid resin (DuPont Kevlar®), and 3 kg of alumina thermal conductivity enhancer was added. The mixture was stirred for 0.5 hours at 4000 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 38.8%. The calculation method was: 40 kg microcapsules / (40 kg microcapsules + 60 kg aramid resin + 3 kg alumina) × 100%; (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 350°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 200℃ with a stretch ratio of 3.0, and then heat treat it at 250℃ for 10 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and Kevlar aramid fiber woven fabric are used to reinforce the composite material (area density 180 g / m²). 2 Through a blending and implantation process, the final temperature-regulating textile material is formed.

[0022] Example 4 A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 40 kg of n-octadecane core material (CAS 593-45-3) and 120 kg of Tween 60 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 3000 r / min for 1.5 hours at 110°C until the core material was completely emulsified. 8 kg of ammonium persulfate initiator and 20 kg of phenolic resin prepolymer were added and stirred and refluxed at 110°C for 4.5 hours to form organic wall material microcapsules. 8 kg of carbon nanotube inorganic wall material oxidized by Hummer method was added and heated in a water bath at 95°C for 2.5 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 250 kg of ethanol solvent, 2 kg of KH-560 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 75 °C for 1.2 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: 30 kg of surface-modified phase change energy storage microcapsules were mixed with 70 kg of polyimide resin (DuPont Vespel® SP-1), and 2 kg of boron nitride thermal conductivity enhancer was added. The mixture was stirred for 0.8 hours at 3500 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 29.4%. The calculation method was: 30 kg microcapsules / (30 kg microcapsules + 70 kg polyimide resin + 2 kg boron nitride) × 100%. (4) Spinning process: The melt spinning method is used for spinning, the spinning temperature is 340℃, and the temperature-regulating fiber is formed by spinning through a spinneret; (5) Stretching heat treatment: Stretch the fiber at 180°C with a stretch ratio of 2.5, and then heat treat it at 220°C for 15 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and T300 grade carbon fiber plain weave fabric are used to reinforce the composite material (area density 200g / m²). 2 Through a combination of three-dimensional weaving techniques, the final temperature-regulating textile material is formed.

[0023] Example 5 A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 35 kg of n-hexadecyl alcohol core material (CAS 36653-82-4) and 105 kg of polyvinyl alcohol emulsifier (NOVELUTION-S90K) were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2800 r / min for 2 hours at 95°C until the core material was completely emulsified. 7 kg of toluene diisocyanate and 35 kg of polyurethane prepolymer were added and stirred and refluxed at 95°C for 5 hours to form organic wall material microcapsules. 35 kg of graphene inorganic wall material oxidized by the Hummer method was added and heated in a water bath at 85°C for 3.5 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 200 kg of ethanol solvent, 2 kg of KH-550 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 65 °C for 1.8 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: 25 kg of surface-modified phase change energy storage microcapsules were mixed with 75 kg of aramid resin (DuPont Kevlar®), and 2 kg of carbon nanotube thermal conductivity enhancer was added. The mixture was stirred for 1 hour at 3200 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 24.5%. The calculation method was: 25 kg microcapsules / (25 kg microcapsules + 75 kg aramid resin + 2 kg carbon nanotubes) × 100%. (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 330°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 160℃ with a stretch ratio of 2.2, and then heat treat it at 210℃ for 18 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and ultra-high molecular weight polyethylene (UHMWPE) unidirectional fabric reinforced composite material (area density 150 g / m²) were prepared. 2 Through lamination, the final temperature-regulating textile material is formed.

[0024] Example 6 A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 25 kg of stearic acid core material (CAS 57-11-4) and 100 kg of polyvinyl alcohol emulsifier (NOVELUTION-S90K) were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2200 r / min for 2.5 hours at 90°C until the core material was completely emulsified. 4 kg of benzoyl peroxide initiator and 25 kg of polystyrene monomer were added and stirred and refluxed at 90°C for 5.5 hours to form organic wall material microcapsules. 5 kg of a mixture of graphene and carbon nanotubes oxidized by the Hummer method (mass ratio 1:1) was added and heated in a water bath at 88°C for 3 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 180 kg of ethanol solvent, 1.5 kg of KH-560 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 68 °C for 1.6 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: Take 10 kg of surface-modified phase change energy storage microcapsules and mix them with 90 kg of a mixture of aramid and polyimide (mass ratio 1:1). Add 1.5 kg of a mixture of alumina and boron nitride (mass ratio 1:1) as a thermal conductivity enhancer. Mix the mixture for 1.2 hours at 2800 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution is 9.9%. The calculation method is: 10 kg microcapsules / (10 kg microcapsules + 45 kg aramid resin + 45 kg polyimide resin + 1.5 kg thermal conductivity enhancer) × 100%; (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 325°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 140℃ with a stretch ratio of 1.8, and then heat treat it at 190℃ for 22 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and E-glass fiber plain weave fabric are used to reinforce the composite material (area density 300 g / m²). 2 Through lamination, the final temperature-regulating textile material is formed.

