CN113388939A - Preparation method and application of core-shell type composite fluorescent fiber - Google Patents
Preparation method and application of core-shell type composite fluorescent fiber Download PDFInfo
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- CN113388939A CN113388939A CN202110684669.7A CN202110684669A CN113388939A CN 113388939 A CN113388939 A CN 113388939A CN 202110684669 A CN202110684669 A CN 202110684669A CN 113388939 A CN113388939 A CN 113388939A
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/12—Threads containing metallic filaments or strips
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/16—Yarns or threads made from mineral substances
- D02G3/18—Yarns or threads made from mineral substances from glass or the like
- D02G3/182—Yarns or threads made from mineral substances from glass or the like the glass being present only in part of the structure
- D02G3/185—Yarns or threads made from mineral substances from glass or the like the glass being present only in part of the structure in the core
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/14—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a preparation method and application of a core-shell type composite fluorescent fiber, wherein the method comprises the steps of mixing a fluorescent polymer, an organic solvent and a volatility adjusting solvent, oscillating until the fluorescent polymer is fully dissolved, and preparing to obtain a polymer solution; and then, taking the polymer solution as spinning solution for electrostatic spinning, receiving by using a core fiber bundle, and forming a coating film on the surface of the core fiber bundle, wherein the core fiber bundle keeps a rotating state in the receiving process and moves left and right in the rotating axis direction. The method can uniformly coat the core fiber bundle in all directions, has simple process and easy operation, and can be applied to surface coating of filaments and strips such as glass fibers, yarns, metal wires, fine rods and the like; the prepared core-shell type composite fluorescent fiber has good cladding property, uniform surface fiber winding, random arrangement, obvious fluorescent intensity, excellent flexibility effect and wider application range.
Description
Technical Field
The invention belongs to the technical field of surface coating of composite fiber yarns, and particularly relates to a preparation method and application of a core-shell type composite fluorescent fiber.
Background
Most of the existing fluorescent fibers are prepared by doping fluorescent particles or blending the fluorescent particles with composite fibers, and the fluorescent effect of the existing fluorescent fibers cannot meet the requirements of more application scenes and limits materials.
Most of the surface coating methods of the composite fiber filaments are soaking and scraping methods, however, the polymer composite fibers prepared by the soaking and scraping methods have the problems of insufficient and uniform surface coating, poor flexibility effect, easy brittle fracture and the like. The electrostatic spinning method can be used for preparing fibers with the diameter ranging from a few nanometers to a few micrometers, the formed fibers have outstanding scale effect and surface/interface effect, and the prepared composite material has good flexibility effect. However, in the conventional electrospinning process, the composite fibers of the core are mostly fixed during the receiving process, which also causes uneven surface coating of the composite fiber bundle of the core.
Disclosure of Invention
The invention aims to overcome the defects, and provides a preparation method of a core-shell type composite fluorescent fiber, which has the advantages of simple process and easy operation, and the obtained composite fluorescent fiber material is uniformly coated, has obvious fluorescent intensity and excellent flexibility effect, and can be applied to surface coating of filaments and strips such as glass fibers, yarns, metal wires, thin rods and the like.
In order to realize the purpose, the invention is realized by the following technical scheme:
a preparation method of a core-shell type composite fluorescent fiber comprises the following steps:
mixing a fluorescent polymer, an organic solvent and a volatility adjusting solvent, and oscillating until the fluorescent polymer is fully dissolved to prepare a polymer solution;
the polymer solution is used as spinning solution for electrostatic spinning, a core fiber bundle is used for receiving, a coating film is formed on the surface of the core fiber bundle, and the core fiber bundle keeps a rotating state in the receiving process and moves left and right in the rotating axis direction.
Preferably, the fluorescent polymer is one of polyimide containing pyrene, polyimide containing fluorene, polyimide containing naphthalene, polyarylether containing pyrene, polyarylether containing fluorene or polyarylether containing naphthalene.
Preferably, the concentration of the polymer solution is 8 wt% to 25 wt%, and the concentration of the prepared polymer solution is 18 wt%.
