CN116376313A - Preparation method and application of responsive structural color liquid drop - Google Patents
Preparation method and application of responsive structural color liquid drop Download PDFInfo
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- CN116376313A CN116376313A CN202310306447.0A CN202310306447A CN116376313A CN 116376313 A CN116376313 A CN 116376313A CN 202310306447 A CN202310306447 A CN 202310306447A CN 116376313 A CN116376313 A CN 116376313A
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- 238000002360 preparation method Methods 0.000 title abstract description 13
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- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 32
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- GTELLNMUWNJXMQ-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical class OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.CCC(CO)(CO)CO GTELLNMUWNJXMQ-UHFFFAOYSA-N 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 14
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 claims description 11
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- CDXFIRXEAJABAZ-UHFFFAOYSA-N 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F CDXFIRXEAJABAZ-UHFFFAOYSA-N 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 5
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 5
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 5
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000136 polysorbate Polymers 0.000 claims description 5
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- 238000004519 manufacturing process Methods 0.000 claims description 4
- LCPUCXXYIYXLJY-UHFFFAOYSA-N 1,1,2,4,4,4-hexafluorobutyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(F)(F)C(F)CC(F)(F)F LCPUCXXYIYXLJY-UHFFFAOYSA-N 0.000 claims description 3
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
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- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 3
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 3
- BNWCETAHAJSBFG-UHFFFAOYSA-N tert-butyl 2-bromoacetate Chemical compound CC(C)(C)OC(=O)CBr BNWCETAHAJSBFG-UHFFFAOYSA-N 0.000 claims description 3
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/006—Preparation of organic pigments
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0084—Dispersions of dyes
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Abstract
The invention belongs to the field of responsive structural color materials, and discloses a preparation method and application of responsive structural color liquid drops, wherein the preparation method specifically comprises the following steps: (1) Preparing a first surfactant solution and a second surfactant solution; (2) Preparing liquid hydrocarbon and liquid fluorocarbon as oil phase substances; (3) Uniformly mixing the first surfactant solution, the second surfactant solution, hydrocarbon and fluorocarbon to form an oil-in-water system, wherein the formed liquid drops are responsive structural color liquid drops; the mass ratio of the first surfactant to the second surfactant in the system is changed, so that the structural color of the liquid drop can appear or disappear, and the response of the structural color to the surfactant is realized. The structural color liquid drop can regulate and control the appearance of the liquid drop through the competitive action of the two surfactants, so that the display and disappearance of the structural color are controlled, the responsiveness is realized, and the method is very suitable for anti-counterfeiting.
Description
Technical Field
The invention belongs to the field of responsive structural color materials, and particularly relates to a preparation method and application of responsive structural color liquid drops, which have the characteristic of surfactant response.
Background
The responsive structural color material is a material capable of changing color under external stimulus such as temperature, humidity, electric field, magnetic field, etc. The device can feed back external stimulus in real time, and convert the external stimulus which is difficult to observe into an optical signal visible to naked eyes. Therefore, the responsive structural color material has great potential in the fields of intelligent display, anti-counterfeiting, information encryption, biological detection and the like.
However, the present responsive structural color materials are mainly focused on the responsive photonic crystal structural color materials, and most of the present photonic crystal material preparation still adopts a "top-down" strategy, such as photolithography and layer-by-layer deposition technology, to prepare the large-size material into the desired micro-nano structure. Although a plurality of high-quality micro-nano structures can be prepared by adopting a top-down strategy, the method has the defects of high cost, material waste, low time efficiency, limited structure size and the like, and the application of the method in the field of high-flux application is hindered. Therefore, developing new structural color materials, reducing the preparation period and cost thereof has important significance for further expanding the application of the structural color materials.
