A phase change temperature regulating fiber, a preparation method and a temperature regulating fabric prepared by using the same
By preparing core spinning solution and shell material with phase change temperature of 26-35℃, and combining titanium dioxide and organic-inorganic hybrid polymers, the problem of poor cooling effect of existing phase change temperature-regulating fibers in high-temperature environments has been solved, providing a comfortable wearing experience and improving the overall performance of the fiber.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- JIANGSU INTCO MEDICAL PROD CO LTD
- Filing Date
- 2023-12-05
- Publication Date
- 2026-06-05
AI Technical Summary
Existing phase change temperature-regulating fibers and the temperature-regulating fabrics they prepare have poor cooling effects and poor breathability and water permeability in high-temperature environments, which affects wearing comfort and work efficiency.
By compounding polyethylene glycol of different molecular weights, a core spinning solution with a phase change temperature of 26-35℃ was prepared. An organic-inorganic hybrid polymer with amino and siloxy functional groups was synthesized as a support material by in-situ polymerization. Titanium dioxide was used as an additive. Polyethylene glycol was encapsulated in the shell as a core layer using a coaxial electrospinning process to obtain phase change temperature-regulating fiber.
It achieves the absorption or release of heat when the temperature changes, maintains a comfortable body temperature, improves the softness, strength, heat resistance and UV shielding effect of the fiber, provides a comfortable wearing experience, and enhances the abrasion resistance and weather resistance of the fiber.
Abstract
Description
Technical Field
[0001] This invention relates to the field of phase change materials technology, specifically to a phase change temperature-regulating fiber, its preparation method, and a temperature-regulating fabric prepared using the same. Background Technology
[0002] With increasingly stringent requirements for industrial production and occupational safety, the demand for phase change materials (PCMs) is growing for workers in high-temperature environments. PCMs are materials capable of absorbing or releasing large amounts of heat within a specific temperature range. When the temperature exceeds the phase change temperature, the PCM changes from a solid to a liquid state, absorbing heat; when the temperature falls below the phase change temperature, the PCM changes from a liquid to a solid state, releasing heat. This characteristic allows PCMs to regulate the ambient temperature within a certain range, providing a comfortable wearing experience for the human body.
[0003] Currently, the market lacks phase change temperature-regulating fibers and temperature-regulating fabrics made from them that offer good cooling, breathability, water permeability, and comfort. Traditional protective clothing suffers from poor cooling and poor breathability and water permeability in high-temperature environments. Furthermore, protective clothing made from monolithic gel blocks is not only inconvenient to wear but also affects work efficiency.
[0004] Therefore, we propose a phase change temperature-regulating fiber and the temperature-regulating fabric prepared therefrom. Summary of the Invention
[0005] The purpose of this invention is to provide a phase change temperature-regulating fiber, a preparation method thereof, and a temperature-regulating fabric prepared therefrom, in order to solve the problems mentioned in the background art.
[0006] To solve the above-mentioned technical problems, the present invention provides the following technical solution:
[0007] A method for preparing phase change temperature-regulating fiber includes the following steps:
[0008] Step S1: Mix polyethylene glycols of different molecular weights, heat to 40-50℃, stir evenly, and then prepare the core spinning solution.
[0009] Step S2: Under nitrogen protection, 4-ethyleneaniline, organosilicon containing double bonds, and chloroform are mixed evenly, and azobisisobutyronitrile is added dropwise. The mixture is heated to 75-85℃ and stirred for 10-12 hours. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. The support material, titanium dioxide, and N,N-dimethylformamide are mixed, heated to 40-50℃, and stirred evenly to obtain the shell spinning solution.
[0010] Step S3: Inject the core spinning solution and the shell spinning solution into the syringe respectively to obtain phase change temperature-regulating fiber.
