Polybutylene succinate composite fiber and preparation method thereof

Abstract

The invention discloses a poly (butylene succinate) composite fiber and a preparation method thereof. The preparation method comprises the following steps: 1) dissolving the photochromic dye, the antioxidant A and the ultraviolet light absorber in an oil-soluble solvent to obtain an oil-phase solution; 2) adding the oil phase solution into an aqueous solution containing an emulsifier, and emulsifying to obtain an oil-in-water emulsion; adjusting the pH value of the emulsion to 3-8 and the temperature to 20-100 DEG C; (3) adding a capsule wall material and a magnetic substance into water, adding the mixture into the emulsion at a constant speed, putting the mixture into an external magnetic field with controllable strength, and keeping the temperature at 20-90 DEG C for 0.3-5 hours to obtain the photochromic microcapsule with a shell with a special structure; and 4) adding the photochromic microcapsule into a spinning solution of the poly (butylene succinate) fiber, and then spinning to obtain the poly (butylene succinate) composite fiber.

Description

Technical Field

[0001] The present invention relates to the field of textile technology, and particularly relates to a polybutylene succinate composite fiber and a preparation method thereof. Background Art

[0002] The use of polymer materials has greatly facilitated people's lives. However, after being discarded, they often take decades to degrade under natural conditions, causing great harm to the natural environment and wasting resources. With the continuous improvement of people's environmental awareness and the introduction of the plastic restriction order, degradable polymers have received increasing attention. Currently, there are already various types of degradable polymers. Among them, polybutylene succinate (PBS) has excellent comprehensive properties and biodegradability, and its mechanical properties can be comparable to those of traditional polyolefin polymer materials. It is one of the most promising materials to replace traditional polyolefin polymer materials.

[0003] The fibers prepared from polybutylene succinate (PBS) are widely used in the textile field, which can effectively reduce the environmental damage and resource waste caused by discarded fabrics. With people's pursuit of beauty and novelty, more and more requirements are put forward for the functionality and diversity of textiles. The single and fixed color of clothing can no longer satisfy people's curiosity. Therefore, a textile that can change color dynamically is needed. In the dynamic color change of fibers, photoinduced fiber color change is an ideal color change method because of its simple operation, rapid reaction, and rich color changes. The principle of photoinduced fiber color change is mainly divided into two types. One is that photochromic substances are added inside or adhered to the surface of the fiber. The photochromic fiber can display different colors with the change of the external light environment conditions, having a unique visual effect. The other is to use liquid crystal spinning to manufacture fibers with liquid crystal structures inside, which have different reflection effects on the incident light, forming photochromism at different angles. It can not only meet consumers' pursuit of novelty, diversity, and variability of clothing colors but also be widely used in fields such as anti-counterfeiting and advertising.

[0004] CN112323168A discloses a method for preparing photochromic fibers by spinning a spinning solution in which a photochromic masterbatch is mixed into a polyethylene fiber or polypropylene fiber raw material; however, its preparation process is complex and variable, and a large number of toxic reagents are used.

[0005] CN114367249A discloses a method for preparing nanocellulose-based photochromic microcapsules with a modified nanocellulose solution as the aqueous phase and an organic photochromic compound mixture as the oil phase; the preparation process is complex and variable, and it can only be used for coatings, with a narrow application range.

[0006] CN111334880A discloses a method for preparing photochromic lyocell fibers by spinning a spinning solution in which a photochromic raw material is mixed into a lyocell fiber raw material; the durability and strength of the obtained product are poor.

[0007] At present, photochromic fibers are mainly prepared by grafting spirooxazine groups or spiropyran groups, adding fluorescent agents, liquid crystal spinning, electrospinning, or using coatings with adhesives for high-temperature baking, printing, and coating. The preparation process is complex and variable, uses many toxic reagents, and the durability and comfort of the obtained products are poor. Moreover, the vast majority of photochromic fibers cannot be degraded after being discarded, causing environmental damage and waste of resources. Summary of the Invention

[0008] The purpose of the present invention is to provide a polybutylene succinate composite fiber and a preparation method thereof.