Disclosure of Invention
In view of the above-mentioned drawbacks or improvements of the prior art, an object of the present invention is to provide a method for preparing a responsive structural color droplet and an application thereof, wherein the structural color droplet is obtained by modifying and controlling the structure and composition of the droplet, using two different surfactants, and using the combination of the first surfactant, the second surfactant, the hydrocarbon and the fluorocarbon. The structural color liquid drop can regulate and control the appearance of the liquid drop through the competitive action of two surfactants, so that the display and disappearance of the structural color are controlled, and the responsiveness is realized. The size and the color of the structural color liquid drop obtained by the invention have randomness, can avoid being copied or imitated, and is very suitable for anti-counterfeiting. In addition, the preparation process is simple, and the raw materials are cheap and can be prepared in batches. In addition, the structural color has the advantages of fading resistance, environmental protection, high saturation and the like, and is similar to other structural colors.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for producing a droplet of a responsive structural color, comprising the steps of:
(1) Dissolving a first surfactant in deionized water to obtain a first surfactant solution; dissolving a second surfactant in deionized water to obtain a second surfactant solution; the first surfactant solution and the second surfactant solution correspond to aqueous solutions of continuous phases of responsive structural color droplets; wherein the first surfactant is one of FC-4430, FC301, capstone FS-30, capstone 62MA, ZY-FC327, ZY-823, ZONLY FS300, TF282 and TF 328; the second surfactant is one of SDS, PVA, CTAB, F-108, F-127, TWEEN20, TWEEN 40, TWEEN 60 and TWEEN 80;
(2) Preparing liquid hydrocarbon and liquid fluorocarbon as oil phase substances; wherein the hydrocarbon has a density less than the fluorocarbon, a refractive index greater than the fluorocarbon, and the hydrocarbon and the fluorocarbon are immiscible at room temperature; an oil phase material of the hydrocarbon and the fluorocarbon corresponding to the dispersed phase of the responsive structural color droplets;
(3) Uniformly mixing the first surfactant solution, the second surfactant solution, the hydrocarbon and the fluorocarbon to form an oil-in-water system, wherein the formed liquid drops are responsive structural color liquid drops; according to the mass ratio of the first surfactant to the second surfactant in the system, the liquid drops can have structural colors or not;
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system is 1:1-1:5, the liquid drops are Janus liquid drops and have structural colors;
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system is not 1:1-1:5, the liquid drops do not have structural color.
As a further preferred aspect of the present invention, the method further comprises the step (4):
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system is 1:1-1:5, adding the first surfactant solution and/or the second surfactant solution into the oil-in-water system again to enable the mass ratio of the first surfactant to the second surfactant in the system to deviate from 1:1-1:5, and obtaining liquid drops with disappeared structural color by utilizing diffusion;
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system does not meet 1:1-1:5, the first surfactant solution and/or the second surfactant solution are added into the oil-in-water system again, so that the mass ratio of the first surfactant to the second surfactant in the system meets 1:1-1:5 again, and the liquid drops with the structural color reproduction can be obtained by utilizing the diffusion effect.
As a further preferred aspect of the present invention, in the step (1), the concentration of the first surfactant solution is 1 to 50mg/mL, and the concentration of the second surfactant solution is 1 to 50mg/mL.
As a further preferred aspect of the present invention, in the step (2), the hydrocarbon is one of octadecyl methacrylate, ethoxylated trimethylolpropane triacrylate, ethylene glycol dimethacrylate, t-butyl bromoacetate, n-butyl acrylate, and dodecyl acrylate;
the fluorocarbon is 1H, 2H-heptadecafluorodecyl acrylate 1, 3-hexafluoroisopropyl methacrylate 2, 2-trifluoroethyl methacrylate one of hexafluorobutyl methacrylate, 2,3, 4-hexafluorobutyl acrylate and trifluoroethyl methacrylate;
in the step (3), the volume ratio of the hydrocarbon to the fluorocarbon is 1:1-1:8.
As a further preferred aspect of the present invention, in the step (3), the mixing is performed in a vortex oscillator at a shaking speed of 300 to 2000rpm for a shaking time of 0.5 to 5 minutes;
the diameter of the responsive structural color drop is 20-200 mu m.
According to another aspect of the invention, the invention provides a responsive structural color drop obtained by the preparation method.
According to a further aspect of the invention, the invention provides the use of a responsive structural colour droplet as described above in the anti-counterfeiting of a liquid.
As a further preferred aspect of the present invention, specifically, the first surfactant solution and/or the second surfactant solution is added again to the oil-in-water system, so that the mass ratio of the first surfactant to the second surfactant in the system deviates from or satisfies 1:1 to 1:5, and the disappearance and reproduction of the structural color are controlled by using diffusion.
