CN114574993A - Preparation method of nylon 66 photonic crystal fiber with opal structure or inverse opal structure - Google Patents
Preparation method of nylon 66 photonic crystal fiber with opal structure or inverse opal structure Download PDFInfo
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- CN114574993A CN114574993A CN202011383607.4A CN202011383607A CN114574993A CN 114574993 A CN114574993 A CN 114574993A CN 202011383607 A CN202011383607 A CN 202011383607A CN 114574993 A CN114574993 A CN 114574993A
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- 229920002302 Nylon 6,6 Polymers 0.000 title claims abstract description 163
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- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 20
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
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- 239000002131 composite material Substances 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
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- 229910021389 graphene Inorganic materials 0.000 claims description 3
- HTEAGOMAXMOFFS-UHFFFAOYSA-N methyl 2-methylprop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.COC(=O)C(C)=C HTEAGOMAXMOFFS-UHFFFAOYSA-N 0.000 claims description 3
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 6
- 238000000879 optical micrograph Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 239000011022 opal Substances 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 239000002121 nanofiber Substances 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 241000238367 Mya arenaria Species 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
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Images
Classifications
-
- 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
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
-
- 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
-
- 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
-
- 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
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a preparation method of a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure, which is characterized by comprising the following steps: preparing nylon 66 photonic crystal fiber with an opal structure by using electrospinning liquid containing polystyrene microsphere latex and nylon 66 through a directional electrostatic spinning technology; or the nylon 66 photonic crystal fiber with the opal structure is prepared into the nylon 66 photonic crystal fiber with the inverse opal structure by adopting a sacrificial template method. The opal-structure or inverse opal-structure nylon 66 photonic crystal fiber has high color saturation, good mechanical property and waterproof property, and good shape retention when being attached to a 3D structure, so that the opal-structure or inverse opal-structure nylon 66 photonic crystal fiber has a good application prospect in the field of textile or intelligent electronic skin.
Description
Technical Field
The invention relates to the technical field of photonic crystal fibers. More particularly, relates to a preparation method of a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure.
Background
The photonic crystal is a substance formed by periodically arranging two or more nano structures with different refractive indexes in space, and the regular microstructure in the photonic crystal generates a photonic band gap so as to control the motion state of photons and select visible light to generate structural color. The colloidal crystal fiber is a fiber material with structural color obtained by combining colloidal crystals and fibers. The light is selected by diffraction, scattering, refraction and the like of the colloidal crystal fiber to present certain color. The traditional dyes used in the textile industry at present pollute water resources and cannot be naturally degraded. Whilst the interaction of the dye with components in the air can lead to fading of the fabric. The structural color is generated by utilizing a periodic structure of the structural color, so that the structural color material has the characteristics of environmental friendliness, no toxicity, no pollution, no fading, high saturation and high brightness. Therefore, the structural color material is of great significance to replace the traditional dye. At present, the methods for obtaining the colloidal crystal fiber mainly comprise a template assembly method, an electrostatic spinning method, an extrusion assembly method, a multilayer crimp assembly method, a micro-fluidic spinning method, a fabric assembly method and the like. The electrostatic spinning is a simple and effective method for preparing the nano-fibers, and the fiber membrane prepared by electrostatic spinning is formed by stacking and interweaving the nano-fibers, has the characteristics of high specific surface area, high porosity, small pore diameter and the like, and has wide application prospects in the aspects of intelligent electronic skin, catalysis, filtration, solar cells and the like. At present, in the prior art, a mixture of polyvinyl alcohol and polymer microspheres is subjected to electrostatic spinning to obtain a fiber membrane with various colors, and the photonic crystal fiber can obtain various high-quality patterns by utilizing an ink-jet printing technology, and has important significance for the research and development of wearable materials. Although the photonic crystal fiber has a good prospect in the aspect of improving the traditional textile industry, the raw material polyvinyl alcohol used in the prior art is easy to dissolve in water and has poor mechanical properties.
Polyhexamethylene adipamide, commonly known as nylon-66, is a thermoplastic resin generally prepared by the polycondensation of adipic acid and hexamethylene diamine. Insoluble in general solvents, and soluble only in hexafluoroisopropanol and the like. High mechanical strength and hardness, and high rigidity. It can be used as engineering plastics and mechanical accessories, such as gear and lubricating bearing, and can be used to replace nonferrous metal material to make machine shell and blade of car engine, etc. and also can be used to make synthetic fibre.
