A light colour thermal fibre, a method of manufacture and use on a fabric
By introducing polyacrylonitrile-modified silica aerogel and cationic modified nano zinc oxide into polyacrylonitrile fibers, light-colored thermal insulation fibers were prepared, solving the problems of insufficient thermal insulation and antibacterial and antistatic properties, and achieving high-efficiency thermal insulation and excellent antibacterial and antistatic effects of the fibers.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- BOSIDENG DOWN WEAR LTD
- Filing Date
- 2026-01-21
- Publication Date
- 2026-05-01
AI Technical Summary
Existing polyacrylonitrile fibers have limitations in thermal insulation performance, making it difficult to meet the requirements of thermal insulation and heat preservation applications. Furthermore, the dispersion uniformity and interfacial bonding strength of silica aerogel in the matrix are insufficient, affecting its performance improvement.
Polyacrylonitrile-modified silica aerogel was used as a heat-insulating functional filler, combined with cationic modified nano zinc oxide as an antistatic and antibacterial agent, and light-colored polyacrylonitrile fibers were prepared by melt spinning to optimize the antibacterial and antistatic properties of the fibers.
It improves the thermal insulation performance of the fiber, optimizes the antibacterial and antistatic properties, and improves the dispersibility and compatibility of silica aerogel in the matrix.
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Figure CN121538751B_ABST
Abstract
Description
A light-colored thermal fiber, its preparation method, and its application in fabrics. Technical Field
[0001] This invention relates to the field of fiber technology, specifically to a light-colored warm fiber, its preparation method, and its application in fabrics. Background Technology
[0002] Acrylic fiber, also known as polyacrylonitrile (PAN) fiber, is commonly called artificial wool. It has a low thermal conductivity and excellent warmth retention. Because the homopolymer of acrylonitrile monomers has high crystallinity and poor elasticity and spinnability, polyacrylonitrile is copolymerized with second and third monomers (such as itaconic acid and methyl acrylate) to disrupt its regular structure and improve spinnability. Due to its excellent mechanical properties, superior thermal stability, and outstanding chemical resistance, polyacrylonitrile fiber has become an ideal matrix for developing thermal insulation fibers.
[0003] However, single polyacrylonitrile fibers have limitations in thermal insulation performance, making it difficult to meet the requirements of thermal insulation applications. Therefore, existing technologies improve the thermal insulation performance of polyacrylonitrile fibers by adding nanofillers. The thermal insulation mechanism of silica aerogel stems from its unique nanoporous structure, which synergistically inhibits heat transfer through multiple mechanisms. However, the uniformity of silica aerogel dispersion and the interfacial bonding strength with the matrix remain key challenges limiting its performance improvement.
[0004] Therefore, the preparation of a light-colored polyacrylonitrile fiber that provides heat insulation and warmth, while also possessing antibacterial and antistatic properties, has significant practical application value. Summary of the Invention
[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide a light-colored warm fiber, a preparation method, and its application in fabrics. It utilizes polyacrylonitrile-modified silica aerogel as a heat-insulating functional filler and cationic modified nano zinc oxide as an antistatic and antibacterial agent. Light-colored polyacrylonitrile fiber is prepared by melt spinning. The fiber has good heat insulation and warmth retention properties, and the antibacterial and antistatic properties of the fiber are optimized by introducing a cationic inorganic-organic composite antibacterial and antistatic agent.
[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0007] A method for preparing a light-colored thermal insulation fiber includes the following steps:
[0008] Step (1): Mix nano zinc oxide, ethanol, and water, disperse by ultrasonication, adjust the pH value, add KH560, react, after the reaction is completed, centrifuge to collect the precipitate, wash, dry, and obtain epoxidized nano zinc oxide;
[0009] Step (2): Mix epoxidized nano zinc oxide and methanol, disperse by ultrasonication, add propargylamine, react, filter, wash, and dry to obtain alkynylated nano zinc oxide;
[0010] Alkyne-modified nano-zinc oxide was mixed with methanol, ultrasonically dispersed, cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was subjected to light irradiation. After the reaction was completed, the mixture was filtered, washed, and dried to obtain cationic modified nano-zinc oxide.
