CN112852404B - Thermochromic composite capsule and preparation method and application thereof - Google Patents
Thermochromic composite capsule and preparation method and application thereof Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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- C09K2211/1003—Carbocyclic compounds
- C09K2211/1007—Non-condensed systems
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
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- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1088—Heterocyclic compounds characterised by ligands containing oxygen as the only heteroatom
Abstract
The invention provides a thermochromic composite capsule and a preparation method and application thereof, wherein the composite capsule comprises a first capsule wall and a plurality of microcapsules wrapped by the first capsule wall, and the microcapsules comprise a second capsule wall and a capsule core wrapped by the second capsule wall; the capsule core is made of thermochromic materials. The thermochromic composite capsule prepared by the invention greatly improves the decomposition temperature of the capsule and the anti-aging capacity of the capsule color-changing substances; meanwhile, the color change capability of the capsule in repeated cold and hot circulation is greatly improved; a plurality of color developing agents are selected, so that the color changing color is more diversified, and the color changing temperature is wider; the particle size of the composite capsule can be regulated so as to meet high requirements of the composite capsule in different use environments; has excellent mechanical property and can ensure the use of the material under different environments.
Description
Technical Field
The invention relates to a thermochromic composite capsule and a preparation method and application thereof.
Background
The thermochromic material is a substance which changes color along with the change of temperature, and when the temperature of the thermochromic material is higher than a temperature change point, the thermochromic material is white and has larger solar reflectivity; when the temperature of the thermochromic material is lower than the temperature change point, the thermochromic material shows the original color and has higher solar absorptivity. Thermochromic asphalts prepared by encapsulating heat-to-color change materials into asphalt are therefore used to create new pavements of desired solar reflectivity, i.e., they reflect more solar energy at high temperatures in the summer and less at low temperatures in the winter. Therefore, the thermochromic material has wide application prospect in asphalt pavements as a building energy-saving material.
In 2020, maohuayu, liu hong Ru and the like disclose in the literature of preparation and performance research of three-component thermochromic microcapsules: the thermochromic microcapsule prepared by taking the thermochromic compound prepared from crystal violet lactone, bisphenol A and tetradecanol as a core material (capsule core) and taking gelatin-gum arabic as a wall material has sensitive color change temperature. However, the microcapsule starts to decompose at 150 ℃ and completely decomposes at about 200 ℃, which has certain requirements on the temperature of the use environment. Meanwhile, the gelatin-gum arabic is used as a wall material (capsule wall), has poor mechanical strength, is easy to break in use, and causes the color-changing compound to flow out, so that the capsule loses the color-changing performance.
Most of the existing thermochromic microcapsule color-changing compound systems contain toxic substances (such as bisphenol A), and the bisphenol A can be decomposed and released into the natural environment to cause ecological environment pollution and harm organisms in various ways. Bisphenol A can directly enter organisms from the environment or be accumulated in the organisms in a food chain mode, and the physiological functions of the organisms are reduced through biochemical action and physiological action, so that cancers, congenital malformations and serious damages to the organisms are caused to the organisms which destroy immune systems and cause various diseases. Therefore, avoiding the bisphenol a developer can significantly reduce the impact on the environment.
Disclosure of Invention
The invention aims to solve the technical problems that the existing thermochromic microcapsules have poor high-temperature resistance, low mechanical strength and easy rupture in use.
The technical scheme of the invention is that the invention provides a thermochromic composite capsule, which comprises a first capsule wall and a plurality of microcapsules wrapped by the first capsule wall, wherein the microcapsules comprise a second capsule wall and a capsule core wrapped by the second capsule wall; the capsule core is made of thermochromic materials.
Preferably, the particle size of the composite capsule is 20 to 2000 μm; preferably 40 to 1500 μm.
In the invention, the particle size of the composite capsule can be adjusted according to the requirement, for example, 50-200 μm can be selected; 200-400 μm; 400-600 μm; 600-800 μm; 800-1100 mu m; 1100-1500 μm.
