CN113956511B - Humidity response color-changing hydrogel and preparation method and application thereof - Google Patents
Humidity response color-changing hydrogel and preparation method and application thereof Download PDFInfo
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/81—Indicating humidity
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/12—Agar-agar; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
Abstract
The invention relates to the technical field of intelligent sensing, in particular to humidity-response color-changing hydrogel and a preparation method and application thereof, wherein the preparation method of the humidity-response color-changing hydrogel comprises the following steps: (1) preparing gold nanoparticles by adopting a citrate reduction method; (2) a surfactant-modified gold nanoparticle; (3) And adding the hydrogel precursor into the gold nanoparticle solution modified by the surfactant to prepare the humidity-responsive color-changing hydrogel. Gold nanoparticles are introduced into a hydrogel network, the distance between the gold nanoparticles is reversibly regulated and controlled according to expansion or contraction caused by absorption/dehydration of the hydrogel, so that the dynamic reversible regulation and control of the plasmon resonance characteristics of the gold nanoparticles are realized, and finally the color of the gold nanoparticle hydrogel is reversibly changed, so that the humidity intelligent response hydrogel is constructed.
Description
Technical Field
The invention relates to the technical field of intelligent sensing, in particular to humidity response color-changing hydrogel and a preparation method and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Humidity control plays a very important role in detection in the fields of agriculture, industry, aerospace, goods storage and the like, and is particularly important for humidity monitoring. The humidity sensors are classified according to detection mechanism, and can be classified into capacitive, resistive, acoustic surface wave, optical and mass type humidity sensors; the current widely studied humidity sensors mainly comprise capacitance type humidity sensors and resistance type humidity sensors, but the sensors have the defects of high cost, poor portability, high use threshold and complex detection process, and high-end equipment and professional detection personnel are needed. Hydrogel is used as a stretchable elastomer material and is widely applied to the fields of flexible conductive materials, supercapacitors, drug sustained release, sensors, intelligent soft robots and the like at present; the inventor finds that the research on the hydrogel used for preparing the humidity sensor in the prior art is very little, and has good research and development prospect.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a humidity response color-changing hydrogel, a preparation method and application thereof, gold nanoparticles are introduced into a hydrogel network, the spacing between the gold nanoparticles is reversibly regulated and controlled according to expansion or contraction caused by absorption/dehydration of the hydrogel, so that the dynamic reversible regulation and control of the plasma resonance characteristics of the gold nanoparticles are realized, and finally the color of the gold nanoparticle hydrogel is reversibly changed, so that the humidity intelligent response hydrogel is constructed.
In order to achieve the above object, the technical scheme of the present invention is as follows:
in a first aspect of the present invention, there is provided a method for preparing a humidity-responsive color-changing hydrogel, the method comprising the steps of:
(1) Preparing gold nanoparticles by adopting a citrate reduction method;
(2) Modifying gold nanoparticles with a surfactant;
(3) And adding the hydrogel precursor into the gold nanoparticle solution modified by the surfactant to prepare the humidity-responsive color-changing hydrogel.
In one or more embodiments, the gold nanoparticles in step (1) are prepared by: heating chloroauric acid aqueous solution to boiling, adding sodium citrate aqueous solution, and continuing to stir vigorously to obtain gold nanoparticles;
in one or more embodiments, the surfactant in step (2) is selected from polyvinylpyrrolidone;
in one or more embodiments, the step of surfactant-modifying the gold nanoparticles in step (2) is:
centrifuging the gold nanoparticle aqueous solution obtained in the step (1), re-dispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution, heating and refluxing for reaction, and re-dispersing the obtained product into ethanol solution to obtain polyvinylpyrrolidone-modified gold nanoparticles;
in one or more embodiments, the hydrogel precursor in step (3) is selected from agarose;
in one or more embodiments, in the step (3), agarose powder is dispersed into the obtained polyvinylpyrrolidone modified gold nanoparticle solution under stirring, and the gold nanoparticle modified hydrogel is obtained through stirring and heating reaction, and the humidity response color-changing hydrogel is obtained after drying.
In a second aspect of the present invention, there is provided a humidity-responsive color-changing hydrogel prepared by the method for preparing a humidity-responsive color-changing hydrogel according to the first aspect.
In a third aspect of the invention, there is provided the use of the humidity-responsive color-changing hydrogel of the second aspect in the field of intelligent sensing.
The specific embodiment of the invention has the following beneficial effects:
(1) The humidity response color-changing hydrogel is sensitive to humidity response, can quickly generate color change, and has excellent cycle performance.
(2) The gold nanoparticles are prevented from agglomerating and denaturing by modifying the surfactant, the gold nanoparticles are mixed with the hydrogel precursor solution to prepare the gold nanoparticle modified hydrogel material, the hydrogel is utilized to absorb, dehydrate, expand and shrink to regulate the distance between the gold nanoparticles, so that reversible color change is realized, the preparation process is simple, and the preparation method is nontoxic and harmless to the environment.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a schematic diagram of the working principle of a humidity-responsive color-changing hydrogel;
FIG. 2 shows the change in ultraviolet absorbance peak at different humidities of the humidity-responsive color-changing hydrogel prepared in example 1 of the present invention.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
In one embodiment of the present invention, there is provided a method for preparing a humidity-responsive color-changing hydrogel, the method comprising the steps of:
(1) Preparing gold nanoparticles by adopting a citrate reduction method;
(2) Modifying gold nanoparticles with a surfactant;
(3) And adding the hydrogel precursor into the gold nanoparticle solution modified by the surfactant to prepare the humidity-responsive color-changing hydrogel.