[0025] Comparative Example 1 (using only organic wall material microcapsules) A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 30 kg of paraffin core material (Changyingtong RK-58) and 120 kg of Tween 60 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2500 r / min for 2 hours at 100°C until the core material was completely emulsified. 5 kg of potassium persulfate initiator and 50 kg of methyl methacrylate monomer were added and stirred and refluxed at 100°C for 5 hours to form organic wall material microcapsules. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain pure organic wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 200 kg of ethanol solvent, 1 kg of KH-550 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 70 °C for 1.5 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: Take 20 kg of surface-modified phase change energy storage microcapsules and mix them with 80 kg of polyimide resin (DuPont Vespel® SP-1), add 2 kg of boron nitride thermal conductivity enhancer, and mix them for 1 hour at 3000 r / min using a high-speed shear disperser to form a spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution is 19.6%, and the calculation method is the same as in Example 1.

[0026] (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 320°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 150°C with a stretch ratio of 2.0, and then heat treat it at 200°C for 20 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and T300 grade carbon fiber plain weave fabric are used to reinforce the composite material (area density 200g / m²). 2 Through a combination of three-dimensional weaving technology, temperature-regulating textile materials are formed.

[0027] Comparative Example 2 (without surface modification treatment) A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 30 kg of paraffin core material (Changyingtong RK-58) and 120 kg of Tween 60 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2500 r / min for 2 hours at 100°C until the core material was completely emulsified. 5 kg of potassium persulfate initiator and 50 kg of methyl methacrylate monomer were added and stirred and refluxed at 100°C for 5 hours to form organic wall material microcapsules. 15 kg of graphene inorganic wall material oxidized by Hummer method was added and heated in a water bath at 90°C for 3 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Preparation of spinning solution: 20 kg of phase change energy storage microcapsules and 80 kg of polyimide resin (DuPont Vespel® SP-1) were mixed and 2 kg of boron nitride thermal conductivity enhancer was added. The mixture was mixed for 1 hour at 3000 r / min using a high-speed shear disperser to form a spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 19.6%, and the calculation method was the same as in Example 1.

[0028] (3) Spinning process: The spinning process is carried out by melt spinning at a temperature of 320°C, and temperature-regulating fibers are formed by spinning through a spinneret. (4) Stretching heat treatment: Stretch the fiber at 150°C with a stretch ratio of 2.0, and then heat treat it at 200°C for 20 minutes; (5) Preparation of composite materials: The temperature-regulating fiber and T300 grade carbon fiber plain weave fabric are used to reinforce the composite material (area density 200g / m²). 2 Through a combination of three-dimensional weaving technology, temperature-regulating textile materials are formed.

[0029] Comparative Example 3 (without thermal conductivity enhancer) A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 30 kg of paraffin core material (Changyingtong RK-58) and 120 kg of Tween 60 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2500 r / min for 2 hours at 100°C until the core material was completely emulsified. 5 kg of potassium persulfate initiator and 50 kg of methyl methacrylate monomer were added and stirred and refluxed at 100°C for 5 hours to form organic wall material microcapsules. 15 kg of graphene inorganic wall material oxidized by Hummer method was added and heated in a water bath at 90°C for 3 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 200 kg of ethanol solvent, 1 kg of KH-550 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 70 °C for 1.5 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: 20 kg of surface-modified phase change energy storage microcapsules were mixed with 80 kg of polyimide resin (DuPont Vespel® SP-1) and mixed for 1 hour at 3000 r / min using a high-speed shear disperser to form a spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution was 19.6%, and the calculation method was the same as in Example 1.

[0030] (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 320°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 150°C with a stretch ratio of 2.0, and then heat treat it at 200°C for 20 minutes; (6) Preparation of composite materials: The temperature-regulating fiber and T300 grade carbon fiber plain weave fabric are used to reinforce the composite material (area density 200g / m²). 2 Through a combination of three-dimensional weaving technology, temperature-regulating textile materials are formed.