[0011] Step (3): Mix polyacrylonitrile, polyacrylonitrile-modified silica aerogel, and cationic modified nano zinc oxide evenly, melt blend, extrude granulation, melt spin spinning, cool and stretch to obtain light-colored warm fiber.
[0012] Preferably, in step (1), the mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:8-20:8-20:0.1-0.3; the reaction conditions are: reacting at a pH of 8-9 and a temperature of 50-70℃ for 3-6 hours.
[0013] Preferably, in step (2), the mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:0.8-1.2:100; the reaction conditions are: stirring at room temperature for 60-84 hours.
[0014] Preferably, in step (2), the mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1-1.2:0.05-0.1:80-100; the photoreaction conditions are: photoreaction for 8-12 hours under ultraviolet light at a temperature of 20-30℃ and a wavelength of 365nm in a nitrogen atmosphere.
[0015] Preferably, in step (3): the mass ratio of polyacrylonitrile, polyacrylonitrile-modified silica aerogel, and cationic modified nano zinc oxide is 90-98:1-5:1-5; the melt spinning conditions are: spinning temperature is 180-190℃ in zone 1, 190-195℃ in zone 2, 200-210℃ in zone 3, and 210-220℃ in zone 4, spinning speed is 100-500m / min; drawing temperature is 110-120℃, and drawing ratio is 3-5 times.
[0016] Preferably, in step (3), the polyacrylonitrile-modified silica aerogel is prepared by the following steps:
[0017] S1. After soaking the silica aerogel in ethanol, remove it, transfer it to water, add vinyltriethoxysilane, disperse it by ultrasound, adjust the pH value, and react. After the reaction is completed, filter, wash, and dry to obtain vinylsilane modified silica aerogel.
[0018] S2. Mix acrylonitrile, ethanol, and water, add photoinitiator and vinylsilane-modified silica aerogel, disperse by ultrasonication, and react under light. After the reaction is complete, filter, wash, and dry to obtain polyacrylonitrile-modified silica aerogel.
[0019] Preferably, in step (3), when preparing polyacrylonitrile-modified silica aerogel, the mass ratio of silica aerogel, vinyltriethoxysilane, and water in S1 is 1-3:10:150-250; the reaction conditions are: stirring and reacting at pH 10 and 40-60℃ for 4-6 hours.
[0020] Preferably, in step (3), when preparing polyacrylonitrile-modified silica aerogel, the mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator in S2 is 17-20:30-40:1-1.5:4:1-2; the photoreaction conditions are: photoreaction for 2-5 hours under ultraviolet light at a temperature of 20-30℃ and a wavelength of 365nm.
[0021] Preferably, a light-colored thermal fiber is prepared using the method described above for preparing light-colored thermal fibers.
[0022] Preferably, an application of light-colored thermal fibers as described above on a fabric.
[0023] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0024] This invention utilizes polyacrylonitrile-modified silica aerogel as a heat-insulating functional filler and cationic modified nano zinc oxide as an antistatic and antibacterial agent. Light-colored polyacrylonitrile fibers are prepared by melt spinning. The fibers have good heat insulation and warmth retention properties. Furthermore, the introduction of cationic inorganic-organic composite antibacterial and antistatic agents optimizes the antibacterial and antistatic properties of the fibers.