According to the technical scheme, compared with the prior art, the liquid drop with the responsive structural color is obtained by using two different surfactants and utilizing the cooperation of the first surfactant, the second surfactant, the hydrocarbon and the fluorocarbon.
The invention can accurately regulate and control the structural color by regulating and controlling the morphology of the liquid drops, thereby realizing responsiveness. The invention uses surfactants such as FC-4430, FC301, capstone FS-30, capstone 62MA, ZY-FC327, ZY-823, ZONLY FS300, TF282 and TF328 as first surfactants, and the first surfactants can preferentially reduce the interfacial tension between fluorocarbon and water; the use of surfactants SDS, PVA, CTAB, F-108, F-127, TWEEN20, TWEEN 40, TWEEN 60, TWEEN 80 as the second surfactant preferentially reduces the interfacial tension between hydrocarbons and water. By controlling the mass ratio of the first surfactant to the second surfactant in the system, the morphology of the liquid drops can be changed by utilizing the competing action of the first surfactant and the second surfactant, and the response of structural color to the surfactants can be realized. Specifically, when the mass ratio of the first surfactant to the second surfactant in the system is 1:1-1:5, the liquid drops are Janus liquid drops and have structural colors; when the mass ratio of the first surfactant to the second surfactant in the system does not meet 1:1-1:5, the system does not have structural color; thus, the mass ratio of the first surfactant to the second surfactant in the system is controlled, so that the structural color of the liquid drop can appear or disappear, and the response is realized.
The liquid drop consists of hydrocarbon and fluorocarbon which are mutually insoluble, and when the appearance of the liquid drop is Janus liquid drop, the characteristic that the density of the hydrocarbon is smaller than that of the fluorocarbon but the refractive index is larger than that of the fluorocarbon is utilized, so that the liquid drop can generate structural color based on the combination of total internal reflection and an interference mechanism.
After the oil-in-water system is formed by uniform mixing, the first surfactant solution and/or the second surfactant solution can be added into the system again through simple steps, the secondary oscillation is not needed, and the interface between the hydrocarbon and the fluorocarbon in the hydrocarbon-fluorocarbon liquid drop can be influenced by utilizing the diffusion action of the water phase, so that the form of the liquid drop is further changed, and the structural color of the liquid drop is disappeared or reproduced. The structural color liquid drop with the surfactant response, which is obtained by the invention, has the structural color displayed and disappeared, and the circulation of the structural color displayed and disappeared can be realized by repeatedly changing the mass ratio of the two surfactants.
In particular, the invention can achieve the following beneficial effects:
(1) The preparation method of the structural color liquid drop provided by the invention is simple, is simple to operate, has low technical requirements, can conveniently prepare the structural color liquid drop with controllable micro-nano size, has cheap and easily available required raw materials, and is suitable for mass production.
(2) The structural color liquid drops obtained by the invention can realize the display and disappearance of the structural color by adjusting the mass ratio of the two used surfactants, and the liquid drops display the structural color when the mass ratio is 1:1-1:5; and when the mass ratio is outside 1:1-1:5, the structural color disappears, and the anti-counterfeiting method is suitable for the fields of anti-counterfeiting and the like.
(3) The structural color liquid drop prepared by the method has the characteristic of physical unclonable property, and is very suitable for anti-counterfeiting. Taking the oil-in-water system formed by oscillation treatment as an example, the overall condition of the liquid drop obtained by slightly changing the condition during oscillation will change, and the physical unclonable characteristic is provided.
Drawings
Fig. 1 is a reflection mode optical microscope photograph of structural color droplets having different sizes prepared by a vortex mixing method in example 1 and a reflection mode optical microscope photograph of different cases obtained by circularly adding the surfactant 1 and the surfactant 2.
Fig. 2 is a reflection mode optical microscope photograph of droplets having different sizes prepared by the vortex mixing method of example 2 and a reflection mode optical microscope photograph of different cases obtained by circularly adding the surfactant 1 and the surfactant 2.