[0031] Comparative Example 4 (Traditional Composite Process) A method for preparing a temperature-regulating textile material includes the following steps: (1) Preparation of phase change energy storage microcapsules: 30 kg of paraffin core material (Changyingtong RK-58) and 120 kg of Tween 60 emulsifier were added to the reaction vessel and mixed. The mixture was stirred and emulsified at 2500 r / min for 2 hours at 100°C until the core material was completely emulsified. 5 kg of potassium persulfate initiator and 50 kg of methyl methacrylate monomer were added and stirred and refluxed at 100°C for 5 hours to form organic wall material microcapsules. 15 kg of graphene inorganic wall material oxidized by Hummer method was added and heated in a water bath at 90°C for 3 hours to carry out the composite reaction. The reaction product was cooled to 25°C, filtered, washed 3 times with deionized water, and dried in a vacuum drying oven at 80°C for 12 hours to obtain inorganic / organic composite wall material phase change energy storage microcapsules. (2) Surface modification treatment: 100 kg of phase change energy storage microcapsules were dispersed in 200 kg of ethanol solvent, 1 kg of KH-550 silane coupling agent was added, and the mixture was stirred at 1500 r / min at 70 °C for 1.5 hours; the mixture was then filtered, washed twice with ethanol, and dried in a vacuum drying oven at 80 °C for 8 hours to obtain surface-modified phase change energy storage microcapsules; (3) Preparation of spinning solution: Take 20 kg of surface-modified phase change energy storage microcapsules and mix them with 80 kg of polyimide resin (DuPont Vespel® SP-1). Add 2 kg of boron nitride thermal conductivity enhancer and mix them for 1 hour at 3000 r / min using a high-speed shear disperser to form a uniform and stable spinning solution. The mass percentage of phase change energy storage microcapsules in the spinning solution is 19.6%, and the calculation method is the same as in Example 1.

[0032] (4) Spinning process: The spinning process is carried out by melt spinning at a temperature of 320°C, and temperature-regulating fibers are formed by spinning through a spinneret. (5) Stretching heat treatment: Stretch the fiber at 150°C with a stretch ratio of 2.0, and then heat treat it at 200°C for 20 minutes; (6) Traditional composite: combining temperature-regulating fibers with conventional polyester fabric (area density 150g / m²). 2 (0.3mm thick) are combined through a simple sewing process to form a temperature-regulating textile material.

[0033] The performance of Examples 1-6 and Comparative Examples 1-4 was compared and tested using the following methods: 1. Temperature resistance of microcapsules: Thermogravimetric analysis (TGA) was used to heat the sample from room temperature to 600℃ at a heating rate of 10℃ / min under a nitrogen atmosphere. The temperature at which the sample mass loss was 5% was recorded as the temperature resistance temperature.

[0034] 2. Microcapsule phase transition enthalpy: Using a differential scanning calorimeter (DSC), under nitrogen protection, the temperature was cyclically increased and decreased at a rate of 10℃ / min within the range of -20℃ to 100℃. The phase transition enthalpy was calculated by integrating the phase transition peak area.

[0035] 3. Material phase change enthalpy: DSC test was also used, with a sample size of 5-10 mg. The test conditions were the same as those for microcapsule phase change enthalpy test, reflecting the overall energy storage capacity of the final textile material.

[0036] 4. Tensile strength: According to GB / T 3923.1-2013 standard, a universal testing machine was used with a clamping distance of 100mm, a tensile speed of 100mm / min, and a test sample width of 25mm. The maximum force value at break was recorded to calculate the tensile strength.

[0037] 5. Elongation at break: Recorded simultaneously during the tensile strength test, and the percentage of elongation at break relative to the original gauge length is calculated.

[0038] 6. Thermal conductivity: The thermal constant was measured using a Hot Disk thermal constant analyzer with a TPS 2500S probe at room temperature (25°C), with a power of 100mW and a measurement time of 20s.

[0039] 7. Microcapsule breakage rate: The sample was extracted with n-hexane in a Soxhlet extractor for 24 hours. The microcapsule breakage rate was calculated by the change in mass before and after extraction. Breakage rate = (mass before extraction - mass after extraction) / mass before extraction × 100%.

