[0071] By adopting the preparation method provided by the invention, the composite spinning of the polymer and the aggregation-induced luminescent AIE molecule is realized to prepare the composite luminescent fiber. Because the AIE molecule has high luminescence under the excitation of ultraviolet light, and the polymer can provide the mechanical properties required by the composite fiber, the formed polymer/AIE composite luminescent fiber has excellent luminescence and mechanical properties that meet the requirements.
[0072] According to the present invention, the first solvent and the second solvent are each independently selected from at least one of dichloromethane, cyclohexane, phenol, toluene, acetonitrile, chlorobenzene, and methyl acetate.
[0073] According to the present invention, in step 4), the conditions of the pre-curing treatment are: the pre-curing temperature is 40-80° C., and the pre-curing time is 5-40 min.
[0074] In the present invention, the pre-curing treatment can be performed in an oven.
[0075] According to the present invention, the cooling conditions include: the cooling time is 1-50 min.
[0076] In the present invention, the inventors have observed that the pre-curing treatment can adjust the viscosity of the polymer/AIE composite liquid to make it suitable for subsequent spinning processing, and can realize that such (polymer/AIE composite liquid) materials can be made into fibers. And after research, it is found that when the pre-curing temperature is in the range of 40-80°C, the pre-curing is 5-40 min, and the cooling time is in the range of 1-50 min, the composite liquid has the most suitable viscosity.
[0077] In the present invention, during the process of transferring the spinning solution to the spinning equipment for spinning, it is necessary to avoid the generation of bubbles in the spinning solution, so as to reduce the influence of the bubbles in the spinning solution on the spinning process, thereby leading to the spinning process. The mechanical properties of the fiber are reduced.
[0078] According to the present invention, the spinning step specifically includes: transferring the spinning solution to an extrusion device, extruding the spinning solution into an oil bath at a speed of 1-10ml/min for solidification and molding, and then at a speed of 1-3m The line speed of /min is collected on the spool.
[0079] In the present invention, an extrusion device commonly used in the field can be selected, and preferably, a syringe is selected as the extrusion device.
[0080] More preferably, the volume of the extrusion device is 50-100 ml.
[0081] In the present invention, the curing time is 1-10s.
[0082] Preferably, the pre-curing temperature is 50-70°C, the pre-curing time is 10-25 min, and the cooling time is 5-30 min.
[0083] In the present invention, it is necessary to ensure that the curing bath forms a uniform temperature field during the spinning process. Because the fiber is cured very fast in the spinning curing bath, if the temperature field is not uniform, the polymer/AIE composite obtained by spinning The diameter of the luminescent fiber is uneven, which affects the fiber quality.
[0084] According to the present invention, in step 5), the temperature of the spinning curing bath is 110°C-240°C, preferably 150°C-200°C.
[0085] In the present invention, the spinning solidification bath is an oil bath system, preferably a silicone oil system.
[0086] In the present invention, the diameter of the polymer/aggregation-induced luminescent molecule composite luminescent fiber with different diameters is obtained by adjusting the diameter of the outlet of the extrusion device.
[0087] In the present invention, the diameter of the polymer/aggregation-inducing light-emitting molecule composite light-emitting fiber is 100 μm-1000 μm, preferably 500 μm.
[0088] According to the present invention, in step 5), the washing detergent is deionized water and/or ethanol, preferably deionized water.
[0089] In the present invention, the washing process includes: washing with deionized water is 1-3 times.
[0090] According to the present invention, in step 5), the drying conditions include: a drying temperature of 40-90°C, preferably 50-70°C, and a drying time of 10-60 min, preferably 20-40 min.
