CN111499885A - Photo-stimulus response reversible color-changing hydrogel and preparation method thereof and optical device - Google Patents
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Abstract
The invention belongs to the technical field of hydrogel, and particularly relates to light stimulus response reversible color-changing hydrogel, a preparation method thereof and an optical device. The light stimulus response reversible color-changing hydrogel comprises hydrogel colloid, 10,12-pentacosadiynoic acid substituted by spiropyran, and 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules; 10,12-pentacosadiynoic acid substituted by spiropyran and 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules are uniformly doped in the hydrogel colloid, the light stimulus response reversible color-changing hydrogel color-changing process takes light as a driving force, the light stimulus can accurately adjust the intensity, the irradiation time and the irradiation site of illumination, further the light stimulus response of the light stimulus response reversible color-changing hydrogel can be accurately controlled, and the process control can be realized. In addition, the light stimulation response reversible color-changing hydrogel takes light as a driving force to perform light stimulation response reversible color-changing, is clean and soft, and cannot damage a hydrogel system.
Description
Technical Field
The invention belongs to the technical field of hydrogel, and particularly relates to light stimulus response reversible color-changing hydrogel, a preparation method thereof and an optical device.
Background
Hydrogels are flexible and stretchable, and studies have shown that stretchable hydrogels have potential applications in conductors, displays, capacitors, and batteries. In particular, display devices, which are important media for human-computer interaction, have been widely designed and produced and rely on light emission or color change.
However, the conventional color-changeable hydrogel requires the use of heat, pH, electrical stimulation, and the like as response conditions, and causes energy loss.
Disclosure of Invention
In view of the above, the invention provides a light-stimulated-response reversible color-changing hydrogel, a preparation method thereof and an optical device, which are used for solving the problem that the existing color-changing hydrogel needs to use heat, a pH value, electric stimulation and the like as response conditions to generate energy loss.
The specific technical scheme of the invention is as follows:
a light stimulus response reversible color-changing hydrogel comprises hydrogel colloid and 10,12-pentacosadiynoic acid substituted by spiropyran, and 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules;
the 10,12-pentacosadiynoic acid substituted by the spiropyran and the 10,12-pentacosadiynoic acid and/or the 10,12-pentacosadiynoic acid substituted by the small molecule are uniformly doped in the hydrogel colloid.
The light stimulus response reversible color-changing hydrogel comprises hydrogel colloid, 10,12-pentacosadiynoic acid substituted by spiropyran, 10,12-pentacosadiynoic acid (10,12-pentacosadiynoic acid, DA) and/or 10,12-pentacosadiynoic acid substituted by small molecules, the light stimulus response reversible color-changing hydrogel presents bluish purple after being irradiated under 254nm ultraviolet light for 10min, and then presents blue after being irradiated under visible light for 10min, and the process of color conversion is reversible; the light stimulus response reversible color-changing hydrogel is purple after being irradiated for 10min under 365nm ultraviolet light, and is colorless after being irradiated for 10min under visible light, and the process of color conversion is reversible. In addition, the light stimulation response reversible color-changing hydrogel takes light as a driving force to perform light stimulation response reversible color-changing, is clean and soft, cannot generate energy loss, and cannot damage a hydrogel system.
It is significant to introduce a luminescent substance such as a photochromic material spiropyran into the hydrogel to obtain a light stimulus responsive hydrogel so as to realize a visual display of light stimulus responsive discoloration. Spiropyrans are important photochromic compounds, and become hot spots of research in the current photochromic field due to the characteristics of excellent photochromic properties, thermal stability, fatigue resistance, capability of serving as good organic light storage materials and the like. However, the spiropyrans have low solubility in water, and how to introduce them into hydrogel systems has been a problem to be solved by those skilled in the art.
In the invention, the light stimulus response reversible color-changing hydrogel comprises hydrogel colloid, 10,12-pentacosadiynoic acid substituted by spiropyran, 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules, spiropyran is introduced into the 10,12-pentacosadiynoic acid to obtain 10,12-pentacosadiynoic acid substituted by spiropyran, the 10,12-pentacosadiynoic acid substituted by spiropyran and 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules are co-doped into the hydrogel system, the 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules can increase the solubility of 10,12-pentacosadiynoic acid substituted by spiropyran in water, so that the 10 substituted by spiropyran, the 12-pentacosadiynoic acid is uniformly doped in the hydrogel system, so that the problem that the spiropyran is very low in solubility in water and is difficult to introduce into the hydrogel system is solved.