Fig. 3 is a reflection mode optical microscope photograph of structural color droplets having different sizes prepared by the vortex mixing method of example 3 and a reflection mode optical microscope photograph of different cases obtained by circularly adding the surfactant 1 and the surfactant 2.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Based on the invention, the preparation method of the structural color liquid drop with the surfactant response can be carried out according to the following steps:
(1) Preparing surfactant solution with a certain concentration:
preparing surfactant solution with a certain concentration: respectively dissolving different surfactants (namely surfactant 1 and surfactant 2; the difference between the surfactant 1 and the surfactant 2 is that the surfactant 1 can preferentially reduce the interfacial tension between fluorocarbon and water, and the surfactant 2 can preferentially reduce the interfacial tension between hydrocarbon and water) in a certain volume of deionized water to obtain a continuous phase aqueous solution of the responsive structural color liquid drops, and naming the continuous phase aqueous solution as a surfactant 1 solution and a surfactant 2 solution; the surfactant 1 can be one of FC-4430, FC301, capstone FS-30, capstone 62MA, ZY-FC327, ZY-823, ZONLY FS300, TF282 and TF328, and the concentration of the surfactant 1 can be 1-50mg/mL; surfactant 2 may be one of SDS, PVA, CTAB, F-108, F-127, TWEEN20, TWEEN 40, TWEEN 60, TWEEN 80, and the concentration of surfactant 2 may be 1-50mg/mL.
(2) The hydrocarbon and the fluorocarbon are added into a centrifuge tube according to a certain volume ratio. The hydrocarbon can be one of octadecyl methacrylate, ethoxylated trimethylolpropane triacrylate, ethylene glycol dimethacrylate, tert-butyl bromoacetate, n-butyl acrylate and dodecyl acrylate;
the fluorocarbon may be 1H, 2H-heptadecafluorodecyl acrylate 1, 3-hexafluoroisopropyl methacrylate 2, 2-trifluoroethyl methacrylate, hexafluorobutyl methacrylate, 2,3, 4-hexafluorobutyl acrylate, trifluoroethyl methacrylate. The volume ratio of hydrocarbon to fluorocarbon may be 1:1 to 1:8.
(3) And placing a centrifuge tube filled with hydrocarbon and fluorocarbon in a certain volume ratio in a vortex oscillator, and setting the oscillation speed so that the hydrocarbon and the fluorocarbon can be fully and uniformly mixed to obtain an oil phase substance of a disperse phase of the responsive structural color liquid drops. The oscillating speed can be 300-2000rpm, and the oscillating time can be 0.5-5min.
(4) After the hydrocarbon and the fluorocarbon can be fully and uniformly mixed, adding the surfactant 1 and the surfactant 2 with a certain mass ratio into the solution, and oscillating again through a vortex oscillator to prepare the structural color liquid drops. And (3) dripping the prepared structural color liquid drop solution system on a surface dish, and observing the relation between the color and the size under a reflection mode optical microscope. The volume ratio of the oil phase material to the surfactant solution may be 1:1 to 1:20. The mass ratio of the solute surfactant 1 to the surfactant 2 may be 1:1 to 1:5, and the obtained liquid droplets will show structural color at this time (of course, if the mass ratio of the solute surfactant 1 to the surfactant 2 deviates from 1:1 to 1:5, the obtained liquid droplets do not have structural color, and the structural color can be recovered by adjusting the mass ratio of the solute surfactant 1 to the surfactant 2 in the following steps). The diameter of the structural color liquid drop is 20-200 mu m.
The preparation process is that the oil phase substances are mixed in the step (3) and the step (4) respectively to form an oil-in-water system, and besides the step mixing, the two surfactant aqueous solutions and the two oil phase substances can be added into the same centrifuge tube at one time, so that the oil-in-water system which is uniformly mixed can be obtained through one-time oscillation treatment. In addition, besides the mixing realized by adopting the oscillation of a vortex oscillator, other mixing modes such as hand shaking, ultrasonic mixing, cell pulverizer treatment and the like can be adopted.
Further, in order to detect the responsiveness of the droplet, the following steps may be performed:
s1: a certain amount of surfactant 2 was added again to the droplet solution system in which the structural color had been generated, and the morphology of the droplets and the change in color were observed by a reflection-mode optical microscope. The mass of the surfactant 2 added again needs to be such that the mass ratio of the solute surfactant 1 to the surfactant 2 of the whole system is out of the range of 1:1 to 1:5.
S2: and (3) adding a certain amount of surfactant 1 into the liquid drop solution system obtained in the step (S1), and observing the shape and color change of the liquid drops through a reflection mode optical microscope. The mass of the re-added surfactant 1 needs to be such that the mass ratio of the solute surfactant 1 to the surfactant 2 of the whole system satisfies the range of 1:1 to 1:5.
