CN114605807A - Polycarbonate diol-based structural color elastomer and preparation method thereof - Google Patents
Polycarbonate diol-based structural color elastomer and preparation method thereof Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/103—Detecting, measuring or recording devices for testing the shape, pattern, colour, size or movement of the body or parts thereof, for diagnostic purposes
- A61B5/11—Measuring movement of the entire body or parts thereof, e.g. head or hand tremor, mobility of a limb
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- A—HUMAN NECESSITIES
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- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
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- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
Abstract
The invention provides a polycarbonate diol-based structural color elastomer and a preparation method thereof. The polycarbonate diol elastomer is obtained by bulk polymerization of polycarbonate diol, glycerol and 4,4' -dicyclohexylmethane diisocyanate under the action of a catalyst dibutyltin dilaurate; the photonic crystal is obtained by self-assembling PS @ SiO2 microsphere particles; the PS @ SiO2 microsphere particles are prepared by polymerizing styrene through emulsion, and then coating the polystyrene microsphere particles with vinyltriethoxysilane. The structural color elastomer has potential application in visual sensing and intelligent wearable devices.
Description
Technical Field
The invention relates to the technical field of opal photonic crystal materials, in particular to a polycarbonate diol-based structural color elastomer and a preparation method and application thereof.
Background
The structural color is the color generated by the interaction of light waves and the nano-microstructures, and is widely researched due to the advantages of bright color, easy color adjustment, fading resistance and the like. The structural color of the photonic crystal is an effective means for artificially designing and preparing the structural color. The photonic crystal is an ordered structural material formed by arranging two or more dielectric materials with different dielectric constants according to a certain periodic sequence, and has a photonic band gap, when the photonic band gap falls in a visible light range, visible light beams with specific frequencies are prohibited from being transmitted through the photonic crystal and reflected back to show structural color. Many researchers combine photonic crystal and elastomer to prepare structural color elastomer, adjust its colour through the lattice spacing of adjusting colloidal particle in the mechanical deformation process, because its easy tensile force discolours the characteristics, structural color elastomer has wide application prospect in fields such as flexible wearable equipment, human motion detection, human health, man-machine interaction.
Tan et al incorporate silica nanoparticles into supramolecular elastomer matrices based on metal coordination interactions between amino-terminated poly (dimethylsiloxane) and trichlorocerium, producing supramolecular structure-colored elastomers whose structural color is not angle-dependent and which have good self-healing properties (adv. Mater.,2019,31(6): 1805496). Li et al incorporate carbon-coated ferroferric oxide nanoparticles into amino-terminated polydimethylsiloxane polymers by supramolecular action, the carbon-coated ferroferric oxide nanoparticles are ordered in short range in the polymer molecular chain, so the color has no angular dependence, in addition, the wide spectral response can be realized, and the cutting opening and the scratch can be quickly healed under the irradiation of laser and sunlight (adv. Funct. Mater.2020,30(16): 2000008). Chinese patent No. CN202010195856.4, entitled "a method for preparing structural color coating with photochromic ability" the method is that a polymer matrix material and nanoparticles are dispersed in a solvent to form a precursor dispersion; and then removing the solvent from the precursor dispersion liquid in a pre-designed mould or on a pre-designed substrate by using a solvent volatilization method or a spraying method to obtain the structural color coating with the mechanochromism capability. The nano particles are orderly arranged in the polymer matrix through the assembly parts, so that the structural color coating can express colors, and the colors can be changed along with the external force action on the color coating to generate force-induced color change. The structural color elastomer prepared by the methods has low mechanical strength, poor creep resistance and insufficient brightness, and the practical application of the material is limited to a great extent.
Disclosure of Invention
In order to solve the problems of the structural color elastomer prepared by the method, the invention provides the structural color elastomer with high mechanical strength and self-healing property and the preparation method thereof, a novel dynamic reversible cross-linked polymer network is constructed by polycarbonate diol, glycerol and 4,4' -dicyclohexylmethane diisocyanate, and the assembled photonic crystal and the dynamic reversible cross-linked polymer network are compounded to prepare the photonic elastomer with stable optical function, high mechanical strength and better self-healing property. The photon elastomer can be applied to human joint motion detection, and the color of the photon elastomer generates blue shift along with the motion of joints, so that the photon elastomer has good visualization capability.
It is an object of the present invention to provide structural color elastomers based on polycarbonate diols.
Another object of the present invention is to provide a process for producing the above-mentioned polycarbonate diol-based structural color elastomer.
The invention also provides the use of the structural color elastomer based on polycarbonate diol.
The technical scheme adopted by the invention is as follows:
polycarbonate diol-based structural color elastomerIs compounded by polycarbonate diol elastomer and opal photonic crystal. The elastomer based on polycarbonate diol is obtained by bulk polymerization of polycarbonate diol, glycerol and 4,4' -dicyclohexylmethane diisocyanate under the action of a catalyst dibutyltin dilaurate; the photonic crystal is formed by PS @ SiO2Self-assembling the microsphere particles; the PS @ SiO2The microsphere particles are prepared by polymerizing styrene through emulsion to obtain polystyrene microsphere particles, and then coating the polystyrene microsphere particles with vinyltriethoxysilane.