[0025] To improve the interfacial compatibility between silica aerogel and polyacrylonitrile fiber matrix, this invention modifies silica aerogel with vinyltriethoxysilane and then polymerizes acrylonitrile monomer, introducing cyano groups. This improves the dispersibility and compatibility of the aerogel in the matrix, reduces the thermal conductivity of the fiber, and enhances its heat insulation effect. This invention also modifies the surface of nano-zinc oxide using the silane coupling agent KH560, introducing propargylamine through the reaction of epoxy and amino groups to prepare alkynylated nano-zinc oxide. Further, a thiol-alkynyl click reaction is initiated by the alkynyl group and cysteine hydrochloride under ultraviolet light to obtain cationic modified nano-zinc oxide with amino hydrochloride end groups. The organic antibacterial and antistatic components synergistically improve the antibacterial and antistatic properties of polyacrylonitrile fibers through the inorganic antibacterial and antistatic material nano-zinc oxide. Simultaneously, the formation of hydrogen bonds between the cations and the polyacrylonitrile matrix optimizes the dispersibility and compatibility of the nano-zinc oxide in the matrix. Attached Figure Description
[0026] Figure 1 is a bar chart of thermal conductivity in performance testing of Examples 1-5 and Comparative Examples 1-2 of the present invention;
[0027] Figure 2 is a line graph of the static voltage half-life of Examples 1-5 and Comparative Examples 1-2 in the performance test of the present invention;
[0028] Figure 3 is a bar chart showing the antibacterial rate of Examples 1-5 and Comparative Examples 1-2 in the performance test of this invention. Detailed Implementation
[0029] The present invention will be further illustrated below through specific embodiments. The following embodiments are specific implementations of the present invention, but the implementation of the present invention is not limited to the following embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and are included within the protection scope of the present invention.
[0030] Example 1
[0031] This embodiment discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0032] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0033] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0034] Step (2): Epoxidized nano zinc oxide and methanol are mixed and ultrasonically dispersed for 30 min. Propylene amine is added and the mixture is stirred and reacted at room temperature for 72 h. After the reaction is completed, the mixture is washed by ether filtration and dried at 50 °C for 12 h to obtain alkynylated nano zinc oxide.
[0035] The mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:0.8:100.
[0036] Alkyne-modified nano-zinc oxide was mixed with methanol and ultrasonically dispersed for 10 min. Cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was irradiated at room temperature for 10 h under a nitrogen atmosphere and ultraviolet light with a wavelength of 365 nm. After the reaction was completed, the mixture was washed by ether filtration and dried at 50 °C for 12 h to obtain cationic modified nano-zinc oxide.
[0037] The mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1-1.2:0.05-0.1:80-100.
[0038] Step (3): Polyacrylonitrile, polyacrylonitrile-modified silica aerogel and cationic modified nano zinc oxide are mixed evenly at a mass ratio of 98:1:1, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0039] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0040] The preparation of polyacrylonitrile-modified silica aerogel includes the following steps:
[0041] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0042] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0043] S2. Mix acrylonitrile, ethanol and water, add photoinitiator and vinylsilane modified silica aerogel, ultrasonically disperse for 2 hours, and react at room temperature under ultraviolet light with a wavelength of 365 nm for 4 hours. After the reaction is completed, wash with ethanol by vacuum filtration and dry at 50°C for 48 hours to obtain polyacrylonitrile modified silica aerogel.
[0044] The mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator is 17:30:1:4:1.
[0045] Example 2
[0046] This embodiment discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0047] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0048] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0049] Step (2): Epoxidized nano zinc oxide and methanol are mixed and ultrasonically dispersed for 30 min. Propylene amine is added and the mixture is stirred and reacted at room temperature for 72 h. After the reaction is completed, the mixture is washed by ether filtration and dried at 50 °C for 12 h to obtain alkynylated nano zinc oxide.
[0050] The mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:0.9:100.
[0051] Alkyne-modified nano-zinc oxide was mixed with methanol and ultrasonically dispersed for 10 min. Cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was irradiated at room temperature for 10 h under a nitrogen atmosphere and ultraviolet light with a wavelength of 365 nm. After the reaction was completed, the mixture was washed by ether filtration and dried at 50 °C for 12 h to obtain cationic modified nano-zinc oxide.
[0052] The mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1.05:0.08:90.
[0053] Step (3): Polyacrylonitrile, polyacrylonitrile-modified silica aerogel, and cationic modified nano zinc oxide are mixed evenly at a mass ratio of 96:2:2, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0054] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0055] The preparation of polyacrylonitrile-modified silica aerogel includes the following steps:
[0056] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0057] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0058] S2. Mix acrylonitrile, ethanol and water, add photoinitiator and vinylsilane modified silica aerogel, ultrasonically disperse for 2 hours, and react at room temperature under ultraviolet light with a wavelength of 365 nm for 4 hours. After the reaction is completed, wash with ethanol by vacuum filtration and dry at 50°C for 48 hours to obtain polyacrylonitrile modified silica aerogel.
