High-temperature stable long-afterglow fiber or yarn and preparation method thereof

By combining trivalent metal salts and carbon quantum dots in fibers or yarns, high-temperature stable long-afterglow fibers or yarns are prepared, which solves the problems of luminescence stability and shedding in high-temperature environments and achieves high color fastness and high-temperature resistance.

CN119308155BActive Publication Date: 2025-09-19QINGDAO UNIV
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Patent Information

Application Number
CN202411507480.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-28
Publication Date
2025-09-19
Estimated Expiration
2044-10-28

AI Technical Summary

Technical Problem

Existing luminous fabrics have poor luminous stability in high-temperature environments, and the coating easily falls off, affecting safety and visibility.

Method used

By combining trivalent metal salts with carbon quantum dots and forming trivalent metal oxide-complexed carbon quantum dots through high-temperature calcination, high-temperature stable long-afterglow fibers or yarns are prepared. Molecular covalent bonds are formed between trivalent metal oxides and carbon quantum dots to inhibit thermal radiation transitions and form strong interactions in the fibers or yarns to improve bonding strength.

Benefits of technology

It achieves luminous stability and long afterglow emission at high temperatures. The material is not easy to fall off, has high color fastness and high temperature resistance, and is suitable for high temperature environments.

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Abstract

The present invention discloses a high-temperature stable long-afterglow fiber or yarn and a preparation method thereof, comprising the following steps: (1) adding aminobenzenesulfonic acid and a trivalent metal salt to deionized water and anhydrous ethanol, then adding a sufficient amount of ammonia water and fully precipitating; (2) fully washing, centrifuging and drying the mixed solution containing the precipitate to obtain a dried powder; (3) fully grinding the dried powder, placing it in a muffle furnace for high-temperature calcination to obtain a long-afterglow luminescent material; (4) placing a high-temperature resistant fiber or yarn in a pretreatment solution for pretreatment, then taking out the pretreated fiber or yarn and placing it in a dye vat, adding a dyeing solution containing a long-afterglow luminescent material to dye the fiber or yarn, and after dyeing, performing reduction cleaning on the fiber or yarn, then washing and drying it to obtain a long-afterglow fiber or yarn. The long-afterglow fiber or yarn prepared by the present invention can not only maintain stable luminescence performance in a high-temperature environment, but also produce a long afterglow at high temperatures.
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Description

Technical Field

[0001] The present invention relates to the field of fiber technology, and in particular to a high-temperature stable long-afterglow fiber or yarn and a preparation method thereof. Background Art

[0002] In daily life and modern industry, safety and visibility are always key issues, especially in low-light or nighttime environments. Wearable luminescent fabrics can currently address this issue. However, these luminescent fabrics typically use a fabric as a base fabric. Luminescent functional materials are then mixed with an adhesive to form a coating, which is then applied to the fabric to form a coating. This coating process reduces the inherent properties of the textile, such as softness, flexibility, and breathability. The coating also easily falls off, causing the fabric's luminescent properties to fail. In addition, these luminescent materials cannot maintain luminescence stability for long periods of time in high-temperature environments, which limits their use in certain high-temperature environments, such as firefighting uniforms and heat-resistant work clothes. Furthermore, after the light is removed, they also lose their luminescence or have only a short afterglow, which reduces their safety. Carbon quantum dots are quantum materials with particle sizes below 10 nanometers. They have a band gap structure controlled by both structure and surface groups, and have excellent optical properties. They have been widely used in fields such as biological detection, optoelectronic devices, and catalysis. Carbon quantum dots mainly contain non-toxic elements such as carbon, nitrogen, and oxygen. Compared with toxic materials such as organic fluorescent dyes and inorganic quantum dots, they are green and non-toxic. However, most carbon quantum dot materials react easily with oxygen and chemicals in the surrounding environment at high temperatures, resulting in a complete or significant reduction in optical performance. Even though a small number of optical materials are high-temperature stable and can maintain structural stability at high temperatures, high-temperature thermal shock triggers thermal radiation, which seriously affects the luminous efficiency of the luminescent material. Therefore, it is urgent to prepare a carbon quantum dot-based fiber material that can maintain stable luminescence performance in high-temperature environments to improve safety in high-temperature environments. Summary of the Invention