[0009] The polybutylene succinate composite fiber of the present invention is a photochromic fiber that can be biodegradable. By adding a certain amount of photochromic microcapsules with a special structural design to the traditional spinning process of biodegradable polybutylene succinate (PBS) fibers, it has the properties of photochromism and biodegradability, with variable colors, no pollution to the environment, and almost no impact on the wearing comfort of fabrics.

[0010] In order to achieve the above purposes, the present invention adopts the following technical solutions:

[0011] On the one hand, the present invention provides a preparation method of a polybutylene succinate composite fiber, wherein the preparation method includes:

[0012] 1) Dissolve a photochromic dye, antioxidant A, and ultraviolet absorber in an oil-soluble solvent to obtain an oil-phase solution;

[0013] 2) Add the oil-phase solution to an aqueous solution containing an emulsifier, and emulsify to obtain an oil-in-water emulsion; adjust the pH of the emulsion to 3 - 8 and the temperature to 20 - 100 °C;

[0014] 3) Add a capsule wall material and a magnetic substance to water, and uniformly add it to the emulsion. Place it in an externally applied magnetic field with a controllable intensity, and keep it warm at 20 - 90 °C for 0.3 - 5 hours to obtain photochromic microcapsules with a special structure on the shell;

[0015] 4) Add the photochromic microcapsules to the spinning dope of polybutylene succinate fiber, and then carry out spinning to obtain the polybutylene succinate composite fiber.

[0016] According to the preparation method of the present invention, preferably, in step 1), the mass ratio of the photochromic dye, antioxidant, ultraviolet absorber, and oil-soluble solvent is (20 - 60):(0.5 - 10):(1 - 5):100; more preferably (20 - 60):(0.5 - 7):(1.2 - 2.5):100.

[0017] According to the preparation method of the present invention, preferably, in step 2), in the aqueous solution containing an emulsifier, the concentration of the emulsifier is 0.1 wt% to 15 wt%.

[0018] According to the preparation method of the present invention, preferably, in step 2), the mass ratio of the oil phase solution to the aqueous solution containing an emulsifier is 1:(5 - 10).

[0019] According to the preparation method of the present invention, preferably, in step 3), the mass ratio of the capsule wall material, magnetic substance and water is (25 - 30):(5 - 20):(30 - 40).

[0020] According to the preparation method of the present invention, preferably, in step 3), the mass ratio of the aqueous solution containing the capsule wall material and the magnetic substance to the emulsion is 1:(4 - 18), more preferably 1:(5.5 - 18); further preferably 1:(5.5 - 8).

[0021] According to the preparation method of the present invention, preferably, in step 3), the magnetic field is an alternating electromagnetic field, and the intensity range is 1 - 2 mT.

[0022] According to the preparation method of the present invention, preferably, in step 4), based on the total mass of the spinning dope and the photochromic microcapsules being 100 parts, the mass parts of the photochromic microcapsules are 1 - 5.

[0023] According to the preparation method of the present invention, preferably, antioxidant B is further added to the spinning dope. In addition, other additives commonly used in spinning solutions, such as spinning aids, heat stabilizers, etc., may be further added to the spinning dope, and the present invention does not limit this.

[0024] According to the preparation method of the present invention, preferably, based on the total mass of the spinning dope and the photochromic microcapsules being 100 parts, the mass parts of antioxidant B are 0.5 - 1.5.

[0025] According to the preparation method of the present invention, preferably, the pH of the emulsion is adjusted to 3 - 8 with a hydrochloric acid solution.

[0026] According to the preparation method of the present invention, preferably, the photochromic dye is selected from at least one of naphthospiropyrans, spirooxazines, diarylethylenes, azobenzenes, fulgides, naphthopyrans, transition metal oxides, metal halides, and rare earth complexes. More preferably, the photochromic dye is diarylethylene, spirooxazine, azobenzene, or naphthopyran.