[0059] The mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator is 17.5:35:1.3:4:1.5.
[0060] Example 3
[0061] This embodiment discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0062] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0063] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0064] Step (2): Epoxidized nano zinc oxide and methanol are mixed and ultrasonically dispersed for 30 min. Propylene amine is added and the mixture is stirred and reacted at room temperature for 72 h. After the reaction is completed, the mixture is washed by ether filtration and dried at 50 °C for 12 h to obtain alkynylated nano zinc oxide.
[0065] The mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:1:100.
[0066] Alkyne-modified nano-zinc oxide was mixed with methanol and ultrasonically dispersed for 10 min. Cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was irradiated at room temperature for 10 h under a nitrogen atmosphere and ultraviolet light with a wavelength of 365 nm. After the reaction was completed, the mixture was washed by ether filtration and dried at 50 °C for 12 h to obtain cationic modified nano-zinc oxide.
[0067] The mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1.1:0.08:90.
[0068] Step (3): Polyacrylonitrile, polyacrylonitrile-modified silica aerogel and cationic modified nano zinc oxide are mixed evenly in a mass ratio of 94:3:3, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0069] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0070] The preparation of polyacrylonitrile-modified silica aerogel includes the following steps:
[0071] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0072] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0073] S2. Mix acrylonitrile, ethanol and water, add photoinitiator and vinylsilane modified silica aerogel, ultrasonically disperse for 2 hours, and react at room temperature under ultraviolet light with a wavelength of 365 nm for 4 hours. After the reaction is completed, wash with ethanol by vacuum filtration and dry at 50°C for 48 hours to obtain polyacrylonitrile modified silica aerogel.
[0074] The mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator is 18.5:35:1.3:4:1.5.
[0075] Example 4
[0076] This embodiment discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0077] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0078] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0079] Step (2): Epoxidized nano zinc oxide and methanol are mixed and ultrasonically dispersed for 30 min. Propylene amine is added and the mixture is stirred and reacted at room temperature for 72 h. After the reaction is completed, the mixture is washed by ether filtration and dried at 50 °C for 12 h to obtain alkynylated nano zinc oxide.
[0080] The mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:1.1:100.
[0081] Alkyne-modified nano-zinc oxide was mixed with methanol and ultrasonically dispersed for 10 min. Cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was irradiated at room temperature for 10 h under a nitrogen atmosphere and ultraviolet light with a wavelength of 365 nm. After the reaction was completed, the mixture was washed by ether filtration and dried at 50 °C for 12 h to obtain cationic modified nano-zinc oxide.
[0082] The mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1.15:0.08:90.
[0083] Step (3): Polyacrylonitrile, polyacrylonitrile-modified silica aerogel, and cationic modified nano zinc oxide are mixed evenly at a mass ratio of 92:4:4, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0084] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0085] The preparation of polyacrylonitrile-modified silica aerogel includes the following steps:
[0086] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0087] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0088] S2. Mix acrylonitrile, ethanol and water, add photoinitiator and vinylsilane modified silica aerogel, ultrasonically disperse for 2 hours, and react at room temperature under ultraviolet light with a wavelength of 365 nm for 4 hours. After the reaction is completed, wash with ethanol by vacuum filtration and dry at 50°C for 48 hours to obtain polyacrylonitrile modified silica aerogel.
[0089] The mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator is 19.5:35:1.3:4:1.5.
[0090] Example 5
[0091] This embodiment discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0092] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0093] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0094] Step (2): Epoxidized nano zinc oxide and methanol are mixed and ultrasonically dispersed for 30 min. Propylene amine is added and the mixture is stirred and reacted at room temperature for 72 h. After the reaction is completed, the mixture is washed by ether filtration and dried at 50 °C for 12 h to obtain alkynylated nano zinc oxide.
[0095] The mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:1.2:100.
[0096] Alkyne-modified nano-zinc oxide was mixed with methanol and ultrasonically dispersed for 10 min. Cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was irradiated at room temperature for 10 h under a nitrogen atmosphere and ultraviolet light with a wavelength of 365 nm. After the reaction was completed, the mixture was washed by ether filtration and dried at 50 °C for 12 h to obtain cationic modified nano-zinc oxide.