S3: and (3) sequentially repeating the steps S1 and S2, and observing the shape and the color change of the liquid drop by using a reflection mode optical microscope. The number of repeated cycles can reach more than 8.
Of course, besides adding the surfactant 2 and then adding the surfactant 1 to the system in the step S1 and the step S2, the mass ratio of the solute surfactant 1 to the surfactant 2 may deviate from 1:1 to 1:5 by adding the surfactant 1 and then adding the surfactant 2 to restore the mass ratio of the solute surfactant 1 to the surfactant 2 to 1:1 to 1:5.
The following are specific examples:
example 1
The structural color droplets in this example were prepared as follows:
(1) Preparing surfactant solution with a certain concentration:
dissolving a certain mass of Capstone FS-30 in a certain volume of deionized water to obtain a Capstone FS-30 aqueous solution (i.e. surfactant 1 solution) with a concentration of 15mg/mL; dissolving a mass of SDS in a volume of deionized water to obtain an aqueous SDS solution (i.e., surfactant 2 solution) with a concentration of 10mg/mL; the surfactant 1 solution and the surfactant 2 solution can be used as aqueous solutions of the continuous phase of the structural color droplets.
(2) Adding ethoxylated trimethylolpropane triacrylate and 1H, 2H-heptadecafluorodecyl acrylate into a centrifuge tube according to a certain volume ratio, wherein the volume ratio of the ethoxylated trimethylolpropane triacrylate to the 1H, 2H-heptadecafluorodecyl acrylate is 1:1.
(3) A centrifuge tube containing ethoxylated trimethylolpropane triacrylate and 1h,2 h-heptadecafluorodecyl acrylate in a volume ratio of 1:1 was placed in a vortex shaker at a shaking speed of 500rpm for 1min to allow the ethoxylated trimethylolpropane triacrylate and the 1h,2 h-heptadecafluorodecyl acrylate to be thoroughly and uniformly mixed to give an oil phase material of a dispersed phase of structural color droplets.
(4) After ethoxylated trimethylolpropane triacrylate and acrylic acid 1H, 2H-heptadecafluorodecyl ester can be fully and uniformly mixed, a Capstone FS-30 aqueous solution and an SDS aqueous solution with a certain mass ratio are added into the solution, and the structural color liquid drops are prepared by oscillating through a vortex oscillator. And (3) dripping the prepared structural color liquid drop solution system on a surface dish, and observing the relation between the color and the size under a reflection mode optical microscope. The volume ratio of the oil phase substance to the surfactant solution is 1:5 (wherein the volume of the surfactant solution is the volume algebraic sum of the surfactant 1 solution and the surfactant 2 solution used in the step), the mass ratio of solute Capstone FS-30 to SDS is 1:2, and the diameter of the structural color liquid drop is 40-150 mu m.
(5) A further amount of Capstone FS-30 aqueous solution was added to the droplet solution system that had generated the structural color, and the morphology of the droplets and the color change were observed by reflection mode optical microscopy. The mass of the added Capstone FS-30 is required to enable the mass ratio of the solute Capstone FS-30 to SDS of the whole system to be 2:1.
(6) And (3) adding a certain amount of SDS aqueous solution into the liquid drop solution system obtained in the step (5), and observing the shape and color change of the liquid drops through a reflection mode optical microscope. The mass of the added SDS again needs to be such that the mass ratio of solute Capstone FS-30 to SDS of the whole system is 1:2.
(7) And (5) repeating the steps (5) and (6) in sequence, and observing the shape and the color change of the liquid drop by a reflection mode optical microscope. The number of repeated cycles is more than 8.
As shown in fig. 1, fig. 1 (a) is an optical microscope image of the structural color obtained in the step (4), wherein the mass ratio of solute Capstone FS-30 to SDS is 1:2; in FIG. 1, (b) is an optical microscope image of the entire system after a certain amount of aqueous solution of Capstone FS-30 was added in step (5) (the mass of Capstone FS-30 added again at this time is such that the mass ratio of Capstone FS-30 to SDS was 2:1), it can be seen that the structural color had disappeared. In FIG. 1, (c) is an optical microscope image of the SDS aqueous solution added in the step (6) (at this time, the mass of SDS added again makes the mass ratio of solute Capstone FS-30 to SDS of the whole system 1:2), and the structural color is seen to be reproduced again, and the cycle is repeated. The cycle times can reach more than 8 times.