[0027] According to the preparation method of the present invention, preferably, antioxidant A and antioxidant B are independently selected from at least one of tert-butylhydroxyanisole (BHA), dibutylhydroxytoluene (BHT), tert-butylhydroquinone (TBHQ), propyl gallate (PG), ascorbyl palmitate (AP), dilauryl thiodipropionate (DLTP), and 4-hexylresorcinol (4-HR).

[0028] According to the preparation method of the present invention, preferably, the ultraviolet absorber is selected from at least one of salicylates, benzophenones, benzotriazoles, substituted acrylonitriles, triazines, and hindered amines.

[0029] More preferably, the ultraviolet absorber is selected from at least one of phenyl salicylate, benzotriazole, 2-(2'-hydroxy-5'-methylphenyl)benzotriazole, 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-n-octoxybenzophenone, 2-(2'-hydroxy-3',5'-diphenyl)-5-chlorobenzotriazole, resorcinol monobenzoate, 2,2'-thiobis(4-tert-octylphenoxy)nickel, tris(1,2,2,6,6-pentamethylpiperidyl) phosphite, 4-benzoyloxy-2,2,6,6-tetramethylpiperidine, 2,4,6-tris(2'-n-butoxyphenyl)-1,3,5-triazine, and hexamethylphosphoric triamide.

[0030] Even more preferably, the ultraviolet absorber is phenyl salicylate, benzotriazole, 2,4-dihydroxybenzophenone, or 4-benzoyloxy-2,2,6,6-tetramethylpiperidine.

[0031] According to the preparation method of the present invention, preferably, the oil-soluble solvent is selected from at least one of isopentane, n-pentane, petroleum ether, hexane, cyclohexane, isooctane, trimethylpentane, cyclopentane, heptane, dioxane in alkanes; methylamine, dimethylamine, 1,1-dichloromethane, 1,1,1-trichloromethane, nitromethane, chloroform, trichlorotrifluoroethane, carbon tetrachloride, trichloroethylene, dichloroethylene, butyl chloride, N,N-dimethylformamide, N,N-dimethylacetamide, N-methylformamide, dimethylformamide, dimethyl sulfoxide in alkane derivatives; isopropyl alcohol, isobutyl alcohol, n-butanol, propyl ether, diethyl ether, phenol in alcohols and ethers; aldehydes and ketones, organic acids, organic esters; benzene, toluene, xylene, p-xylene, m-xylene, chlorobenzene, o-dichlorobenzene, aniline in benzene series.

[0032] More preferably, the oil-soluble solvent is a more commonly used solvent such as isopentane, N,N-dimethylacetamide, or dimethylformamide.

[0033] According to the preparation method of the present invention, preferably, the emulsifier is selected from at least one of Crescent-300, CENTELIUS-XI-01, fatty amine polyoxyethylene ether, de-sugared sodium lignosulfonate M-9, carboxymethyl cellulose and its derivatives.

[0034] According to the preparation method of the present invention, preferably, the capsule wall material is selected from at least one of amino resin, polyacrylamide, polyacrylic acid, polyvinylpyrrolidone, polyvinyl alcohol, polymaleic anhydride, polyquaternary ammonium salt, polyethylene glycol, arabic gum, gelatin, sodium alginate, chitosan.

[0035] More preferably, the capsule wall material is amino resin, chitosan, polyacrylamide or polyacrylic acid.

[0036] According to the preparation method of the present invention, preferably, the magnetic substance is selected from at least one of AlNi(Co), FeCr(Co), FeCrMo, FeAlC, FeCo(V)(W), Re-Fe, FeCrCo, PtCo, MnAlC, CuNiFe, AlMnAg.

[0037] More preferably, the magnetic substance is AlNi, MnAlC, CuNiFe or PtCo.

[0038] According to the preparation method of the present invention, preferably, the particle size range of the magnetic substance is 0.1 nm to 5 nm; for example, 0.2 nm to 0.5 nm, 1 nm to 3 nm, 0.1 nm to 0.5 nm or 2 nm to 5 nm.