Preferably, the small molecule substituted 10,12-pentacosadiynoic acid is selected from amino substituted 10,12-pentacosadiynoic acid, coumarin substituted 10,12-pentacosadiynoic acid and/or nitroazobenzene substituted 10,12-pentacosadiynoic acid.
The structural formulas of the amino-substituted 10,12-pentacosadiynoic acid, the coumarin-substituted 10,12-pentacosadiynoic acid and the nitroazobenzene-substituted 10,12-pentacosadiynoic acid are as follows in sequence:
amino-substituted 10,12-pentacosadiynoic acid;
coumarin-substituted 10,12-pentacosadiynoic acid;
nitroazobenzene-substituted 10,12-pentacosadiynoic acid.
In the present invention, the photostimulation-responsive reversible color-changing hydrogel preferably comprises hydrogel colloids and 10,12-pentacosadiynoic acid substituted by spiropyrans, and 10,12-pentacosadiynoic acid. The structural formulas of the spiropyran substituted 10,12-pentacosadiynoic acid and the 10,12-pentacosadiynoic acid are as follows:
10,12-pentacosadiynoic acid substituted with spiropyran;
10,12-pentacosadiynoic acid.
Preferably, the doping amount of the spiropyran substituted 10,12-pentacosadiynoic acid in the hydrogel colloid is
The invention also provides a preparation method of the light stimulus response reversible color-changing hydrogel, which comprises the following steps:
a) dissolving the 10,12-pentacosadiynoic acid substituted by the spiropyran and the 10,12-pentacosadiynoic acid and/or the 10,12-pentacosadiynoic acid substituted by the small molecule in an organic solvent to obtain a mixed solution, and adding the mixed solution into deionized water to obtain a composite vesicle solution;
b) and adding a colloid raw material into the composite vesicle solution, after swelling the colloid raw material, stirring at 41-52 ℃ to dissolve the colloid raw material, and cooling to obtain the photo-stimulation response reversible color-changing hydrogel.
According to the preparation method, 10,12-pentacosadiynoic acid substituted by spiropyran, 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules are assembled to form a water-soluble composite vesicle solution, and then a hydrogel system is formed by adding a colloid raw material for forming hydrogel, so that the light stimulus response reversible color-changing hydrogel is obtained, the color of the hydrogel system can be regulated and controlled through different light stimuli, and the repeated reversible response can be realized.
The light-stimulated response reversible color-changing hydrogel disclosed by the invention is simple in structure and low in preparation cost.
In the invention, the colloid raw material is dissolved by stirring at 41-52 ℃ in the step b), so that the dissolution of the colloid raw material can be ensured, and the composite vesicles can be prevented from being damaged.
Preferably, the mole ratio of the spiropyran-substituted 10,12-pentacosadiynoic acid to the 10,12-pentacosadiynoic acid and/or the small molecule-substituted 10,12-pentacosadiynoic acid in step a) is (0.8-1.2): (3.8-4.3), and more preferably 1: 4.
Preferably, the organic solvent of step a) is selected from ethanol, tetrahydrofuran, methanol and/or acetone, more preferably ethanol;
the molar concentration of the spiropyran-substituted 10,12-pentacosadiynoic acid in the mixed solution is 1.5 x 10- 4mol/L～3*10-4mol/L。
The molar concentration of the spiropyran substituted 10,12-pentacosadiynoic acid in the complex vesicle solution is 0.8 x 10-5mol/L～1.2*10-5mol/L。
Preferably, the volume ratio of the mixed solution in the step a) to the deionized water is 1: 30.
preferably, the step a) of adding the mixed solution into deionized water to obtain a complex vesicle solution specifically comprises:
and adding the mixed solution into deionized water at the temperature of 60-75 ℃, performing ultrasonic treatment, cooling to 10-32 ℃ under the condition of no illumination, and standing at the temperature of 4 ℃ for 8-15 hours to obtain the composite vesicle solution.
Preferably, the colloid raw material in the step b) is selected from gelatin powder, carrageenan powder, bone glue or pectin.
The light stimulation response reversible color-changing hydrogel can generate different responses to different lights and reversibly change the color of a hydrogel system, the diversity generated in the light stimulation process is absent in heat, pH value and electric stimulation, and the light stimulation can realize contactless remote regulation and control. According to the invention, the organic spiropyran photoisomerization molecules are introduced into the hydrogel in the form of the assembly, the preparation process is simple, the construction of an environment-friendly hydrogel system is realized, the color response process is completely reversible, and energy attenuation is avoided.
