Preparation method of multifunctional temperature-regulating fiber

Abstract

The invention provides a preparation method of multifunctional temperature-regulating fibers. The preparation method comprises the following steps: dispersing silicon dioxide coated polyethylene glycol phase-change microcapsules into a polyethylene matrix; the preparation method comprises the following steps: dispersing nano powder capable of absorbing light and generating heat into polyester and polyamide matrixes; the multifunctional composite fiber with light absorption, heating, cool feeling and antibacterial functions is prepared through a skin-core composite spinning method. The functional fiber prepared by the invention has both heating and cooling properties and has excellent contact antibacterial and photo-thermal rapid sterilization capabilities, and the prepared fabric has good breaking strength, weaving characteristic and excellent washability.

Description

Technical Field

[0001] The present application relates to the technical field of composite functional fiber manufacturing, and in particular to a method for preparing a multifunctional temperature regulating fiber. Background Art

[0002] Current thermal regulation textiles generally achieve functions such as heating, heat preservation and cooling by coating photothermal functional materials on the fiber surface.

[0003] Currently, common photothermal materials are mainly divided into inorganic nanomaterials (such as copper oxide, iron oxide, vanadium dioxide, etc.) and organic materials (carbon nanotubes, graphene, etc.). Coating methods, composite fiber methods and doping methods are usually used to give textiles thermal regulation functions. For example, the invention patent CN118065146A involves intelligent temperature control fabrics, which achieve infrared radiation regulation by coating the surface of the fabric with mesoporous zirconium phosphate wrapped with vanadium dioxide to give the fabric light absorption and heating function. However, although the coating method is simple, it has poor durability and affects comfort; for example, the invention patent CN118007266A involves blending wormwood quercetin powder and nano-titanium dioxide with polyester to prepare functional masterbatch and melt-spinning composite wormwood modified polyester fiber. The composite fiber method improves durability and comfort, but the process is complicated, the cost is high and the dispersibility is poor. In addition, plant extracts such as wormwood have poor heat resistance and continuous production conditions are harsh; for example, the invention patent CN112501922A discloses a heat storage and thermal insulation fabric and its preparation method. The fabric contains phase change microcapsules, which can adjust the material's absorption of heat energy according to the ambient temperature to maintain the temperature of the fabric stable. However, this phase change material has the risk of phase change loss, resulting in unstable heat storage and thermal insulation effects of the fabric, poor durability and easy reduction of fiber performance; for example, the invention patent CN 117586755A discloses a method for preparing a refrigerant material, wherein a rare earth compound, a borate aqueous solution and a metal hydroxide are mixed and reacted under high pressure and high temperature to prepare a rare earth-boron refrigerant material, and the rare earth-boron refrigerant material is given a cooling function by coating the textile. The preparation process is complicated and the raw materials are expensive, and the material can only be given a single cooling function, and is not very applicable in actual production.

[0004] It is difficult to prepare a thermally regulating textile with relatively balanced performance in terms of durability, warmth retention and preparation process with existing technology. Summary of the invention

[0005] The present application provides a method for preparing a multifunctional temperature-regulating fiber, which can be used to solve the problem that the material has high light absorption and heat generation, cooling feeling, antibacterial and bactericidal properties, and has good breaking strength, weaving characteristics and excellent washability.

[0006] A method for preparing a multifunctional temperature regulating fiber comprises the following steps:

[0007] Polyethylene glycol phase change microcapsules coated with silicon dioxide are dispersed in a polyethylene matrix; nanopowders with light absorption and heat generation are dispersed in a polyester and polyamide matrix; and a multi-functional composite fiber with light absorption and heat generation, cooling and antibacterial functions is prepared by a skin-core composite spinning method. The functional fiber prepared by the present invention has both heating and cooling properties, and has excellent contact antibacterial and photothermal rapid sterilization capabilities. The prepared fabric has good breaking strength, weaving characteristics and excellent washability.

[0008] Furthermore, the preparation method of the multifunctional temperature regulating fiber specifically comprises the following steps:

[0009] Step 1, dispersing the phase change microcapsules of polyethylene glycol coated with silica in a polyethylene matrix, wherein the polyethylene matrix is ​​crushed particles, and the mass ratio of the phase change microcapsules to the polyethylene is 40:60, mixing them evenly by vacuum kneading and then crushing them into powder, and then granulating and slicing them through a twin-screw extruder to obtain a polyethylene phase change masterbatch;

[0010] Step 2, dispersing the light-absorbing and heat-generating nanopowder into a polyester or polyamide matrix through a twin-screw extruder, wherein the mass ratio of the light-absorbing and heat-generating nanopowder to the matrix is ​​20-30:70-80, to obtain a light-absorbing and heat-generating masterbatch;

[0011] Step 3, mixing S1 polyethylene phase change masterbatch with polyethylene and S2 light-absorbing heat-generating masterbatch with polyester or polyamide matrix, respectively, and extruding them through the first screw and the second screw, and then spinning, cooling, oiling, winding and collecting through the sheath-core spinning assembly to obtain the multifunctional temperature regulating fiber.