[0003] In order to solve the above technical problems, the present invention provides a high-temperature stable long afterglow fiber or yarn and a preparation method thereof. The long afterglow fiber or yarn can not only maintain stable luminous performance in a high-temperature environment, but also produce long afterglow at high temperature. Moreover, the long afterglow fiber or yarn has high color fastness and the material is not easy to fall off from the fiber.

[0004] The technical solution adopted in the present invention is:

[0005] The present invention provides a high-temperature stable long-afterglow fiber or yarn and a preparation method thereof, wherein the preparation method comprises the steps of:

[0006] (1) Add aminobenzenesulfonic acid and a trivalent metal salt to a mixed solution of deionized water and anhydrous ethanol, stir evenly to mix thoroughly, then add sufficient ammonia water and allow to precipitate for 1 to 5 hours to obtain a mixed solution containing a precipitate;

[0007] (2) washing the mixed solution containing the precipitate thoroughly and centrifuging it, and drying the precipitate in an oven to obtain a dried powder;

[0008] (3) Grinding the dried powder thoroughly and calcining it in a muffle furnace at 400°C to 700°C for 1.5 to 3 hours to obtain a long afterglow luminescent material;

[0009] (4) placing the high-temperature resistant fiber or yarn in a pretreatment solution for pretreatment, then taking out the pretreated high-temperature resistant fiber or yarn and placing it in a dyeing vat, and adding a dyeing solution containing a long afterglow luminescent material to dye the high-temperature resistant fiber or yarn, and after dyeing is completed, using a reducing cleaning solution to perform reduction cleaning on the fiber or yarn, and then washing and drying to obtain a long afterglow fiber or yarn.

[0010] Furthermore, in step (1), the molar ratio of aminobenzenesulfonic acid to trivalent metal salt is 1:10-30.

[0011] Furthermore, in step (1), the aminobenzenesulfonic acid is at least one of 2-aminobenzenesulfonic acid, 3-aminobenzenesulfonic acid, 4-aminobenzenesulfonic acid, 2,4-diaminobenzenesulfonic acid, 2,5-diaminobenzenesulfonic acid, and 3,4-diaminobenzenesulfonic acid.

[0012] Furthermore, in step (1), the trivalent metal salt is one of trivalent aluminum salt, iron salt, cobalt salt, chromium salt, gallium salt, indium salt, and vanadium salt. Furthermore, in step (2), the washing times are 2 to 5 times, the centrifugal speed is 5000 to 8000 r / min, the centrifugal time is 3 to 10 minutes, the drying temperature is 60 to 100° C., and the drying time is 3 to 10 hours.

[0013] Furthermore, in step (4), the bath ratio of the fiber or yarn to the pretreatment liquid is 1:10-30, the pretreatment liquid is a mixed solution of sodium hydroxide and a nonionic surfactant, the concentration of sodium hydroxide is 1-2 g / L, the concentration of the nonionic surfactant is 0.4-1 g / L, and the nonionic surfactant is peregal O, fatty alcohol polyoxyethylene ether, and polyethylene glycol.

[0014] Furthermore, the dyeing solution in step (4) includes a long-lasting luminescent material, an auxiliary agent and a leveling agent, and the concentration of the long-lasting luminescent material is 2-4 g / L, the concentration of the auxiliary agent is 1-2 g / L, and the concentration of the leveling agent is 0.8-1.2 g / L.

[0015] Furthermore, in step (4), the bath ratio of the fiber or yarn to the dyeing solution is 1:20-50, the dyeing temperature is 100-150° C., and the dyeing time is 30-60 min.