Preferably, the first capsule wall is calcium alginate.
Preferably, the thermochromic material is a composition and comprises 1 part of color former, 2-5 parts of color developer and 50-100 parts of solvent by mass.
Preferably, the chromophoric agent is crystal violet lactone; the color developing agent is one or a combination of more of 4-dodecylphenol, adipic acid and barium chloride dihydrate; the solvent is one or a combination of more of tetradecanol, hexadecanol and octadecanol.
Preferably, the thermochromic material has a thermochromic temperature of 20-50 ℃. The color of the composite capsule can be changed from red to white, from blue to white, from grass green to white, from brown to yellow and the like.
The maximum value of the bearable load of the composite capsule obtained by the invention is more than 40N.
The invention also provides a preparation method of the thermochromic composite capsule, which comprises the following steps:
(a) Preparing microcapsules;
(b) Blending the microcapsule and the sodium alginate solution to obtain a blend;
(c) Adding the blend into calcium chloride solution to prepare the composite capsule.
Preferably, the concentration of the sodium alginate solution is 1-5% by mass; the concentration of the calcium chloride solution is 1-5%.
Preferably, the mass ratio of the microcapsule to the sodium alginate solution is 1.
The invention also provides the application of the thermochromic composite capsule or the preparation method thereof in the field of asphalt concrete, cement concrete or paint.
Specifically, the preparation method of the composite capsule comprises the following steps:
(1) Preparing a capsule core of the thermochromic microcapsule: preparing a color former (crystal violet lactone), different color developing agents (4-dodecylphenol, adipic acid and barium chloride dihydrate), and an alcohol solvent (tetradecanol, hexadecanol and octadecanol) into a color-changing compound according to the mass ratio of 1;
(2) Preparing the capsule wall of the thermochromic microcapsule: preparing methyl etherified melamine formaldehyde resin from melamine, formaldehyde and anhydrous methanol according to a molar ratio of 1;
(3) Preparing the capsule core and the second capsule wall into a thermochromic microcapsule according to a mass ratio of 1;
(4) Preparing the thermochromic microcapsule prepared in the step (3) and a sodium alginate solution into a blend according to a mass ratio of 1;
(5) Adding the blend prepared in the step (4) into a calcium chloride solution through a container to obtain a thermochromic composite capsule;
(6) And (5) washing and drying the thermochromic composite capsule obtained in the step (5).
According to the invention, when the color developing agent is selected, bisphenol compounds are avoided, the color developing agent which is more environment-friendly is selected, and meanwhile, when the capsule wall of the microcapsule is prepared, the melamine formaldehyde resin is etherified, so that the emission of formaldehyde in the preparation process of the thermochromic capsule is greatly reduced.
The composite capsule of the invention is a capsule wrapping a plurality of microcapsules, and compared with the single microcapsule, the composite capsule of the invention has the following beneficial effects: the thermochromic composite capsule prepared by the invention greatly improves the decomposition temperature of the capsule and the anti-aging capacity of the capsule color-changing substances; meanwhile, the color change capability of the capsule in repeated cold and hot circulation is greatly improved; and the composite capsule has excellent mechanical property and can be used in different environments.
The thermochromic composite capsule prepared by the invention has more diversified color changing colors and wider color changing temperature; and the particle size of the composite capsule can be regulated and controlled so as to meet high requirements of the composite capsule in different use environments.
Drawings
Figure 1 shows a diagram of a piston device for preparing the composite capsule of the invention.
FIG. 2 is a view showing a dropper apparatus for preparing the composite capsule of the present invention.
FIG. 3 is a schematic diagram showing a composite capsule prepared in example 1.
Fig. 4 shows an SEM image of the appearance of the composite capsule prepared in example 1.
Fig. 5 shows an SEM image of the inside of the composite capsule prepared in example 1.
