CN110042487B - Quantum dot/polyaryletherketone nanocomposite and preparation method thereof - Google Patents
Quantum dot/polyaryletherketone nanocomposite and preparation method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
- C08G65/4018—(I) or (II) containing halogens other than as leaving group (X)
- C08G65/4025—(I) or (II) containing fluorine other than as leaving group (X)
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- 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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- 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
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
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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
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- 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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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/009—Condensation or reaction polymers
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
- D04H3/03—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random
- D04H3/033—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments at random reorientation immediately after yarn or filament formation
Abstract
The invention discloses a quantum dot/polyaryletherketone nano composite material and a preparation method thereof, belonging to the technical field of nano fibers. Firstly, a phenolphthalein monomer and a 4, 4-difluorobenzophenone monomer are subjected to polycondensation reaction to prepare the linear benzene carboxyl side group polyaryletherketone. The linear benzene carboxyl side group polyaryletherketone material is a special plastic with excellent acid and alkali resistance, corrosion resistance and thermal stability, and is mixed with quantum dots in a solution form, namely CdS/hyperbranched polyaryletherketone, so as to form a fiber membrane material by an electrostatic spinning technology. The film has the characteristics of high fluorescence property of quantum dots and stability of linear polymers, and the quantum dots are uniformly dispersed under the electrostatic spinning condition, so that the film material for photoelectric devices is obtained. Compared with the film without the doped quantum dots, the film with the doped quantum dots has greatly improved fluorescence intensity and thermal stability.
Description
Technical Field
The invention belongs to the technical field of nano fibers, and particularly relates to linear benzene carboxyl side group polyaryletherketone, a membrane material which is formed by doping quantum dots into an electro-spun fiber membrane and has a luminous effect, and a preparation method thereof.
Background
The CdS quantum dot can regulate and control the fluorescence color by changing the diameter in a visible light range without changing the chemical composition or the crystal structure, and has wide application in the aspects of solar cells, sensors, fluorescent probes and the like due to the special property. However, the CdS quantum dots have extremely small size, large specific surface area and a large number of defects on the surface, and are easy to agglomerate in the forming process, so that the application of the CdS quantum dots in the aspect of luminescence is limited. The existing method for preparing the quantum dots with high fluorescence performance by using the polymer as the template can effectively improve the dispersibility of the quantum dots, which is an important subject in the field of quantum dots.
The polyaryletherketone has excellent properties of chemical corrosion resistance, good physical properties, flame retardance, heat resistance and the like, is a special engineering plastic with excellent performance, and is widely applied to military, aerospace, electronic information, energy and other aspects. Polyaryletherketone polymers have been studied in recent years to help disperse quantum dots and to improve the luminescent properties of quantum dots. The hyperbranched polyaryletherketone can provide space for the dispersion of the quantum dots and control the size and appearance of the quantum dots, so that the hyperbranched polyaryletherketone can be used for preparing a high-performance luminescent nano composite material. However, the CdS/hyperbranched polyaryletherketone exists in a solution form, and even if the CdS/hyperbranched polyaryletherketone exists in a solution form, the CdS/hyperbranched polyaryletherketone is difficult to become a film material which can be applied to a photoelectric device, so that the CdS/hyperbranched polyaryletherketone needs to be dispersed and formed into a film by means of linear benzene carboxyl polyaryletherketone with a higher molecular weight.
The electrostatic spinning technology is a simple and convenient method for preparing the nanofiber membrane with low cost. Under the combined action of electric field force and surface tension, the solvent is volatilized, the polymer is solidified to form fibers with a certain diameter, and the diameter of the fibers can be regulated and controlled by changing external conditions. The linear benzene carboxyl polyaryletherketone has excellent spinnability and provides extremely high heat resistance for the nanofiber membrane material.
Disclosure of Invention
In order to solve the problem of difficult film formation of the CdS/hyperbranched polyaryletherketone composite material, the invention provides a preparation method of a polyaryletherketone nano composite material.