Example 2
The structural color droplets in this example were prepared as follows:
(1) Preparing surfactant solution with a certain concentration:
dissolving a certain mass of Capstone FS-30 in a certain volume of deionized water to obtain a Capstone FS-30 aqueous solution (i.e. surfactant 1 solution) with a concentration of 10mg/mL; dissolving a mass of SDS in a volume of deionized water to obtain an aqueous SDS solution (i.e., surfactant 2 solution) having a concentration of 20mg/mL; the surfactant 1 solution and the surfactant 2 solution can be used as aqueous solutions of the continuous phase of the structural color droplets.
(2) Adding ethoxylated trimethylolpropane triacrylate and 1H, 2H-heptadecafluorodecyl acrylate into a centrifuge tube according to a certain volume ratio, wherein the volume ratio of the ethoxylated trimethylolpropane triacrylate to the 1H, 2H-heptadecafluorodecyl acrylate is 1:2.
(3) A centrifuge tube containing ethoxylated trimethylolpropane triacrylate and 1h,2 h-heptadecafluorodecyl acrylate in a volume ratio of 1:2 was placed in a vortex shaker at a shaking speed of 600rpm for 1min to allow the ethoxylated trimethylolpropane triacrylate and the 1h,2 h-heptadecafluorodecyl acrylate to be thoroughly and uniformly mixed to give an oil phase material of a dispersed phase of structural color droplets.
(4) After ethoxylated trimethylolpropane triacrylate and acrylic acid 1H, 2H-heptadecafluorodecyl ester can be fully and uniformly mixed, a Capstone FS-30 aqueous solution and an SDS aqueous solution with a certain mass ratio are added into the solution, and the solution is oscillated by a vortex oscillator to prepare liquid drops. And (3) dripping the prepared liquid drop solution system on a surface dish, and observing under a reflection mode optical microscope. The volume ratio of the oil phase substance to the surfactant solution is 1:4 (wherein the volume of the surfactant solution is the volume algebraic sum of the surfactant 1 solution and the surfactant 2 solution used in the step), the mass ratio of solute Capstone FS-30 to SDS is 3:1, and the diameter of the liquid drop is 50-100 mu m.
(5) And adding a certain amount of SDS aqueous solution into the droplet solution system again, and observing the morphology and the color change of the droplets by a reflection mode optical microscope. The mass of the added SDS again needs to be such that the mass ratio of solute Capstone FS-30 to SDS of the whole system is 1:3.
(6) And (3) adding a certain amount of Capstone FS-30 aqueous solution into the liquid drop solution system obtained in the step (5), and observing the shape and color change of the liquid drops through a reflection mode optical microscope. The quality of the added Capstone FS-30 is required to ensure that the mass ratio of the solute Capstone FS-30 to SDS of the whole system is 3:1.
(7) And (5) repeating the steps (5) and (6) in sequence, and observing the shape and the color change of the liquid drop by a reflection mode optical microscope. The number of repeated cycles is more than 10.
As shown in fig. 2, fig. 2 (a) is an optical microscope image of the droplet without structural color, which is obtained in the step (4), wherein the mass ratio of solute capsule FS-30 to SDS is 3:1; in FIG. 2 (b) is an optical microscope image of the SDS aqueous solution added in the step (5) (at this time, the mass of SDS added again is required to make the mass ratio of solute Capstone FS-30 to SDS of the whole system 1:3), and it can be seen that the droplets generate structural color. In FIG. 2 (c) is an optical microscope image of the entire system after a certain amount of aqueous solution of Capstone FS-30 was added in step (6) (at this time, the mass of Capstone FS-30 added again requires a mass ratio of Capstone FS-30 to SDS of 3:1), and it can be seen that the structural color had disappeared again, and the cycle was repeated. The cycle times can reach more than 10 times.