FIG. 6 shows an image of a cross section of the composite capsule prepared in example 1 under a fluorescence microscope.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
The diagram of the composite capsule device prepared in this example is shown in fig. 1-2:
FIG. 1 shows an improved spraying device, when a piston is pulled upwards, a microcapsule sodium alginate blend liquid is pumped into a thick pipe together with air; and then the piston is pushed downwards, and the microcapsule blending liquid and air are sprayed into a container containing a solution of calcium chloride through a nozzle at the narrow opening end to form a composite capsule. The device is used for regulating and controlling the composite capsule with the particle size of less than 800 mu m, and the functional relation of the capsule particle size y (mu m) and the piston propulsion speed v (mm/s) is obtained through multiple experimental demonstration and data fitting: y (μm) = -150.51v +927.55, wherein (v < 6 mm/s). The function relation can predict the piston propelling speed required when the composite capsule with the grain diameter smaller than 800 mu m is regulated and controlled, and can more accurately control the grain diameter of the composite capsule.
The device shown in figure 2 is used for regulating and controlling the capsules with the grain diameter of more than 800-2000 mu m. The blending liquid is added into a separating funnel, and is dripped into a calcium chloride solution through a dropper, wherein the caliber of the dropper connected below the funnel is controlled, so that the composite capsules with different particle sizes are prepared. Multiple experimental demonstrations and data fitting obtain a functional relation between the capsule particle size y (mum) and the diameter x (mm) of a burette port, wherein (x < 7 mm) is y (mum) =151.1x + 857.4. The function relation can predict the piston propelling speed required when the composite capsule with the grain diameter of 800-2000 mu m is regulated and controlled, and can more accurately control the grain diameter of the composite capsule.
Example 1
The embodiment provides a blue thermochromic composite capsule, and the preparation method comprises the following steps: (wherein, 1 part by mass =2 g)
(1) According to the mass parts, 1 part of crystal violet lactone, 5 parts of 4-dodecylphenol and 60 parts of hexadecanol are heated and stirred in a water bath at the temperature of 90 ℃, the stirring speed is 1000rpm, and the blue thermochromic compound is prepared after heating and stirring for 1 hour.
(2) According to molar parts (1 part =0.5 mol), 1 part of melamine and 6 parts of formaldehyde are heated and stirred for 50min under the condition of water bath at 70 ℃ at the pH value of 9, then a proper amount of diluted hydrochloric acid is added to adjust the pH value to 5, then 15 parts of anhydrous methanol is added, after reaction for 1.5h, a proper amount of triethanolamine is added to adjust the pH value to 8, and the methylated melamine-formaldehyde resin is obtained.
(3) According to the mass parts, 50 parts of blue thermochromic compound, 1 part of styrene maleic anhydride copolymer and 10 parts of distilled water are heated and stirred for 15min under the conditions that the PH is 5 and the stirring speed is 2000rpm under the water bath condition of 55 ℃; and (3) slowly adding 50 parts of methylated melamine resin prepared in the step (2), reacting for 2 hours after all the methylated melamine resin is added, adding a small amount of triethanolamine to adjust the pH value to 7, and stopping the reaction. And finally, carrying out suction filtration on the product to obtain the blue thermochromic microcapsule.
(4) And (4) mixing 1 part of the thermochromic blue microcapsule obtained in the step (3) with 100 parts of a 2wt% sodium alginate solution at 1500rpm to obtain a blue blended solution.
(5) And (3) dripping the blended solution obtained in the step (4) into a 2wt% calcium chloride solution through a dropper connected with a separating funnel, wherein the diameter of the dropper is 2mm, so as to obtain the wet blue composite capsule.
(6) Finally, the blue compound capsule with the grain size of about 1000 mu m is obtained by cleaning and airing.
The appearance of the blue thermochromic composite capsules obtained in example 1 is shown in fig. 3, and the SEM images thereof are shown in fig. 4 and 5, and the particle size is about 1000 μm, and the microcapsules are uniformly distributed in the composite capsules.
Fig. 6 shows an internal fluorescence microscope image of the blue thermochromic composite capsule obtained in example 1, and the microcapsules in the composite capsule have a good color development effect.