The invention relates to a preparation method of a quantum dot/polyaryletherketone nano composite material, which comprises the following specific steps:
1) the preparation method of the benzene carboxyl side group linear polyaryletherketone comprises the following specific steps: taking a phenolphthalein monomer and 4,4 '-difluorobenzophenone as raw materials, wherein the molar ratio of the phenolphthalein monomer to the 4, 4' -difluorobenzophenone is 1:1, dimethyl sulfoxide is taken as a solvent, potassium carbonate is taken as a salt forming agent, the mixture is mixed into a solution, the solid content in the solution is 20-30 percent, the potassium carbonate is 12 percent excessive relative to hydroxyl in the phenolphthalein monomer,
all the steps of the reaction are carried out under the protection of nitrogen, firstly, under the condition of 140-150 ℃, carrying out azeotropic dehydration on toluene, carrying out salt forming reaction for 2 hours at the dehydration temperature of 140-150 ℃, wherein the volume ratio of the toluene to the solvent is 1: 2; and continuously reacting for 4 hours at 170-180 ℃ for polycondensation reaction to obtain a crude product, and performing after-treatment, namely pouring the crude product into a hydrochloric acid aqueous solution, crushing, washing with hot water and ethanol respectively, and finally drying to obtain the benzene carboxyl side group linear polyaryletherketone.
2) Preparing a mixed solution of the benzene carboxyl side group linear polyaryletherketone and the CdS/hyperbranched polyaryletherketone, comprising the following steps: weighing 1-2 g of the benzene carboxyl side group linear polyaryletherketone prepared in the step 1), weighing 7-8 g of CdS/hyperbranched polyaryletherketone solution, and stirring for more than 12 hours to obtain a stable and uniform mixed solution;
3) pouring the mixed solution obtained in the step 2) into a 10mL injector, installing the injector on an electrostatic spinning device, using an aluminum foil as a receiving plate, wherein the distance between a needle head and the receiving plate is 15cm, the injection speed is 1-2 mL/h, and the voltage is 15-20 kV; and drying the obtained fiber film for 24 hours at 80-100 ℃ under a real condition to obtain the quantum dot/polyaryletherketone nano composite material.
The preparation method of the CdS/hyperbranched polyaryletherketone solution comprises the following specific steps:
dissolving a carboxyl-containing hyperbranched polyaryletherketone in N, N-dimethylformamide, and stirring to prepare a transparent solution with the concentration of 10-20 mg/mL;
secondly, adding a cadmium precursor solution into the benzene carboxyl-containing hyperbranched polyaryletherketone solution, stirring for 20-30 min, introducing nitrogen for 10-15 min, and heating under the condition of magnetic stirring until the solution flows back;
thirdly, after refluxing for 10-20 min, adding a deoxygenated N, N-dimethylformamide solution of thiourea into the reaction system, continuously introducing nitrogen, reacting for 2-30 min under magnetic stirring and heating conditions, and then cooling to room temperature in an ice-water bath to obtain a CdS/hyperbranched polyaryletherketone solution;
wherein the cadmium precursor solution is Cd (Ac)2The concentration of the cadmium precursor solution is 4 x 10-5～ 8×10-5mol/L，Cd(Ac)2The molar ratio of the carboxyl-containing hyperbranched polyaryletherketone to the carboxyl-containing hyperbranched polyaryletherketone is 1: 1-5.
The content of thiourea in the N, N-dimethylformamide solution of thiourea was 4X 10-5～12×10-5mol/L, wherein the molar ratio of the thiourea to the carboxyl-containing hyperbranched polyaryletherketone is 1: 1-5.
The hyperbranched polyaryletherketone containing the benzene carboxyl is prepared by taking a phenolphthalein monomer and a 2,4', 6-trifluorobenzophenone monomer as raw materials.