Therefore, it is required to provide a method for preparing a nylon 66 photonic crystal fiber with an opal structure or an inverse opal structure having good mechanical properties and waterproof properties, and the photonic crystal fiber prepared by the method can fully embody the high saturation and high brightness of the photonic crystal fiber and simultaneously has the strong mechanical properties and waterproof properties of nylon 66.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure, the method can prepare the photonic crystal fiber with high color saturation and good mechanical property and waterproof property, and the method can regulate and control the structural color of the photonic crystal fiber by regulating the particle size of polystyrene microspheres.
The second purpose of the invention is to provide a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure.
The third purpose of the invention is to provide the application of the nylon 66 photonic crystal fiber with the opal structure or the inverse opal structure in the field of textile or intelligent electronic skin.
In order to achieve the first purpose, the invention adopts the following technical scheme:
a preparation method of a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure comprises the following steps: preparing nylon 66 photonic crystal fiber with an opal structure by using electrospinning liquid containing polystyrene microsphere latex and nylon 66 through a directional electrostatic spinning technology;
or preparing the nylon 66 photonic crystal fiber with the opal structure by adopting a sacrificial template method.
Further, in the above method, the polystyrene microsphere in the polystyrene microsphere latex is of a core-shell structure, with polystyrene as a core and poly (acrylic acid-methyl methacrylate) as a shell.
Further, the particle size of the polystyrene microspheres in the polystyrene microsphere latex is 150-300 nm.
Further, the preparation method of the polystyrene microsphere latex comprises the following steps: adding 0.8-1.2 parts by mass of methyl methacrylate, 0.8-1.2 parts by mass of acrylic acid and 17-21 parts by mass of styrene into 80-100 parts by mass of water, and then adding 0-0.027 parts by mass of emulsifier and 0.45-0.55 parts by mass of buffer to obtain a reaction solution; reacting at 60-80 ℃ for 0.5-2h, then adding 0.45-0.5 part by mass of 2-3 wt% ammonium persulfate aqueous solution, reacting at 70-90 ℃ for 10-15h, and then concentrating to obtain the catalyst.
Further, the preparation method of the electrospinning solution containing the polystyrene microsphere latex and the nylon 66 comprises the following steps: dissolving nylon 66 in hexafluoroisopropanol to obtain a nylon 66 solution, then mixing the polystyrene microsphere latex with the nylon 66 solution to obtain a mixed solution, adding triton x-100, and stirring uniformly to obtain the composite material;
or dissolving nylon 66 in hexafluoroisopropanol to obtain nylon 66 solution, mixing the polystyrene microsphere latex with the nylon 66 solution to obtain a mixed solution, adding black powder and Latong x-100, and stirring uniformly to obtain the composite material; wherein the black powder is selected from one or more of cuttlefish powder, graphene, carbon nanotubes and carbon black.
Further, the mass percentage of the nylon 66 in the nylon 66 solution is as follows: 10 to 15 percent; the polystyrene microsphere latex comprises the following polystyrene microspheres in percentage by mass: 30 to 50 percent; the mass of the polystyrene microspheres in the mixed solution is 2-4 times of that of the nylon 66; the addition amount of the black powder is 2-3% of the mass of the polystyrene microsphere; the addition amount of the triton x-100 is 5-10% of the mass of the polystyrene microsphere.
Further, the operating parameters of the electrostatic spinning are as follows: the spinning positive voltage is 5-10kV, and the spinning negative voltage is-4 to-3 kV; the flow rate of the electrospinning liquid is 0.2-0.5mL/h, and the distance from the spinneret to the collector is 15-25 cm; the external conditions of the directional electrostatic spinning are as follows: the indoor humidity is 15-50%.
Further, the conditions of the sacrificial template method are as follows: soaking in tetrahydrofuran or toluene for 10-12 hr.
In order to achieve the second object, the invention provides the following technical scheme:
the nylon 66 photonic crystal fiber with the opal structure or the inverse opal structure is obtained by the preparation method.