[0040] 8. High temperature stability: After heat-treating the sample in an oven at 280℃ for 30 minutes, observe the changes in surface state and test the enthalpy retention rate of phase transition. A retention rate >95% is rated as excellent, and <90% is rated as poor.

[0041] 9. Temperature adjustment response time: Using an infrared thermal imager, the sample is rapidly transferred from a 20℃ environment to a 35℃ environment, and the time required for the sample temperature to reach 32℃ is recorded.

[0042] 10. Composite interface bonding strength: According to GB / T 1456-2005 standard, the peel strength test is adopted, the sample width is 25mm, the peel speed is 100mm / min, and the average peel force is recorded to calculate the bonding strength.

[0043] All tests were conducted in a standard laboratory environment (temperature 23±2℃, relative humidity 50±5%). Each sample was tested 5 times and the average value was taken to ensure the accuracy and reproducibility of the data.

[0044] The test data is shown in the table below: Test Project Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Temperature resistance of microcapsules (°C) >300 >300 >300 >300 >300 >300 180 >300 >300 >300 Microencapsulation phase transition enthalpy (J / g) 220 150 250 190 210 170 225 220 220 220 Material phase transition enthalpy (J / g) 45 24 58 42 38 16 42 38 35 40 Tensile strength (MPa) 320 400 260 300 340 380 310 280 300 250 Elongation at break (%) 25 28 18 22 24 26 23 18 22 20 Thermal conductivity (W / m·K) 0.85 0.78 0.92 0.88 0.82 0.80 0.82 0.80 0.45 0.83 Microcapsule breakage rate (%) 3.2 2.8 4.5 3.5 3.0 3.8 4.5 8.7 3.5 3.8 High temperature stability excellent excellent excellent excellent excellent excellent Difference excellent excellent excellent Temperature response time (min) 2.5 3.0 2.0 2.3 2.7 2.9 3.2 3.0 5.8 2.7 Composite interfacial bonding strength (MPa) 28 25 30 28 26 24 26 24 27 15 Analyzing the data in the table, we can obtain: Each embodiment of the present invention demonstrates significant advantages in different application scenarios. Embodiment 1, as the preferred embodiment, achieves an optimal balance in key indicators such as phase change enthalpy (45 J / g), tensile strength (320 MPa), and temperature regulation response time (2.5 min), making it suitable for fields with high overall performance requirements. Embodiment 2, although having a lower phase change enthalpy (24 J / g), exhibits the highest tensile strength (400 MPa) and the lowest microcapsule breakage rate (2.8%), making it particularly suitable for applications with stringent mechanical performance requirements. Embodiment 3 demonstrates the highest phase change enthalpy (58 J / g) and optimal thermal conductivity (0.92 W / m·K), excelling in scenarios requiring large-capacity thermal storage and rapid thermal response. Embodiments 4-6, through different component combinations, achieve diverse configurations across different performance indicators, proving the good adaptability and flexibility of the technical solution of the present invention.

[0045] The comparison with comparative examples and conventional products fully reveals the synergistic effect of various technical features. Comparative Example 1, using only organic wall materials, exhibits a significantly lower temperature resistance (180°C) than the embodiments of this invention (>300°C), demonstrating the crucial role of inorganic / organic composite wall materials in high-temperature processing performance. Comparative Example 2, without surface modification, shows a significantly higher microcapsule breakage rate (8.7%) than Example 1 (3.2%), highlighting the improving effect of surface modification on interfacial bonding. Comparative Example 3, without the addition of thermal conductivity enhancers, shows a significantly prolonged temperature regulation response time (5.8 min) and a substantial decrease in thermal conductivity (0.45 W / m·K), indicating the significant contribution of thermal conductivity enhancers to thermal management efficiency. Comparative Example 4, employing a conventional composite process, exhibits an interfacial bonding strength (15 MPa) that is only about half that of Example 1 (28 MPa), demonstrating the improvement effect of advanced composite processes on the overall material performance.

[0046] In summary, this invention, through the synergistic innovation of inorganic / organic composite wall materials, surface modification treatment, thermal conductivity enhancers, and advanced composite processes, successfully solves the technical bottlenecks of traditional temperature-regulating textile materials in terms of temperature resistance, energy storage density, mechanical properties, and thermal management efficiency. The performance of all embodiments is significantly superior to the comparative examples and traditional commercially available products, particularly achieving breakthroughs in core indicators such as material phase change enthalpy (increased by over 350%) and temperature regulation response time (reduced by over 60%). This technical solution not only demonstrates clear technological advancement but also exhibits promising prospects for industrial application, capable of meeting diverse needs in different application scenarios.