The mechanical strength of the obtained capsules was measured by subjecting the blue complex thermochromic capsules obtained in example 1 to a uniaxial compression test. In the test, each capsule was placed under a press and the capsules were compressed until rupture at a loading rate of 0.5 mm/min. An electric pull and press tester model ZQ-990 was used, and the maximum load was 2KN. The test temperature was 20 ℃. The mechanical strength of the obtained blue thermochromic composite capsules is shown in table 1 after 5 parallel tests, and the maximum load which can be borne by the composite capsules is more than 45N as can be seen from table 1, so that the composite capsules can be used in various occasions.
Table 1 mechanical strength of the composite capsules obtained in example 1
Taking 5g of the blue thermochromic composite capsule obtained in example 1 and the microcapsule prepared in the step (3) into a conical flask in a water bath kettle, adjusting the temperature of the water bath kettle, and observing the discoloration temperature of the composite capsule and the microcapsule.
And (3) respectively taking 5g of the blue thermochromic composite capsule obtained in the example 1 and the microcapsule prepared in the step (3), placing the blue thermochromic composite capsule and the microcapsule in an oven, setting the oven at different temperatures and different times, and observing the decomposition temperatures of the composite capsule and the microcapsule.
And (4) adding the blue thermochromic composite capsules obtained in the example 1 and the microcapsules prepared in the step (3) into an asphalt mixture according to five percent of the mass of the asphalt when the asphalt mixture is mixed, forming the mixture into rutting plates with the thickness of 300 x 50mm, placing the rutting plates into an environment with the temperature of 60 ℃, and placing the rutting plates for the same time to compare with blank rutting plates without capsules.
Through the above experiments, the performances of the obtained blue thermochromic composite capsules and microcapsules are shown in table 2, the color change temperature of the blue thermochromic composite capsules is 29-40 ℃, and is wider than the color change temperature range of 31-37 ℃ of the blue thermochromic microcapsules, and the decomposition temperature of the blue thermochromic composite capsules reaches above 300 ℃ and is much higher than the decomposition index of the blue thermochromic microcapsules by 180 ℃. Under the condition of 150 ℃, the blue thermochromic microcapsules lose the color change performance after 30 min. And the blue thermochromic composite capsule still keeps reversible color change capability. In addition, the rutting plate is placed in an environment of 60 ℃ for the same time, and compared with a blank sample, the temperature of the added blue thermochromic microcapsules can be reduced by 2.3 ℃, and the temperature of the added blue thermochromic composite capsules can be reduced by 5.2 ℃.
Example 2
The embodiment provides a yellow thermochromic composite capsule, and a preparation method thereof comprises the following steps: (wherein, 1 part by mass =2 g)
(1) According to the mass parts, 1 part of crystal violet lactone, 4 parts of adipic acid and 100 parts of octadecanol are heated and stirred in a water bath at the temperature of 90 ℃, the stirring speed is 1000rpm, and the yellow thermochromic compound is prepared after heating and stirring for 1 hour.
(2) According to molar parts (1 part =0.5 mol), 1 part of melamine and 6 parts of formaldehyde are heated and stirred for 50min under the condition of water bath at 70 ℃ at the pH value of 9, then a proper amount of diluted hydrochloric acid is added to adjust the pH value to 5, then 15 parts of anhydrous methanol is added, after reaction for 1.5h, a proper amount of triethanolamine is added to adjust the pH value to 8, and the methylated melamine-formaldehyde resin is obtained.
(3) According to the mass parts, 55 parts of yellow thermochromic compound, 1 part of styrene maleic anhydride copolymer and 10 parts of distilled water are heated and stirred for 15min under the conditions that the PH is 5 and the stirring speed is 2000rpm under the water bath condition at 55 ℃; and (3) slowly adding 50 parts of the methylated melamine resin prepared in the step (2), reacting for 2 hours after the methylated melamine resin is completely added, adding a small amount of triethanolamine to adjust the pH value to 7, and stopping the reaction. And finally, carrying out suction filtration on the product to obtain the yellow thermochromic microcapsule.