The preparation method of the structural color elastomer based on the polycarbonate diol comprises the following steps:
(1) dispersing styrene in deionized water under the emulsification action of sodium dodecyl sulfate, adding an initiator, and performing emulsion polymerization to obtain a polystyrene microsphere stock solution; the amount of the surfactant sodium dodecyl sulfate can regulate and control the size of the polystyrene colloidal particle microspheres;
(2) dispersing the polystyrene microsphere stock solution prepared in the step (1) in deionized water, adding vinyltriethoxysilane under the action of ammonia water, and coating polystyrene microsphere particles to obtain PS @ SiO2The microsphere particles are prepared by centrifuging the reaction solution and then centrifuging the centrifuged PS @ SiO2Washing, and then ultrasonically dispersing the solution uniformly in ethanol to obtain PS @ SiO2A microsphere dispersion;
(3) mixing PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and carrying out self-assembly on a heating plate to ensure that the opal photonic crystal template with bright color can be formed after the solvent is completely volatilized;
(4) uniformly mixing polycarbonate diol, glycerol, 4' -dicyclohexylmethane diisocyanate and dibutyltin dilaurate to prepare an elastomer precursor solution;
(5) and (3) injecting the elastomer precursor liquid in the step (4) into the opal photonic crystal template in the step (3), removing bubbles, and then heating and curing to obtain the polycarbonate diol-based structural color elastomer.
According to the above technical solution, preferably, the mass ratio of the sodium dodecyl sulfonate to the styrene in the step (1) is 0.0043-0.0053: 1.
according to the technical scheme, preferably, the mass ratio of the initiator to the styrene in the step (1) is 0.0067-0.01: 1.
according to the technical scheme, preferably, the mass ratio of the deionized water to the styrene in the step (1) is 9-10: 1.
according to the above technical scheme, the initiator in the step (1) is preferably potassium persulfate or ammonium persulfate.
According to the above technical scheme, the reaction conditions of the emulsion polymerization in the step (1) are preferably full nitrogen protection.
According to the above technical scheme, preferably, the reaction temperature of the emulsion polymerization in the step (1) is 80-90 ℃.
According to the above technical scheme, preferably, the reaction time of the emulsion polymerization in the step (1) is 4-6 hours, and the size of the microspheres can be controlled.
According to the technical scheme, the particle size of the polystyrene microsphere particles in the step (1) is 438.6-497.8 nm.
According to the technical scheme, preferably, the volume ratio of the deionized water to the polystyrene microsphere stock solution in the step (2) is 28-30: 1.
according to the technical scheme, preferably, the volume ratio of the ammonia water to the polystyrene microsphere stock solution in the step (2) is 1.5-1.67: 1.
according to the above technical solution, preferably, the volume ratio of the vinyltriethoxysilane to the polystyrene microsphere stock solution in the step (2) is 0.33-0.5: 1.
according to the technical scheme, preferably, the reaction temperature of the whole coating process in the step (2) is 20-30 ℃.
According to the above technical scheme, preferably, in the coating process in the step (2), the reaction time is 2-4 hours.
According to the technical scheme, preferably, the rotation speed of the ammonia water during the coating reaction in the step (2) is 500-600 rpm.
According to the technical scheme, preferably, the rotation speed of the vinyl triethoxysilane added in the coating reaction in the step (2) is 300-350 rpm.
According to the above technical solution, preferably, the centrifugation rate of the reaction solution in the step (2) is 8000-9500 rpm.
According to the technical scheme, in the preferable case, the PS @ SiO in the step (2)2The washing is as follows: washing with deionized water, and washing with anhydrous ethanol for 3 times.
According to the technical scheme, the PS @ SiO alcohol washing by absolute ethyl alcohol in the step (2) is preferably performed2In the process of the microsphere particles, centrifugal washing can be used, and the centrifugal speed is 6000-6500 rpm.
According to the technical scheme, the absolute ethanol washed PS @ SiO in the step (2) is preferable2The microsphere particles are dispersed in a proper amount of absolute ethyl alcohol, for example, the dosage of the absolute ethyl alcohol is 20-30 ml.
According to the technical scheme, the PS @ SiO dispersed in absolute ethyl alcohol in the step (2) is preferably used2The mass concentration is 1-5%.
According to the technical scheme, in the preferable case, the PS @ SiO in the step (3)2The self-assembly temperature of the microsphere particles is 40-60 ℃.