Example 3
The structural color droplets in this example were prepared as follows:
(1) Preparing surfactant solution with a certain concentration:
dissolving a certain mass of Capstone FS-30 in a certain volume of deionized water to obtain a Capstone FS-30 aqueous solution (i.e. surfactant 1 solution) with a concentration of 20mg/mL; dissolving a certain mass of PVA in a certain volume of deionized water, wherein the concentration of the obtained PVA aqueous solution (namely surfactant 2 solution) is 15mg/mL; the surfactant 1 solution and the surfactant 2 solution can be used as aqueous solutions of the continuous phase of the structural color droplets.
(2) Adding ethoxylated trimethylolpropane triacrylate and 2, 2-trifluoroethyl methacrylate into a centrifuge tube according to a certain volume ratio, wherein the volume ratio of the ethoxylated trimethylolpropane triacrylate to the 2, 2-trifluoroethyl methacrylate is 1:1.
(3) A centrifuge tube filled with ethoxylated trimethylolpropane triacrylate and 2, 2-trifluoroethyl methacrylate in a volume ratio of 1:1 is placed in a vortex oscillator, the oscillation speed is set to be 500rpm, and the oscillation time is set to be 1min, so that the ethoxylated trimethylolpropane triacrylate and the 2, 2-trifluoroethyl methacrylate can be fully and uniformly mixed, and an oil phase substance of a disperse phase of structural color liquid drops is obtained.
(4) After ethoxylated trimethylolpropane triacrylate and 2, 2-trifluoroethyl methacrylate can be fully and uniformly mixed, a Capstone FS-30 aqueous solution and a PVA aqueous solution with a certain mass ratio are added into the solution, and the structural color liquid drops are prepared by oscillating through a vortex oscillator. And (3) dripping the prepared structural color liquid drop solution system on a surface dish, and observing the relation between the color and the size under a reflection mode optical microscope. The volume ratio of the oil phase substance to the surfactant solution is 1:5 (wherein the volume of the surfactant solution is the volume algebraic sum of the surfactant 1 solution and the surfactant 2 solution used in the step), the mass ratio of solute Capstone FS-30 to PVA is 2:3, and the diameter of the structural color liquid drop is 40-120 mu m.
(5) A further amount of Capstone FS-30 aqueous solution was added to the droplet solution system that had generated the structural color, and the morphology of the droplets and the color change were observed by reflection mode optical microscopy. The quality of the added Capstone FS-30 is required to enable the mass ratio of the solute Capstone FS-30 to PVA of the whole system to be 2:1.
(6) And (3) adding a certain amount of PVA aqueous solution into the liquid drop solution system obtained in the step (5) again, and observing the shape and color change of the liquid drops through a reflection mode optical microscope. The quality of the added PVA needs to be such that the mass ratio of solute Capstone FS-30 to PVA of the whole system is 2:3.
(7) And (5) repeating the steps (5) and (6) in sequence, and observing the shape and the color change of the liquid drop by a reflection mode optical microscope. The number of repeated cycles is more than 10.
As shown in fig. 3, fig. 3 (a) is an optical microscope image of the structure color obtained in the step (4), wherein the mass ratio of solute Capstone FS-30 to PVA is 2:3; in FIG. 3 (b) is an optical microscope image of the aqueous solution of Capstone FS-30 added in step (5) (at this time, the mass of Capstone FS-30 added again requires the mass ratio of Capstone FS-30 to PVA of the whole system to be 2:1), and it can be seen that the structural color has disappeared. In FIG. 3, (c) is an optical microscope image of the PVA added in step (6) in an amount such that the mass of PVA added again is required to give a mass ratio of solute Capstone FS-30 to PVA of 2:3 for the whole system, and it can be seen that the structural color is reproduced again, and the cycle is thus repeated. The cycle times can reach more than 10 times.
The above examples are only examples, and surfactant 1 may be any of FC-4430, FC301, capstone 62MA, ZY-FC327, ZY-823, ZONLY FS300, TF282, TF328, similar to Capstone FS-30, which is capable of preferentially reducing the interfacial tension between fluorocarbon and water; surfactant 2 may be any of CTAB, F-108, F-127, TWEEN20, TWEEN 40, TWEEN 60, TWEEN 80, similar to SDS, PVA, which can preferentially reduce interfacial tension between hydrocarbon and water; the specific type of hydrocarbon, fluorocarbon, can also be flexibly adjusted as long as they are all liquid at room temperature and are mutually immiscible, hydrocarbon having a density less than fluorocarbon and a refractive index greater than fluorocarbon. In addition, the preparation process and the subsequent detection process of each of the above examples were carried out at room temperature.