[0016] Furthermore, in step (4), the bath ratio of the fiber or yarn to the reducing cleaning solution is 1:30-50, the reducing cleaning solution is a mixed solution of sodium hydroxide and hydrosulfite, the concentration of sodium hydroxide is 1-2 g / L, and the concentration of hydrosulfite is 1-3 g / L.

[0017] Furthermore, the high temperature resistant fiber or yarn in step (4) is polyester fiber, aramid fiber, carbon fiber, polyimide fiber, and corresponding yarns.

[0018] The beneficial effects of the present invention are:

[0019] (1) The present invention provides a high-temperature stable long afterglow fiber or yarn and a preparation method thereof, wherein the long afterglow luminescent material is prepared in situ by a high-temperature calcination method, and in the preparation process, trivalent metal salts are used to form trivalent metal oxide-complexed carbon quantum dots, and molecular covalent bonds can be formed between the trivalent metal oxide and the carbon quantum dots to anchor the luminescent groups on the surface of the carbon quantum dots, thereby effectively inhibiting thermal radiation transitions at high temperatures and ensuring their luminescence efficiency; at the same time, the trivalent metal oxide has a dense crystal structure, which protects the carbon quantum dots from the reaction of external oxygen and chemical groups, making them highly stable; in addition, the confinement effect of the trivalent metal oxide further ensures the luminescence performance and long afterglow emission of the long afterglow luminescent material, and at the same time, it is wrapped on the surface of the carbon quantum dots to make them have high temperature resistance, thereby ensuring that the prepared long afterglow luminescent material can maintain luminescence stability and long afterglow emission at high temperatures, and the preparation method of the present invention is relatively simple, with a short reaction time, and is easy to control and prepare on a large scale;

[0020] (2) The present invention provides a high-temperature stable long afterglow fiber or yarn and a preparation method thereof. In the process of preparing the fiber or yarn, the fiber or yarn is pretreated with alkali solution, and a leveling agent and an auxiliary agent are added to the dye solution. The fiber or yarn is dyed at a high temperature. This is not only conducive to the dye solution entering the interior of the fiber or yarn, improving the dyeing rate, shortening the dyeing time, and making the dyeing more uniform, but also promotes the efficient combination of the fiber or yarn and the long afterglow luminescent material. Under high temperature conditions, the long afterglow luminescent material moves more vigorously in the liquid phase, the diffusion rate is increased, and it can penetrate the micropores of organic fibers such as polyester fibers and enter When the luminescent material enters the non-crystalline region, it can not only be adsorbed on the fiber through weak interactions such as van der Waals forces and hydrogen bonds, but also penetrate into the interior of the fiber molecular chain, forming strong interactions with the ester bonds of the fiber through the functional groups on its surface, thereby achieving a firm bond, thereby making it have high color fastness and preventing the long-lasting luminescent material from falling off after washing or friction and affecting the luminescence performance; in addition, the long-lasting luminescent material is evenly dispersed in the fiber or yarn, and due to the limitation of the fiber or yarn, it does not aggregate, and can also avoid the quenching phenomenon caused by the aggregation of the long-lasting luminescent material, thereby further stabilizing the luminescence performance and long-lasting emission;

[0021] (3) The high-temperature stable long afterglow fiber or yarn of the present invention has high-temperature stability and acid and alkali resistance, which depends on its unique material composition and structural characteristics. First, the surface of the long afterglow luminescent material is coated with a trivalent metal oxide network structure. This structure is not easy to undergo hydrolysis or other reactions in acidic, alkaline or high-temperature environments, and can resist the erosion of acidic and alkaline media and high temperatures, thereby maintaining the stability of its chemical properties to the greatest extent. Secondly, the matrix of the long afterglow fiber or yarn, such as polyester, also has excellent high-temperature resistance and tolerance to weak acids and alkalis, so that it will not undergo significant degradation in high-temperature environments or harsh environments. In addition, a strong interaction is formed between the dyed fiber or yarn and the long afterglow luminescent material, further improving its overall high-temperature resistance and acid and alkali resistance, thereby ensuring that the fiber can still maintain its excellent luminescence performance and long afterglow emission characteristics under extreme conditions, thereby enhancing the application value of the fiber or yarn in extreme environments. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0023] Figure 1 Transmission electron microscope image and particle size distribution diagram of the long afterglow luminescent material prepared in Example 2 of the present invention;