[0011] In the above technical solution, by compounding polyethylene glycol of different molecular weights, a core spinning solution with a phase change temperature of 26-35℃ is obtained, which can absorb or release heat when the temperature changes, helping to maintain a comfortable body temperature. An organic-inorganic hybrid polymer with amino and siloxy functional groups is successfully synthesized by in-situ polymerization and used as a support material, which can combine the softness of organic materials with the strength and heat resistance of inorganic materials. Titanium dioxide is used as an additive to improve the ultraviolet shielding effect. Polyethylene glycol is encapsulated in the shell as a core layer through coaxial electrospinning process to produce phase change temperature-regulating fibers. Using these fibers, textiles with temperature-regulating functions can be produced to provide a comfortable wearing experience.
[0012] Furthermore, in step S1, the polyethylene glycol is PEG-800, PEG-1000, or PEG-1500, with a mass ratio of 1:(0.15-0.20):(0.10-0.15).
[0013] Furthermore, in step S2, the mass ratio of 4-vinylaniline and organosilicon containing double bonds and chloroform is 1:(0.3-0.5):(3-4).
[0014] Furthermore, in step S2, the mass of azobisisobutyronitrile is 0.2-0.4% of the mass of 4-vinylaniline.
[0015] Furthermore, in step S2, the mass ratio of the support material to N,N dimethylformamide is 1:(4-5).
[0016] Furthermore, in step S2, the mass ratio of titanium dioxide to the supporting material is 1:(10-12).
[0017] Furthermore, the preparation method of the double-bonded organosilicon in step S2 is as follows:
[0018] Potassium hydroxide and octamethylcyclotetrasiloxane were mixed evenly and heated to 80-90℃. The mixture was reacted for 1-2 hours. A mixed solution of 3-methacryloyloxypropyltris(methoxyethoxy)silane, dimethyl sulfoxide, and hexamethylsiloxane was added and stirred evenly. The reaction was continued for 3-4 hours. After vacuum distillation and drying, organosilicon containing double bonds was obtained.
[0019] In the above technical solution, octamethylcyclotetrasiloxane, 3-methacryloyloxypropyltris(methoxyethoxy)silane, hexamethyldisiloxane, and dimethyl sulfoxide are used as raw materials to react under the catalysis of potassium hydroxide to synthesize organosilicon macromolecules containing carbon-carbon double bonds, i.e., organosilicon containing double bonds.
[0020] Furthermore, the mass ratio of potassium hydroxide to octamethylcyclotetrasiloxane is 1:(180-200).
[0021] Furthermore, the mass ratio of 3-methacryloxypropyltris(methoxyethoxy)silane, dimethyl sulfoxide, and hexamethylsiloxane is 3:(1-2):(0.1-0.2).
[0022] Furthermore, in step S2, the titanium dioxide undergoes a modification treatment, the specific process of which is as follows:
[0023] Titanium dioxide was dispersed in deionized water and stirred evenly. Sodium hexametaphosphate was added and ultrasonically stirred for 30-50 minutes. The mixture was heated to 70-80℃, and the pH of the system was adjusted to 9-10 with sodium hydroxide solution. Sodium silicate solution was added dropwise, and the pH of the system was adjusted to 7-8 with hydrochloric acid solution. The temperature was raised to 85-90℃ and kept at that temperature for 1-2 hours. The mixture was then cooled to room temperature, filtered, washed, and dried to obtain modified titanium dioxide.
[0024] In the above technical solution, modified titanium dioxide is prepared by using titanium dioxide as the core material, sodium silicate as the coating material, and sodium hexametaphosphate as the dispersant. Coating the surface of titanium dioxide with a layer of SiO2 film can significantly improve the dispersion stability and ultraviolet absorption performance of titanium dioxide.
[0025] Furthermore, the mass ratio of titanium dioxide to deionized water is 1:(40-50).
[0026] Furthermore, the mass of the sodium hexametaphosphate is 0.6-0.8 times the mass of the titanium dioxide.
[0027] Furthermore, the mass of the sodium silicate solution is 6-8 times the mass of the titanium dioxide, and its concentration is 0.5-0.8 mol / L.
[0028] Furthermore, the concentration of the sodium hydroxide solution is 0.8-1.0 mol / L.
[0029] Furthermore, the concentration of the hydrochloric acid solution is 0.10-0.12 mol / L.