[0012] Preferably, in step 1, the phase change component in the phase change microcapsule is polyethylene glycol, and its molecular weight is 3000-6000 g / mol.

[0013] Preferably, in step 1, the content of polyethylene glycol in the microcapsule is 10 to 30 wt%.

[0014] Preferably, in step 1, the particle size of the silicon dioxide is 500 to 800 nm.

[0015] Preferably, in step 1, the particle size of the polyethylene powder is 6 to 20 μm, the kneading temperature is 80 to 120° C., and the kneading time is 6 to 12 hours.

[0016] Preferably, in step 2, the light-absorbing and heat-generating nanopowder is one or more of cesium tungsten bronze nanoparticles, copper sulfide, cuprous sulfide, and carbon nanotubes, with a particle size of 300 to 600 nm, the polyester matrix is ​​polybutylene terephthalate or polyethylene terephthalate, and the polyamide matrix is ​​nylon 6, nylon 56, or nylon 66.

[0017] Preferably, in step 3, the heating temperature of the first screw extruder is 160-180°C, and the heating temperature of the second screw extruder is 220-290°C.

[0018] Preferably, in step 3, the polyethylene masterbatch is added in an amount of 20 to 40 wt%, and the light-absorbing heat-generating masterbatch is added in an amount of 10 to 25 wt%.

[0019] Preferably, in step 3, the winding speed is 3200-4000 m / min, the heat setting temperature is 100-120° C.; and the drafting multiple is 1.5-3.5 times.

[0020] The beneficial effects of the present invention are:

[0021] Functional particles are evenly dispersed: By combining silica coating technology and vacuum mixing and crushing technology, the dispersion uniformity of phase change microcapsules in the polyethylene substrate is improved, thereby increasing the loading amount of phase change materials in polymer masterbatch and textiles, and improving the thermal storage performance of textiles.

[0022] Excellent temperature regulation function: through the fiber skin-core structure design, the textile can heat up and cool down at the same time according to the light and heat changes in the use environment.

[0023] Excellent cooling properties: The surface polyamide material itself has an excellent cooling effect, and the core polyethylene material has a fast thermal conductivity and works synergistically with the phase change material to achieve rapid thermal conductivity, giving the fabric an excellent cooling effect.

[0024] Excellent mechanical properties and batch production capabilities: The sheath-core hollow fiber prepared by the melt spinning method has good chemical stability, can maintain its photothermal performance under different environmental conditions, and is not easily affected by external factors such as humidity and temperature. It has both efficient photothermal heating and cooling functions, and maintains good breaking strength and weaving characteristics. At the same time, the fiber's washability is also significantly improved, which increases its service life.

[0025] Excellent antibacterial properties: Nanomaterials have a high photothermal conversion efficiency and can effectively convert the absorbed light energy into heat energy to achieve rapid heating. They cooperate with the ion contact antibacterial mechanism of metal oxides and can carry out broad-spectrum antibacterial sterilization. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 A flow chart of the method provided in an embodiment of the present application.

[0027] Figure 2 This is a comparison chart of the average temperature rise of the embodiment provided in the present application and the comparative example before and after washing for 20 minutes.

[0028] Figure 3This is a comparison chart of the cooling performance test before and after washing of the embodiments and comparative examples provided in the present application.

[0029] Figure 4 This is a comparison chart of the Escherichia coli antibacterial test bacterial discs after washing between Example C1 and Comparative Example γ1 provided in the embodiments of the present application. DETAILED DESCRIPTION

[0030] In order to make the objectives, technical solutions and advantages of the present application clearer, the implementation methods of the present application will be further described in detail below with reference to the accompanying drawings.

[0031] The present invention adopts the following test methods to test the heating performance, breaking strength and washability:

[0032] Temperature rise performance: Under the conditions of temperature of (20±2)℃ and relative humidity of (65±2)%, use XR-3 light thermal storage performance tester and xenon arc lamp as the irradiation light source. Place the sample under a certain irradiation intensity. The sample absorbs light energy and causes the temperature to change. Use a temperature sensor to test the sample temperature. Record the temperature change of the sample at each time point within 10 minutes of irradiation and 10 minutes of turning off the light source. Calculate the maximum temperature rise value, average temperature rise value and test endpoint temperature rise value of the sample within 20 minutes.

