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

Abstract

The preparation method comprises the following steps: (1) taking aminobenzene sulfonic acid and trivalent metal salt, adding the aminobenzene sulfonic acid and the trivalent metal salt into deionized water and absolute ethyl alcohol, then adding sufficient ammonia water, and fully precipitating; (2) fully washing, centrifuging and drying the mixed solution containing the precipitate to obtain dried powder; and (3) fully grinding the dried powder, and calcining in a muffle furnace at high temperature to obtain the long-afterglow luminescent material. And (4) putting the high-temperature-resistant fibers or yarns into the pretreatment liquid for pretreatment, then taking out the pretreated fibers or yarns, putting the pretreated fibers or yarns into a dye vat, adding a dyeing solution containing a long-afterglow luminescent material to dye the fibers or yarns, performing reduction cleaning on the fibers or yarns after dyeing is completed, and then performing water washing and drying to obtain the high-temperature-resistant fibers or yarns. The long afterglow fiber or yarn is obtained. The long afterglow fiber or yarn prepared by the invention not only can keep stable luminescence performance in a high-temperature environment, but also can generate long afterglow at a high temperature.

Description

Technical Field

[0001] The 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. Currently, wearable luminous fabrics can solve this problem, but such luminous fabrics usually use fabrics as base fabrics, and then mix luminous functional materials with adhesives to form coatings, which are then coated on fabrics to form coatings. This coating treatment method reduces the inherent properties of textiles such as softness, flexibility and breathability, and the coating is also easy to fall off, resulting in the failure of the luminous performance of the fabric; in addition, this luminous material cannot maintain the luminous stability in a high temperature environment for a long time, which limits its use in certain high temperature environments, such as firefighting suits, high temperature resistant work clothes, etc., and after losing light, it also loses its luminescence or has only a short afterglow, thereby reducing its safety. Carbon quantum dots are quantum materials with a particle size of less than 10 nanometers, with a band gap structure controlled by structure and surface groups, and excellent optical properties. They have been widely used in biological detection, optoelectronic devices, catalysis and other fields. At the same time, 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 are prone to react with oxygen, chemicals, etc. in the surrounding environment under high temperature conditions, resulting in complete or significant reduction in optical performance; even if a small number of optical materials have high temperature stability and can maintain structural stability at high temperatures, high temperature thermal shock will induce thermal radiation, which will seriously affect the luminous efficiency of the luminescent material. Therefore, it is urgent to prepare a carbon quantum dot-based fiber material that can maintain stable luminous performance in a high temperature environment to improve safety in a high temperature environment. 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, and the long afterglow fiber or yarn has high color fastness, and the material is not easy to fall off the fiber.

[0004] The technical solution adopted by 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) adding aminobenzenesulfonic acid and trivalent metal salt to a mixed solution of deionized water and anhydrous ethanol, stirring evenly to fully mix, then adding sufficient ammonia water and fully precipitating 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, 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 the 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 min, the drying temperature is 60 to 100° C., and the drying time is 3 to 10 h.

[0013] Furthermore, in the 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 non-ionic surfactant, the concentration of sodium hydroxide is 1-2 g / L, the concentration of the non-ionic surfactant is 0.4-1 g / L, and the non-ionic surfactant is peregrin O, fatty alcohol polyoxyethylene ether, and polyethylene glycol.

[0014] Furthermore, in step (4), the dyeing solution comprises a long afterglow luminescent material, an auxiliary agent and a leveling agent, and the concentration of the long afterglow 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 their 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. The long afterglow luminescent material is prepared in situ by a high-temperature calcination method. During the preparation process, trivalent metal salts are used to form carbon quantum dots complexed with trivalent metal oxides, and molecular covalent bonds can be formed between the trivalent metal oxides 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. In addition, the preparation method of the present invention is relatively simple, has 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 an 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 rapidly 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 it enters the non-crystalline area, it can not only adsorb with the fiber through weak interactions such as van der Waals force and hydrogen bond, but also penetrate into the fiber molecular chain, and form strong interactions with the ester bond of the fiber through the functional groups on its surface, so as to achieve a firm bond, so that it has high color fastness, and prevents the long afterglow luminescent material from falling off after washing or friction, thereby affecting the luminescent performance; in addition, the long afterglow luminescent material is evenly dispersed in the fiber or yarn, and does not aggregate due to the limitation of the fiber or yarn, and can also avoid the quenching phenomenon caused by the aggregation of the long afterglow luminescent material, thereby further stabilizing the luminescent performance and long afterglow 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, which is not easy to hydrolyze or other reactions in acid, alkali or high temperature environment, and can resist the erosion of acid and alkali medium and high temperature, so that the stability of its chemical properties can be maintained 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 be significantly degraded in high temperature environment or harsh environment. In addition, a strong interaction is formed between the dyed fiber or yarn and the long afterglow luminescent material, which further improves 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 drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. 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 creative work.