[0030] Furthermore, the coaxial electrospinning process conditions in step S3 are as follows: spinning voltage 16-18kV, distance between coaxial needle and receiver 12-18cm, core layer spinning solution propulsion speed 0.5-0.8mL / h, shell layer spinning solution propulsion speed 3-4mL / h, roller speed 300-400r / min, spinning temperature 25-40℃, and spinning time 2-3h.
[0031] The phase change temperature-regulating fiber prepared by the aforementioned method.
[0032] Temperature-regulating fabric prepared using the aforementioned phase change temperature-regulating fiber.
[0033] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0034] 1. This invention discloses a phase change temperature-regulating fiber. By compounding polyethylene glycol of different molecular weights, a core spinning solution with a phase change temperature of 26-35°C is obtained. This solution can absorb or release heat when the temperature changes, helping to maintain a comfortable body temperature. An organic-inorganic hybrid polymer with siloxy functional groups is successfully synthesized through in-situ polymerization and used as a support material. This combines the softness of organic materials with the strength and heat resistance of inorganic materials. Titanium dioxide is added to the shell to improve the ultraviolet shielding effect. Polyethylene glycol is encapsulated in the shell as a core layer through a coaxial electrospinning process to obtain a core-shell phase change temperature-regulating fiber. Using these fibers, textiles with temperature-regulating functions can be produced, providing a comfortable wearing experience.
[0035] 2. This invention discloses a phase change temperature-regulating fiber, using titanium dioxide as the core material, sodium silicate as the coating material, and sodium hexametaphosphate as the dispersant. A SiO2 film is coated onto the surface of titanium dioxide, significantly improving its dispersion stability and UV absorption performance. Simultaneously, the amino groups in the organic-inorganic hybrid polymer (supporting material) containing amino and siloxy functional groups react with the hydroxyl groups on the coated titanium dioxide surface, thereby enhancing the interaction between titanium dioxide and the supporting material, improving the stability of titanium dioxide and the bonding strength with the supporting material. This not only improves the UV resistance and antibacterial properties of the shell spinning solution but also enhances the fiber's abrasion resistance and weather resistance, making the phase change temperature-regulating fiber more durable and suitable for various environments. Detailed Implementation
[0036] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0037] In this embodiment, polyethylene glycol (PEG-800, PEG-1000, PEG-1500) is sourced from Nanjing Yingguan New Materials Technology Co., Ltd.; titanium dioxide (anatase type, particle size 5-15nm) is sourced from Nanjing Baoket New Materials Co., Ltd.
[0038] Example 1: A method for preparing phase change temperature-regulating fibers, comprising the following processes:
[0039] Step S1: Mix 10g PEG-800, 1.5g PEG-1000 and 1g PEG-1500, heat to 40℃, stir evenly, and obtain the core layer spinning solution.
[0040] Step S2: Under nitrogen protection, 10g of 4-vinylaniline, 3g of organosilicon containing double bonds, and 30g of chloroform are mixed evenly, and 0.02g of azobisisobutyronitrile is added dropwise. The mixture is heated to 75℃ and stirred for 10h. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. 10g of the support material, 1g of titanium dioxide, and 40g of N,N-dimethylformamide are mixed, heated to 40℃, and stirred evenly to obtain the shell spinning solution.
[0041] Step S3: Inject the core spinning solution and the shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process (spinning voltage 16kV, coaxial needle and receiver distance 12cm, core spinning solution feed speed 0.5mL / h, shell spinning solution feed speed 3mL / h, roller speed 300r / min, spinning temperature 25℃, spinning time 2h).
[0042] The preparation method of the organosilicon containing double bonds in step S2 is as follows:
[0043] 0.1g of potassium hydroxide and 18g of octamethylcyclotetrasiloxane were mixed evenly, heated to 80℃, and reacted for 1h. Then, a mixed solution of 3g of 3-methacryloyloxypropyltris(methoxyethoxy)silane, 1g of dimethyl sulfoxide, and 0.1g of hexamethylsiloxane was added, stirred evenly, and reacted for another 3h. After vacuum distillation and drying, organosilicon containing double bonds was obtained.