The invention has the beneficial effects that:
the invention discloses a quantum dot/polyaryletherketone nano composite material, which is a polyaryletherketone film material capable of emitting light. The linear polyaryletherketone has excellent spinnability and thermal stability, and electrostatic spinning can realize the regulation and control of the morphology and the size of the polymer by changing spinning conditions. On one hand, the linear benzene carboxyl side group polyaryletherketone can change the quantum dots from a solution form to a film material which can be used as a photoelectric device. On the other hand, the quantum dot solution is introduced into the linear benzene carboxyl side group polyaryletherketone, so that the luminous performance of the polymer can be greatly enhanced, the polymer has a fluorescent effect, and the film material is endowed with excellent performance in the aspect of photoelectric devices. The electrostatic spinning technology adopted by the method can better disperse the quantum dots in the polymer, is not easy to agglomerate, and has the advantages of high efficiency, low cost, simple and convenient operation, uniform fiber diameter distribution and the like.
Drawings
FIG. 1: infrared pattern of fibrous membranes
FIG. 2: transmission electron microscopy of fibers
FIG. 3: fluorescence spectrum of fiber membrane
FIG. 4: TGA Profile of fibrous membranes
Detailed Description
Example 1:
the first step is as follows: in a 50mL three-necked flask to which a nitrogen port, a stirring paddle and a water-carrying device were connected with a thermometer, 4.3246g (13.5mmol) of a phenolphthalein monomer and 3.5429g (15mmol) of 2,4', 6-trifluoro-benzophenone were put in this order, followed by addition of 0.9781g (4.725mmol) of anhydrous potassium carbonate and 1.5026g (9.45mmol) of anhydrous sodium carbonate.
The second step is that: adding 18mL of sulfolane solvent and 15mL of toluene as a water-carrying agent into the system, introducing nitrogen, heating under stirring until the toluene is refluxed (130 ℃, corresponding to the salifying step in the invention content), refluxing for 3h to ensure that the toluene is discharged after water in the system is removed.
The third step: by using a staged heating method, the system is sequentially heated to 160 ℃, 180 ℃, 200 ℃ and 220 ℃ for reaction for 2 hours respectively. And after the reaction is finished, discharging the mixture solution into a hydrochloric acid aqueous solution, crushing by using a powder machine, washing materials for multiple times by adopting boiling distilled water and room-temperature ethanol respectively, and removing residual inorganic salt and solvent. Drying in an oven to obtain the yellow benzene carboxyl-containing hyperbranched polyaryletherketone polymer.
The fourth step: 100mg of benzene carboxyl-containing hyperbranched polyaryletherketone is added into a 50mL reaction bottle, 5mL of N, N-dimethylformamide is added to dissolve the benzene carboxyl-containing hyperbranched polyaryletherketone, and the mixture is stirred at normal temperature.
The fifth step: adding a solution containing 4X 10 of N, N-dimethylformamide obtained above-5Molar Cd (Ac)2Stirring the solution at room temperature for 30min, introducing nitrogen for 10min, and heating the solution to reflux under magnetic stirring.
And a sixth step: refluxing for 20min, adding 2mL of a solution containing 4X 10-5And (3) deoxidizing the N, N-dimethylformamide solution of the molar thiourea, reacting for 2min, and cooling to room temperature in ice water bath to obtain a clear pale yellow CdS/hyperbranched polyaryletherketone solution.
Example 2:
the first step is as follows: a100 mL three-necked flask was charged with 4.0827g (12.74mmol) of phenolphthalein monomer, 2.7819g (12.74mmol) of 4, 4-difluorobenzophenone monomer, and 3.1659g (22.93mmol) of anhydrous potassium carbonate.
The second step is that: to a three-necked flask was added 18mL of dimethyl sulfoxide and 13mL of toluene. A nitrogen port, a stirring paddle and a water carrying device are arranged on a three-neck flask, the three-neck flask is heated under the condition of introducing nitrogen until toluene refluxes (145 ℃, namely salifying of the invention content), and water and toluene are discharged after 3 hours.