In order to achieve the third object, the invention provides the following technical scheme:
the application of the nylon 66 photonic crystal fiber with the opal structure or the inverse opal structure in the fields of textile or intelligent electronic skin.
The invention has the following beneficial effects:
the invention combines nylon 66 with polystyrene microspheres with core-shell structures, and prepares the uniform nylon 66 photonic crystal fiber with opal structure or inverse opal structure with structural color by utilizing the electrostatic spinning technology. Meanwhile, the structural color of the nylon 66 photonic crystal fiber can be regulated and controlled by adjusting the diameter of the polystyrene microsphere.
The invention adopts two methods to improve the structural color brightness of the nylon 66 photonic crystal fiber, one is that tetrahydrofuran is adopted to etch polystyrene microspheres to prepare the inverse opal structure photonic crystal fiber, and the structure increases the structural color saturation of the nylon 66 photonic crystal fiber; secondly, black powder such as cuttlefish powder is doped in the electrospinning liquid, and the cuttlefish powder absorbs scattered light, so that the nylon 66 photonic crystal fiber has higher color saturation, and the fiber has a non-iridescent structural color and can replace the traditional dye in the textile industry, thereby achieving the purpose of protecting the environment.
The preparation method is simple and low in cost, and can prepare a large amount of the nylon 66 photonic crystal fibers with opal structures or inverse opal structures in a short time.
The opal-structured or inverse opal-structured nylon 66 photonic crystal fiber has high color saturation, good mechanical property and waterproof property, and good shape retention when being attached to a 3D structure, so that the opal-structured or inverse opal-structured nylon 66 photonic crystal fiber has good application prospect in the textile industry fields of wearable materials and the like.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 shows an optical microscope image of a nylon 66 photonic crystal fiber; (A) optical microscope images of opal-structured nylon 66 photonic crystal fibers prepared in example 1 are shown; (B) optical microscopy images of opal-structured nylon 66 photonic crystal fibers prepared in example 2 are shown; (C) optical microscopy images of opal-structured nylon 66 photonic crystal fibers prepared in example 3 are shown; (D) an optical microscope image of the opal structured nylon 66 photonic crystal fiber prepared in example 4 is shown.
FIG. 2 shows a scanning electron microscope image of a nylon 66 photonic crystal fiber; (A) scanning electron microscope images of opal-structured nylon 66 photonic crystal fibers prepared in example 1 are shown; (B) scanning electron microscope images of opal-structured nylon 66 photonic crystal fibers prepared in example 2 are shown; (C) scanning electron microscope images of opal-structured nylon 66 photonic crystal fibers prepared in example 3 are shown; (D) scanning electron microscope images of opal-structured nylon 66 photonic crystal fibers prepared in example 4 are shown.
Fig. 3 shows a water contact angle image of an opal-structured nylon 66 photonic crystal fiber prepared in example 1.
Fig. 4 shows a scanning electron microscope image of the inverse opal structured nylon 66 photonic crystal fiber prepared in example 2.
FIG. 5 shows a reflection spectrum of a photonic crystal fiber of a nylon 66 photonic crystal fiber; (A) shows a reflection spectrum of the opal-structured nylon 66 photonic crystal fiber prepared in example 1; (B) shows the reflection spectrum of the opal-structured nylon 66 photonic crystal fiber prepared in example 2; (C) shows a reflection spectrogram of the opal-structured nylon 66 photonic crystal fiber prepared in example 3; (D) the reflection spectrum of the opal-structured nylon 66 photonic crystal fiber prepared in example 4 is shown.
Fig. 6 shows a scanning electron microscope image of the opal-structured nylon 66 photonic crystal fiber prepared in comparative example 1.
FIG. 7 shows the reflection spectrum of a nylon 66 photonic crystal fiber; (A) shows the reflection spectrum of the opal-structured nylon 66 photonic crystal fiber prepared in example 9; (B) the reflection spectrum of the opal-structured nylon 66 photonic crystal fiber prepared in example 5 is shown.
Detailed Description
In order to more clearly illustrate the present invention, the present invention is further described below with reference to preferred embodiments and the accompanying drawings. Similar components in the figures are denoted by the same reference numerals. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The specific embodiment of the invention provides a preparation method of a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure, which comprises the following steps: preparing nylon 66 photonic crystal fiber with an opal structure by using electrospinning liquid containing polystyrene microsphere latex and nylon 66(PA66) through a directional electrospinning technology;
or the nylon 66 photonic crystal fiber with the opal structure is prepared into the nylon 66 photonic crystal fiber with the inverse opal structure by adopting a sacrificial template method.