[0044] In step S2, the titanium dioxide undergoes a modification treatment, the specific process of which is as follows:
[0045] 1g of titanium dioxide was dispersed in 40g of deionized water and stirred until homogeneous. 0.6g of sodium hexametaphosphate was added, and the mixture was ultrasonically stirred for 30min. The mixture was then heated to 70℃, and the pH of the system was adjusted to 9 with 0.8mol / L sodium hydroxide solution. 6g of 0.5mol / L sodium silicate solution was added dropwise, and the pH of the system was adjusted to 7 with 0.1mol / L hydrochloric acid solution. The temperature was raised to 85℃ and maintained for 1h. After cooling to room temperature, the modified titanium dioxide was obtained by filtration, washing, and drying.
[0046] Example 2: A method for preparing phase change temperature-regulating fiber, comprising the following processes:
[0047] Step S1: Mix 10g PEG-800, 1.8g PEG-1000 and 1.2g PEG-1500, heat to 45℃, stir evenly, and the core layer spinning solution is obtained.
[0048] Step S2: Under nitrogen protection, 10g of 4-vinylaniline, 4g of organosilicon containing double bonds, and 35g of chloroform are mixed evenly, and 0.03g of azobisisobutyronitrile is added dropwise. The mixture is heated to 80℃ and stirred for 11h. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. 11g of the support material, 1g of titanium dioxide, and 50g of N,N-dimethylformamide are mixed, heated to 45℃, and stirred evenly to obtain the shell spinning solution.
[0049] Step S3: Inject the core spinning solution and shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process (spinning voltage 17kV, coaxial needle and receiver distance 15cm, core spinning solution feed rate 0.6mL / h, shell spinning solution feed rate 3.5mL / h, roller speed 350r / min, spinning temperature 30℃, spinning time 2.5h).
[0050] The preparation method of the organosilicon containing double bonds in step S2 is as follows:
[0051] 0.1g of potassium hydroxide and 19g of octamethylcyclotetrasiloxane were mixed evenly, heated to 85℃, and reacted for 1.5h. Then, a mixed solution of 3g of 3-methacryloyloxypropyltris(methoxyethoxy)silane, 1.5g of dimethyl sulfoxide, and 0.15g of hexamethylsiloxane was added, stirred evenly, and reacted for another 3.5h. After vacuum distillation and drying, organosilicon containing double bonds was obtained.
[0052] In step S2, the titanium dioxide undergoes a modification treatment, the specific process of which is as follows:
[0053] 1g of titanium dioxide was dispersed in 45g of deionized water and stirred evenly. 0.7g of sodium hexametaphosphate was added, and the mixture was ultrasonically stirred for 40min. The mixture was heated to 75℃, and the pH of the system was adjusted to 9.5 with 0.9mol / L sodium hydroxide solution. 7g of 0.6mol / L sodium silicate solution was added dropwise, and the pH of the system was adjusted to 7.5 with 0.11mol / L hydrochloric acid solution. The temperature was raised to 88℃ and kept at that temperature for 1.5h. After cooling to room temperature, the modified titanium dioxide was obtained by filtration, washing, and drying.
[0054] Example 3: A method for preparing phase change temperature-regulating fibers, comprising the following processes:
[0055] Step S1: Mix 10g PEG-800, 2g PEG-1000 and 1.5g PEG-1500, heat to 50℃, stir evenly to obtain core spinning solution;
[0056] Step S2: Under nitrogen protection, 10g of 4-vinylaniline, 5g of organosilicon containing double bonds, and 40g of chloroform are mixed evenly, and 0.04g of azobisisobutyronitrile is added dropwise. The mixture is heated to 85℃ and stirred for 12h. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. 12g of the support material, 1g of titanium dioxide, and 50g of N,N-dimethylformamide are mixed, heated to 50℃, and stirred evenly to obtain the shell spinning solution.