The third step: heating the reaction system to 180 ℃, reacting for 4 hours, and discharging the reaction product into an aqueous solution of hydrochloric acid after the reaction is finished. The polymer was pulverized and washed 3 times with hot water and cold ethanol, respectively, to remove solvent and small molecules. Vacuumizing and drying at 90 ℃ to obtain the linear benzene carboxyl side group polyaryletherketone.
Example 3:
7.7108g of N, N-dimethylformamide and 1.0479g of linear benzene carboxyl side group polyaryletherketone are added into a sample bottle, stirred for 12 hours, poured into a 10mL injector, installed on an electrostatic spinning device, an aluminum foil is used as a receiving plate, the distance between a needle head and the receiving plate is 15cm, the injection speed is 1-2 mL/h, and the voltage is 15-20 kv. And drying the obtained fiber membrane for 24 hours at 80-100 ℃ under a vacuum condition to obtain the linear benzene carboxyl side group polyaryletherketone fiber membrane.
Example 4:
7.7455g of CdS/hyperbranched polyaryletherketone quantum dot solution and 1.0526g of linear benzene carboxyl side group polyaryletherketone are added into a sample bottle, stirred for 12 hours, poured into a 10mL injector, installed on an electrostatic spinning device, an aluminum foil is used as a receiving plate, the distance between a needle head and the receiving plate is 15cm, the injection speed is 1-2 mL/h, and the voltage is 15-20 kv. And drying the obtained fiber membrane for 24 hours at 80-100 ℃ under a real condition to obtain the high-temperature-resistant quantum dot/polyaryletherketone nanofiber membrane material.
Curve a in FIG. 1 corresponds to the linear phenylcarboxyl side group polyaryletherketone of example 3, and the carbon on the phenylcarboxyl group has a stretching vibration peak at 1718 cm-1; curve c corresponds to the CdS/hyperbranched polyaryletherketone solution of example 1, and carbon on the hyperbranched polymer carboxyl side group has a stretching vibration peak at 1739cm < -1 >; the curve b corresponds to the composite material of the two of the embodiment 4, and the vibration peak is shifted to 1722 cm-1.
Fig. 2 is a transmission electron microscope image of the high temperature resistant quantum dot/polyaryletherketone nanofiber membrane material of example 4, it can be seen that the diameter of the fiber is about 100nm, the lattice of the quantum dot can be clearly seen in the fiber, and the particle size is about 5-6 nm, which indicates that the quantum dot is successfully introduced and uniformly dispersed in the fiber.
In fig. 3, curves a and b are excitation and emission spectra of the linear phenylcarboxy side group polyaryletherketone nanofiber membrane, and curves c and d are excitation and emission spectra of the quantum dot/linear phenylcarboxy side group polyaryletherketone nanofiber membrane. It can be seen that the polymer film has a certain fluorescence intensity, but due to the introduction of the quantum dots, the fluorescence excitation and emission intensity of the film material are obviously improved, and the maximum excitation and emission wavelengths are respectively changed from 390nm and 447nm to 404nm and 460nm, which have certain shifts compared with the maximum excitation and emission wavelengths 410nm and 463nm of the CdS/hyperbranched polyaryletherketone solution obtained in the sixth step of example 1.
In fig. 4, a curve a is a thermal weight loss curve of the linear benzene carboxyl side group polyaryletherketone nanofiber membrane, a curve b is a thermal weight loss curve of the quantum dot/polyaryletherketone nanofiber membrane, and a curve c is a thermal weight loss curve of the CdS/hyperbranched polyaryletherketone settled out. The introduction of the quantum dots can be seen to improve the heat resistance of the polyaryletherketone nanofiber membrane. Compared with TGA data measured after the hyperbranched polyaryletherketone/CdS quantum dot solution obtained in the sixth step of the embodiment 1 is dried, the heat resistance of the hyperbranched polyaryletherketone/CdS quantum dot solution is slightly reduced, but the application range of the hyperbranched polyaryletherketone/CdS quantum dot solution is greatly widened by doping the quantum dot solution into a fiber film.