[0091] In the present invention, the preparation steps of selecting polydimethylsiloxane PDMS as a polymer and aggregation-induced luminescence AIE molecules to prepare a luminescent composite material include:
[0092] Step 1): Add the aggregation-induced luminescence AIE molecules to an organic solvent to dissolve them to obtain an aggregation-induced luminescence AIE molecule solution;
[0093] Step 2): Add the A component of the polydimethylsiloxane PDMS to the aggregation-induced luminescence AIE molecule solution, stir until the mixture is uniform, and vacuum dry to obtain the A component composite solution of AIE@PDMS;
[0094] Step 3): Add the B component of the polydimethylsiloxane PDMS to the A component composite liquid of AIE@PDMS, and stir until the mixture is uniform to obtain the AIE@PDMS composite liquid;
[0095] Step 4): Pre-solidify the AIE@PDMS composite solution and cool to obtain a spinning solution;
[0096] Step 5): In the spinning equipment, the spinning solution is placed in a spinning curing bath for spinning, washing, and drying to obtain composite luminescent fiber.
[0097] In the present invention, the polydimethylsiloxane PDMS is composed of two parts: the body (A) and the curing agent (B). Specifically, the polydimethylsiloxane PDMS is commercially available, for example, Sylgard 184 product of Dow Corning, USA.
[0098] In the present invention, it is preferable to use polydimethylsiloxane PDMS as the polymer and aggregation-induced luminescence AIE molecules to prepare the luminescent composite material. As polydimethylsiloxane PDMS has excellent elasticity and transparency, the formed PDMS/AIE composite luminescent fiber has excellent luminescence and elasticity.
[0099] Further, in step 2), the weight ratio of the aggregation-induced luminescence AIE molecule to the A component of the polydimethylsiloxane PDMS is (0.5:1000)-(65:1000), preferably (1.1 :1000)-(57:1000), more preferably (5:1000)-(15:1000).
[0100] In the present invention, the bulk A component of the PDMS and the aggregation-induced luminescence AIE molecule are mixed in advance, and dried in a vacuum to obtain the A component composite liquid of AIE@PDMS. Through research, it is found that when the weight ratio of the aggregation-induced luminescence AIE molecule to the A component of the polydimethylsiloxane PDMS is (0.5:1000)-(65:1000), the final composite luminescent fiber is simultaneously It has excellent light-emitting properties and flexibility.
[0101] More preferably, when the weight ratio of the aggregation-inducing luminescence AIE molecule to the A component of the polydimethylsiloxane PDMS is (1.1:1000)-(57:1000), further preferably, when the aggregation-inducing When the weight ratio of the light-emitting AIE molecule to the A component of the polydimethylsiloxane PDMS is (5:1000)-(15:1000), the prepared composite light-emitting fiber has more excellent performance.
[0102] In order to remove the adverse effects of organic solvents on subsequent operation steps, in the present invention, preferably, the uniform mixture of polydimethylsiloxane and aggregation-inducing luminescent molecules is vacuum dried. Research has found that the drying temperature is 30°C. After drying for 1-6h at -90℃, the organic solvent in the aforementioned mixed solution can be removed.
[0103] Further research has found that the drying temperature of vacuum drying is preferably 40°C-80°C, and the drying time is preferably 2-4h.
[0104] When the body A and the curing agent B are mixed and heated, the mixture will undergo a cross-linking reaction to solidify the liquid PDMS to form a solid product. Different weight ratios of the body and curing agent will affect the performance of the final product.
[0105] In order to obtain a composite luminescent fiber with excellent luminescence performance, flexibility and elasticity, the inventors studied the weight ratio of the body A to the curing agent B, the pre-curing temperature and the pre-curing time in PDMS. When the weight ratio of the B component of the polysiloxane PDMS to the A component of the polydimethylsiloxane PDMS is 0.1-6:10, the prepared composite light-emitting fiber has excellent elasticity and does not affect the composite light-emitting fiber The luminous performance.
[0106] Preferably, the weight ratio of the body A to the curing agent B is 0.5-3:10, more preferably 1-2:10.
[0107] According to the present invention, the drying conditions include: a drying temperature of 40-90°C, preferably 50-70°C, and a drying time of 10-60 min, preferably 20-40 min.
[0108] The third aspect of the present invention provides an application of the composite light-emitting fiber according to the present invention or the composite light-emitting fiber produced by the method of the present invention, wherein the application is a flexible wearable device.