[0033] Cooling performance: Test the cooling coefficient according to GB / T35263-2017, compare with the standard of Q-MAX≥0.15, and evaluate the instantaneous cooling effect of the material.

[0034] Washability: The multifunctional thermostatic fiber was tested for 50 wash cycles using a standard washing machine and a phosphorus-free detergent, and the sample was dried after each wash. After every 10 washes, the breaking strength of the sample was tested using a tensile testing machine according to the ASTM D2256 standard, and its photothermal heating performance was evaluated. The test results showed that after 50 washes, the photothermal heating and cooling properties of the fiber remained at a high level, indicating that the fiber has good washability.

[0035] Antibacterial performance: The antibacterial performance of textiles was tested in accordance with GB / T 20944.3 standard, and the comparison standard required an antibacterial effect of >70%.

[0036] Example 1

[0037] (1) 4 kg of phase change microcapsules of 500 nm silica coated with 3000 g / mol molecular weight polyethylene glycol were dispersed in 6 kg of polyethylene 6 μm powder, crushed and kneaded at 80° C. in a vacuum environment for 6 h, and then granulated by a twin-screw granulator at a heating temperature of 160° C. to obtain polyethylene phase change masterbatch A1;

[0038] (2) 2 kg of cuprous sulfide mixed powder was dispersed in 8 kg of polyester matrix through a twin-screw extruder, and heated at 290° C. in a twin-screw granulator to obtain light-absorbing and heat-generating masterbatch B1;

[0039] (3) The polyethylene phase change masterbatch A1 is mixed with polyethylene at an addition amount of 20%, and the light-absorbing heat-generating masterbatch B1 is mixed with a polyester matrix at an addition amount of 10%, and the two are extruded through the first screw and the second screw respectively. The fibers are spun through a sheath-core spinning assembly, and the fibers are collected under the conditions of a winding speed of 3200 m / min, a heat setting temperature of 100°C, and a stretching multiple of 1.5 times to obtain the multifunctional temperature-regulating fiber C1.

[0040] Example 2

[0041] (1) 10 kg of phase change microcapsules of 550 nm silica coated with 4500 g / mol molecular weight polyethylene glycol were dispersed in 15 kg of 10 μm polyethylene powder, crushed and kneaded at 88° C. in a vacuum environment for 7 h, and then granulated by a twin-screw granulator at a heating temperature of 178° C. to obtain polyethylene phase change masterbatch A2;

[0042] (2) 6 kg of cuprous sulfide and carbon nanotubes were dispersed in 14 kg of polyamide 6 matrix through a twin-screw extruder, and then heated at 275° C. in a twin-screw granulator to obtain light-absorbing and heat-generating masterbatch B2;

[0043] (3) The polyethylene phase change masterbatch A2 is mixed with polyethylene at an addition amount of 40%, and the light-absorbing heat-generating masterbatch B2 is mixed with a polyamide 6 matrix at an addition amount of 25%, and the two are extruded through the first screw and the second screw respectively. The fibers are spun through a sheath-core spinning assembly, and the fibers are collected under the conditions of a winding speed of 3400 m / min, a heat setting temperature of 110°C, and a stretching multiple of 2.5 times to obtain the multifunctional temperature-regulating fiber C2.

[0044] Example 3

[0045] (1) 1.2 kg of phase change microcapsules of 720 nm silica coated with 5800 g / mol molecular weight polyethylene glycol were dispersed in 1.8 kg of polyethylene 18 μm particle powder, crushed and kneaded at 100 ° C in a vacuum environment for 10 h, and then granulated by a twin-screw granulator at a heating temperature of 180 ° C to obtain polyethylene phase change masterbatch A3;

[0046] (2) 2.5 kg of cesium tungsten bronze nanoparticles and carbon nanotubes mixed powder was dispersed in 7.5 kg of polyamide 56 matrix through a twin-screw extruder, and heated at 275° C. in a twin-screw granulator to obtain light-absorbing and heat-generating masterbatch B3;

[0047] (3) The polyethylene phase change masterbatch A3 is mixed with polyethylene at an addition amount of 30%, and the light-absorbing heat-generating masterbatch B3 is mixed with a polyamide 56 matrix at an addition amount of 16%, and the two are extruded through the first screw and the second screw respectively. The fibers are spun through a sheath-core spinning assembly, and the fibers are collected under the conditions of a winding speed of 3880 m / min, a heat setting temperature of 120°C, and a stretching multiple of 2.8 times to obtain the multifunctional temperature-regulating fiber C3.