In addition, in the above method, the polystyrene microspheres in the polystyrene microsphere latex are of a core-shell structure, with polystyrene as a core and poly (acrylic acid-methyl methacrylate) as a shell. Because the polystyrene microsphere has a hard core and soft shell structure, the polystyrene microsphere is more favorable for compact arrangement in the assembling process, and is further easier to assemble into photonic crystals in the electrostatic spinning process, so that the photonic crystal fiber with uniform surface is obtained.
Wherein the particle size of the polystyrene microsphere is 150-300 nm. It should be noted that the photonic crystal assembled in the particle size range has a photonic band gap in the visible light range, and the structural color of the photonic crystal fiber can be controlled by adjusting the particle size, and too large or too small a particle size not only makes assembly difficult but also affects subsequent observation and application.
Illustratively, the preparation method of the polystyrene microsphere latex comprises the following steps: adding 0.8-1.2 parts by mass of methyl methacrylate, 0.8-1.2 parts by mass of acrylic acid and 17-21 parts by mass of styrene into 80-100 parts by mass of water, and then adding 0-0.027 parts by mass of emulsifier and 0.45-0.55 parts by mass of buffer to obtain a reaction solution; reacting at 60-80 deg.C for 0.5-2h, adding 2-3 wt% ammonium persulfate aqueous solution 0.45-0.5, reacting at 70-90 deg.C for 10-15h, and concentrating.
In the preparation method, the emulsifier can be selectively added or not added according to actual needs; when the emulsifier is selected, the addition amount concentration is required to be lower than the critical micelle concentration. The added emulsifier includes but is not limited to sodium dodecylbenzene sulfonate, fatty acid soap or alkyl sulfate (sodium dodecyl sulfate) and the like, and the buffer includes but is not limited to sodium bicarbonate, ammonium chloride or sodium acetate and the like.
For example, the preparation method of the electrospinning solution containing polystyrene microsphere latex and nylon 66 is as follows: dissolving nylon 66 in hexafluoroisopropanol to obtain a nylon 66 solution, then mixing the polystyrene microsphere latex with the nylon 66 solution to obtain a mixed solution, adding triton x-100, and stirring uniformly to obtain the composite material;
or dissolving nylon 66 in hexafluoroisopropanol to obtain nylon 66 solution, mixing the polystyrene microsphere latex with the nylon 66 solution to obtain a mixed solution, adding black powder and triton x-100, and stirring uniformly to obtain the product; wherein the black powder is selected from one or more of cuttlefish powder, graphene, carbon nanotubes and carbon black.
The mass percentage of nylon 66 in the nylon 66 solution is as follows: 10 to 15 percent; the mass percentage of the polystyrene microspheres in the polystyrene microsphere latex is 30-50%; the mass of the polystyrene microspheres in the mixed solution is 2-4 times of that of the nylon 66; the addition amount of the black powder is 2-3% of the mass of the polystyrene microsphere; the addition amount of the triton x-100 is 5-10% of the mass of the polystyrene microsphere.
In the above method, nylon 66 is dissolved in hexafluoroisopropanol, whereas in the prior art, nylon 66 is dissolved in formic acid, hexafluoroisopropanol, etc., but selecting hexafluoroisopropanol as a solvent makes the electrostatic spinning process more stable and the fiber diameter more uniform.
The invention also discovers that the adding amount of nylon 66, polystyrene microspheres and triton x-100 influences the spinning quality, and the photonic crystal fiber with excellent surface appearance and excellent mechanical property can be spun only within the range of the invention.
For example, the addition amount of the triton x-100 is 5-10% of the mass of the polystyrene microsphere, which is not easy to be too high or too low, if the addition amount is too high, the viscosity of the electrostatic spinning solution is reduced, which is not favorable for forming uniform fibers in the electrostatic spinning process, even for forming electrospinning spray, and if the addition amount is too low, the polystyrene microsphere is not uniformly dispersed, which is not favorable for forming uniform nylon 66 photonic crystal fibers.