The invention also provides an optical device, which comprises the light stimulation response reversible color-changing hydrogel.
The optical device may be applied in optical storage and memory devices or intelligent display and communication devices.
In conclusion, the invention provides a light stimulus response reversible color-changing hydrogel, which comprises hydrogel colloid, 10,12-pentacosadiynoic acid substituted by spiropyran, and 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules; the 10,12-pentacosadiynoic acid substituted by the spiropyran and the 10,12-pentacosadiynoic acid and/or the 10,12-pentacosadiynoic acid substituted by the small molecule are uniformly doped in the hydrogel colloid. The color change process of the photo-stimulation response reversible color-changing hydrogel takes light as a driving force, and the intensity, the irradiation time and the irradiation site of illumination can be accurately adjusted by photo-stimulation, so that the photo-stimulation response of the photo-stimulation response reversible color-changing hydrogel can be accurately controlled, and the process control can be realized. In addition, the light stimulation response reversible color-changing hydrogel takes light as a driving force to perform light stimulation response reversible color-changing, is clean and soft, and cannot damage a hydrogel system.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic diagram showing the operation of example 1 of the present invention;
FIG. 2 is a photograph of photo-stimulus responsive reversible color-changing hydrogel prepared in example 1 of the present invention under different illumination;
FIG. 3 is a diagram of the corresponding UV-VIS absorption spectra of the reversible color-changing hydrogel with light stimulus response prepared in example 1 according to the present invention;
wherein DA is 10,12-pentacosadiynoic acid, substituted DA is 10,12-pentacosadiynoic acid substituted by spiropyran, and PDA is poly-10, 12-pentacosadiynoic acid.
Detailed Description
The invention provides a light stimulus response reversible color-changing hydrogel, a preparation method thereof and an optical device, which are used for solving the problem that the existing color-changing hydrogel needs to use heat, pH value, electric stimulation and the like as response conditions to generate energy loss.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Fig. 1 is a schematic diagram of an operation process according to embodiment 1 of the present invention.
In this embodiment, the preparation of the photo-stimulus responsive reversible color-changing hydrogel is performed first, and includes the following steps:
(1) preparation of Complex vesicle solution
Weigh 1.2 x 10-5mol of 10,12-pentacosadiynoic acid (DA) and 0.3X 10-5Putting mol 10,12-pentacosadiynoic acid substituted by spiropyran into a beaker, adding 10m L ethanol, completely dissolving under 120W ultrasonic power to obtain a mixed solution, adding the mixed solution into 300m L deionized water at 75 ℃, performing ultrasonic power of 48W for 90min, naturally cooling to 25 ℃ in the shade after the ultrasonic power is over, and putting the mixture into a refrigerator at 4 ℃ for overnight to obtain the composite vesicle solution.
(b) Preparation of photo-stimulus responsive reversible color-changing hydrogel
Adding 0.2g of gelatin powder into the composite vesicle solution, soaking for 4h at room temperature, swelling the gelatin powder, heating to 50 ℃, stirring to dissolve the gelatin powder, pouring the dissolved gelatin powder into a culture dish, and forming the light stimulation response reversible color-changing hydrogel in the cooling process.
In this example, the photo-stimulus responsive reversible color-changing hydrogel prepared by the method is further subjected to photo-stimulus responsive color-changing property detection. FIG. 2 is a photograph of the photo-stimulus responsive reversible color-changing hydrogel prepared in example 1 of the present invention under different illumination. The prepared light stimulus response reversible color-changing hydrogel presents an approximately colorless and transparent state when not being processed. After the irradiation is carried out for 10min under an ultraviolet lamp with the wavelength of 254nm, the light-stimulated response reversible color-changing hydrogel presents bluish purple, and presents blue after the irradiation is carried out for 10min under visible light, and the color conversion process is reversible; after the reversible color-changing hydrogel is irradiated under a 365nm ultraviolet lamp for 10min, the reversible color-changing hydrogel responding to light stimulation presents purple, and then presents colorless after being irradiated under visible light for 10min, and the color conversion process is reversible.