According to the above technical means, it is preferable that the molar ratio of the polycarbonate diol to the hydroxyl groups of glycerin in the step (4) is 0.1 to 0.33: 1.
according to the above technical solution, it is preferable that the molar ratio of the sum of the molar amounts of the hydroxyl groups of the polycarbonate diol and the glycerol in the step (4) to the isocyanate of the 4,4' -dicyclohexylmethane diisocyanate is 0.9 to 1.1: 1.
according to the above technical means, it is preferable that the polycarbonate diol in the step (4) has a weight average molecular weight of 1000g/mol to 3000 g/mol.
According to the technical scheme, preferably, the temperature of the elastomer precursor liquid prepared in the step (4) is controlled to be 45-60 ℃.
According to the above technical solution, preferably, the ratio of the mass of the dibutyltin dilaurate in the step (4) to the total mass of the reactants (polycarbonate diol, glycerol, 4' -dicyclohexylmethane diisocyanate) is 0.6-1%.
According to the above technical solution, preferably, the means for removing bubbles from the photonic crystal injected with the elastic precursor liquid in step (5) is to use an oil pump to evacuate, that is, to put the photonic crystal into a vacuum drying oven to evacuate.
According to the above technical solution, preferably, the time for vacuuming the photonic crystal injected with the elastic precursor liquid in the step (5) is 1 to 2 hours when removing bubbles.
According to the above technical solution, preferably, the temperature of the photonic crystal injected with the elastic precursor liquid in the step (5) is 60 to 80 ℃ when the photonic crystal is heated and cured.
According to the above technical solution, preferably, the time for heating and curing the photonic crystal injected with the elastic precursor liquid in the step (5) is 2 to 6 hours.
The invention has the beneficial effects that:
(1) the invention has good force-induced discoloration performance, and the color of the elastomer gradually blueshifts with the stress applied to the structural color elastomer based on the polycarbonate diol. After stretching, the color gradually shifts from red to blue to cyan, the corresponding reflection wavelength gradually shifts from 610nm to 570nm in the short wave direction, the color is uniform, and the optical performance is excellent.
(2) The elongation at break of the invention can reach 5500%, the mechanical strength can reach 4.5MPa, after the self-healing is carried out for 48 hours at 80 ℃, the self-healing efficiency based on stress can reach 74%, and the self-healing efficiency based on strain can reach 84%.
(3) The invention can be applied to human joint motion detection, and the color of the joint generates blue shift along with the motion of the joint, so that the invention has good visualization capability and potential application in visual sensing and intelligent wearable equipment.
Drawings
FIG. 1 depicts PS microspheres and PS @ SiO synthesized as described in example 12Scanning electron microscope image of microsphere, wherein a is PS microsphere, b is PS @ SiO2And (3) microspheres.
FIG. 2 is a tensile stress strain plot of structural color elastomers based on polycarbonate diol in examples 1-3. The graphical information shows that as the glycerol crosslinker is increased, the tensile strength of the elastomer increases and the elongation at break decreases.
Fig. 3 is a tensile stress-strain curve of the unrepaired sample and the original sample in example 2, in which the middle of the tensile sample is cut with a scalpel to a depth of half the thickness of the sample, the tensile stress-strain curve showing that the self-healing efficiency of the polymer at 80 ℃ for 48 hours is 74% and 84% based on the stress and the self-healing efficiency of the polymer at 80 ℃ for 48 hours.
FIG. 4 is PS @ SiO in example 22Reflectance spectra of opal photonic crystal templates and polycarbonate diol-based structurally colored elastomers. The graphical information shows that the reflection wavelength of the assembled opal photonic crystal template is 525nm, and the reflection wavelength of the structural color elastomer based on the polycarbonate diol is 620nm, namely the reflection wavelength of the assembled opal photonic crystal template is red-shifted after the assembled opal photonic crystal template is injected into the elastomer precursor liquid, because the air in the gaps of the opal photonic crystal template microspheres is replaced by the elastomer, the difference of the effective refractive indexes is increased, and according to the Bragg formula, the reflection wavelength is increased and red-shifted.
FIG. 5 is a scanning electron micrograph of a cross section of a structural color elastomer based on polycarbonate diol of example 2. The graphical information shows that after the assembled opal photonic crystal template is injected with the elastomer precursor liquid, the spacing between the microspheres is increased to form a non-close-packed face-centered cubic lattice.
FIG. 6 is a digital photograph of a stretched structural color elastomer based on polycarbonate diol of example 2, with increasing applied force from left to right. The graphical information shows that the color gradually shifts from red to cyan after stretching.
FIG. 7 is a chart of the tensile reflectance spectra of polycarbonate diol-based structural color elastomers of example 2. The graphical representation shows that as the structural color elastomer based on polycarbonate diol is stressed, the reflection wavelength gradually shifts from 610nm to 570nm in the short wave direction, and the reflection wavelength gradually decreases with the increase of stress.
Detailed Description
The present invention is further illustrated in detail below with reference to specific examples, which are intended to better explain the invention without limiting it.