[0024] Figure 2The ultraviolet diffuse reflectance spectrum of the long afterglow luminescent material prepared in Example 2 of the present invention and afterglow spectra at different excitation wavelengths;

[0025] Figure 3 The afterglow lifetime spectrum and quantum efficiency spectrum of the long afterglow luminescent material prepared in Example 2 of the present invention at an excitation wavelength of 365nm;

[0026] Figure 4 These are photos of the long afterglow luminescent material and yarn prepared in Example 2 of the present invention under 365nm ultraviolet light irradiation and after irradiation is stopped;

[0027] Figure 5 These are photos of the long afterglow yarn obtained in Example 2 of the present invention after being treated with acid / alkali, and the changes over time under sunlight, 365nm ultraviolet light, and after irradiation is stopped;

[0028] Figure 6 The afterglow intensity of the long afterglow yarn obtained in Example 2 of the present invention before and after acid / alkali treatment;

[0029] Figure 7 The afterglow intensity of the long afterglow yarn obtained in Example 2 of the present invention before and after the washing fastness test;

[0030] Figure 8 These are photos of the long afterglow yarn obtained in Example 2 of the present invention changing over time after being treated with high temperature under sunlight, irradiated by a 365nm ultraviolet lamp, and after irradiation is stopped;

[0031] Figure 9 The afterglow intensity of the long afterglow yarn obtained in Example 2 of the present invention before and after high temperature treatment. DETAILED DESCRIPTION

[0032] The present invention provides a high-temperature stable long-lasting fiber or yarn and a method for preparing the same. To clarify the objectives, technical solutions, and effects of the present invention, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are intended only to illustrate the present invention and are not intended to limit the present invention.

[0033] The present invention will be described in detail below with reference to the accompanying drawings.

[0034] Example 1

[0035] This embodiment provides a high-temperature stable long-lasting yarn, the preparation process of which is as follows:

[0036] (1) 0.25 mmol of 2,5-diaminobenzenesulfonic acid and 7.5 mmol of ferric chloride hexahydrate were added to a mixed solution of 10 mL of deionized water and 10 mL of anhydrous ethanol, and ultrasonicated for 10 minutes. The mixture was stirred evenly to mix thoroughly, and then sufficient ammonia water was added and allowed to precipitate for 3 hours to obtain a mixed solution containing a precipitate.

[0037] (2) The mixed solution containing the precipitate was centrifuged at 5000 r / min for 3 min, the precipitate was added to deionized water, ultrasonically mixed and then centrifuged and washed again, and the mixture was repeated 3 times. The obtained precipitate was placed in an oven at 60°C and dried for 3 h to obtain a dried powder;

[0038] (3) Grinding the dried powder thoroughly and calcining it in a muffle furnace at 400°C for 2.5 hours to obtain a long-lasting luminescent material;