Claims (3)
1. A preparation method of a quantum dot/polyaryletherketone nano composite material comprises the following specific steps:
1) the preparation method of the benzene carboxyl side group linear polyaryletherketone comprises the following specific steps: taking a phenolphthalein monomer and 4, 4' -difluorobenzophenone as raw materials, mixing the raw materials in a molar ratio of 1:1, dimethyl sulfoxide as a solvent and potassium carbonate as a salt forming agent to form a solution, wherein the solid content in the solution is 20-30%, the potassium carbonate is 12% excessive relative to hydroxyl in the phenolphthalein monomer,
carrying out the following reactions under the protection of nitrogen, firstly carrying out azeotropic dehydration on toluene at 140-150 ℃, carrying out salt forming reaction for 2 hours at the dehydration temperature of 140-150 ℃, wherein the volume ratio of the toluene to the solvent is 1: 2; continuously reacting for 4 hours at 170-180 ℃ for polycondensation reaction to obtain a crude product, and performing after-treatment, namely pouring the crude product into a hydrochloric acid aqueous solution, crushing, washing with hot water and ethanol respectively, and finally drying to obtain the benzene carboxyl side group linear polyaryletherketone;
2) preparing a mixed solution of the benzene carboxyl side group linear polyaryletherketone and the CdS/hyperbranched polyaryletherketone, comprising the following steps: weighing 1-2 g of the benzene carboxyl side group linear polyaryletherketone prepared in the step 1), weighing 7-8 g of CdS/hyperbranched polyaryletherketone solution, and stirring for more than 12 hours to obtain a stable and uniform mixed solution;
3) pouring the mixed solution obtained in the step 2) into a 10mL injector, installing the injector on an electrostatic spinning device, using an aluminum foil as a receiving plate, wherein the distance between a needle head and the receiving plate is 15cm, the injection speed is 1-2 mL/h, and the voltage is 15-20 kV; and drying the obtained fiber film for 24 hours at 80-100 ℃ under a real condition to obtain the quantum dot/polyaryletherketone nano composite material.
2. The preparation method of the quantum dot/polyaryletherketone nanocomposite as claimed in claim 1, wherein the preparation method of the CdS/hyperbranched polyaryletherketone solution comprises the following specific steps:
dissolving a carboxyl-containing hyperbranched polyaryletherketone in N, N-dimethylformamide, and stirring to prepare a transparent solution with the concentration of 10-20 mg/mL;
secondly, adding a cadmium precursor solution into the benzene carboxyl-containing hyperbranched polyaryletherketone solution, stirring for 20-30 min, introducing nitrogen for 10-15 min, and heating under the condition of magnetic stirring until the solution flows back;
thirdly, after refluxing for 10-20 min, adding a deoxygenated N, N-dimethylformamide solution of thiourea into the reaction system, continuously introducing nitrogen, reacting for 2-30 min under magnetic stirring and heating conditions, and then cooling to room temperature in an ice-water bath to obtain a CdS/hyperbranched polyaryletherketone solution;
wherein the cadmium precursor solution is Cd (Ac)2The concentration of the cadmium precursor solution is 4 x 10-5～8×10-5mol/L，Cd(Ac)2The molar ratio of the carboxyl-containing hyperbranched polyaryletherketone to the carboxyl-containing hyperbranched polyaryletherketone is 1: 1-5;
the content of thiourea in the N, N-dimethylformamide solution of thiourea was 4X 10-5～12×10-5mol/L, wherein the molar ratio of thiourea to the carboxyl-containing hyperbranched polyaryletherketone is 1: 1-5;
the hyperbranched polyaryletherketone containing the benzene carboxyl is prepared by taking a phenolphthalein monomer and a 2,4', 6-trifluorobenzophenone monomer as raw materials.
3. A quantum dot/polyaryletherketone nanocomposite obtained by the preparation method of claim 1 or 2.
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