The invention relates to a polycarbonate diol-based structural color elastomer, which is formed by compounding a polycarbonate diol elastomer and a photonic crystal. The polycarbonate diol elastomer is obtained by bulk polymerization of polycarbonate diol, glycerol and 4,4' -dicyclohexylmethane diisocyanate under the action of a catalyst dibutyltin dilaurate; the photonic crystal is formed by PS @ SiO2Self-assembling the microsphere particles; the PS @ SiO2The microsphere particles are prepared by polymerizing styrene through emulsion to obtain polystyrene microsphere particles, and then coating the polystyrene microsphere particles with vinyltriethoxysilane. The structural color elastomer has potential application in visual sensing and intelligent wearable devices.
Example 1
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.072g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10 minutes at the temperature of 80 ℃ oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of potassium persulfate initiator, continuously stirring for reacting for 6 hours, stopping the reaction, pouring the reaction solution into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mLPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring at the rotating speed of 300rpm for 10 minutes, uniformly mixing, and then adding into a reaction bottle4.5mL of ammonia water and 27mL of deionized water were added and stirring was continued for 15 minutes, and 1500. mu.l of vinyltriethoxysilane was added dropwise to the reaction flask and reacted at 200rpm for about 3 hours. Then centrifuging the reaction liquid at 6500rpm for 15 minutes, pouring out the supernatant in a centrifugal tube, adding 30mL of deionized water, putting the centrifugal tube into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the centrifugal tube into a centrifuge for centrifugal treatment at 6500rpm for 15 minutes, then pouring out the supernatant, cleaning the centrifugal tube with deionized water for 3 times in the above manner, adding 30mL of absolute ethyl alcohol into the centrifugal tube, putting the centrifugal tube into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, then putting the centrifugal tube into the centrifuge for centrifugal treatment at 6000rpm for 10 minutes, pouring out the supernatant in the centrifugal tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly washing with absolute ethyl alcohol for three times, and then washing the PS SiO with absolute ethyl alcohol again, and finally pouring out the supernatant in the centrifugal tube2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with the weight-average molecular weight of 2000g/mol in a vacuum drying oven at 100 ℃ for vacuumizing for 3 hours, taking 4g of dried polycarbonate diol and 0.01227g of glycerol, placing the dried polycarbonate diol and the 0.01227g of glycerol in a 20mL sample bottle, stirring the mixture for 15 minutes at the rotating speed of 700rpm at the temperature of 50 ℃, uniformly mixing the mixture, adding 625 mu l of 4,4' -dicyclohexylmethane diisocyanate, continuously stirring the mixture for 20 minutes at the reaction temperature of 60 ℃, reducing the temperature to 50 ℃, uniformly mixing the mixture, adding 1 wt% of dibutyltin dilaurate, stirring the mixture for 3 minutes at the rotating speed of 1000rpm, injecting the mixture into the assembled PS @ SiO2And (3) scraping the opal photonic crystal template by using a glass plate, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the red structural color elastomer based on the polycarbonate diol.
Example 2
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.072g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10 minutes at the temperature of 80 ℃ oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of potassium persulfate initiator, continuously stirring for reacting for 6 hours, stopping the reaction, pouring the reaction solution into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mL LPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring for 10 minutes at the rotating speed of 300rpm, uniformly mixing, adding 4.5mL ammonia water and 27mL deionized water into a reaction bottle, continuously stirring for 15 minutes, dropwise adding 1500 mu l vinyltriethoxysilane into the reaction bottle, and reacting for about 3 hours at the rotating speed of 200 rpm. Then centrifuging the reaction solution at 6500rpm for 15 minutes, pouring out the supernatant in a centrifuge tube, adding 30mL of deionized water, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the mixture into a centrifuge for centrifugal treatment at 6500rpm for 15 minutes, pouring out the supernatant, cleaning the mixture for 3 times by using deionized water in the above manner, adding 30mL of absolute ethyl alcohol into the centrifuge tube, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, then putting the mixture into the centrifuge for centrifugal treatment at 6000rpm for 10 minutes, pouring out the supernatant in the centrifuge tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly wash the mixture for three times by using absolute ethyl alcohol, and then washing the cleaned PS @ SiO by using absolute ethyl alcohol again2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with weight average molecular weight of 2000g/mol in a vacuum drying oven at 100 deg.C, vacuumizing for 3 hr, placing 4g of dried polycarbonate diol and 0.0245g of glycerol in a 20mL sample bottle, stirring at 50 deg.C and 700rpm for 15min, mixing, adding 680 μ l of 4,4' -dicyclohexylmethane diisocyanate, stirring at 60 deg.C for 20 min, mixing, and dryingCooling to 50 deg.C, mixing, adding 1 wt% dibutyltin dilaurate, stirring at 1000rpm for 3 min, and injecting into the PS @ SiO2And (3) scraping the opal photonic crystal template by using a glass plate, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the red structural color elastomer based on the polycarbonate diol.