[0097] The mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1.2:0.1:100.
[0098] Step (3): Polyacrylonitrile, polyacrylonitrile-modified silica aerogel and cationic modified nano zinc oxide are mixed evenly at a mass ratio of 90:5:5, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0099] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0100] The preparation of polyacrylonitrile-modified silica aerogel includes the following steps:
[0101] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0102] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0103] S2. Mix acrylonitrile, ethanol and water, add photoinitiator and vinylsilane modified silica aerogel, ultrasonically disperse for 2 hours, and react at room temperature under ultraviolet light with a wavelength of 365 nm for 4 hours. After the reaction is completed, wash with ethanol by vacuum filtration and dry at 50°C for 48 hours to obtain polyacrylonitrile modified silica aerogel.
[0104] The mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator is 20:40:1.5:4:2.
[0105] Comparative Example 1
[0106] This comparative example discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0107] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0108] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0109] Step (2): Polyacrylonitrile, polyacrylonitrile-modified silica aerogel, and epoxidized nano zinc oxide are mixed evenly at a mass ratio of 98:1:1, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0110] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0111] The preparation of polyacrylonitrile-modified silica aerogel includes the following steps:
[0112] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0113] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0114] S2. Mix acrylonitrile, ethanol and water, add photoinitiator and vinylsilane modified silica aerogel, ultrasonically disperse for 2 hours, and react at room temperature under ultraviolet light with a wavelength of 365 nm for 4 hours. After the reaction is completed, wash with ethanol by vacuum filtration and dry at 50°C for 48 hours to obtain polyacrylonitrile modified silica aerogel.
[0115] The mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator is 17:30:1:4:1.
[0116] Comparative Example 2
[0117] This comparative example discloses a method for preparing light-colored thermal insulation fibers, including the following steps:
[0118] Step (1): Mix nano zinc oxide, ethanol and water, ultrasonically disperse for 30 min, adjust the pH value to 8, add KH560, react at 60℃ for 4 h, after the reaction is completed, centrifuge to collect the precipitate, wash with water, and dry at 50℃ for 12 h to obtain epoxidized nano zinc oxide.
[0119] The mass ratio of nano zinc oxide, ethanol, water, and KH560 is 1:10:10:0.3.
[0120] Step (2): Epoxidized nano zinc oxide and methanol are mixed and ultrasonically dispersed for 30 min. Propylene amine is added and the mixture is stirred and reacted at room temperature for 72 h. After the reaction is completed, the mixture is washed by ether filtration and dried at 50 °C for 12 h to obtain alkynylated nano zinc oxide.
[0121] The mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:0.8:100.
[0122] Alkyne-modified nano-zinc oxide was mixed with methanol and ultrasonically dispersed for 10 min. Cysteine hydrochloride and benzoin dimethyl ether were added, and the mixture was irradiated at room temperature for 10 h under a nitrogen atmosphere and ultraviolet light with a wavelength of 365 nm. After the reaction was completed, the mixture was washed by ether filtration and dried at 50 °C for 12 h to obtain cationic modified nano-zinc oxide.
[0123] The mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1-1.2:0.05-0.1:80-100.
[0124] Step (3): Polyacrylonitrile, vinylsilane modified silica aerogel and cationic modified nano zinc oxide are mixed evenly at a mass ratio of 98:1:1, melt-blended at 180°C, extruded and granulated, melt-spun in a twin-screw spinning machine, cooled and stretched to obtain light-colored warm fiber.
[0125] The melt spinning conditions were as follows: spinning temperature was 185℃ in zone 1, 195℃ in zone 2, 205℃ in zone 3, and 215℃ in zone 4; spinning speed was 300m / min; drawing temperature was 110℃; and drawing ratio was 5.
[0126] The preparation of vinylsilane-modified silica aerogel includes the following steps:
[0127] S1. After soaking the silica aerogel in ethanol for 8 hours, remove it, transfer it to water, add vinyltriethoxysilane, ultrasonically disperse for 1 hour, adjust the pH to 10, stir the reaction at 40°C for 6 hours, after the reaction is completed, wash it by ethanol filtration, and dry it at 50°C for 48 hours to obtain vinylsilane modified silica aerogel.