[0023] Figure 1 The 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 the afterglow spectrum 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 stopping the irradiation;

[0027] Figure 5 These are photos of the long afterglow yarn obtained in Example 2 of the present invention changing over time after being treated with acid / alkali under sunlight, irradiated with a 365nm ultraviolet lamp, 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 at high temperature under sunlight, irradiated by a 365nm ultraviolet lamp, and after irradiation is stopped;

[0031] Fig. 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 afterglow fiber or yarn and a preparation method thereof. To make the purpose, technical scheme and effect of the present invention clearer and more specific, the present invention is further described in detail below. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

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

[0034] Example 1

[0035] This embodiment provides a high temperature stable long afterglow yarn, and the preparation process 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, stirred evenly to make them fully mixed, and then a sufficient amount of ammonia water was added and fully precipitated for 3 hours to obtain a mixed solution containing a precipitate;

[0037] (2) centrifuging the mixed solution containing the precipitate at 5000 r / min for 3 min, adding deionized water to the precipitate, mixing it evenly with ultrasound, and then centrifuging and washing it again, repeating this process 3 times, and drying the obtained precipitate in an oven at 60° C. for 3 h to obtain a dried powder;

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

[0039] (4) A pretreatment solution made of sodium hydroxide and chlorpyrifos O was prepared, wherein the concentration of sodium hydroxide was 1 g / L and the concentration of chlorpyrifos O was 0.4 g / L. 50 g of polyester yarn was added to the pretreatment solution for alkaline treatment for 10 min, and the bath ratio was 1:20. A dye solution made of a long afterglow luminescent material, an auxiliary agent, and a leveling agent was prepared, wherein the concentration of the long afterglow luminescent material was 2 g / L, the concentration of the auxiliary agent was 1 g / L, and the concentration of the leveling agent was 0.8 g / L. The polyester yarn after alkaline treatment was placed in a dye vat, and the prepared dye solution was added, and the bath ratio was 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, wherein the concentration of sodium hydroxide was 1 g / L and the concentration of insurance powder was 1 g / L. The dyed polyester yarn was cleaned with the reducing cleaning solution for 10 min, and the bath ratio was 1:20. The yarn was 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 afterglow yarn, and the preparation process 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, stirred evenly to make them fully mixed, and then a sufficient amount of ammonia water was added and fully precipitated for 3 hours to obtain a mixed solution containing a precipitate;

[0043] (2) centrifuging the mixed solution containing the precipitate at 5000 r / min for 3 min, adding deionized water to the precipitate, mixing it evenly with ultrasound, and then centrifuging and washing it again, repeating this process 3 times, and drying the obtained precipitate in an oven at 60° C. 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 afterglow luminescent material;