[0057] Step S3: Inject the core spinning solution and the shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process (spinning voltage 16-18kV, coaxial needle and receiver distance 18cm, core spinning solution feed speed 0.8mL / h, shell spinning solution feed speed 4mL / h, roller speed 300-400r / min, spinning temperature 40℃, spinning time 3h).
[0058] The preparation method of the organosilicon containing double bonds in step S2 is as follows:
[0059] 0.1g of potassium hydroxide and 20g of octamethylcyclotetrasiloxane were mixed evenly, heated to 90℃, and reacted for 2h. Then, a mixed solution of 3g of 3-methacryloyloxypropyltris(methoxyethoxy)silane, 2g of dimethyl sulfoxide and 0.2g of hexamethylsiloxane was added, stirred evenly, and reacted for another 4h. After vacuum distillation and drying, organosilicon containing double bonds was obtained.
[0060] In step S2, the titanium dioxide undergoes a modification treatment, the specific process of which is as follows:
[0061] 1g of titanium dioxide was dispersed in 50g of deionized water and stirred until homogeneous. 0.8g of sodium hexametaphosphate was added, and the mixture was ultrasonically stirred for 50min. The mixture was then heated to 80℃, and the pH of the system was adjusted to 10 with 1.0mol / L sodium hydroxide solution. 8g of 0.8mol / L sodium silicate solution was added dropwise, and the pH of the system was adjusted to 8 with 0.12mol / L hydrochloric acid solution. The temperature was raised to 90℃ and maintained for 2h. After cooling to room temperature, the modified titanium dioxide was obtained by filtration, washing, and drying.
[0062] Comparative Example 1: A method for preparing phase change temperature-regulating fibers, comprising the following processes:
[0063] Step S1: Mix 4g PEG-800, 4g PEG-1000 and 4g PEG-1500, heat to 45℃, stir evenly, and obtain the core layer spinning solution.
[0064] Step S2: Under nitrogen protection, 10g of 4-vinylaniline, 4g of organosilicon containing double bonds, and 35g of chloroform are mixed evenly, and 0.03g of azobisisobutyronitrile is added dropwise. The mixture is heated to 80℃ and stirred for 11h. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. 11g of the support material, 1g of titanium dioxide, and 50g of N,N-dimethylformamide are mixed, heated to 45℃, and stirred evenly to obtain the shell spinning solution.
[0065] Step S3: Inject the core spinning solution and shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process (spinning voltage 17kV, coaxial needle and receiver distance 15cm, core spinning solution feed rate 0.6mL / h, shell spinning solution feed rate 3.5mL / h, roller speed 350r / min, spinning temperature 30℃, spinning time 2.5h).
[0066] Compared with Example 2, in step S1 of Comparative Example 1, the mass ratio of PEG-800, PEG-1000, and PEG-1500 is 1:1:1; the other steps are the same as in Example 2.
[0067] Comparative Example 2: A method for preparing phase change temperature-regulating fiber, comprising the following processes:
[0068] Step S1: Mix 10g PEG-800, 1.8g PEG-1000 and 1.2g PEG-1500, heat to 45℃, stir evenly, and the core layer spinning solution is obtained.
[0069] Step S2: Under nitrogen protection, 10g of 4-vinylaniline, 4g of organosilicon containing double bonds, and 35g of chloroform are mixed evenly, and 0.03g of azobisisobutyronitrile is added dropwise. The mixture is heated to 80℃ and stirred for 11h. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. 11g of the support material, 0.5g of titanium dioxide, and 50g of N,N-dimethylformamide are mixed, heated to 45℃, and stirred evenly to obtain the shell spinning solution.
[0070] Step S3: Inject the core spinning solution and shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process (spinning voltage 17kV, coaxial needle and receiver distance 15cm, core spinning solution feed rate 0.6mL / h, shell spinning solution feed rate 3.5mL / h, roller speed 350r / min, spinning temperature 30℃, spinning time 2.5h).
[0071] Compared with Example 2, 0.5g of titanium dioxide was added in step S2 of Comparative Example 2; the other steps were the same as in Example 2.