[0039] According to the preparation method of the present invention, preferably, the particle size of the photochromic microcapsule is 0.01 nm to 10,000 nm.

[0040] In the preparation method of the present invention, the spinning dope of the polybutylene succinate fiber can be prepared by existing processes. The spinning can be carried out by existing conventional spinning processes such as melt spinning, electrospinning, etc. The present invention does not make any limitation in this regard.

[0041] On the other hand, the present invention provides a polybutylene succinate composite fiber obtained by any one of the above preparation methods.

[0042] The capsule wall material of the photochromic microcapsules of the present invention contains magnetic substances. The magnetic substances will be attracted by an external magnetic field and tend to disperse away from the wall material. However, as the degree of polymerization of the capsule wall material increases, its viscosity also increases, which will restrict the escape of the magnetic substances, thereby forming a star-shaped radiation structure on the outside of the capsule wall material, increasing the surface roughness of the microcapsules, avoiding the aggregation of the microcapsules, and being more conducive to its combination with the spinning solution of polybutylene succinate, so that it is more evenly dispersed in the fiber, and thus has a better light-emitting effect. By controlling the self-polymerization rate of the capsule wall material and the intensity of the external magnetic field, the movement of the magnetic substances can be controlled, thereby the shape of the microcapsule shell can be controlled, and thus various spinning methods can be matched.

[0043] The polybutylene succinate composite fiber prepared by the method of the present invention has the advantages of excellent photochromism, uniform photochromism, fast response time, simple production method, etc., and is biodegradable, avoiding environmental pollution and resource waste, and can be widely used in the fields of advertising, anti-counterfeiting, clothing and apparel, etc., and can meet the diverse and functional needs of the market. Specific embodiments

[0044] In order to more clearly illustrate the present invention, the present invention will be further described below in conjunction with preferred embodiments. Those skilled in the art should understand that the specific content described below is illustrative rather than restrictive, and should not be used to limit the protection scope of the present invention.

[0045] All numerical designations of the present invention (such as temperature, time, concentration, weight, etc., including the range of each of them) can generally be approximate values that can be appropriately changed (+) or (-) in increments of 0.1 or 1.0. All numerical designations can be understood as being preceded by the term "about".

[0046] Example 1

[0047] This example prepares a polybutylene succinate composite fiber, which includes the following steps:

[0048] 1) Add 30 g of diarylethene, 1 g of tert-butylhydroxyanisole, and 0.6 g of phenyl salicylate to 50 g of isopentane and stir evenly at 70 °C.

[0049] 2) Add the uniformly mixed solution to 410 g of an aqueous solution containing 0.1 wt% CENTELIUS-XI-01, and then stir at a speed of 20000 rpm for 30 min to obtain an oil-in-water emulsion. Adjust the pH of the emulsion to 7 with hydrochloric acid solution, and control the temperature at 60 °C.

[0050] 3) Dissolve 30 g of amino resin in 40 mL of water, then add 20 g of AlNi with a particle size of 0.2 nm to 0.5 nm, stir evenly, and then slowly add it to the oil-in-water emulsion obtained above. Place it in an external magnetic field with a strength of 1 mT and keep it at 60 °C for 3 hours to prepare photochromic microcapsules with a special star-shaped structure on the shell; then filter, wash, and dry.

[0051] 4) Add the photochromic microcapsules prepared above to the melt spinning stock solution of polybutylene succinate in a mass ratio of 99:1. In addition, add 0.5 parts of antioxidant dibutylhydroxytoluene and mix evenly. Then carry out spinning through the process of melt spinning, adjust the temperature of each zone of the torque rheometer and the screw extruder, control the appropriate extrusion speed, extrude polybutylene succinate fibers containing photochromic microcapsules, and then carry out side blowing for cooling at a wind speed of 0.3 m / s, a humidity of 70% RH, and a temperature of 25 °C, oiling, winding, and stretching with a draw ratio of 1:3 to obtain degradable polybutylene succinate composite fibers.