In addition, black powder can be added during the preparation of the electrospinning liquid so as to obtain the electrospinning liquid with high contrast, and nylon 66 photonic crystal fibers with higher color saturation can be obtained after electrostatic spinning. More specifically, the black powder can enable the photonic crystal fiber material to absorb more scattered light, the photonic crystal fiber material can improve the color saturation of the material by absorbing the scattered light, and meanwhile, a long-range disordered short-range ordered amorphous photonic structure can be formed, so that the material presents a non-iridescent structural color, and the structural color does not change along with the change of an observation angle.
Illustratively, the operating parameters of the electrospinning are: the spinning positive voltage is 6.5kV, and the spinning negative voltage is-3.5 kV; the flow rate of the electrospinning liquid is 0.3mL/h, and the distance from the spinneret to the collector is 20 cm; the external conditions of the directional electrostatic spinning are as follows: the indoor humidity was 20%.
The electrostatic spinning voltage affects the amount of charge charged in electrospinning and the fiber diameter, and generally, the larger the electrostatic spinning voltage, the smaller the fiber diameter. The electrospinning liquid flow rate (bolus rate) affects the fiber diameter, and in general, the larger the bolus rate, the larger the diameter of the resulting fiber. In addition, increased room humidity affects the speed of fiber curing, and the fibers take more time to complete the curing process and therefore the smaller the diameter of the resulting fiber. Therefore, the nylon 66 photonic crystal fiber prepared within the range of the operating parameters of the invention has excellent surface appearance and excellent mechanical properties, and can maintain the good color of the photonic crystal fiber, and if the range of the invention is exceeded, the nylon 66 photonic crystal fiber can not obtain the nanofiber with excellent surface appearance.
In addition, the nylon 66 photonic crystal fiber with the inverse opal structure is prepared by a sacrificial template method, which is a template etching process, polystyrene microspheres are used as a template, tetrahydrofuran is used as an etching agent, the polystyrene microspheres are etched, and generated holes form a regular microstructure to generate photonic band gaps, so that the nylon 66 photonic crystal fiber with the opal structure is converted into the nylon 66 photonic crystal fiber with the inverse opal structure.
The invention adopts two methods to improve the structural color brightness of the nylon 66 photonic crystal fiber film, one is that the tetrahydrofuran is adopted to etch the polystyrene microspheres to prepare the inverse opal structure photonic crystal fiber, so that the structural color saturation of the photonic crystal fiber film is increased; secondly, by doping black powder substances such as cuttlefish powder in the electrospinning liquid, the black powder absorbs scattered light, so that the photonic crystal fiber formed by electrospinning has higher color saturation, and meanwhile, the photonic crystal fiber has a non-iridescent structural color.
Example 1
1. Preparing core-shell structure polystyrene microsphere latex:
adding 1 part by mass of methyl methacrylate, 1 part by mass of acrylic acid and 19 parts by mass of styrene into 100 parts by mass of water, then adding 0.017 parts by mass of emulsifier sodium dodecyl benzene sulfonate and 0.49 parts by mass of buffer ammonium bicarbonate to obtain a reaction liquid, reacting the reaction liquid at 70 ℃ for 1 hour, adding 0.48 part by mass of an aqueous solution of ammonium persulfate, reacting at 80 ℃ for 12 hours to obtain a polystyrene microsphere emulsion with a core-shell structure and a particle size of 160nm, and concentrating the polystyrene microsphere emulsion into a latex (colloidal emulsion) with a concentration of 30%.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol solvent to obtain nylon 66 solution with mass concentration of 13%, mixing 0.6g of the colloidal emulsion prepared in the step 1 with 0.5169g of 13% PA66 solution, adding 20mg of triton x-100, and performing magnetic stirring for 4h and ultrasonic treatment for 30min to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of the opal-structured nylon 66 photonic crystal fiber:
and transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
From fig. 3, it can be seen that the water contact angle of the nylon 66 photonic crystal fiber with the opal structure is 133.3 °, so that the nylon 66 photonic crystal fiber obtained by the method has waterproof performance.