Preferably, the volume ratio of the organic solvent to the volatility adjusting solvent is 7: 3-9: 1. The organic solvent may be DMAc, DMF or CHCl3The volatility adjusting solvent can be NMP, ethanol, acetone or CHCl2。
Preferably, the core fiber bundle may use a glass fiber bundle.
Preferably, the electrostatic spinning process is as follows: the spinning voltage is 12-14 kV, the orifice aperture is 0.5mm, the receiving distance is 15-20 cm, the spinning solution is 1-5 mL, the spinning solution propelling speed is 2-5 mL/h, and the room temperature and the air relative humidity are 25-50%.
Preferably, the form of the spun fiber can be controlled by adjusting the electrospinning process and the concentration of the spinning solution, and long fibers are formed when the polymer solution having a concentration of 11 to 25 wt% is used for electrospinning, and short fibers are formed when the polymer solution having a concentration of 6 to 10 wt% is used for electrospinning.
Preferably, the invention can adopt a speed-adjustable receiving device provided with a detachable movable rotating plate and a multi-filament fixed rotating disc, and the speed-adjustable receiving device is replaced according to the required receiving method; when short fibers are received, a multi-filament fixed rotation method is used, namely a plurality of single-bundle core fibers are fixed around a disc of a receiving device, the circle center of the disc is used as an axis, and the fixed core fiber bundles are driven to receive by rotating the disc, so that more efficient production is realized.
Preferably, if concentrated solution is used for spinning fiber coating, 1mL of spinning solution is sucked; if the thin solution spinning fiber is used for coating, 3mL of spinning solution is absorbed, so that the coating layer is prevented from being too thick.
Preferably, the adjustable range of the rotation speed of the core fiber bundle is 50-200 r/min, and the adjustable range of the movement speed is 5-15 m/h.
Preferably, the diameter of the core fiber bundle is 200-300 μm, and the thickness of the coating film is 100-150 μm.
The invention also provides application of the core-shell type composite fluorescent fiber in fluorescent anti-counterfeiting, flexible imaging or intelligent wearable equipment.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the core-shell type composite fluorescent fiber provided by the invention can uniformly coat the core fiber bundle in all directions, has simple process and easy operation, and can be applied to surface coating of filaments and strips such as glass fibers, yarns, metal wires, fine rods and the like.
(2) The preparation method can control the form of the spinning fiber by adjusting the electrostatic spinning process and the concentration of the spinning solution according to different requirements, and adopts different receiving methods aiming at different fiber forms, thereby being beneficial to fiber coating and improving the production efficiency.
(3) The core-shell type composite fluorescent fiber prepared by the method has good cladding property, uniform winding of surface fibers, random arrangement, obvious fluorescent intensity, excellent flexibility effect and wider application range.
Drawings
FIG. 1 is a process flow chart of the preparation of pyrene-containing polyimide-glass fiber composite fluorescent fiber.
FIG. 2 is a surface SEM image of pyrene-containing polyimide-glass fiber composite fluorescent fiber prepared in example 1 of the present invention;
FIG. 3 is a SEM image of a section of a pyrene-containing polyimide-glass fiber composite fluorescent fiber prepared in example 1 of the present invention;
FIG. 4 is a fluorescence emission spectrum of a pyrene-containing polyimide-glass fiber composite fluorescent fiber prepared in example 2 of the present invention;
FIG. 5 is a TGA spectrum of pyrene-containing polyimide-glass fiber composite fluorescent fiber prepared in example 3 of the present invention;
FIG. 6 is a comparison graph of a pure glass fiber and a pyrene-containing polyimide-glass fiber composite fluorescent fiber prepared in example 1 of the present invention under daily light irradiation and ultraviolet light irradiation, respectively.
Detailed Description
Preferred embodiments of the present invention will be described in more detail with reference to specific examples.
The following are the raw materials or drugs used in the examples:
pyrene-containing polyimide: prepared according to patent 201910686570.3.