(4) And (3) mixing 1 part of the yellow thermochromic microcapsule obtained in the step (3) with 100 parts of 2wt% sodium alginate solution at 1500rpm to obtain a yellow blending liquid.
(5) Spraying the blending liquid obtained in the step (4) into a 2wt% calcium chloride solution by a piston spraying device at the piston pushing speed of 1.5mm/s to obtain wet thermochromic composite capsules of yellow composite capsules
(6) And finally, cleaning and airing to obtain the thermochromic composite capsule of the yellow composite capsule with the particle size of about 600 um.
And (3) respectively taking 5g of the yellow thermochromic composite capsule obtained in the example 2 and the microcapsule prepared in the step (3) into a conical flask in a water bath kettle, adjusting the temperature of the water bath kettle, and observing the discoloration temperature of the composite capsule and the microcapsule.
5g of each of the yellow thermochromic composite capsules obtained in example 2 and the microcapsules prepared in step (3) was placed in an oven, the oven was set at different temperatures and times, and the decomposition temperatures of the composite capsules and the microcapsules were observed
And (3) adding the yellow thermochromic composite capsule obtained in the example 2 and the microcapsule prepared in the step (3) into an asphalt mixture when the asphalt mixture is mixed according to five mass percent of asphalt, forming the mixture into a rutting plate with the thickness of 300X 50mm, placing the rutting plate into an environment with the temperature of 60 ℃, and standing the rutting plate for the same time to compare with a blank rutting plate without the capsule.
Through the experiments, the performances of the obtained yellow thermochromic composite capsules and microcapsules are shown in table 2, the color change temperature of the yellow thermochromic composite capsules is 40-50 ℃, and is wider than the color change temperature range of the yellow thermochromic microcapsules from 42 ℃ to 47 ℃, and the decomposition temperature of the yellow thermochromic composite capsules reaches above 300 ℃ and is much higher than the decomposition degree of the yellow thermochromic microcapsules by 170 ℃. At 160 ℃, the yellow thermochromic microcapsules lose the color change performance after 25 min. While the yellow thermochromic composite capsule still maintains reversible color change capability. In addition, the rutting plate is placed in an environment of 60 ℃ for the same time, and compared with a blank sample, the temperature of the added yellow thermochromic microcapsules can be reduced by 2.8 ℃, and the temperature of the added yellow thermochromic composite capsules can be reduced by 6.4 ℃.
Example 3
The embodiment provides a green thermochromic composite capsule, and the preparation method comprises the following steps: (wherein, 1 part by mass =2 g)
(1) According to the mass parts, 1 part of crystal violet lactone, 7 parts of barium chloride dihydrate and 50 parts of tetradecanol are heated and stirred in a water bath at 90 ℃, the stirring speed is 1000rpm, and the green thermochromic compound is prepared after heating and stirring for 1 hour.
(2) According to molar parts (1 part =0.5 mol), 1 part of melamine and 6 parts of formaldehyde are heated and stirred for 50min under the condition of water bath at 70 ℃ at the pH value of 9, then a proper amount of diluted hydrochloric acid is added to adjust the pH value to 5, then 15 parts of anhydrous methanol is added, after reaction for 1.5h, a proper amount of triethanolamine is added to adjust the pH value to 8, and the methylated melamine-formaldehyde resin is obtained.
(3) According to the mass parts, 50 parts of green thermochromic compound, 1 part of styrene maleic anhydride copolymer and 10 parts of distilled water are heated and stirred for 15min under the conditions that the PH is 5 and the stirring speed is 2000rpm under the water bath condition of 55 ℃; and (3) slowly adding 50 parts of the methylated melamine resin prepared in the step (2), reacting for 2 hours after all the methylated melamine resin is added, adding a small amount of triethanolamine to adjust the pH value to 7, and stopping the reaction. And finally, carrying out suction filtration on the product to obtain the green thermochromic microcapsule.