It will be readily appreciated by those skilled in the art that the foregoing description is merely a preferred embodiment of the invention and is not intended to limit the invention, but any modifications, equivalents, improvements or alternatives falling within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (8)
1. A method for preparing responsive structural color droplets, comprising the steps of:
(1) Dissolving a first surfactant in deionized water to obtain a first surfactant solution; dissolving a second surfactant in deionized water to obtain a second surfactant solution; the first surfactant solution and the second surfactant solution correspond to aqueous solutions of continuous phases of responsive structural color droplets; wherein the first surfactant is one of FC-4430, FC301, capstone FS-30, capstone 62MA, ZY-FC327, ZY-823, ZONLY FS300, TF282 and TF 328; the second surfactant is one of SDS, PVA, CTAB, F-108, F-127, TWEEN20, TWEEN 40, TWEEN 60 and TWEEN 80;
(2) Preparing liquid hydrocarbon and liquid fluorocarbon as oil phase substances; wherein the hydrocarbon has a density less than the fluorocarbon, a refractive index greater than the fluorocarbon, and the hydrocarbon and the fluorocarbon are immiscible at room temperature; an oil phase material of the hydrocarbon and the fluorocarbon corresponding to the dispersed phase of the responsive structural color droplets;
(3) Uniformly mixing the first surfactant solution, the second surfactant solution, the hydrocarbon and the fluorocarbon to form an oil-in-water system, wherein the formed liquid drops are responsive structural color liquid drops; according to the mass ratio of the first surfactant to the second surfactant in the system, the liquid drops can have structural colors or not;
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system is 1:1-1:5, the liquid drops are Janus liquid drops and have structural colors;
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system is not 1:1-1:5, the liquid drops do not have structural color.
2. The method of producing a responsive structural color drop of claim 1, further comprising the step (4):
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system is 1:1-1:5, adding the first surfactant solution and/or the second surfactant solution into the oil-in-water system again to enable the mass ratio of the first surfactant to the second surfactant in the system to deviate from 1:1-1:5, and obtaining liquid drops with disappeared structural color by utilizing diffusion;
when the mass ratio of the first surfactant to the second surfactant in the oil-in-water system does not meet 1:1-1:5, the first surfactant solution and/or the second surfactant solution are added into the oil-in-water system again, so that the mass ratio of the first surfactant to the second surfactant in the system meets 1:1-1:5 again, and the liquid drops with the structural color reproduction can be obtained by utilizing the diffusion effect.
3. The method of claim 1, wherein in step (1), the concentration of the first surfactant solution is 1 to 50mg/mL, and the concentration of the second surfactant solution is 1 to 50mg/mL.
4. The method for producing a responsive structural color droplet according to claim 1, wherein in the step (2), the hydrocarbon is one of octadecyl methacrylate, ethoxylated trimethylolpropane triacrylate, ethylene glycol dimethacrylate, t-butyl bromoacetate, n-butyl acrylate, dodecyl acrylate;
the fluorocarbon is 1H, 2H-heptadecafluorodecyl acrylate 1, 3-hexafluoroisopropyl methacrylate 2, 2-trifluoroethyl methacrylate one of hexafluorobutyl methacrylate, 2,3, 4-hexafluorobutyl acrylate and trifluoroethyl methacrylate;
in the step (3), the volume ratio of the hydrocarbon to the fluorocarbon is 1:1-1:8.
5. The method for producing a responsive structural color droplet according to claim 1, wherein in the step (3), the mixing is performed in a vortex oscillator at a vibration speed of 300 to 2000rpm for a vibration time of 0.5 to 5min;
the diameter of the responsive structural color drop is 20-200 mu m.
6. Responsive structural color droplets obtained by the method of any one of claims 1 to 5.
7. The use of the responsive structural color drop of claim 6 in anti-counterfeiting.
8. The use according to claim 7, wherein the first surfactant solution and/or the second surfactant solution is added to the oil-in-water system again to provide a first surface in the system
The mass ratio of the surfactant to the second surfactant deviates from or meets 1:1-1:5, and by utilizing the diffusion effect,
the disappearance and reproduction of the structural color is controlled.
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