[0072] Comparative Example 3: A method for preparing phase change temperature-regulating fibers, comprising the following processes:
[0073] Step S1: Mix 10g PEG-800, 1.8g PEG-1000 and 1.2g PEG-1500, heat to 45℃, stir evenly, and the core layer spinning solution is obtained.
[0074] Step S2: Mix 11g of polyamide, 1g of titanium dioxide and 50g of N,N-dimethylformamide, heat to 45℃ and stir evenly to obtain the shell spinning solution;
[0075] Step S3: Inject the core spinning solution and shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process (spinning voltage 17kV, coaxial needle and receiver distance 15cm, core spinning solution feed rate 0.6mL / h, shell spinning solution feed rate 3.5mL / h, roller speed 350r / min, spinning temperature 30℃, spinning time 2.5h).
[0076] Compared with Example 2, Comparative Example 3 does not include the preparation method of double-bonded organosilicon in step S2, and the supporting material is replaced with polyamide (PA66, from Yuyao Huali Nylon Technology Co., Ltd.); the other steps are the same as in Example 2.
[0077] Comparative Example 4: A method for preparing phase change temperature-regulating fiber, comprising the following processes:
[0078] The preparation method of the organosilicon containing double bonds in step S2 is as follows:
[0079] 0.1g of potassium hydroxide and 19g of octamethylcyclotetrasiloxane were mixed evenly, heated to 85℃, and reacted for 1.5h. Then, a mixed solution of 3g of 3-methacryloyloxypropyltris(methoxyethoxy)silane, 3g of dimethyl sulfoxide, and 3g of hexamethylsiloxane was added, stirred evenly, and reacted for another 3.5h. After vacuum distillation and drying, organosilicon containing double bonds was obtained.
[0080] Compared with Example 2, the mass ratio of 3-methacryloyloxypropyltris(methoxyethoxy)silane, dimethyl sulfoxide, and hexamethylsiloxane in Comparative Example 4 was 1:1:1; other steps were the same as in Example 2.
[0081] Experiment: The phase change temperature-regulating fibers obtained in Examples 1-3 and Comparative Examples 1-4 were used to prepare samples. Their properties were tested and the test results were recorded.
[0082] Tensile properties test: The test was conducted using an XLB yarn tensile strength tester with a pre-tension of 0.05 cN / dtex, a clamping distance of 250 mm, and a tensile speed of 500 mm / min. The elongation at break was calculated.
[0083] DSC test: The phase change performance of the sample was tested using a differential scanning calorimeter. 10mg of phase change temperature-regulating fiber was used as the sample. N2 was used as the protective gas with a flow rate of 30mL / min. The heating and cooling range was -20-120℃, and the heating and cooling rate was 10℃ / min.
[0084] Test Results
[0085] Elongation at break / % Phase transition J / g Phase transition temperature / °C Example 1 24.6 161.8 31.8 Example 2 25.5 174.6 34.6 Example 3 25.2 167.5 33.2 Comparative Example 1 21.7 192.3 45.2 Comparative Example 2 20.3 156.2 29.5 Comparative Example 3 18.4 140.7 24.3 Comparative Example 4 22.9 170.4 32.7
[0086] Based on the data in the table above, the following conclusions can be clearly drawn:
[0087] 1. Compared with Examples 1-3, the phase change saturation and phase change temperature of the product obtained in Comparative Example 1 are both increased, which does not meet the requirements of human comfort. It can be seen that the phase change temperature regulating fiber prepared by the present invention is affected by the ratio of each reagent in its preparation process. By selecting the mass ratio within the range mentioned above, a more comfortable phase change temperature regulating fiber can be prepared.
[0088] 2. Compared with Examples 1-3, the elongation at break, phase transition temperature, and phase transition temperature of the products obtained in Comparative Examples 2 and 3 all changed, indicating that the present invention can improve the mechanical properties and stability of the shell spinning solution by effectively combining titanium dioxide with the support material, thereby improving the comprehensive performance of the phase change temperature-regulating fiber.