[0052] Example 2

[0053] This example prepares a polybutylene succinate composite fiber, including the following steps:

[0054] 1) Add 25 g of spiropyran, 0.8 g of dibutylhydroxytoluene, and 1 g of benzotriazole to 60 g of N,N-dimethylacetamide and stir evenly at 80 °C.

[0055] 2) Add the evenly mixed solution to 567 g of an aqueous solution containing 15 wt% CENTELIUS-XI-01, and then stir at a speed of 10,000 rpm for 20 min to obtain an oil-in-water emulsion. Adjust the pH of the emulsion to 8 with hydrochloric acid solution and control the temperature at 100 °C.

[0056] 3) Dissolve 28 g of chitosan in 38 mL of water, then add 15 g of MnAlC powder with a particle size of 1 nm to 3 nm, stir evenly, and then slowly add it to the oil-in-water emulsion obtained above. Place it in an external magnetic field with a strength of 1 mT and keep it at 90 °C for 0.3 hours to prepare photochromic microcapsules with a special star-shaped structure on the shell, and then filter, wash, and dry.

[0057] 4) Add the above-prepared photochromic microcapsules to the electrospinning stock solution of polybutylene succinate in a mass ratio of 95:5. In addition, add 1 part of antioxidant propyl gallate and mix evenly. Then, perform electrospinning. After high-speed shear emulsification, filtration, and vacuum degassing, electrospinning is carried out (the electrospinning process parameters are voltage of 18 KV, flow rate of 10 mL / h, receiving distance of 20 cm, and rotation speed of the receiving hub of 400 rpm) to obtain a degradable polybutylene succinate composite fiber containing photochromic microcapsules.

[0058] Example 3

[0059] This example prepares a polybutylene succinate composite fiber, including the following steps:

[0060] 1) Add 20 g of azobenzene, 0.6 g of ascorbyl palmitate, and 2 g of 2,4-dihydroxybenzophenone to 90 g of N,N-dimethylformamide and stir evenly at 75 °C.

[0061] 2) Add the evenly mixed solution to 1126 g of an aqueous solution containing 0.1 wt% Crescent-300, and then stir at a speed of 30000 rpm for 10 min to obtain an oil-in-water emulsion. Adjust the pH of the emulsion to 3 with hydrochloric acid solution, and control the temperature at 20 °C.

[0062] 3) Dissolve 26 g of polyacrylamide in 35 mL of water, add 10 g of CuNiFe powder with a particle size of 0.1 nm - 0.5 nm, stir evenly, and then slowly add it to the above-obtained oil-in-water emulsion. Place it in an external magnetic field with a strength of 2 mT and keep it at 20 °C for 5 hours to prepare photochromic microcapsules with a special star-shaped structure on the shell. Then, perform filtration, washing, and drying.

[0063] 4) Add the above-prepared photochromic microcapsules to the electrospinning stock solution of polybutylene succinate in a mass ratio of 97:3. In addition, add 0.6 part of antioxidant dilauryl thiodipropionate and mix evenly. Then, perform electrospinning. After high-speed shear emulsification, filtration, and vacuum degassing, electrospinning is carried out (the electrospinning process parameters are voltage of 25 KV, flow rate of 15 mL / h, receiving distance of 22 cm, and rotation speed of the receiving hub of 520 rpm) to obtain a degradable polybutylene succinate composite fiber containing photochromic microcapsules.

[0064] Example 4

[0065] This example prepares a polybutylene succinate composite fiber, including the following steps:

[0066] 1) Add 15 g of naphthopyran, 2 g of dilauryl thiodipropionate, and 0.5 g of 4-benzoyloxy-2,2,6,6-tetramethylpiperidine to 30 g of N,N-dimethylformamide and stir evenly at 70 °C.

[0067] 2) Then add the evenly mixed solution to 475 g of an aqueous solution containing 5 wt% of de-sugared lignosulfonate M-9, and then stir at a speed of 15000 rpm for 20 min to obtain an oil-in-water emulsion. Adjust the pH of the emulsion to 5 with a hydrochloric acid solution and control the temperature at 50 °C.