[0045] (4) A pretreatment solution made of sodium hydroxide and chlorpyrifos O was prepared, wherein the concentration of sodium hydroxide was 1 g / L and the concentration of chlorpyrifos O was 0.4 g / L. 50 g of polyester yarn was added to the pretreatment solution for alkaline treatment for 10 min, and the bath ratio was 1:20. A dye solution made of a long afterglow luminescent material, an auxiliary agent, and a leveling agent was prepared, wherein the concentration of the long afterglow luminescent material was 2 g / L, the concentration of the auxiliary agent was 1 g / L, and the concentration of the leveling agent was 0.8 g / L. The polyester yarn after alkaline treatment was placed in a dye vat, and the prepared dye solution was added, and the bath ratio was 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, wherein the concentration of sodium hydroxide was 1 g / L and the concentration of insurance powder was 1 g / L. The dyed polyester yarn was cleaned with the reducing cleaning solution for 10 min, and the bath ratio was 1:20. The yarn was 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 microscopy image of the long afterglow luminescent material prepared in Example 2 ( Figure 1 (a) 、High resolution transmission electron microscopy image ( Figure 1 (b)) and particle size distribution diagram ( 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 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 long afterglow luminescent materials 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 shown, 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 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 tested for acid resistance and alkali resistance. 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 was 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 resistance and alkali resistance tests. The long afterglow polyester yarn after the acid resistance 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 to washing of long afterglow polyester yarn was tested according to the standard GB / T 3921-2008, and the afterglow intensity after washing was tested. Six groups of samples were prepared, and three groups were randomly selected for the color fastness to washing test. The original samples were compared with the washed and dried samples using a gray sample card to evaluate the color change of the samples. The color fastness of the three groups of samples were 4-5, 4-5, and 4-5, respectively, which met the qualified requirements of general dyeing 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 intensifies, the diffusion rate increases, and they penetrate the micropores of the polyester fiber into the non-crystalline region. They can not only adsorb to the fiber through weak interactions such as van der Waals forces and hydrogen bonds, but 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 firm bond; and in some cases the fiber matrix can serve as a good afterglow enhancement medium, because the aggregation of afterglow materials will result in quenching, and after entering the fiber, they will not aggregate due to restriction, 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, 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 , Fig. 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, and the afterglow luminescence intensity is tested after maintaining each temperature gradient for 10 minutes. 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, ultrasonicated for 10 minutes, stirred evenly to make them fully mixed, and then a sufficient amount of ammonia water was added and fully precipitated for 3 hours to obtain a mixed solution containing a precipitate;

[0059] (2) centrifuging the mixed solution containing the precipitate at 5000 r / min for 10 min, adding deionized water to the precipitate, mixing it evenly with ultrasound, and then centrifuging and washing it again, repeating this process 5 times, and drying the obtained precipitate in an oven at 80° C. for 3 h to obtain a dried powder;

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

[0061] (4) preparing a pretreatment solution made of sodium hydroxide and polyethylene glycol, wherein the concentration of sodium hydroxide is 2 g / L and the concentration of is 1 g / L, adding 50 g of polyethylene glycol polyimide yarn into the pretreatment solution for alkaline treatment for 10 min, and the bath ratio is 1:40; preparing a dyeing solution made of a long afterglow luminescent material, an auxiliary agent, and a leveling agent, wherein the concentration of the long afterglow luminescent material is 4 g / L, the concentration of the auxiliary agent is 2 g / L, and the concentration of the leveling agent is 1.2 g / L, and adding the alkaline-treated polyethylene glycol polyimide yarn to the pretreatment solution for alkaline treatment for 10 min. The polyester yarn was placed in a dye 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 and dried to obtain long afterglow polyethylene glycol polyimide yarn.

[0062] It should be noted that some 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 protection scope of the present invention.

Claims

1. A method for preparing high temperature stable long afterglow fiber or yarn, characterized in that: Includes steps: (1) adding aminobenzenesulfonic acid and trivalent metal salt to a mixed solution of deionized water and anhydrous ethanol, stirring evenly to fully mix, then adding sufficient ammonia water and fully precipitating for 1 to 5 hours to obtain a mixed solution containing a precipitate; (2) washing the mixed solution containing the precipitate thoroughly and centrifuging it, and drying the precipitate in an oven to obtain a dried powder; (3) Grinding the dried powder thoroughly, and calcining it at 400° C. to 700° C. in a muffle furnace 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, 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.

2. The method for preparing a high temperature stable long afterglow 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 afterglow 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 afterglow fiber or yarn according to claim 1, characterized in that: The trivalent metal salt in step (1) is one of trivalent aluminum salts, iron salts, cobalt salts, chromium salts, gallium salts, indium salts and vanadium salts.

5. The method for preparing a high temperature stable long afterglow fiber or yarn according to claim 1, characterized in that: In the 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.

6. The method for preparing a high temperature stable long afterglow fiber or yarn according to claim 1, characterized in that: In the 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 peregrin O, fatty alcohol polyoxyethylene ether, and polyethylene glycol.

7. The method for preparing a high temperature stable long afterglow fiber or yarn according to claim 1, characterized in that: In the step (4), the dyeing solution comprises a long afterglow luminescent material, an auxiliary agent and a leveling agent, wherein the concentration of the long afterglow 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.

8. The method for preparing a high temperature stable long afterglow fiber or yarn according to claim 1, characterized in that: In the 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.

9. The method for preparing a high temperature stable long afterglow fiber or yarn according to claim 1, characterized in that: In the 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.

10. A high temperature stable long afterglow fiber or yarn, prepared by the preparation method according to any one of claims 1 to 9.

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