[0039] (4) A pretreatment solution made of sodium hydroxide and chlorinated polyol was prepared, with the concentration of sodium hydroxide being 1 g / L and the concentration of chlorinated polyol being 0.4 g / L. 50 g of polyester yarn was added to the pretreatment solution for alkaline treatment for 10 min at a bath ratio of 1:20. A dye solution made of a long afterglow luminescent material, an auxiliary agent, and a leveling agent was prepared, with the concentration of the long afterglow luminescent material being 2 g / L, the concentration of the auxiliary agent being 1 g / L, and the concentration of the leveling agent being 0.8 g / L. The polyester yarn after alkaline treatment was placed in a dye vat and the prepared dye solution was added thereto at a bath ratio of 1:50. The yarn was dyed at 150°C for 30 min. A reducing cleaning solution made of sodium hydroxide and insurance powder was prepared, with the concentration of sodium hydroxide being 1 g / L and the concentration of insurance powder being 1 g / L. The dyed polyester yarn was cleaned with the reducing cleaning solution for 10 min at a bath ratio of 1:20, and then washed twice with water and dried to obtain a long afterglow polyester yarn.

[0040] Example 2

[0041] This embodiment provides a high-temperature stable long-lasting yarn, the preparation process of which is as follows:

[0042] (1) 0.25 mmol of 2,5-diaminobenzenesulfonic acid and 7.5 mmol of aluminum chloride hexahydrate were added to a mixed solution of 10 mL of deionized water and 10 mL of anhydrous ethanol, and ultrasonicated for 10 minutes. The mixture was stirred evenly to mix thoroughly, and then sufficient ammonia water was added and allowed to precipitate for 3 hours to obtain a mixed solution containing a precipitate.

[0043] (2) The mixed solution containing the precipitate was centrifuged at 5000 r / min for 3 min, the precipitate was added to deionized water, ultrasonically mixed and then centrifuged and washed again, and the mixture was repeated 3 times. The obtained precipitate was placed in an oven at 60°C and dried for 3 h to obtain a dried powder;

[0044] (3) Grinding the dried powder thoroughly and calcining it in a muffle furnace at 500°C for 100 min to obtain a long-lasting luminescent material;

[0045] (4) A pretreatment solution made of sodium hydroxide and chlorinated polyol was prepared, with the concentration of sodium hydroxide being 1 g / L and the concentration of chlorinated polyol being 0.4 g / L. 50 g of polyester yarn was added to the pretreatment solution for alkaline treatment for 10 min at a bath ratio of 1:20. A dye solution made of a long afterglow luminescent material, an auxiliary agent, and a leveling agent was prepared, with the concentration of the long afterglow luminescent material being 2 g / L, the concentration of the auxiliary agent being 1 g / L, and the concentration of the leveling agent being 0.8 g / L. The polyester yarn after alkaline treatment was placed in a dye vat and the prepared dye solution was added thereto at a bath ratio of 1:50. The yarn was dyed at 150°C for 30 min. A reducing cleaning solution made of sodium hydroxide and insurance powder was prepared, with the concentration of sodium hydroxide being 1 g / L and the concentration of insurance powder being 1 g / L. The dyed polyester yarn was cleaned with the reducing cleaning solution for 10 min at a bath ratio of 1:20, and then washed twice with water and dried to obtain a long afterglow polyester yarn.

[0046] Reference Figure 1-4 The long afterglow luminescent material and yarn prepared in Example 2 were tested as follows:

[0047] in, Figure 1 This is a low-resolution transmission electron microscope image of the long afterglow luminescent material prepared in Example 2 ( Figure 1 (a) 、High resolution transmission electron microscopy ( Figure 1 (b)) and particle size distribution ( Figure 1 (c)). Figure 1 (a) shows that the long afterglow luminescent material is aluminum oxide crystal with a cubic structure; Figure 1 (b) shows that the synthesized long afterglow luminescent material has good dispersion, no agglomeration, and is approximately spherical. Figure 1 (c) The particle size distribution diagram shows that the particle size of the long afterglow luminescent material is distributed in the range of 3.0 to 7.0 nm, with an average particle size of 5.25 nm.