Referring to fig. 3, it is a corresponding uv-vis absorption spectrum diagram when the photo-stimulus responsive reversible color-changing hydrogel prepared in example 1 of the present invention exhibits different colors. FIG. 3 shows that after 254nm illumination, the reversible color-changing hydrogel shows bluish purple color in response to light stimulation, and absorption peaks appear at 564nm and 627nm, which correspond to the absorption peak of ring opening of spiropyran and the absorption peak of poly-10, 12-pentacosadiynoic acid (PDA) synthesized by poly-10, 12-pentacosadiynoic acid (DA). When the reversible color-changing hydrogel shows purple color in response to light stimulation, only an absorption peak is at 564nm, but no absorption peak is at 627nm, which indicates that only spiropyran has ring-opening reaction in the state, and 10,12-pentacosadiynoic acid (DA) has no polymerization reaction. When the light stimulus response reversible color-changing hydrogel presents blue, the absorption peak of blue-phase diyne at 627nm is not changed, the absorption peak of the open ring of the spiropyran at 564nm disappears, because the spiropyran gradually changes from the open ring body to the closed ring body under the illumination condition of visible light, the absorption peak disappears, the purple color of the open ring body also disappears, and the color of the light stimulus response reversible color-changing hydrogel changes to the blue color of poly 10,12-pentacosadiynoic acid (PDA). Repeating the above process with light of different wavelengths can observe the same change of the ultraviolet-visible absorption spectrum.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A light stimulus response reversible color-changing hydrogel is characterized by comprising hydrogel colloid, 10,12-pentacosadiynoic acid substituted by spiropyran, and 10,12-pentacosadiynoic acid and/or 10,12-pentacosadiynoic acid substituted by small molecules;
the 10,12-pentacosadiynoic acid substituted by the spiropyran and the 10,12-pentacosadiynoic acid and/or the 10,12-pentacosadiynoic acid substituted by the small molecule are uniformly doped in the hydrogel colloid.
2. The photostimulation-responsive reversible color-changing hydrogel according to claim 1, wherein said small molecule substituted 10,12-pentacosadiynoic acid is selected from the group consisting of amino-substituted 10,12-pentacosadiynoic acid, coumarin-substituted 10,12-pentacosadiynoic acid and/or nitroazobenzene-substituted 10,12-pentacosadiynoic acid.
3. The photostimulation-responsive reversible color-changing hydrogel according to claim 1, wherein said spiropyran-substituted 10,12-pentacosadiynoic acid is doped in said hydrogel colloid in an amount of
4. A method for preparing a light stimuli-responsive reversible color-changing hydrogel according to any one of claims 1 to 3, comprising the steps of:
a) dissolving the 10,12-pentacosadiynoic acid substituted by the spiropyran and the 10,12-pentacosadiynoic acid and/or the 10,12-pentacosadiynoic acid substituted by the small molecule in an organic solvent to obtain a mixed solution, and adding the mixed solution into deionized water to obtain a composite vesicle solution;
b) and adding a colloid raw material into the composite vesicle solution, after swelling the colloid raw material, stirring at 41-52 ℃ to dissolve the colloid raw material, and cooling to obtain the photo-stimulation response reversible color-changing hydrogel.
5. The preparation method according to claim 4, wherein the molar ratio of the spiropyran-substituted 10,12-pentacosadiynoic acid to the 10,12-pentacosadiynoic acid and/or the small molecule-substituted 10,12-pentacosadiynoic acid in step a) is (0.8-1.2): (3.8-4.3).
6. The process according to claim 4, wherein the organic solvent of step a) is selected from ethanol, tetrahydrofuran, methanol and/or acetone;
the molar concentration of the spiropyran-substituted 10,12-pentacosadiynoic acid in the mixed solutionIs 1.5 x 10-4mol/L～3*10-4mol/L。
7. The preparation method according to claim 4, wherein the volume ratio of the mixed solution of the step a) to the deionized water is 1: 30.
8. the preparation method according to claim 4, wherein the step a) of adding the mixed solution into deionized water to obtain the complex vesicle solution specifically comprises the following steps:
and adding the mixed solution into deionized water at the temperature of 60-75 ℃, performing ultrasonic treatment, cooling to 10-32 ℃ under the condition of no illumination, and standing at the temperature of 4 ℃ for 8-15 hours to obtain the composite vesicle solution.
9. The preparation method according to claim 4, wherein the colloid material in step b) is selected from gelatin powder, carrageenan powder, bone glue or pectin.
10. An optical device comprising the light stimuli-responsive reversibly color-changing hydrogel of any one of claims 1 to 3.
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