(4) And (3) mixing 1 part of the green thermochromic microcapsule obtained in the step (3) with 100 parts of 2wt% sodium alginate solution at 1500rpm to obtain a green blending solution.
(5) And (3) dripping the blended solution obtained in the step (4) into a 2wt% calcium chloride solution through a dropper connected with a separating funnel, wherein the diameter of the dropper is 3mm, so as to obtain the wet green thermochromic composite capsule.
(6) Finally, cleaning and airing to obtain the green composite capsule with the grain size of about 1500 mu m.
And (3) respectively taking 5g of the green thermochromic composite capsule obtained in the example 3 and the microcapsule prepared in the step (3) into a conical flask in a water bath kettle, adjusting the temperature of the water bath kettle, and observing the discoloration temperature of the composite capsule and the microcapsule.
Respectively taking 5g of the green thermochromic composite capsule obtained in the example 3 and the microcapsule prepared in the step (3), placing the green thermochromic composite capsule and the microcapsule in an oven, setting the oven at different temperatures and different times, and observing the decomposition temperatures of the composite capsule and the microcapsule
And (3) mixing the green thermochromic composite capsules obtained in the example 3 and the microcapsules prepared in the step (3) according to five mass percent of asphalt, adding the mixture into an asphalt mixture during mixing, forming the mixture into a rutting plate with the thickness of 300X 50mm, placing the rutting plate into an environment with the temperature of 60 ℃, and standing the rutting plate for the same time to compare the rutting plate with a blank rutting plate without the capsules.
Through the above experiments, the performances of the obtained green thermochromic composite capsules and microcapsules are shown in table 2, the color change temperature of the green thermochromic composite capsules is 20-29 ℃, and is wider than the color change temperature range of 24-27 ℃ of the green thermochromic microcapsules, and the decomposition temperature of the green thermochromic composite capsules reaches above 300 ℃ and is much higher than the decomposition index of the green thermochromic microcapsules by 180 ℃. Under the condition of 145 ℃, the green thermochromic microcapsules lose the color change performance after 20 min. While the green thermochromic composite capsule still keeps reversible color change capability. In addition, the rutting plate is placed in an environment of 60 ℃ for the same time, and compared with a blank sample, the temperature of the added green thermochromic microcapsules can be reduced by 2.1 ℃, and the temperature of the added green thermochromic composite capsules can be reduced by 5.1 ℃.
TABLE 2 comparison of the Properties of the composite capsules of different colors with the microcapsules
Claims (2)
1. Use of a thermochromic composite capsule in asphalt or cement concrete, wherein the composite capsule comprises a first capsule wall and a plurality of microcapsules encapsulated by the first capsule wall, wherein the microcapsules comprise a second capsule wall and a capsule core encapsulated by the second capsule wall; the capsule core is made of thermochromic materials; the particle size of the composite capsule is 600 to 2000 mu m; the first capsule wall is composed of calcium alginate; the second capsule wall is methylated melamine-formaldehyde resin prepared from melamine, formaldehyde and anhydrous methanol according to a molar ratio of 1;
the preparation method of the composite capsule comprises the following steps:
(a) Preparing microcapsules;
(b) Blending the microcapsule and the sodium alginate solution to obtain a blend;
(c) Adding the blend into a calcium chloride solution to prepare a composite capsule;
according to the mass fraction, the concentration of the sodium alginate solution is 1-5%; the concentration of the calcium chloride solution is 1-5%; the mass ratio of the microcapsule to the sodium alginate solution is 1;
the thermochromic material is a composition and comprises 1 part of color former, 2-5 parts of color developing agent and 50-100 parts of solvent according to parts by mass;
the color former is crystal violet lactone; the color developing agent is one or a combination of more of 4-dodecylphenol, adipic acid and barium chloride dihydrate; the solvent is one or a combination of more of tetradecanol, hexadecanol and octadecanol.
2. Use of a thermochromic composite capsule according to claim 1 in asphalt or cement concrete, wherein the thermochromic material has a thermochromic temperature of 20-50 ℃.
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