[0048] Figure 2 This is the ultraviolet diffuse reflectance spectrum of the long afterglow luminescent material prepared in Example 2 ( Figure 2 (a)) and afterglow spectra at different excitation wavelengths ( Figure 2 (b)). Figure 2 From (a), we can see that the absorption range of the long afterglow luminescent material is 200~600nm; Figure 2As can be seen in (b), under the excitation light of 300nm, 330nm, 360nm, and 390nm, emission peaks of ~450nm and ~550nm are all displayed, indicating that the long-afterglow luminescent material has two emission centers.

[0049] Figure 3 This is the lifetime spectrum of the long afterglow luminescent material prepared in Example 2 at an excitation wavelength of 365 nm ( Figure 3 (a)), quantum efficiency spectrum ( Figure 3 (b)). Figure 3 The lifetime decay curve and fitting data in (a) show that the lifetime of the long afterglow luminescent material prepared in Example 2 is 1.12 seconds; Figure 3 It can be seen from the quantum efficiency curve and data calculation in (b) that the quantum efficiency of the long afterglow luminescent material prepared in this Example 2 is 19.8%.

[0050] Figure 4 (a) and (b) are photos of the long afterglow luminescent material and the long afterglow yarn prepared in Example 2 under 365nm ultraviolet light irradiation and after the irradiation is stopped. The above ultraviolet light irradiation is at room temperature. Figure 4 It can be seen that the long afterglow luminescent material prepared in Example 2 emits green light when irradiated by a 365nm ultraviolet lamp at room temperature. When the ultraviolet lamp is turned off, it exhibits a dynamic color-changing afterglow that turns yellow first and then green, and the afterglow can last for 10 seconds. In addition, the long afterglow polyester yarn also exhibits a green afterglow at room temperature, and the afterglow can last for 5 seconds.

[0051] It should be noted that after the yarn is made, the concentration of the long afterglow luminescent material is relatively low and is distributed in the solid phase, which affects the duration of its afterglow, but the afterglow duration of the yarn can reach 5 seconds, which is still relatively long.

[0052] In addition, the long afterglow polyester yarn prepared in Example 2 was subjected to acid and alkali resistance tests. Specifically, the long afterglow polyester yarn was placed in an acetic acid solution with a pH value of 2.5 and a sodium hydroxide solution with a pH value of 10, respectively, with a bath ratio of 1:30, and immersed at a constant temperature for 1 hour at room temperature. During the period, it was stirred every 10 minutes to avoid unevenness. After the immersion, the polyester yarn was taken out, rinsed with running water, and placed in an oven for drying to obtain the long afterglow polyester yarn after the acid and alkali resistance tests. The long afterglow polyester yarn after the acid and alkali resistance tests was irradiated with a 365nm ultraviolet lamp. Figure 5 As shown, from Figure 5 It can be observed that under acid and alkali conditions, the yarn still maintains a good long afterglow intensity; in addition, the afterglow intensity of the long afterglow polyester yarn before and after acid / alkali treatment was measured using a spectrometer, such as Figure 6 As shown, from Figure 6It can be seen that the afterglow intensity of the long afterglow polyester yarn after acid / alkali treatment decreases to a certain extent, but the attenuation is below 20%, indicating that the long afterglow polyester yarn has certain acid and alkali resistance.

[0053] In addition, the color fastness of long-lasting polyester yarn to washing was tested according to standard GB / T 3921-2008, and the intensity of the afterglow after washing was measured. Six sets of samples were prepared, and three were randomly selected for color fastness to washing. Discoloration was assessed using a gray scale to compare the original samples with the washed and dried samples. The color fastness of the three sets of samples was rated 4-5, 4-5, and 4-5, respectively, meeting the standard for general dyed products. This shows that the long afterglow luminescent material of the long afterglow polyester yarn prepared in this embodiment is relatively stably and firmly bonded to the polyester yarn with good durability. This is because under high-temperature dyeing conditions, the movement of long afterglow dye molecules in the liquid phase is intensified, the diffusion rate is increased, and they penetrate the micropores of the polyester fiber into the non-crystalline region. Not only can they be adsorbed with the fiber through weak interactions such as van der Waals forces and hydrogen bonds, but they can also penetrate into the interior of the fiber molecular chains, and form strong interactions with the ester bonds of the fiber through the functional groups on their own surface to achieve a strong bond; and in some cases, the fiber matrix can serve as a good afterglow enhancement medium, because the aggregation of afterglow materials will cause quenching, and after entering the interior of the fiber, they will not aggregate due to restrictions, thereby stabilizing the long afterglow emission of the material.