[0068] 3) Dissolve 25 g of polyacrylic acid in 30 mL of water, add 5 g of PtCo powder with a particle size of 2 nm to 5 nm, stir evenly, and then slowly add it to the above-obtained oil-in-water emulsion. Place it in an external magnetic field with a strength of 2 mT and keep it at 50 °C for 2.5 hours to prepare photochromic microcapsules with a special star-shaped structure on the shell. Then filter, wash, and dry.

[0069] 4) Add the above-prepared photochromic microcapsules to the melt spinning stock solution of polybutylene succinate in a mass ratio of 97:3. In addition, add 1.5 parts of the antioxidant 4-hexylresorcinol and mix evenly. Then carry out spinning through the melt spinning process, adjust the temperatures of each zone of the torque rheometer and the screw extruder, control the appropriate extrusion speed, extrude polybutylene succinate fibers containing photochromic microcapsules, and then carry out side blowing for cooling with a wind speed of 0.5 m / s, a humidity of 85% RH, and a temperature of 27 °C, oiling, winding, and stretching with a draw ratio of 1:1 to obtain degradable polybutylene succinate composite fibers.

[0070] Comparative Example 1

[0071] This comparative example prepares a polybutylene succinate composite fiber, including the following steps:

[0072] 1) Add 30 g of diarylethene, 1 g of tert-butylhydroxyanisole, and 0.6 g of phenyl salicylate to 50 g of isopentane and stir evenly at 70 °C.

[0073] 2) Add the evenly mixed solution to 410 g of an aqueous solution containing 0.1 wt% of CENTELIUS-XI-01, and then stir at a speed of 20000 rpm for 30 min to obtain an oil-in-water emulsion. Adjust the pH of the emulsion to 7 with a hydrochloric acid solution and control the temperature at 60 °C.

[0074] 3) Dissolve 30 g of amino resin in 40 mL of water, stir evenly, and then slowly add it to the above-obtained oil-in-water emulsion. Place it in an external magnetic field with a strength of 1 mT and keep it at 60 °C for 3 hours to prepare photochromic microcapsules; then filter, wash, and dry.

[0075] 4) Add the above-prepared photochromic microcapsules to the melt spinning stock solution of polybutylene succinate in a mass ratio of 99:1. In addition, add 0.5 parts of antioxidant dibutylhydroxytoluene and mix evenly. Then, carry out spinning through the process of melt spinning, adjust the temperatures of each zone of the torque rheometer and the screw extruder, control the appropriate extrusion speed, extrude the polybutylene succinate fiber containing photochromic microcapsules, and then carry out side blowing for cooling with a wind speed of 0.3 m / s, a humidity of 70% RH, and a temperature of 25 °C, oiling, winding, and stretching with a draw ratio of 1:3 to obtain the degradable polybutylene succinate composite fiber.

[0076] Comparative Example 2

[0077] This comparative example prepares a polybutylene succinate composite fiber, including the following steps:

[0078] 1) Add 20 g of azobenzene, 0.6 g of ascorbyl palmitate, and 2 g of 2,4-dihydroxybenzophenone to 90 g of N,N-dimethylformamide and stir evenly at 75 °C.

[0079] 2) Add the evenly mixed solution to 1126 g of an aqueous solution containing 0.1 wt% Crescent-300, and then stir at a speed of 30000 rpm for 10 min to obtain an oil-in-water emulsion. Adjust the pH of the emulsion to 3 with a hydrochloric acid solution and control the temperature at 20 °C.

[0080] 3) Dissolve 26 g of polyacrylamide in 35 mL of water, add 10 g of CuNiFe powder with a particle size of 0.1 nm - 0.5 nm, stir evenly, and then slowly add it to the above-obtained oil-in-water emulsion. Place it in an external magnetic field with a strength of 2 mT and keep it warm at 20 °C for 5 hours to prepare photochromic microcapsules with a special star-shaped structure on the shell; then carry out filtration and washing, and drying.