Example 2
1. Preparing core-shell structure polystyrene microsphere latex:
adding 1 part by mass of methyl methacrylate, 1 part by mass of acrylic acid and 19 parts by mass of styrene into 100 parts by mass of water, then adding 0.012 part by mass of emulsifier sodium dodecyl benzene sulfonate and 0.49 part by mass of buffer sodium bicarbonate to obtain a reaction solution, reacting the reaction solution at 70 ℃ for 1h, then adding 0.48 part by mass of an aqueous solution of ammonium persulfate, reacting at 80 ℃ for 12h to obtain a polystyrene microsphere emulsion with a core-shell structure and a particle size of 198nm, and then concentrating the polystyrene microsphere emulsion into a colloidal emulsion with a concentration of 40%.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol as a solvent to obtain a nylon 66 solution with the mass concentration of 13%, mixing 0.5123g of the colloidal emulsion prepared in the step 1 with 0.5691g of the nylon 66 solution with the mass concentration of 13%, adding 20mg of triton x-100, and performing magnetic stirring for 4 hours and ultrasonic treatment for 30 minutes to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
and transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
4. Preparing a nylon 66 photonic crystal fiber film with an inverse opal structure:
soaking the nylon 66 photonic crystal fiber with the opal structure in tetrahydrofuran for 10-12h to obtain the nylon 66 photonic crystal fiber with the inverse opal structure.
Example 3
1. Preparing core-shell structure polystyrene microsphere latex:
adding 1 part by mass of methyl methacrylate, 1 part by mass of acrylic acid and 19 parts by mass of styrene into 100 parts by mass of water, then adding 0.010 part by mass of emulsifier sodium dodecyl benzene sulfonate and 0.49 part by mass of buffer sodium bicarbonate to obtain a reaction solution, reacting the reaction solution at 70 ℃ for 1 hour, adding 0.48 part by mass of an aqueous solution of ammonium persulfate, reacting at 80 ℃ for 12 hours to obtain a polystyrene microsphere emulsion with a core-shell structure and a particle size of 222nm, and concentrating the polystyrene microsphere emulsion into a colloidal emulsion with a concentration of 40%.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol as a solvent to obtain a nylon 66 solution with the mass concentration of 13%, mixing 0.625g of the colloidal emulsion prepared in the step 1 with 0.6592g of the nylon 66 solution with the mass concentration of 13%, adding 20mg of triton x-100, and carrying out magnetic stirring for 4 hours and ultrasonic treatment for 30 minutes to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
Example 4
1. Preparing core-shell structure polystyrene microsphere latex:
adding 1 part by mass of methyl methacrylate, 1 part by mass of acrylic acid and 19 parts by mass of styrene into 100 parts by mass of water, then adding 0.0065 part by mass of emulsifier sodium dodecyl benzene sulfonate and 0.49 part by mass of buffer sodium bicarbonate, reacting the reaction solution at 70 ℃ for 1h, then adding 0.48 part by mass of ammonium persulfate aqueous solution, reacting at 80 ℃ for 12h to obtain the polystyrene microsphere emulsion with the core-shell structure and the particle size of 245nm, and then concentrating the polystyrene microsphere emulsion into 30% colloidal emulsion.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol serving as a solvent to obtain a nylon 66 solution with the mass concentration of 13%, mixing 0.6g of the colloidal emulsion prepared in the step 1 with 0.5169g of the nylon 66 solution with the mass concentration of 13%, adding 20mg of triton x-100, and carrying out magnetic stirring for 4 hours and ultrasonic stirring for 30min to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
Example 5
1. Preparing core-shell structure polystyrene microsphere latex:
adding 1 part by mass of methyl methacrylate, 1 part by mass of acrylic acid and 19 parts by mass of styrene into 100 parts by mass of water, then adding 0.005 part by mass of emulsifier sodium dodecyl benzene sulfonate and 0.49 part by mass of buffer sodium bicarbonate to obtain a reaction solution, reacting the reaction solution at 70 ℃ for 1h, then adding 0.48 part by mass of an aqueous solution of ammonium persulfate, reacting at 80 ℃ for 12h to obtain a polystyrene microsphere emulsion with a core-shell structure and a particle size of 255nm, and then concentrating the polystyrene microsphere emulsion into a colloidal emulsion with a concentration of 40%.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol as a solvent to obtain a nylon 66 solution with the mass concentration of 13%, mixing 0.61g of the colloidal emulsion prepared in the step 1 with 0.63g of the nylon 66 solution with the mass concentration of 13%, adding 20mg of triton x-100, and carrying out magnetic stirring for 4 hours and ultrasonic treatment for 30 minutes to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of the opal-structured nylon 66 photonic crystal fiber:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