Example 3
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.072g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10 minutes at the temperature of 80 ℃ oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of potassium persulfate initiator, continuously stirring for reacting for 6 hours, stopping the reaction, pouring the reaction solution into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mL LPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring for 10 minutes at the rotating speed of 300rpm, uniformly mixing, adding 4.5mL ammonia water and 27mL deionized water into a reaction bottle, continuously stirring for 15 minutes, dropwise adding 1500 mu l vinyltriethoxysilane into the reaction bottle, and reacting for about 3 hours at the rotating speed of 200 rpm. Then centrifuging the reaction solution at 6500rpm for 15 minutes, pouring out the supernatant in a centrifuge tube, adding 30mL of deionized water, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the mixture into a centrifuge for centrifugal treatment at 6500rpm for 15 minutes, pouring out the supernatant, cleaning the mixture for 3 times by using deionized water in the above manner, adding 30mL of absolute ethyl alcohol into the centrifuge tube, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, then putting the mixture into the centrifuge for centrifugal treatment at 6000rpm for 10 minutes, pouring out the supernatant in the centrifuge tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly wash the mixture for three times by using absolute ethyl alcohol, and then washing the cleaned PS @ SiO by using absolute ethyl alcohol again2Adding 30mL of absolute ethyl alcohol, and putting the mixture into a 180W ultrasonic cleanerAfter 30 minutes of medium ultrasonic treatment, PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with weight average molecular weight of 2000g/mol in a vacuum drying oven at 100 ℃ for vacuumizing for 3 hours, taking 4g of dried polycarbonate diol and 0.0409g of glycerol, placing the dried polycarbonate diol and 0.0409g of glycerol into a 20mL sample bottle, stirring the mixture for 15 minutes at the rotating speed of 700rpm at the temperature of 50 ℃, uniformly mixing the mixture, adding 755 mu l of 4,4' -dicyclohexylmethane diisocyanate, continuously stirring the mixture for 20 minutes at the reaction temperature of 60 ℃, reducing the temperature to 50 ℃, uniformly mixing the mixture, adding 1 wt% of dibutyltin dilaurate, stirring the mixture for 3 minutes at the rotating speed of 1000rpm, injecting the mixture into the assembled PS @ SiO @2And (3) scraping the opal photonic crystal template by using a glass plate, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the red structural color elastomer based on the polycarbonate diol.
Example 4
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.065g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10 minutes at the temperature of 80 ℃ in an oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of potassium persulfate initiator, continuously stirring for reaction for 6 hours, stopping the reaction, pouring the reaction liquid into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mL LPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring for 10 minutes at the rotating speed of 300rpm, uniformly mixing, adding 4.5mL ammonia water and 27mL deionized water into a reaction bottle, continuously stirring for 15 minutes, dropwise adding 1500 mu l vinyltriethoxysilane into the reaction bottle, and reacting for about 3 hours at the rotating speed of 200 rpm. Then, after the reaction solution was centrifuged at 6500rpm for 15 minutes, the supernatant in the centrifuge tube was poured off,adding 30mL of deionized water, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the mixture into a centrifuge, centrifuging the mixture for 15 minutes at the rotating speed of 6500rpm, pouring out the supernatant, cleaning the mixture for 3 times by using the deionized water in the manner, adding 30mL of absolute ethyl alcohol into a centrifuge tube, putting the centrifuge tube into the 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, putting the centrifuge tube into the centrifuge, centrifuging the mixture for 10 minutes at the rotating speed of 6000rpm, pouring out the supernatant in the centrifuge tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly wash the mixture for three times by using the absolute ethyl alcohol, and then washing the cleaned PS @ SiO @ film by using the absolute ethyl alcohol2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with the weight-average molecular weight of 2000g/mol in a vacuum drying oven at 100 ℃ for vacuumizing for 3 hours, taking 4g of dried polycarbonate diol and 0.0245g of glycerol, placing the mixture in a 20mL sample bottle, stirring the mixture for 15 minutes at the temperature of 50 ℃ and the rotating speed of 700rpm, adding 680 mu l of 4,4' -dicyclohexylmethane diisocyanate after uniformly mixing, continuing stirring the mixture for 20 minutes at the reaction temperature of 60 ℃, reducing the temperature to 50 ℃, adding 1 wt% of dibutyltin dilaurate after uniformly mixing, stirring the mixture for 3 minutes at the rotating speed of 1000rpm, and injecting the mixture into the assembled PS @ SiO2And (3) putting the opal photonic crystal template into a glass plate, leveling the opal photonic crystal template, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the orange polycarbonate diol-based structural color elastomer.