[0089] 3. Compared with Examples 1-3, the breaking elongation, phase transition elongation, and phase transition temperature of the product obtained in Comparative Example 4 all changed, indicating that the performance of the double-bonded organosilicon prepared by the present invention is affected by the ratio of each reagent in its preparation process. By selecting the mass ratio within the range described above, better phase transition temperature-regulating fibers can be obtained.
[0090] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process method article or apparatus.
[0091] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A method for preparing phase change temperature-regulating fibers, characterized in that: Includes the following steps: Step S1: Mix polyethylene glycols of different molecular weights, heat to 40-50℃, stir evenly, and then prepare the core spinning solution. Step S2: Under nitrogen protection, 4-ethyleneaniline, organosilicon containing double bonds, and chloroform are mixed evenly, and azobisisobutyronitrile is added dropwise. The mixture is heated to 75-85℃ and stirred for 10-12 hours. After cooling to room temperature, the mixture is filtered and dried to obtain the support material. The support material, titanium dioxide, and N,N-dimethylformamide are mixed, heated to 40-50℃, and stirred evenly to obtain the shell spinning solution. Step S3: Inject the core spinning solution and the shell spinning solution into the syringe respectively, and prepare phase change temperature-regulating fibers by coaxial electrospinning process; The preparation method of the double-bonded organosilicon in step S2 is as follows: Potassium hydroxide and octamethylcyclotetrasiloxane were mixed evenly and heated to 80-90℃. The reaction was carried out for 1-2 hours. A mixed solution of 3-methacryloyloxypropyltris(methoxyethoxy)silane, dimethyl sulfoxide and hexamethylsiloxane was added. After stirring evenly, the reaction was continued for 3-4 hours. After vacuum distillation and drying, organosilicon containing double bonds was obtained. In step S2, the titanium dioxide undergoes a modification treatment, the specific process of which is as follows: Titanium dioxide was dispersed in deionized water and stirred evenly. Sodium hexametaphosphate was added and ultrasonically stirred for 30-50 minutes. The mixture was heated to 70-80℃, and the pH of the system was adjusted to 9-10 with sodium hydroxide solution. Sodium silicate solution was added dropwise, and the pH of the system was adjusted to 7-8 with hydrochloric acid solution. The temperature was raised to 85-90℃ and kept at that temperature for 1-2 hours. The mixture was then cooled to room temperature, filtered, washed, and dried to obtain modified titanium dioxide.
2. The method for preparing a phase change temperature-regulating fiber according to claim 1, characterized in that: In step S1, the polyethylene glycol is PEG-800, PEG-1000, or PEG-1500, and the mass ratio is 1:(0.15-0.20):(0.10-0.15).
3. The method for preparing a phase change temperature-regulating fiber according to claim 1, characterized in that: In step S2, the mass ratio of 4-vinylaniline and organosilicon containing double bonds to chloroform is 1:(0.3-0.5):(3-4).
4. The method for preparing a phase change temperature-regulating fiber according to claim 1, characterized in that: In step S2, the mass ratio of titanium dioxide to the supporting material is 1:(10-12).
5. The method for preparing a phase change temperature-regulating fiber according to claim 1, characterized in that: The mass ratio of 3-methacryloyloxypropyltris(methoxyethoxy)silane, dimethyl sulfoxide, and hexamethylsiloxane is 3:(1-2):(0.1-0.2).
6. The method for preparing a phase change temperature-regulating fiber according to claim 1, characterized in that: The coaxial electrospinning process conditions in step S3 are as follows: spinning voltage 16-18kV, distance between coaxial needle and receiver 12-18cm, core layer spinning solution propulsion speed 0.5-0.8mL / h, shell layer spinning solution propulsion speed 3-4mL / h, roller speed 300-400r / min, spinning temperature 25-40℃, and spinning time 2-3h.
7. A phase change temperature-regulating fiber prepared by the preparation method according to any one of claims 1-6.
8. The application of a phase change temperature-regulating fiber according to claim 7, characterized in that: Phase change temperature-regulating fibers are used to prepare temperature-regulating fabrics.