[0128] The mass ratio of silica aerogel, vinyltriethoxysilane, and water is 3:10:200.
[0129] In the above examples and comparative examples: the particle size of nano zinc oxide is 30-50 nm; KH560 is γ-glycidyl etheroxypropyltrimethoxysilane, CAS number 2530-83-8; silica aerogel is in powder form, with a thermal conductivity of 0.017~0.023 W / (m∙K) and a bulk density of 40-120 kg / m³; polyacrylonitrile is in powder form as an acrylonitrile / methyl acrylate / itaconic acid copolymer, with a viscosity-average relative molecular mass of Mη = 78000; and the photoinitiator is photoinitiator 1173.
[0130] Test case
[0131] The performance of the light-colored thermal fibers prepared in Examples 1-5 and Comparative Examples 1-2 was tested. Specific test results are shown in Table 1.
[0132] Table 1
[0133]
[0134] The tests for each indicator in Table 1 were conducted according to the following standards: thermal insulation performance was expressed by thermal conductivity and measured using a thermal conductivity meter; the electrostatic half-life was determined by weaving the light-colored thermal insulation fibers prepared in Examples 1-5 and Comparative Examples 1-2 into fabrics, and referring to GB / T12703 "Evaluation of Electrostatic Properties of Textiles"; the antibacterial rate was determined according to GB / T20944.3 "Evaluation of Antibacterial Properties of Textiles Part 3: Shaking Method", and Escherichia coli was selected as the bacterial strain.
[0135] As can be seen from the test results in Table 1, the light-colored polyacrylonitrile fiber prepared by this invention has good thermal insulation, antibacterial and antistatic properties. This is because the invention uses polyacrylonitrile-modified silica aerogel as a thermal insulation functional filler, cationic modified nano zinc oxide as an antistatic agent and antibacterial agent, and prepares light-colored polyacrylonitrile fiber by melt spinning. The fiber has good thermal insulation properties, and the introduction of cationic inorganic-organic composite antibacterial and antistatic agent optimizes the antibacterial and antistatic properties of the fiber.
[0136] Comparative Example 1 uses epoxidized nano zinc oxide instead of cationic modified nano zinc oxide. Since the organic antibacterial components and antistatic agents can synergistically enhance the antibacterial and antistatic properties of the inorganic antibacterial and antistatic material nano zinc oxide, the antibacterial and antistatic properties of the polyacrylonitrile fiber are improved. Furthermore, hydrogen bonds can be formed between the cationic components and the polyacrylonitrile matrix, which optimizes the dispersion and compatibility of the nano zinc oxide in the matrix. Therefore, the antibacterial and antistatic properties of the fiber prepared in Comparative Example 1 are reduced.
[0137] Comparative Example 2 uses vinylsilane-modified silica aerogel instead of polyacrylonitrile-modified silica aerogel. Since polyacrylonitrile introduces cyano groups when modifying silica aerogel, it improves the dispersibility and compatibility of aerogel in the matrix. Therefore, in the fiber prepared in Comparative Example 2, the dispersibility of aerogel is reduced, which affects the thermal insulation performance of the fiber.
[0138] It should be noted that the embodiments described above are only for explaining the present invention and do not constitute any limitation on the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory terms, not limiting terms. Modifications can be made to the present invention within the scope of the claims, and revisions can be made to the present invention without departing from the scope and spirit of the present invention. Although the present invention described herein relates to specific methods, materials, and embodiments, it does not mean that the present invention is limited to the specific examples disclosed herein; on the contrary, the present invention can be extended to all other methods and applications with the same function.