Example 5
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.068g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at 200rpm for 10 minutes at the temperature of 80 ℃ oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of sodium dodecyl sulfate, and addingAnd (3) continuing stirring the potassium sulfate initiator for reaction for 6 hours, stopping the reaction, pouring the reaction liquid into a standby beaker, carrying out ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mL LPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring for 10 minutes at the rotating speed of 300rpm, uniformly mixing, adding 4.5mL ammonia water and 27mL deionized water into a reaction bottle, continuously stirring for 15 minutes, dropwise adding 1500 mu l vinyltriethoxysilane into the reaction bottle, and reacting for about 3 hours at the rotating speed of 200 rpm. Then centrifuging the reaction solution at 6500rpm for 15 minutes, pouring out the supernatant in a centrifuge tube, adding 30mL of deionized water, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the mixture into a centrifuge for centrifugal treatment at 6500rpm for 15 minutes, pouring out the supernatant, cleaning the mixture for 3 times by using deionized water in the above manner, adding 30mL of absolute ethyl alcohol into the centrifuge tube, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, then putting the mixture into the centrifuge for centrifugal treatment at 6000rpm for 10 minutes, pouring out the supernatant in the centrifuge tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly wash the mixture for three times by using absolute ethyl alcohol, and then washing the cleaned PS @ SiO by using absolute ethyl alcohol again2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with weight average molecular weight of 2000g/mol in a vacuum drying oven at 100 ℃ for vacuumizing for 3 hours, taking 4g of dried polycarbonate diol and 0.0245g of glycerol, placing the mixture in a 20mL sample bottle, stirring the mixture for 15 minutes at 50 ℃ and 700rpm, adding 680 mu l of 4,4' -dicyclohexylmethane diisocyanate after uniform mixing, continuing stirring the mixture for 20 minutes at 60 ℃ reaction temperature, reducing the temperature to 50 ℃, adding 1 wt% of dibutyltin dilaurate after uniform mixing, stirring the mixture for 3 minutes at 1000rpm, injecting the mixture into the assembled PS @ SiO2The opal photonic crystal template is scraped by a glass plate and put into a drying oven, and the drying oven is vacuumized for 1 hour at room temperatureAfter this time, the reaction was carried out in an oven at 80 ℃ for 4 hours to obtain a red structural color elastomer based on polycarbonate diol.
Example 6
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.075g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10min at the temperature of 80 ℃ in an oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15min, adding 0.15g of potassium persulfate initiator, continuously stirring for reaction for 6h, stopping the reaction, pouring the reaction solution into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 h, and sealing for standby. Taking the prepared 3mLPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring at the rotating speed of 300rpm for 10 minutes, uniformly mixing, adding 4.5mL ammonia water and 27mL deionized water into a reaction bottle, continuously stirring for 15 minutes, dropwise adding 1500 mu l vinyltriethoxysilane into the reaction bottle, and reacting at the rotating speed of 200rpm for about 3 hours. Then centrifuging the reaction solution at 6500rpm for 15 minutes, pouring out the supernatant in a centrifuge tube, adding 30mL of deionized water, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the mixture into a centrifuge for centrifugal treatment at 6500rpm for 15 minutes, pouring out the supernatant, cleaning the mixture for 3 times by using deionized water in the above manner, adding 30mL of absolute ethyl alcohol into the centrifuge tube, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, then putting the mixture into the centrifuge for centrifugal treatment at 6000rpm for 10 minutes, pouring out the supernatant in the centrifuge tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly wash the mixture for three times by using absolute ethyl alcohol, and then washing the cleaned PS @ SiO by using absolute ethyl alcohol again2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Mixing a polycarbonate with a weight average molecular weight of 2000g/molPlacing diol in a vacuum drying oven at 100 deg.C, vacuumizing for 3 hr, placing 4g dried polycarbonate diol and 0.0245g glycerol in a 20mL sample bottle, stirring at 700rpm for 15min at 50 deg.C, adding 680 μ l 4,4' -dicyclohexylmethane diisocyanate, stirring at 60 deg.C for 20 min, cooling to 50 deg.C, mixing, adding 1 wt% dibutyltin dilaurate, stirring at 1000rpm for 3 min, and injecting into the above assembled PS @ SiO2And (3) scraping the opal photonic crystal template by using a glass plate, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the red structural color elastomer based on the polycarbonate diol.