[0054] This embodiment also uses a spectrometer to characterize the long afterglow polyester yarn before and after washing, such as Figure 7 As shown in the figure, the attenuation of the afterglow intensity of the long afterglow polyester yarn after washing is less than 20%, with no obvious decrease.

[0055] like Figure 8 、 Figure 9 As shown, this embodiment also tests the luminescence performance of the long afterglow polyester yarn at high temperature. It also has luminescence performance at high temperature, and is placed at temperatures of 50°C, 100°C and 200°C, respectively. After maintaining each temperature gradient for 10 minutes, the afterglow luminescence intensity is tested. The afterglow intensity decays by less than 20%, with no obvious decrease, indicating that the long afterglow polyester yarn has high temperature stability.

[0056] Example 3

[0057] This embodiment provides a high-temperature stable long-afterglow fiber, the preparation process of which is as follows:

[0058] (1) 0.5 mmol of 2,5-diaminobenzenesulfonic acid and 5 mmol of aluminum chloride hexahydrate were added to a mixed solution of 20 mL of deionized water and 20 mL of anhydrous ethanol, and ultrasonicated for 10 minutes. The mixture was stirred evenly to mix thoroughly, and then sufficient ammonia water was added and allowed to precipitate for 3 hours to obtain a mixed solution containing a precipitate.

[0059] (2) The mixed solution containing the precipitate was centrifuged at 5000 r / min for 10 min, the precipitate was added to deionized water, ultrasonically mixed and then centrifuged and washed again, and the mixture was repeated 5 times. The obtained precipitate was placed in an oven at 80°C and dried for 3 h to obtain a dried powder;

[0060] (3) Grinding the dried powder thoroughly and calcining it at 600°C in a muffle furnace for 150 min to obtain a long-lasting luminescent material;

[0061] (4) A pretreatment solution made of sodium hydroxide and polyethylene glycol was prepared, wherein the concentration of sodium hydroxide was 2 g / L and the concentration of nitrite was 1 g / L. 50 g of polyethylene glycol polyimide yarn was added into the pretreatment solution for alkaline treatment for 10 min, and the bath ratio was 1:40. A dye solution made of long afterglow luminescent material, auxiliary agent and leveling agent was prepared, wherein the concentration of long afterglow luminescent material was 4 g / L, the concentration of auxiliary agent was 2 g / L and the concentration of leveling agent was 1.2 g / L. The polyethylene glycol after alkaline treatment was added into the pretreatment solution. The polyester yarn was placed in a dyeing vat, and the prepared dye solution was added at a bath ratio of 1:40. The yarn was dyed at 120°C for 40 minutes. A reducing cleaning solution made of sodium hydroxide and insurance powder was prepared. The concentration of sodium hydroxide was 2 g / L and the concentration of insurance powder was 3 g / L. The dyed polyester yarn was cleaned with the reducing cleaning solution for 10 minutes at a bath ratio of 1:40, and then washed twice with water and dried to obtain a long-lasting polyethylene glycol polyimide yarn.

[0062] It should be noted that the parts not described in the present invention can be implemented by adopting or drawing on existing technologies.

[0063] Of course, the above description is not a limitation of the present invention, and the present invention is not limited to the above examples. Changes, modifications, additions or substitutions made by technicians in this technical field within the essential scope of the present invention should also fall within the scope of protection of the present invention.