Example 6
1. The core-shell polystyrene microsphere latex was prepared as in example 2.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol as a solvent to obtain a nylon 66 solution with the mass concentration of 13%, mixing 0.6g of the colloidal emulsion prepared in the step 1 with 0.5169g of the nylon 66 solution with the mass concentration of 13%, adding 20mg of triton x-100, and carrying out magnetic stirring for 4 hours and ultrasonic treatment for 30 minutes to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
Example 7
1. The core-shell structure polystyrene-containing microsphere latex was prepared as in example 3.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol serving as a solvent to obtain a nylon 66 solution with the mass concentration of 13%, mixing 0.61g of the colloidal emulsion prepared in the step 1 with 0.4808g of the nylon 66 solution with the mass concentration of 13%, adding 20mg of triton x-100, and carrying out magnetic stirring for 4 hours and ultrasonic stirring for 30 minutes to uniformly stir the mixture to obtain the electro-spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
Example 8
1. The core-shell polystyrene microsphere latex was prepared as in example 4.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol solvent to obtain nylon 66 solution with mass concentration of 13%, mixing 0.6g of the colloidal emulsion prepared in the step 1 with 0.6154g of the nylon 66 solution with mass concentration of 13%, adding 7mg of cuttlefish powder and 20mg of triton x-100, and stirring uniformly by magnetic stirring for 4h and ultrasonic treatment for 30min to obtain uniform electrospinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the opal-structured nylon 66 photonic crystal fiber with high color saturation by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
Example 9
1. The core-shell polystyrene microsphere latex was prepared as in example 5.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol solvent to obtain nylon 66 solution with mass concentration of 13%, mixing 0.6g of the colloidal emulsion prepared in the step 1 with 0.6g of the nylon 66 solution with mass concentration of 13%, adding 7mg of cuttlefish powder and 20mg of triton x-100, and stirring for 4h by magnetic stirring and ultrasonic treatment for 30min to uniformly stir the materials to obtain the electric spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the opal-structured nylon 66 photonic crystal fiber with high color saturation by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
And (3) knotting: by comparing the reflection spectra of the photonic crystal fibers in fig. 7(a) and fig. 7(B), it can be seen that the photonic crystal fiber film added with cuttlefish powder has higher reflectivity and higher reflection peak compared to the photonic crystal fiber film without cuttlefish powder, thus indicating that the structural color of the fiber is more obvious by adding cuttlefish powder, and concluding that the cuttlefish powder can increase the color saturation of the structural color.
Comparative example 1
1. The core-shell polystyrene microsphere latex was prepared as in example 1.
2. Preparing an electrospinning solution:
dissolving nylon 66 in hexafluoroisopropanol solvent to obtain nylon 66 solution with mass concentration of 13%, mixing 0.6g of the colloidal emulsion prepared in the step 1 with 1.38g of the nylon 66 solution with mass concentration of 13%, adding 20mg of triton x-100, and stirring uniformly by magnetic stirring for 4h and ultrasonic treatment for 30min to obtain the electro-spinning solution.
3. Preparation of nylon 66 photonic crystal fiber of opal structure:
transferring the electrospinning solution into a 5ml plastic needle tube with a metal needle (20#), and preparing the nylon 66 photonic crystal fiber with the opal structure by using electrostatic spinning equipment when the indoor humidity is 20%. The operating parameters of electrostatic spinning are as follows: the spinning positive voltage is 6.5kV, the spinning negative voltage is-3.5 kV, the flow rate of the electrospinning solution is 0.3ml/h, and the distance from the spinning nozzle to the collector is 20 cm.
The scanning electron microscope image of fig. 6 shows that under the spinning condition, that is, the mass ratio of the colloidal emulsion of the polystyrene microspheres to the nylon 66 solution is not within the range of the invention, the photonic crystal fiber with good morphology cannot be prepared, that is, the invention cannot be realized
It should be understood that the above-described embodiments of the present invention are examples for clearly illustrating the invention, and are not to be construed as limiting the embodiments of the present invention, and it will be obvious to those skilled in the art that various changes and modifications can be made on the basis of the above description, and it is not intended to exhaust all embodiments, and obvious changes and modifications can be made on the basis of the technical solutions of the present invention.