Example 7
The embodiment discloses a preparation method of a structural color elastomer based on polycarbonate diol, which comprises the following specific steps:
adding 0.072g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10 minutes at the temperature of 80 ℃ oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of potassium persulfate initiator, continuously stirring for reacting for 6 hours, stopping the reaction, pouring the reaction solution into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mL LPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring for 10 minutes at the rotating speed of 300rpm, uniformly mixing, adding 5mL ammonia water and 27mL deionized water into a reaction bottle, continuously stirring for 15 minutes, dropwise adding 1000 mu l vinyltriethoxysilane into the reaction bottle, and reacting for about 3 hours at the rotating speed of 200 rpm. Then centrifuging the reaction solution at 6500rpm for 15 minutes, pouring out the supernatant in a centrifuge tube, adding 30mL of deionized water, placing the centrifuge tube into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, placing the centrifuge tube into a centrifuge for centrifuging at 6500rpm for 15 minutes, then pouring out the supernatant, cleaning the centrifuge tube with deionized water for 3 times in the above manner, adding 30mL of anhydrous ethanol into the centrifuge tube, and then adding the anhydrous ethanol into the centrifuge tubePutting the PS @ SiO solid into a 180W ultrasonic cleaner for 30 minutes, putting the PS @ SiO solid into a centrifugal machine, centrifuging the PS @ SiO solid for 10 minutes at 6000rpm, pouring out supernate in a centrifugal tube, continuously adding 30ml of absolute ethyl alcohol, continuously and repeatedly washing the PS @ SiO solid with the absolute ethyl alcohol for three times, and then washing the PS @ SiO solid with the washed PS @ SiO solid2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with weight average molecular weight of 2000g/mol in a vacuum drying oven at 100 ℃ for vacuumizing for 3 hours, taking 4g of dried polycarbonate diol and 0.0245g of glycerol, placing the mixture in a 20mL sample bottle, stirring the mixture for 15 minutes at 50 ℃ and 700rpm, adding 680 mu l of 4,4' -dicyclohexylmethane diisocyanate after uniform mixing, continuing stirring the mixture for 20 minutes at 60 ℃ reaction temperature, reducing the temperature to 50 ℃, adding 1 wt% of dibutyltin dilaurate after uniform mixing, stirring the mixture for 3 minutes at 1000rpm, injecting the mixture into the assembled PS @ SiO2And (3) putting the opal photonic crystal template into a glass plate, leveling the opal photonic crystal template, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the orange polycarbonate diol-based structural color elastomer.
Example 8
The embodiment discloses a preparation method of a porous colored carbon fiber material, which comprises the following specific steps:
adding 0.072g of sodium dodecyl sulfate into a 250mL three-neck flask, adding 135mL of deionized water, mechanically stirring at the rotation speed of 200rpm for 10 minutes at the temperature of 80 ℃ oil bath, uniformly mixing, adding 15g of styrene, performing nitrogen protection in the whole process, continuously mechanically stirring for 15 minutes, adding 0.15g of potassium persulfate initiator, continuously stirring for reacting for 6 hours, stopping the reaction, pouring the reaction solution into a standby beaker, performing ultrasonic treatment in a 180W ultrasonic cleaner for 2 hours, and sealing for standby. Taking the prepared 3mLPS stock solution into a 100mL three-neck flask, adding 57mL deionized water into the flask, stirring at the rotating speed of 300rpm for 10 minutes, and mixingAfter the mixture was homogeneous, 4.5mL of ammonia and 27mL of deionized water were added to the flask and stirring was continued for 15 minutes, and 1500. mu.l of vinyltriethoxysilane was added dropwise to the flask and allowed to react at 200rpm for 4 hours. Then centrifuging the reaction solution at 6500rpm for 15 minutes, pouring out the supernatant in a centrifuge tube, adding 30mL of deionized water, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 20 minutes, putting the mixture into a centrifuge for centrifugal treatment at 6500rpm for 15 minutes, pouring out the supernatant, cleaning the mixture for 3 times by using deionized water in the above manner, adding 30mL of absolute ethyl alcohol into the centrifuge tube, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, then putting the mixture into the centrifuge for centrifugal treatment at 6000rpm for 10 minutes, pouring out the supernatant in the centrifuge tube, continuing adding 30mL of absolute ethyl alcohol, continuing to repeatedly wash the mixture for three times by using absolute ethyl alcohol, and then washing the cleaned PS @ SiO by using absolute ethyl alcohol again2Adding 30mL of absolute ethyl alcohol, putting the mixture into a 180W ultrasonic cleaner for ultrasonic treatment for 30 minutes, and then adding PS @ SiO2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and completely volatilizing the solvent on a heating plate at 45 ℃ to form the opal photonic crystal template with bright color.
Placing polycarbonate diol with the weight-average molecular weight of 2000g/mol in a vacuum drying oven at 100 ℃ for vacuumizing for 3 hours, taking 4g of dried polycarbonate diol and 0.0245g of glycerol, placing the mixture in a 20mL sample bottle, stirring the mixture for 15 minutes at the temperature of 50 ℃ and the rotating speed of 700rpm, adding 680 mu l of 4,4' -dicyclohexylmethane diisocyanate after uniformly mixing, continuing stirring the mixture for 20 minutes at the reaction temperature of 60 ℃, reducing the temperature to 50 ℃, adding 1 wt% of dibutyltin dilaurate after uniformly mixing, stirring the mixture for 3 minutes at the rotating speed of 1000rpm, and injecting the mixture into the assembled PS @ SiO2And (3) scraping the opal photonic crystal template by using a glass plate, putting the opal photonic crystal template into a drying oven, vacuumizing the opal photonic crystal template for 1 hour at room temperature, and then putting the opal photonic crystal template into an oven at 80 ℃ for reaction for 4 hours to obtain the red structural color elastomer based on the polycarbonate diol.
