CN112301449A - Fluorescent fiber material and preparation method thereof - Google Patents
Fluorescent fiber material and preparation method thereof Download PDFInfo
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- CN112301449A CN112301449A CN202011086734.8A CN202011086734A CN112301449A CN 112301449 A CN112301449 A CN 112301449A CN 202011086734 A CN202011086734 A CN 202011086734A CN 112301449 A CN112301449 A CN 112301449A
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- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
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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
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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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
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Textile Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Dispersion Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a fluorescent fiber material and a preparation method thereof, wherein the fluorescent fiber material is a cuprous complex modified cellulose acetate fiber. The invention carries out spinning on the cuprous complex modified cellulose acetate by an electrostatic spinning technology to finally obtain the fluorescent fiber material. The fluorescent fiber material provided by the invention is environment-friendly, high in luminous efficiency and good in stability, and provides a new theory and technical support for the research of novel fluorescent fiber materials. Moreover, the preparation process of the fluorescent fiber material is simple, the yield is high, the cost is low, and the fluorescent fiber material is suitable for large-scale preparation of fluorescent fiber materials with different colors and has good application prospect.
Description
Technical Field
The invention relates to the technical field of functional fibers, in particular to a fluorescent fiber material and a preparation method thereof.
Background
The fluorescent fiber has wide application in the aspects of anti-counterfeiting, trademark, personalized clothes and the like. The traditional fluorescent fiber is mainly compounded by fluorescent dye (such as azo fluorescent dye) with a conjugated structure through a dyeing process, and has the defects of high toxicity, serious environmental pollution, poor light stability and the like. In recent years, researchers modify fibers with rare earth metal ions to solve the problem of pollution of traditional fluorescent fibers, but the fibers have the defect of poor water stability, and the application of the materials is limited. There is a need to find a fluorescent fiber material which is environmentally friendly and has good stability.
The metal-organic complex luminescent material has the advantages of high fluorescence efficiency, adjustable luminescence and the like of small molecular organic compounds, has the advantage of good thermal stability of inorganic compounds, and is increasingly concerned. The metal-organic complex luminescent materials containing noble metals (such as ir (iii), pt (ii), os (ii), etc.) which are widely researched have the disadvantages of high cost, toxicity and environmental pollution.
The cuprous-organic complex serving as a novel luminescent material has the advantages of low price, small environmental pollution, adjustable luminescence, high fluorescence efficiency and the like, and is applied to the fields of organic luminescent devices, optical sensors, electrochemical cells and the like. Researches show that the cuprous halide-organic complex has the characteristic of structural diversity, can generate a fluorescent color change phenomenon under the stimulation of different external environments, and has potential application prospects in the aspects of information storage, damage detectors and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a fluorescent fiber material and a preparation method thereof, the fluorescent fiber material provided by the invention has the advantages of environmental friendliness, high luminous efficiency and good stability, provides new theoretical and technical support for the research of novel fluorescent fiber materials, and has very wide application prospect.
In order to solve the technical problem, in one aspect, the invention provides a fluorescent fiber material, wherein the fluorescent fiber material is a cuprous complex modified cellulose acetate fiber.
Preferably, the cuprous complex is a cuprous iodide complex.
Further, the cuprous iodide complex is selected from one or more of the following materials: cu2I2(3-picoline)4、Cu2I2(3-picoline)2(PPh3)2、[Cu2I2(PPh3)2(4,4′-bpy)]nAnd [ Cu ]2I2(PPh3)2(pyrazine)]n(ii) a Wherein 3-picoline is 3-methylpyridine, PPh3Triphenylphosphine, 4,4 '-bpy 4, 4' -bipyridine and pyrazine.
In another aspect, the present invention further provides a method for preparing a fluorescent fiber material, comprising the following steps:
(1) dissolving cellulose acetate in a solvent to obtain a solution A;
(2) adding a cuprous complex into the solution A, and stirring to form a solution to be spun;
(3) and performing electrostatic spinning on the solution to be spun to finally form the fluorescent fiber material.