[0081] 4) Add 0.6 parts of antioxidant dilauryl thiodipropionate to 97 parts of the electrospinning stock solution of polybutylene succinate and mix evenly. Then, carry out spinning through the process of electrospinning. After high-speed shear emulsification, filtration, and vacuum degassing, electrospinning is carried out (the electrospinning process parameters are a voltage of 25 KV, a flow rate of 15 mL / h, a receiving distance of 22 cm, and a rotation speed of the receiving hub of 520 rpm) to obtain the degradable polybutylene succinate fiber.

[0082] 5) 3 parts of photochromic microcapsules, taking a proportion of 3 parts compared to 97 parts of the spinning dope, are dispersed in 100 parts of a water / ethanol solution. The polybutylene succinate fiber is dip-dyed and padded in the solution and then dried at a constant temperature of 50 °C to obtain a degradable polybutylene succinate composite fiber containing photochromic microcapsules.

[0083] The photochromic properties of the composite fibers prepared in Examples 1 to 4 and Comparative Examples 1 to 2 were tested: in an indoor environment of 20 to 25 °C, the samples were irradiated with a 32W ultraviolet lamp from a distance of 10 cm for 30 s, and a CIE software was used for color analysis of the color change stability. The test results are shown in Table 1 below:

[0084] Table 1 Photochromic test results

[0085] Sample ΔE L* a* b* Pure PBS fiber 0 89.51 0.09 1.21 Example 1 65.32 25.74 3.11 -16.27 Example 2 62.76 28.46 2.61 -16.53 Example 3 59.44 30.49 2.03 -14.98 Example 4 57.21 32.53 1.01 -13.47 Comparative Example 1 1.05 88.47 0.12 1.16 Comparative Example 2 11.54 77.32 0.42 0.17

[0086] It can be seen from the results in Table 1 that the photochromic effect of the fiber is closely related to the dispersion or aggregation state of the photochromic microcapsules in the PBS matrix. When the microcapsules were dispersed and attached to the fiber by the dip-rolling method in Comparative Example 2, the photochromic property was weak. However, when the microcapsules were introduced by preparing a homogeneous spinning solution for spinning, the microcapsules were evenly dispersed inside the fiber and the photochromic property was strong. And the photochromism is directly related to the magnetic material, and the magnetic material undergoes magneto-optical effect and magnetostrictive effect under the action of an electromagnetic field. By adjusting the content of the microcapsules, the fiber color-changing function can be achieved.

[0087] Obviously, the above-mentioned embodiments of the present invention are merely examples for clearly illustrating the present invention, rather than limitations on the implementation manners of the present invention. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is impossible to list all the implementation manners here. Any obvious changes or modifications derived from the technical solutions of the present invention still fall within the protection scope of the present invention.

Claims

1. A method for preparing a polybutylene succinate composite fiber, wherein, The preparation method includes: 1) Dissolve a photochromic dye, antioxidant A, and an ultraviolet absorber in an oil-soluble solvent to obtain an oil-phase solution; 2) Add the oil-phase solution to an aqueous solution containing an emulsifier and emulsify to obtain an oil-in-water emulsion; adjust the pH of the emulsion to 3-8 and the temperature to 20-100 °C; 3) Add a capsule wall material and a magnetic substance to water and uniformly add it to the emulsion, place it in an externally applied magnetic field with a controllable intensity, and keep it at 20-90 °C for 0.3-5 hours to obtain a photochromic microcapsule with a special structure on the shell; 4) Add the photochromic microcapsule to the spinning dope of polybutylene succinate fiber, and then carry out spinning to obtain the polybutylene succinate composite fiber.

2. The preparation method according to claim 1, wherein In step 1), the mass ratio of the photochromic dye, antioxidant A, ultraviolet absorber, and oil-soluble solvent is (20-60):(0.5-10):(1-5):

100.

3. The preparation method according to claim 1, wherein, In the aqueous solution containing the emulsifier, the concentration of the emulsifier is 0.1 wt% - 15 wt%.