DMAc: chemical purity; shanghai Lingfeng Chemicals, Inc.
Ethanol: analyzing and purifying; chemical agents of the national drug group, ltd.
Glass fiber: the diameter of each fiber is 12 micrometers, and the length of each fiber is 55 centimeters; shanghai Guang rubber and Plastic hardware Limited.
Example 1
The preparation method of the core-shell pyrene-containing polyimide-glass fiber composite fluorescent fiber comprises the following basic steps:
(1) adding pyrene-containing polyimide, DMAc and ethanol into a reaction bottle, and slightly oscillating to fully dissolve the polymer; wherein the volume ratio of DMAc to ethanol is 9:1, and the pyrene-containing polyimide solution with the mass concentration of 18 wt% is prepared.
(2) And (3) taking the 18 wt% pyrene-containing polyimide solution as a spinning solution, spraying the spinning solution on the surface of a glass fiber bundle by using an electrostatic spinning method to form a coating film, and adopting a receiving device which is a speed-adjustable and rotatable receiving device.
The electrospinning process used in this example was: taking 1mL of spinning solution, adjusting the voltage to be 12kV, the receiving distance to be 15cm, the advancing speed of the spinning solution to be 2mL/h, and using a single-shaft rotation method, as shown in figure 1, the rotating speed of a receiving device is 100r/min, and the moving speed is 7.5 m/h.
In the core-shell type composite fluorescent fiber prepared in the embodiment, the diameter of the glass fiber bundle is 300 μm, the thickness of the coating film is 100 μm, and SEM images of the surface and the cross section are shown in fig. 2 and fig. 3. From the magnified magnification plot of the larger fiber morphology inserted in fig. 2, it can be seen that the formulated electrospinning solution can be uniformly stretched in the electrostatic field, resulting in uniform fiber morphology.
Example 2:
preparation of core-shell pyrene-containing polyimide-glass fiber composite fluorescent fiber, 8 wt% pyrene-containing polyimide solution was prepared, and the preparation process was the same as in example 1.
The prepared pyrene-containing polyimide solution with the concentration of 8 wt% is used as spinning solution, and is sprayed on the surface of glass fiber by an electrostatic spinning method to form a coating film, and the adopted receiving device is a speed-adjustable and rotatable receiving device.
The electrospinning process used in this example was: taking 3mL of spinning solution, adjusting the voltage to be 12kV, the receiving distance to be 20cm, the advancing speed of the spinning solution to be 2mL/h, using a multi-filament fixed rotation method, the rotating speed of a receiving device to be 150r/min and the moving speed to be 5 m/h.
The diameter of the glass fiber bundle of the core-shell type composite fluorescent fiber prepared by the embodiment is 250 μm, the thickness of the coating film is 150 μm, the fluorescence emission spectrum of the core-shell type composite fluorescent fiber under the condition of 410nm excitation wavelength is shown in fig. 4, and it can be observed in the graph that the composite fluorescent fiber has significant emission wavelength at 500-510 nm, and the fluorescence emission spectrum can show that the fluorescent fiber prepared by the invention has good fluorescence effect.
Example 3:
preparation of a core-shell pyrene-containing polyimide-glass fiber composite fluorescent fiber, 25 wt% pyrene-containing polyimide solution was prepared, and the preparation process was the same as in example 1.
And (3) taking the prepared 25 wt% pyrene-containing polyimide solution as a spinning solution, spraying the spinning solution on the surface of a glass fiber bundle by using an electrostatic spinning method to form a coating film, and adopting a receiving device which is a speed-adjustable and rotatable receiving device.
The electrospinning process used in this example was: taking 1mL of spinning solution, adjusting the voltage to be 12kV, the receiving distance to be 25cm, the advancing speed of the spinning solution to be 2.5mL/h, and using a single-shaft autorotation method, as shown in figure 1, the rotating speed of a receiving device is 200r/min, and the moving speed is 10 m/h.
In the core-shell type composite fluorescent fiber prepared in this example, the diameter of the glass fiber bundle is 200 μm, and the thickness of the coating film is 100 μm.