Preferably, in the step (1), the solvent is a mixed solution of acetone and dimethylacetamide.
Preferably, the mass ratio of the acetone to the dimethylacetamide is 4-10: 1.
preferably, the mass ratio of the cellulose acetate to the cuprous complex is 10-20: 1.
preferably, in the step (3), the voltage of the electrostatic spinning is 10-25kV, and the flow rate is 1-3 ml/h.
Preferably, in step (3), the diameter of the spinning nozzle is 0.6mm, and the distance between the spinning nozzle and the receiver is 10-18 cm.
The cuprous complex is used for modifying the cellulose acetate, wherein the cellulose acetate has the characteristics of environmental friendliness and biodegradability, and the cuprous complex has the characteristics of environmental friendliness, high luminous efficiency and the like. Therefore, the prepared fluorescent fiber material also has the advantages of environmental friendliness, high luminous efficiency and the like.
The cuprous complex adopted by the invention has different substituents and steric hindrance of the ligand, and the energy transfer modes are different when the substituents and the steric hindrance of the ligand are different, so that the emission wavelengths of fluorescence are different, and the emitted fluorescence colors are different. Therefore, the fluorescent fiber material provided by the invention can have different fluorescent colors, and the fluorescent colors can span the whole visible area.
The fluorescent fiber material provided by the invention is environment-friendly, high in luminous efficiency and good in stability. The cuprous complexes are firstly adopted to modify the cellulose acetate to prepare the fluorescent fiber material, and different cuprous complexes can be selected as modifiers to prepare the fluorescent fiber materials with different fluorescent colors, so that a new theory and technical support is provided for the research of the novel fluorescent fiber material. Moreover, the preparation process of the fluorescent fiber material is simple, the yield is high, the cost is low, and the fluorescent fiber material is suitable for large-scale preparation of fluorescent fiber materials with different colors and has good application prospect.
Drawings
FIG. 1 is a schematic diagram of the synthesis of four modifiers of example 1 of the present invention.
FIG. 2 is an electron micrograph of four fluorescent fiber materials prepared in example 2 of the present invention. Wherein FIG. 2A is 1@ CA at 4000 magnification and FIG. 2A' is 1@ CA at 40000 magnification; FIG. 2B is 2@ CA at 4000 magnification and FIG. 2B' is 2@ CA at 60000 magnification; FIG. 2C is 3@ CA at 4000 magnification and FIG. 2C' is 3@ CA at 40000 magnification; FIG. 2D is 4@ CA at 4000 magnification and FIG. 2D' is 4@ CA at 40000 magnification.
FIG. 3 is an IR spectrum of four fluorescent fiber materials and their corresponding modifiers prepared in example 2 of the present invention.
FIG. 4 is a powder X-ray diffraction diagram of four fluorescent fiber materials and their corresponding modifiers prepared in example 2 of the present invention.
FIG. 5 is a graph showing fluorescence emission spectra of four modifiers prepared in example 1 of the present invention.
FIG. 6 shows fluorescence emission spectra of four fluorescent fiber materials prepared in example 2 of the present invention.
FIG. 7 is a graph showing the light stability of four fluorescent fiber materials prepared in example 2 of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
The figures 1-7 and the embodiments refer to the Chinese meanings of the numbers, symbols and English symbols, respectively: CuI is cuprous iodide, 3-pc is 3-methylpyridine, tpp is triphenylphosphine (also known as PPh)3) Pz (pyrazine) is pyrazine, CA is cellulose acetate, 1 is Cu2I2(3-picoline)42 is Cu2I2(3-picoline)2(PPh3)2And 3 is [ Cu ]2I2(PPh3)2(4,4′-bpy)]nAnd 4 is [ Cu ]2I2(PPh3)2(pyrazine)]n1@ CA is Cu2I2(3-picoline)4Fluorescent fiber material prepared from modified cellulose acetate, 2@ CA being Cu2I2(3-picoline)2(PPh3)2Fluorescent fiber material prepared from modified cellulose acetate, 3@ CA being [ Cu2I2(PPh3)2(4,4′-bpy)]nFluorescent fiber material prepared from modified cellulose acetate, 4@ CA being [ Cu [ ]2I2(PPh3)2(pyrazine)]nThe fluorescent fiber material is prepared by modified cellulose acetate.