[0048] Comparative Example 1

[0049] (1) 4 kg of phase change microcapsules of 500 nm silica coated with 3000 g / mol molecular weight polyethylene glycol were dispersed in 6 kg of polyethylene 6 μm powder, crushed and kneaded at 80° C. in a vacuum environment for 6 h, and then granulated by a twin-screw granulator at a heating temperature of 160° C. to obtain polyethylene phase change masterbatch α1;

[0050] (2) The polyethylene phase change masterbatch α1 is mixed with polyethylene and a polyester matrix at an addition amount of 20%, and the mixture is extruded through a first screw and a second screw respectively. The mixture is spun through a sheath-core spinning assembly, and the multifunctional temperature-regulating fiber γ1 is obtained after being collected under the conditions of a winding speed of 3200 m / min, a heat setting temperature of 100°C, and a stretching multiple of 1.5 times.

[0051] Comparative Example 2

[0052] (1) 2 kg of cuprous sulfide mixed powder is dispersed in 8 kg of polyester matrix through a twin-screw extruder, and heated at 290° C. in a twin-screw granulator to obtain light-absorbing and heat-generating masterbatch β2;

[0053] (3) Polyethylene chips and light-absorbing heat-generating masterbatch β2 are mixed with a polyester matrix at an addition amount of 10%, and the mixture is extruded through a first screw and a second screw respectively. The mixture is spun through a sheath-core spinning assembly, and the multifunctional temperature-regulating fiber γ2 is obtained after being collected under the conditions of a winding speed of 3200 m / min, a heat setting temperature of 100°C, and a stretching multiple of 1.5 times.

[0054] Please see Table 1 for the test results.

[0055] Table 1: Test results comparison table

[0056]

[0057] The above-described embodiments of the present application do not constitute a limitation on the protection scope of the present application.

Claims

1. A method for preparing a multifunctional temperature regulating fiber, characterized in that: The method comprises: Step S1, dispersing the phase change microcapsules of polyethylene glycol coated with silica in a polyethylene matrix; wherein the polyethylene matrix is ​​crushed particles, the mass ratio of the phase change microcapsules to the polyethylene is 40:60, and the mixture is evenly mixed by vacuum kneading and then crushed into powder, and then granulated and sliced ​​by a twin-screw extruder to obtain a polyethylene phase change masterbatch; Step S2, dispersing the light-absorbing heat-generating nanopowder into a polyester or polyamide matrix through a twin-screw extruder, wherein the mass ratio of the light-absorbing heat-generating nanopowder to the matrix is ​​20-30:70-80, to obtain a light-absorbing heat-generating masterbatch; Step S3, mixing S1 polyethylene phase change masterbatch with polyethylene and S2 light-absorbing heat-generating masterbatch with polyester or polyamide matrix, respectively, extruding through the first screw and the second screw, and spinning, cooling, oiling, winding and collecting through the sheath-core spinning assembly to obtain the multifunctional temperature-regulating fiber.

2. The method for preparing the multifunctional temperature regulating fiber according to claim 1, characterized in that: The phase change component in the phase change microcapsule described in step S1 is polyethylene glycol, with a molecular weight of 3000-6000 g / mol, a content of polyethylene glycol in the microcapsule of 10-30 wt%, a particle size of silicon dioxide of 500-800 nm, a particle size of polyethylene powder of 6-20 μm, a kneading temperature of 80-120° C., and a kneading time of 6-12 h.

3. The method for preparing the multifunctional temperature regulating fiber according to claim 1, characterized in that: The light-absorbing and heat-generating nanopowder described in step S2 is one or more of cesium tungsten bronze nanoparticles, copper sulfide, cuprous sulfide, and carbon nanotubes, with a particle size of 300 to 600 nm, the polyester matrix is ​​polybutylene terephthalate or polyethylene terephthalate, and the polyamide matrix is ​​nylon 6, nylon 56, or nylon 66.

4. The method for preparing the multifunctional temperature regulating fiber according to claim 1, characterized in that: The heating temperature of the first screw extruder in step S3 is 160-180°C, and the heating temperature of the second screw extruder is 220-290°C.

5. The method for preparing the multifunctional temperature regulating fiber according to claim 4, characterized in that: The addition amount of the polyethylene masterbatch prepared by S1 is 20-40wt%, and the addition amount of the light-absorbing and heat-generating masterbatch prepared by S2 is 10-25wt%.

6. The method for preparing a multifunctional temperature regulating fiber according to claim 4, characterized in that: In step 3, the winding speed is 3200-4000 m / min, the heat setting temperature is 100-120° C., and the drafting multiple is 1.5-3.5 times.

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