As shown in fig. 5, the thermal stability of pure glass fiber and the composite fluorescent fiber in this example in nitrogen and oxygen atmospheres was investigated by TGA. The initial decomposition temperatures of the pure glass fiber in nitrogen and oxygen are 230 ℃ and 210 ℃ respectively, and the initial decomposition temperatures of the pyrene-containing polyimide-glass fiber composite fluorescent fiber in nitrogen and oxygen are 140 ℃ and 180 ℃ respectively. In addition, the pyrene-containing polyimide-glass fiber composite fluorescent fiber has an obvious weight loss phenomenon at about 500 ℃ in nitrogen. The carbon residue rate in nitrogen at 800 ℃ is over 90 percent, which shows that the material can meet the high-temperature operation condition.
Example 4:
this example provides an application of the core-shell composite fluorescent fiber of the present invention.
As shown in fig. 6, which is a comparison graph of pure glass fiber and the composite fluorescent fiber prepared in example 1 above under daily illumination and ultraviolet irradiation, respectively, it can be observed that the composite fluorescent fiber wound in a crimp manner still has yellow-green fluorescence under the irradiation of ultraviolet light.
In this embodiment, the composite fluorescent fiber is woven into cloth with different patterns to manufacture the fluorescent anti-counterfeiting mark.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and technical principles of the described embodiments, and such modifications and variations should also be considered as within the scope of the present invention.
Claims (10)
1. A preparation method of a core-shell type composite fluorescent fiber is characterized by comprising the following steps:
mixing a fluorescent polymer, an organic solvent and a volatility adjusting solvent, and oscillating until the fluorescent polymer is fully dissolved to prepare a polymer solution;
the polymer solution is used as spinning solution for electrostatic spinning, a core fiber bundle is used for receiving, a coating film is formed on the surface of the core fiber bundle, and the core fiber bundle keeps a rotating state in the receiving process and moves left and right in the rotating axis direction.
2. The method of claim 1, wherein the fluorescent polymer is one of a pyrene-containing polyimide, a fluorene-containing polyimide, a naphthalene-containing polyimide, a pyrene-containing polyarylether, a fluorene-containing polyarylether, or a naphthalene-containing polyarylether.
3. The method of claim 1, wherein the concentration of the polymer solution is 6 wt% to 25 wt%.
4. The method for preparing the core-shell type composite fluorescent fiber according to claim 1, wherein the volume ratio of the organic solvent to the volatility regulating solvent is 7: 3-9: 1.
5. The method for preparing the core-shell type composite fluorescent fiber according to claim 1, wherein the electrospinning process comprises: the spinning voltage is 12-14 kV, the orifice aperture is 0.5mm, the receiving distance is 15-20 cm, the spinning solution is 1-5 mL, the spinning solution propelling speed is 2-5 mL/h, and the room temperature and the air relative humidity are 25-50%.
6. The method for preparing the core-shell type composite fluorescent fiber according to claim 1, wherein the receiving method is as follows: when polymer solution with the concentration of 11 wt% -25 wt% is used for electrostatic spinning, a single-shaft self-rotation method is adopted for receiving; when polymer solution with the concentration of 6 wt% -10 wt% is used for electrostatic spinning, a multi-filament fixed rotation method is adopted for receiving.
7. The method for preparing the core-shell composite fluorescent fiber according to claim 1, wherein the adjustable range of the rotation speed of the core fiber bundle is 50-200 r/min, and the adjustable range of the movement speed is 5-15 m/h.
8. The method of claim 1, wherein the diameter of the core fiber bundle is 200-300 μm.
9. The method for preparing the core-shell type composite fluorescent fiber according to claim 1, wherein the thickness of the coating film is 100 to 150 μm.
10. The application of the core-shell type composite fluorescent fiber is characterized in that the core-shell type composite fluorescent fiber is applied to fluorescent anti-counterfeiting, flexible imaging or intelligent wearable equipment.
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Application publication date: 20210914 |