Example 1 preparation of modifier: as shown in fig. 1:
1、Cu2I2(3-picoline)4the preparation of (1):
CuI (0.38g, 2mmol) and CuI are taken according to the molar ratio of 1:4 at room temperature3-methylpyridine (0.74g, 8mmol) was added to 20mL of acetone to form a mixture 1, which was stirred for 30 min. Filtering, collecting to obtain powder 1, washing with acetone twice, and drying in air to obtain Cu2I2(3-picoline)4。
2、Cu2I2(3-picoline)2(PPh3)2The preparation of (1):
taking Cu2I2(3-picoline)4(0.3g, 0.4mmol) in 10mL acetone to form solution B, and the excess PPh was added with stirring3A toluene solution (4mL) (0.26g, 1mmol) was added to solution B to form a mixture 2, which was stirred for 2 hours to complete the reaction. Filtering, collecting to obtain powder 2, washing with acetone twice, and drying in air to obtain Cu2I2(3-picoline)2(PPh3)2。
3、[Cu2I2(PPh3)2(4,4′-bpy)]nThe preparation of (1):
mixing Cu2I2(3-picoline)2(PPh3)2(0.22g, 0.2mmol) and an excess of 4, 4' -bpy (0.16g, 1mmol) were added to 10mL of toluene to form a mixture 3, which was heated at 80 ℃ for 24 hours. Filtered, collected to give powder 3, washed twice with toluene and acetone, and dried in air to finally obtain [ Cu ]2I2(PPh3)2(4,4′-bpy)]n。
4、[Cu2I2(PPh3)2(pyrazine)]nThe preparation of (1):
mixing Cu2I2(3-picoline)2(PPh3)2(0.22g, 0.2mmol) and excess pyrazine (0.08g, 1mmol) were added to 10mL of toluene to form a mixture 4, which was heated at 80 ℃ for 24 hours. Filtering, collecting to obtain precipitate 4, washing with toluene and acetone twice, and drying in air to obtain [ Cu ]2I2(PPh3)2(pyrazine)]n。
The powder X-ray diffraction patterns of the four modifiers are respectively tested, and the simulated peaks and the experimental peaks of the four modifiers can be well corresponded, which indicates that the four modifiers are pure phases.
EXAMPLE 2 preparation of fluorescent fiber Material
100mg of cellulose acetate (molecular weight Mw: 60000g/mol) was added to 900mg of acetone/dimethylacetamide (4: 1), and stirred for 3 hours to obtain a solution A. And adding 10mg of cuprous complex modifier into the solution A, and stirring for 1 hour to form a solution to be spun. And (3) carrying out electrostatic spinning on the solution to be spun, and finally forming the fluorescent fiber material. The voltage of electrostatic spinning is set to be 15kV, and the flow rate is set to be 1 mL/h. The spinneret had a diameter of 0.6mm and the distance between the spinneret and the receiver was 12 cm.
Four modifier Cu prepared in example 1 were used respectively2I2(3-picoline)4、Cu2I2(3-picoline)2(PPh3)2、[Cu2I2(PPh3)2(4,4′-bpy)]nAnd [ Cu ]2I2(PPh3)2(pyrazine)]nAnd modifying the cellulose acetate to finally prepare four fluorescent fiber materials.
EXAMPLE 3 characterization of fluorescent fiber materials
Four fluorescent fiber materials prepared in example 2 were characterized.
1. The morphology of the fluorescent fiber material was characterized using a Scanning Electron Microscope (SEM): as shown in FIG. 2, the surfaces of the four fluorescent fiber materials are smooth, and the modifying agent is uniformly distributed in the fiber. The diameter of the fluorescent fiber material prepared in example 2 is about 300-600nm, and the fluorescent fiber materials with different diameters can be prepared by adjusting the concentration of the cellulose acetate.