Claims

1. A method for preparing high-temperature stable long-lasting fiber or yarn, characterized in that: Including steps: (1) Add aminobenzenesulfonic acid and trivalent metal salt to a mixed solution of deionized water and anhydrous ethanol, stir evenly to mix thoroughly, then add sufficient ammonia water and allow to precipitate for 1 to 5 hours to obtain a mixed solution containing a precipitate; (2) The mixed solution containing the precipitate is thoroughly washed and centrifuged, and the precipitate is dried in an oven to obtain a dried powder; (3) Grind the dried powder thoroughly and calcine it in a muffle furnace at 400°C to 700°C for 1.5 to 3 hours to obtain a long afterglow luminescent material; (4) placing the high temperature resistant fiber or yarn in a pretreatment solution for pretreatment, then taking out the pretreated high temperature resistant fiber or yarn and placing it in a dyeing vat, and adding a dyeing solution containing a long afterglow luminescent material to dye the high temperature resistant fiber or yarn, and after dyeing is completed, using a reduction cleaning solution to perform reduction cleaning on the fiber or yarn, and then washing and drying to obtain a long afterglow fiber or yarn; The trivalent metal salt in step (1) is one of trivalent aluminum salt, iron salt, cobalt salt, chromium salt, gallium salt, indium salt and vanadium salt; In step (4), the bath ratio of the fiber or yarn to the pretreatment liquid is 1:10-30, the pretreatment liquid is a mixed solution of sodium hydroxide and a nonionic surfactant, the concentration of sodium hydroxide is 1-2 g / L, the concentration of the nonionic surfactant is 0.4-1.0 g / L, and the nonionic surfactant is fatty alcohol polyoxyethylene ether or polyethylene glycol.

2. The method for preparing a high-temperature stable long-lasting fiber or yarn according to claim 1, characterized in that: In the step (1), the molar ratio of aminobenzenesulfonic acid to trivalent metal salt is 1:10-30.

3. The method for preparing a high-temperature stable long-lasting fiber or yarn according to claim 1, characterized in that: In the step (1), the aminobenzenesulfonic acid is at least one of 2-aminobenzenesulfonic acid, 3-aminobenzenesulfonic acid, 4-aminobenzenesulfonic acid, 2,4-diaminobenzenesulfonic acid, 2,5-diaminobenzenesulfonic acid, and 3,4-diaminobenzenesulfonic acid.

4. The method for preparing a high-temperature stable long-lasting fiber or yarn according to claim 1, characterized in that: In step (2), the washing times are 2 to 5 times, the centrifugal speed is 5000 to 8000 r / min, the centrifugal time is 3 to 10 min, the drying temperature is 60 to 100°C, and the drying time is 3 to 10 h.

5. The method for preparing a high-temperature stable long-lasting fiber or yarn according to claim 1, characterized in that: In step (4), the dyeing solution includes a long-lasting luminescent material, an auxiliary agent, and a leveling agent, wherein the concentration of the long-lasting luminescent material is 2-4 g / L, the concentration of the auxiliary agent is 1-2 g / L, and the concentration of the leveling agent is 0.8-1.2 g / L.

6. The method for preparing a high-temperature stable long-lasting fiber or yarn according to claim 1, characterized in that: In step (4), the bath ratio of the fiber or yarn to the dyeing solution is 1:20-50, the dyeing temperature is 100-150° C., and the dyeing time is 30-60 min.

7. The method for preparing a high-temperature stable long-lasting fiber or yarn according to claim 1, characterized in that: In step (4), the bath ratio of the fiber or yarn to the reducing cleaning solution is 1:30-50, the reducing cleaning solution is a mixed solution of sodium hydroxide and hydrosulfite, the concentration of sodium hydroxide is 1-2 g / L, and the concentration of hydrosulfite is 1-3 g / L.

8. A high-temperature stable long-afterglow fiber or yarn, prepared by the preparation method according to any one of claims 1 to 7.

Citation Information

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