4. The preparation method according to claim 1, wherein In step 2), the mass ratio of the oil-phase solution to the aqueous solution containing the emulsifier is 1:(5-10).

5. The preparation method according to claim 1, wherein In step 3), the mass ratio of the capsule wall material, magnetic substance, and water is (25-30):(5-20):(30-40).

6. According to the preparation method described in claim 1, wherein, In step 3), the mass ratio of the aqueous solution containing the capsule wall material and the magnetic substance to the emulsion is 1:(4-18).

7. The preparation method according to claim 1, wherein, The magnetic field is an alternating electromagnetic field, and the intensity range is 1-2 mT.

8. The preparation method according to claim 1, wherein, In step 4), based on the total mass of the spinning dope and the photochromic microcapsule being 100 parts, the mass part of the photochromic microcapsule is 1-5.

9. The preparation method according to claim 8, wherein, Antioxidant B is also added to the spinning dope; based on the total mass of the spinning dope and the photochromic microcapsule being 100 parts, the mass part of antioxidant B is 0.5-1.

5.

10. The preparation method according to claim 1, wherein Adjust the pH of the emulsion to 3-8 with a hydrochloric acid solution.

11. According to the preparation method described in claim 1, wherein, The photochromic dye is selected from at least one of naphthospiropyrans, spirooxazines, diarylethylenes, azobenzenes, fulgides, naphthopyrans, transition metal oxides, metal halides, and rare earth complexes.

12. The preparation method according to claim 9, wherein, Antioxidant A and antioxidant B are independently selected from at least one of tert-butylhydroxyanisole, dibutylhydroxytoluene, tert-butylhydroquinone, propyl gallate, ascorbyl palmitate, dilauryl thiodipropionate, and 4-hexylresorcinol.

13. The preparation method according to claim 1, wherein The ultraviolet absorber is selected from at least one of salicylates, benzophenones, benzotriazoles, substituted acrylonitriles, triazines, and hindered amines.

14. The preparation method according to claim 1, wherein, The oil-soluble solvent is selected from at least one of isopentane, n-pentane, petroleum ether, hexane, cyclohexane, isooctane, trimethylpentane, cyclopentane, heptane, dioxane, methylamine, dimethylamine, 1,1-dichloromethane, 1,1,1-trichloromethane, nitromethane, chloroform, trichlorotrifluoroethane, carbon tetrachloride, trichloroethylene, dichloroethylene, butyl chloride, N,N-dimethylformamide, N,N-dimethylacetamide, N-methylformamide, dimethylformamide, dimethyl sulfoxide, isopropanol, isobutanol, n-butanol, propyl ether, diethyl ether, phenol, aldehyde, ketone, organic acid, organic ester, benzene, toluene, xylene, p-xylene, m-xylene, chlorobenzene, o-dichlorobenzene, aniline.

15. According to the preparation method described in claim 1, wherein The emulsifier is selected from at least one of Crescent-300, CENTELIUS-XI-01, fatty amine polyoxyethylene ether, de-sugared sodium lignosulfonate M-9, and carboxymethyl cellulose and its derivatives.

16. The preparation method according to claim 1, wherein, The capsule wall material is selected from at least one of amino resin, polyacrylamide, polyacrylic acid, polyvinylpyrrolidone, polyvinyl alcohol, poly maleic anhydride, polyquaternary ammonium salt, polyethylene glycol, arabic gum, gelatin, sodium alginate, chitosan.

17. The preparation method according to claim 1, wherein, The magnetic material is selected from at least one of AlNi(Co), FeCr(Co), FeCrMo, FeAlC, FeCo(V)(W), Re-Fe, FeCrCo, PtCo, MnAlC, CuNiFe, AlMnAg.

18. The preparation method according to claim 17, wherein The particle size range of the magnetic material is 0.1 nm to 5 nm.

19. The preparation method according to claim 1, wherein, The particle size of the photochromic microcapsule is 0.01 nm to 10,000 nm.

20. A polybutylene succinate composite fiber obtained by the preparation method according to any one of claims 1-19.