Claims (10)
1. A preparation method of a nylon 66 photonic crystal fiber with a opal structure or an inverse opal structure is characterized by comprising the following steps: preparing nylon 66 photonic crystal fiber with an opal structure by using electrospinning liquid containing polystyrene microsphere latex and nylon 66 through a directional electrostatic spinning technology;
or the nylon 66 photonic crystal fiber with the opal structure is prepared into the nylon 66 photonic crystal fiber with the inverse opal structure by adopting a sacrificial template method.
2. The preparation method of claim 1, wherein the polystyrene microsphere latex has a core-shell structure, wherein polystyrene is used as a core, and poly (acrylic acid-methyl methacrylate) is used as a shell.
3. The method as claimed in claim 1, wherein the polystyrene microsphere latex has a particle size of 150-300 nm.
4. The preparation method of claim 1, wherein the preparation method of the polystyrene microsphere latex comprises the following steps:
adding 0.8-1.2 parts by mass of methyl methacrylate, 0.8-1.2 parts by mass of acrylic acid and 17-21 parts by mass of styrene into 80-100 parts by mass of water, and then adding 0-0.027 parts by mass of emulsifier and 0.45-0.55 parts by mass of buffer to obtain a reaction solution; reacting at 60-80 ℃ for 0.5-2h, then adding 0.45-0.5 part by mass of 2-3 wt% ammonium persulfate aqueous solution, reacting at 70-90 ℃ for 10-15h, and then concentrating to obtain the catalyst.
5. The preparation method of claim 1, wherein the preparation method of the electrospinning solution containing the polystyrene microsphere latex and the nylon 66 comprises the following steps: dissolving nylon 66 in hexafluoroisopropanol to obtain a nylon 66 solution, then mixing the polystyrene microsphere latex with the nylon 66 solution to obtain a mixed solution, adding triton x-100, and stirring uniformly to obtain the composite material;
or dissolving nylon 66 in hexafluoroisopropanol to obtain nylon 66 solution, mixing the polystyrene microsphere latex with the nylon 66 solution to obtain a mixed solution, adding black powder and triton x-100, and stirring uniformly to obtain the product; wherein the black powder is selected from one or more of cuttlefish powder, graphene, carbon nanotubes and carbon black.
6. The preparation method according to claim 5, wherein the mass percent of the nylon 66 in the nylon 66 solution is 10-15%; the mass percentage of the polystyrene microspheres in the polystyrene microsphere latex is 30-50%; the mass of the polystyrene microspheres in the mixed solution is 2-4 times of that of the nylon 66; the addition amount of the black powder is 2-3% of the mass of the polystyrene microsphere; the addition amount of the triton x-100 is 5-10% of the mass of the polystyrene microsphere.
7. The method for preparing the fiber according to claim 1, wherein the operating parameters of the directional electrostatic spinning are as follows: the spinning positive voltage is 5-10kV, and the spinning negative voltage is-4 to-3 kV; the flow rate of the electrospinning liquid is 0.2-0.5mL/h, and the distance from the spinneret to the collector is 15-25 cm; the external conditions of the directional electrostatic spinning are as follows: the indoor humidity is 15-50%.
8. The method according to claim 1, wherein the conditions of the sacrificial template method are: soaking in tetrahydrofuran or toluene for 10-12 hr.
9. An opal-structured or inverse opal-structured nylon 66 photonic crystal fiber obtained by the preparation method according to any one of claims 1 to 8.
10. Use of the opal-structured or inverse opal-structured nylon 66 photonic crystal fiber of claim 9 in textile or smart electronic skin applications.
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| CN105525343A (en) * | 2015-12-18 | 2016-04-27 | 中国科学院理化技术研究所 | Preparation method and application of carbon dot photonic crystal having opal structure or inverse opal structure |
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| CN110079839A (en) * | 2019-04-24 | 2019-08-02 | 上海交通大学 | A kind of method that electro-deposition prepares the 3-D ordered multiporous photonic crystal of metallic aluminium |
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