Claims
1. A method for preparing a light-colored, warm-insulating fiber, characterized in that, Includes the following steps: Step (1): Mix epoxidized nano zinc oxide and methanol, disperse ultrasonically, add propargylamine, react, after the reaction is complete, filter, wash, and dry to obtain acetylated nano zinc oxide; wherein, the epoxidized nano zinc oxide is prepared by the following steps: mix nano zinc oxide, ethanol, and water, disperse ultrasonically, adjust the pH value, add KH560, react, after the reaction is complete, centrifuge to collect the precipitate, wash, and dry to obtain epoxidized nano zinc oxide; mix acetylated nano zinc oxide and methanol, disperse ultrasonically, add cysteine hydrochloride and benzoin dimethyl ether, react under light, after the reaction is complete, filter, wash, and dry to obtain cationic modified nano zinc oxide; Step (2): mix polyacrylonitrile and polyacrylonitrile-modified silica. Aerogel and cationic modified nano zinc oxide are mixed evenly, melt-blended, extruded and granulated, melt-spun, cooled and stretched to obtain light-colored warm fiber; wherein, the polyacrylonitrile modified silica aerogel is prepared by the following steps: S1, after the silica aerogel is immersed in ethanol, it is taken out and transferred to water, vinyltriethoxysilane is added, ultrasonic dispersion is performed, the pH value is adjusted, and the reaction is carried out. After the reaction is completed, it is filtered, washed, and dried to obtain vinylsilane modified silica aerogel; S2, acrylonitrile, ethanol, and water are mixed and stirred, a photoinitiator and vinylsilane modified silica aerogel are added, ultrasonic dispersion is performed, and the reaction is carried out under light. After the reaction is completed, it is filtered, washed, and dried to obtain polyacrylonitrile modified silica aerogel.
2. The method for preparing a light-colored warm fiber according to claim 1, characterized in that, In step (1), when preparing epoxidized nano zinc oxide, the mass ratio of nano zinc oxide, ethanol, water and KH560 is 1:8-20:8-20:0.1-0.3; the reaction conditions are: reacting at pH 8-9 and 50-70℃ for 3-6 hours.
3. The method for preparing a light-colored warm-insulating fiber according to claim 1, characterized in that, In step (1), the mass ratio of epoxidized nano zinc oxide, propargylamine, and methanol is 10:0.8-1.2:100; the reaction conditions are: stirring at room temperature for 60-84 hours.
4. The method for preparing a light-colored warm-insulating fiber according to claim 1, characterized in that, In step (1), the mass ratio of alkynylated nano zinc oxide, cysteine hydrochloride, benzoin dimethyl ether, and methanol is 10:1-1.2:0.05-0.1:80-100; the photoreaction conditions are: photoreaction for 8-12 hours under ultraviolet light at a temperature of 20-30℃ and a wavelength of 365nm in a nitrogen atmosphere.
5. The method for preparing a light-colored warm-insulating fiber according to claim 1, characterized in that, In step (2), the mass ratio of polyacrylonitrile, polyacrylonitrile-modified silica aerogel, and cationic modified nano zinc oxide is 90-98:1-5:1-5; the melt spinning conditions are: spinning temperature is 180-190℃ in zone 1, 190-195℃ in zone 2, 200-210℃ in zone 3, and 210-220℃ in zone 4, and spinning speed is 100-500m / min; the drawing temperature is 110-120℃, and the drawing ratio is 3-5 times.
6. The method for preparing a light-colored warm-insulating fiber according to claim 1, characterized in that, In step (2), when preparing polyacrylonitrile-modified silica aerogel, the mass ratio of silica aerogel, vinyltriethoxysilane, and water in S1 is 1-3:10:150-250; the reaction conditions are: stirring and reacting at pH 10 and 40-60℃ for 4-6 hours.
7. The method for preparing a light-colored warm-insulating fiber according to claim 1, characterized in that, In step (2), when preparing polyacrylonitrile-modified silica aerogel, the mass ratio of acrylonitrile, ethanol, water, vinylsilane-modified silica aerogel, and photoinitiator in S2 is 17-20:30-40:1-1.5:4:1-2; the photoreaction conditions are: photoreaction for 2-5 hours under ultraviolet light at a temperature of 20-30℃ and a wavelength of 365nm.
8. A light-colored thermal fiber prepared by the method for preparing light-colored thermal fiber as described in any one of claims 1-7.
9. An application of the light-colored thermal fiber as described in claim 8 on a fabric.
Citation Information
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