Claims (10)
1. A structural color elastomer based on polycarbonate diol characterized by: the polycarbonate-based diolThe structural color elastomer is formed by compounding a polycarbonate diol-based elastomer and opal photonic crystals; the polycarbonate diol elastomer is obtained by bulk polymerization of polycarbonate diol, glycerol and 4,4' -dicyclohexylmethane diisocyanate under the action of a catalyst dibutyltin dilaurate; the opal photonic crystal is formed by PS @ SiO2Self-assembling the microsphere particles; the PS @ SiO2The microsphere particles are prepared by polymerizing styrene through emulsion to obtain polystyrene microsphere particles, and then coating the polystyrene microsphere particles with vinyltriethoxysilane.
2. The structural color elastomer based on polycarbonate diol according to claim 1, characterized in that: the particle size of the polystyrene microsphere particles is 438.6-497.8 nm.
3. The method for preparing a structural color elastomer based on polycarbonate diol according to claim 1 or 2, characterized by comprising the steps of:
(1) dispersing styrene in deionized water under the emulsification action of sodium dodecyl sulfate, adding an initiator, and carrying out emulsion polymerization to obtain a polystyrene microsphere stock solution;
(2) dispersing the polystyrene microsphere stock solution prepared in the step (1) in deionized water, adding vinyltriethoxysilane under the action of ammonia water to coat polystyrene microsphere particles, centrifuging the reaction solution, and then carrying out PS @ SiO preparation2Washing, and then ultrasonically dispersing in absolute ethyl alcohol to obtain PS @ SiO2A microsphere dispersion;
(3) the PS @ SiO in the step (2) is treated2Spreading the microsphere dispersion liquid on a polytetrafluoroethylene template, and carrying out self-assembly on a heating plate to obtain an opal photonic crystal template;
(4) uniformly mixing polycarbonate diol, glycerol, 4' -dicyclohexylmethane diisocyanate and dibutyltin dilaurate to prepare an elastomer precursor solution;
(5) and (3) injecting the elastomer precursor liquid in the step (4) into the opal photonic crystal template assembled in the step (3), removing bubbles, and then heating and curing to obtain the polycarbonate diol-based structural color elastomer.
4. The method for producing a structural color elastomer based on polycarbonate diol according to claim 3, characterized in that: the initiator in the step (1) is potassium persulfate or ammonium persulfate, and the mass ratio of the sodium dodecyl sulfate to the styrene is 0.0043-0.0053: 1, the mass ratio of the initiator to the styrene is 0.0067-0.01: 1, the mass ratio of the deionized water to the styrene is 9-10: 1, the reaction temperature of the emulsion polymerization is 80-90 ℃, and the reaction time is 4-6 hours.
5. The method for producing a structural color elastomer based on polycarbonate diol according to claim 3, characterized in that: the volume ratio of the deionized water to the polystyrene microsphere stock solution in the step (2) is 28-30: 1, the volume ratio of the ammonia water to the polystyrene microsphere stock solution is 1.5-1.67: 1, the volume ratio of the vinyltriethoxysilane to the polystyrene microsphere stock solution is 0.33-0.5: 1, the reaction temperature in the coating process is 20-30 ℃, the reaction time is 2-4 hours, and the PS @ SiO2The mass concentration in the absolute ethyl alcohol is 1 to 5 percent.
6. The method for producing a structural color elastomer based on polycarbonate diol according to claim 3, characterized in that: the temperature of the photonic crystal self-assembly in the step (3) is 40-60 ℃.
7. The method for producing a structural color elastomer based on polycarbonate diol according to claim 3, characterized in that: the hydroxyl molar ratio of the polycarbonate diol to the glycerol in the step (4) is 0.1-0.33; the molar ratio of the sum of the hydroxyl molar amounts of the polycarbonate diol and the glycerol to the isocyanate of the 4,4 '-dicyclohexylmethane diisocyanate is 0.9-1.1, the ratio of the dibutyltin dilaurate to the total mass of the polycarbonate diol, the glycerol and the 4,4' -dicyclohexylmethane diisocyanate is 0.6-1%, and the temperature for preparing the elastomer precursor liquid is controlled at 45-60 ℃.
8. The method for producing a structural color elastomer based on polycarbonate diol according to claim 3, characterized in that: the weight average molecular weight of the polycarbonate diol in the step (4) is 1000g/mol to 3000 g/mol.
9. The method for producing a structural color elastomer based on polycarbonate diol according to claim 3, characterized in that: and (5) vacuumizing the photonic crystal injected with the elastic precursor liquid to remove bubbles, wherein the temperature of the photonic crystal injected with the elastic precursor liquid is 60-80 ℃ and the time is 2-6 hours when the photonic crystal is heated and cured.
10. Use of the polycarbonate diol-based structural color elastomer of claim 1 or 2 in visual sensing and smart wearable devices.
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