[0047] It should be understood that the above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement it accordingly. It should not be considered that the specific implementation of the present invention is limited to these descriptions. For those skilled in the art, several simple deductions or substitutions can be made without departing from the concept of the present invention. All equivalent changes or modifications made in accordance with the spirit and essence of the present invention should be covered within the protection scope of the present invention.

Claims

1. A method for preparing a temperature-regulating textile material, characterized in that, Includes the following steps: (1) Preparation of phase change energy storage microcapsules: Mix the core material and emulsifier, and stir and emulsify at 1500-3500 r / min at 80-120℃ for 1-3 hours until the core material is completely emulsified; then add the initiator and reactant monomer, and stir and reflux at 80-120℃ for 4-6 hours to form organic wall material microcapsules; then add the oxidized inorganic wall material, and heat in a water bath at 80-100℃ for 2-4 hours to carry out the composite reaction; finally cool, filter, wash and dry to obtain inorganic / organic composite wall material phase change energy storage microcapsules; (2) Surface modification treatment of the phase change energy storage microcapsules obtained in step (1): Disperse the microcapsules in ethanol solvent, add 1-5% of silane coupling agent by mass of microcapsules, stir and react at 60-80℃ for 1-2 hours, then wash and dry to obtain surface-modified phase change energy storage microcapsules. (3) Preparation of spinning solution: The surface-modified phase change energy storage microcapsules obtained in step (2) are mixed with high-performance polymers, and a thermal conductivity enhancer accounting for 0.5~5% of the total mass of the spinning solution is added. The mixture is then mixed using a high-speed shear dispersion apparatus to form a uniform and stable spinning solution, wherein the mass percentage of the phase change energy storage microcapsules in the spinning solution is 5~40%. The high-performance polymer is selected from one or two of aramid and polyimide; The thermal conductivity enhancer is selected from at least one of boron nitride, carbon nanotubes, and alumina; (4) Spinning: The spinning solution is spun into temperature-regulating fibers using melt spinning or solution spinning. (5) Perform stretching heat treatment on the temperature-regulating fiber: stretch the fiber at 100~200℃ with a stretch ratio of 1.5~3.0, and then heat treat it at 150~250℃ for 10~30 minutes; (6) Composite: The temperature-regulating fiber is combined with continuous or discontinuous fiber-reinforced composite material through three-dimensional weaving, lamination or blending implantation process to form a temperature-regulating textile material.

2. The preparation method according to claim 1, characterized in that: The phase change energy storage microcapsules have a particle size of 500~3000nm.

3. The preparation method according to claim 1, characterized in that: The phase change energy storage microcapsules have a mass percentage of 10-30% in the spinning solution.

4. The preparation method according to claim 1, characterized in that: In the wall material of the phase change energy storage microcapsule, the mass ratio of inorganic wall material to organic wall material is (0.1~2):

1.

5. The preparation method according to claim 1, characterized in that: The core material is selected from one or more of paraffin wax, soybean wax, polyethylene glycol, aliphatic hydrocarbons, fatty acids, and fatty alcohols; the organic wall material is selected from one of polyurethane, polymethyl methacrylate, phenolic resin, and polystyrene; and the inorganic wall material is selected from at least one of graphene, carbon nanotubes, and silicon carbide.

6. The preparation method according to claim 1, characterized in that: The phase change enthalpy of the phase change energy storage microcapsule is 150~250 J / g.

7. A temperature-regulating textile material, prepared by the method according to any one of claims 1 to 6, characterized in that: The invention includes temperature-regulating fibers and continuous or discontinuous fiber-reinforced composites, wherein the temperature-regulating fibers contain surface-modified phase change energy storage microcapsules and thermal conductivity enhancers, and the temperature-regulating fibers are formed from at least one high-performance polymer selected from one or two of aramid and polyimide.

8. The temperature-regulating textile material according to claim 7, characterized in that: The phase change energy storage microcapsules have a particle size of 500~3000nm.

9. The temperature-regulating textile material according to claim 7, characterized in that: The phase change energy storage microcapsules account for 5-35% of the mass of the temperature-regulating fiber.

10. The temperature-regulating textile material according to claim 7, characterized in that: The phase transition enthalpy of the temperature-regulating textile material is 10~100 J / g.