2. The structure of the fluorescent fiber material is characterized by the infrared spectrum: as shown in FIG. 3, the characteristic peak of pure cellulose acetate is 3455cm-1And 1752cm-11636cm, due to-OH and C-H groups, respectively, in its structure-1The peaks at (a) are due to water molecules in their structure. In the FT-IR spectra of the four fluorescent fiber materials, 1610, 1497, 1420, 1383, 1226, B,805. 721, 537 and 485cm-1The new peak of (a), which may be attributed to the phenyl group of the organic ligand in the modifier as well as the Cu-I group, indicates successful binding of the cuprous complex modifier to cellulose acetate.
3. The composition and phase purity of the fluorescent fiber material were characterized by powder X-ray diffraction: as shown in fig. 4, the diffraction peaks of pure cellulose acetate show wide bands only at 2 θ ═ 8.5 °, 11 °, 13 °, and 38 °. Characteristic peaks belonging to corresponding modifiers appear in PXRD spectra of four fluorescent fiber materials, which shows that the cuprous complex modifier and cellulose acetate are successfully combined, and also shows that the crystal structure of the cuprous complex modifier can be kept stable in the electrostatic spinning process.
Example 4 fluorescence Spectroscopy testing of fluorescent fiber materials
The four fluorescent fiber materials prepared in example 2 and their corresponding modifiers were tested for their fluorescence emission spectra.
For Cu2I2(3-picoline)4Modified cellulose acetate fluorescent fiber material and corresponding modifier and Cu thereof2I2(3-picoline)2(PPh3)2The modified cellulose acetate fluorescent fiber material and the corresponding modifier thereof select 365nm as the excitation wavelength. For [ Cu ]2I2(PPh3)2(4,4′-bpy)]nModified cellulose acetate fluorescent fiber material and corresponding modifier, [ Cu2I2(PPh3)2(pyrazine)]nThe modified cellulose acetate fluorescent fiber material and the corresponding modifier thereof select 420nm as the excitation wavelength.
The results of the tests are shown in fig. 5 and 6, where the emission of the four modifiers is unimodal and the fluorescence color ranges from violet to orange-red across the entire visible region. The emission of the four fluorescent fiber materials can be well matched with the emission of the corresponding modifiers, and the fluorescence color range of the four fluorescent fiber materials is from purple to orange red and spans the whole visible region.
TABLE 1 fluorescence emission wavelength, emission color and Quantum yield of fluorescent fiber materials and their corresponding modifiers
| Material | Fluorescence emission wavelength (nm) | Emission colour | Quantum yield (%) |
| 1 | 433 | Purple color | 72.3 |
| 1@CA | 438 | Purple color | - |
| 2 | 464 | Blue color | 65.6 |
| 2@CA | 466 | Blue color | - |
| 3 | 538 | Yellow colour | 63.2 |
| 3@CA | 541 | Yellow colour | - |
| 4 | 595 | Orange red | 23.8 |
| 4@CA | 592 | Orange red | - |
According to the test results in table 1, the quantum yields of the four modifiers are relatively high, and are 72.3%, 65.6%, 63.2% and 23.8%, respectively, which indicates that the four modifiers have excellent optical properties and high luminous efficiency, and therefore the luminous efficiencies of the four fluorescent fiber materials corresponding to the four modifiers are high. When the modifier is Cu2I2(3-picoline)4When the fluorescence intensity is high, the fluorescence emission wavelength of the corresponding fluorescent fiber material is 438nm, and the material shows purple fluorescence. When the modifier is Cu2I2(3-picoline)2(PPh3)2When the fluorescence emission wavelength of the corresponding fluorescent fiber material is 466nm, the material shows blue fluorescence. When the modifier is [ Cu ]2I2(PPh3)2(4,4′-bpy)]nWhen the fluorescence intensity is high, the fluorescence emission wavelength of the corresponding fluorescent fiber material is 541nm, and yellow fluorescence is shown. When the modifier is [ Cu ]2I2(PPh3)2(pyrazine)]nWhen the fluorescence emission wavelength of the corresponding fluorescent fiber material is 592nm, the material shows orange-red fluorescence. The fluorescence emission wavelengths and emission colors of the four fluorescent fiber materials and the corresponding modifiers can be well corresponded, which shows that the four modifiers can keep stable in the process of compounding with the cellulose acetate without any structural changeAnd (4) chemical degradation or degradation.
EXAMPLE 5 photostability test of fluorescent fiber materials
The four fluorescent fiber materials prepared in example 2 were subjected to a photostability test.
As shown in FIG. 7, no significant intensity loss or shift in the emission intensity occurred after 48 hours of UV irradiation for any of the four fluorescent fiber materials. The result shows that the fluorescent fiber material provided by the invention has very stable luminescence performance and good light stability. The conventional fluorescent fiber material is generally sensitive to light, and is easily decomposed under the influence of an external environment to cause obvious luminous intensity loss.
The fluorescent fiber material provided by the invention is environment-friendly, high in luminous efficiency and good in stability. The cuprous complexes are firstly adopted to modify the cellulose acetate to prepare the fluorescent fiber material, and different cuprous complexes can be selected as modifiers to prepare the fluorescent fiber materials with different fluorescent colors, so that a new theory and technical support is provided for the research of the novel fluorescent fiber material. Moreover, the preparation process of the fluorescent fiber material is simple, the yield is high, the cost is low, and the fluorescent fiber material is suitable for large-scale preparation of fluorescent fiber materials with different colors and has good application prospect.
The fluorescent fiber material is prepared by skillfully utilizing the luminescent property of the cuprous complex, the problems in the prior art of the fluorescent fiber material are overcome by successfully compounding the cuprous complex and the cellulose acetate, and finally, the fluorescent fiber material which is environment-friendly and has the advantages of high luminescent efficiency, good stability and the like is found. For the fluorescent fiber material, the three properties are all indispensable, and the application of the existing fluorescent fiber material is greatly limited only because the three properties cannot be simultaneously satisfied, and the large-scale application of the fluorescent fiber material cannot be realized at all.
The invention solves the problem that the application of the existing fluorescent fiber material is limited, and can lead the application range and the scale of the fluorescent fiber material to be developed in a breakthrough way, so that the fluorescent fiber material is not limited in scientific research any more, but really realizes the industrial application of the fluorescent fiber material. The improvement of the performance of the fluorescent fiber material is a very advanced research direction in the field, and the substitute of the fluorescent fiber material provided by the invention is not available in the field.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (7)
1. The fluorescent fiber material is characterized by being a cuprous complex modified cellulose acetate fiber.
2. The fluorescent fiber material of claim 1, wherein the cuprous complex is cuprous iodide complex.
3. The fluorescent fiber material of claim 2, wherein the cuprous iodide complex is selected from one or more of the following materials: cu2I2(3-picoline)4、Cu2I2(3-picoline)2(PPh3)2、[Cu2I2(PPh3)2(4,4′-bpy)]nAnd [ Cu ]2I2(PPh3)2(pyrazine)]n(ii) a Wherein 3-picoline is 3-methylpyridine, PPh3Triphenylphosphine, 4,4 '-bpy 4, 4' -bipyridine and pyrazine.
4. The method for preparing a fluorescent fiber material according to any one of claims 1 to 3, comprising the steps of:
(1) dissolving cellulose acetate in a solvent to obtain a solution A;
(2) adding a cuprous complex into the solution A, and stirring to form a solution to be spun;
(3) and performing electrostatic spinning on the solution to be spun to finally form the fluorescent fiber material.
5. The method for preparing a fluorescent fiber material according to claim 4, wherein in the step (1), the solvent is a mixed solution of acetone and dimethylacetamide.
6. The method for preparing the fluorescent fiber material according to claim 5, wherein the mass ratio of acetone to dimethylacetamide is 4-10: 1.
7. the method for preparing a fluorescent fiber material according to claim 4, wherein the mass ratio of the cellulose acetate to the cuprous complex is 10-20: 1.
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