In one or more embodiments, the gold nanoparticles in step (1) are prepared by: heating chloroauric acid aqueous solution to boiling, adding sodium citrate aqueous solution, and continuing to stir vigorously to obtain gold nanoparticles;
preferably, the mass concentration of the chloroauric acid aqueous solution is 0.5% -2%, and more preferably 1%;
preferably, the molar concentration of the aqueous sodium citrate solution is 0.05 to 0.2mol/L, more preferably 0.1mol/L;
the volume ratio of the chloroauric acid aqueous solution to the sodium citrate aqueous solution is 90-110:1, and more preferably 100:1;
in one or more embodiments, the surfactant in step (2) is selected from polyvinylpyrrolidone, polydiene-based propyldimethyl ammonium chloride, or cetyltrimethylammonium bromide;
in one or more embodiments, the step of surfactant-modifying the gold nanoparticles in step (2) is:
centrifuging the gold nanoparticle aqueous solution obtained in the step (1), re-dispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution, heating and refluxing for reaction, and re-dispersing the obtained product into ethanol solution to obtain polyvinylpyrrolidone-modified gold nanoparticles;
preferably, the concentration of the polyvinylpyrrolidone aqueous solution is 0.5 to 2mmol/L, more preferably 1mmol/L;
preferably, the temperature of the heating reflux reaction is 110-130 ℃ and the reaction time is 11-13 h; further preferably 120℃for 12 hours;
preferably, the centrifugation condition is 14000-16000 rpm for 20-40 min; further preferably, the centrifugation is carried out at 15000 rpm for 30min;
preferably, the volume fraction of the ethanol solution is 40-60%, more preferably 50%;
in one or more embodiments, the hydrogel precursor in step (3) is selected from agarose;
in one or more embodiments, in the step (3), agarose powder is dispersed into the obtained polyvinylpyrrolidone modified gold nanoparticle solution under stirring, and the gold nanoparticle modified hydrogel is obtained through stirring and heating reaction, and the humidity response color-changing hydrogel is obtained after drying.
Preferably, the mass ratio of the agarose to the chloroauric acid is 40-60: 1, further preferably 50:1, a step of;
preferably, the temperature of the stirring and heating reaction is 80-100 ℃ and the reaction time is 0.5-1.5 h; further preferably at 90℃for 1h;
preferably, after stirring and heating reaction, pouring the obtained solution into a mould to be placed in a refrigerator at the temperature of 4 ℃ for standing for 2 hours;
preferably, after the gold nanoparticle modified hydrogel is obtained, the gold nanoparticle modified hydrogel is cut to a corresponding size, and finally the cut gold nanoparticle modified hydrogel is freeze-dried, and further freeze-dried for 12 hours at-20 ℃ to remove redundant water.
Specifically, the preparation method of the humidity response color-changing hydrogel comprises the following steps:
(1) Preparing gold nano particles by a citrate reduction method: firstly, dispersing chloroauric acid aqueous solution with certain mass concentration into the aqueous solution, stirring and mixing uniformly, heating to boiling, adding sodium citrate aqueous solution, vigorously stirring for a period of time, and naturally cooling to room temperature after the reaction is finished to obtain gold nanoparticles;
(2) Surfactant-modified gold nanoparticles: centrifuging the obtained gold nanoparticles, re-dispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution, heating and refluxing for reaction for a period of time, and centrifugally washing to obtain gold nanoparticles modified by a surfactant;
(3) Humidity-responsive color-changing hydrogel preparation: firstly, mixing the obtained gold nanoparticles modified by polyvinylpyrrolidone with a certain amount of agarose, heating and stirring for reacting for a period of time, pouring the obtained solution into a mould, standing in a refrigerator for a period of time to obtain the gold nanoparticle modified hydrogel, and then freeze-drying the obtained gold nanoparticle modified hydrogel to remove excessive water to obtain the humidity response color-changing hydrogel.
In one embodiment of the invention, a humidity-responsive color-changing hydrogel prepared by the method for preparing the humidity-responsive color-changing hydrogel is provided.
The humidity response color-changing hydrogel realizes reversible color change by controlling the distance between gold nanoparticles through the dehydration expansion and contraction.
In one embodiment of the invention, the application of the humidity response color-changing hydrogel in the intelligent sensing field is provided.
The invention is further illustrated and described below in connection with specific examples.
Example 1
Preparation of humidity-responsive color-changing hydrogels
(1) Preparing gold nano particles by a citrate reduction method: firstly, dispersing 1mL of 1% chloroauric acid aqueous solution into 100mL of water, stirring for 30min to uniformly mix, heating to boiling, adding 1mL of 0.1mol/L sodium citrate aqueous solution, continuing to vigorously stir for 30s, and naturally cooling to room temperature after the reaction is finished to obtain gold nanoparticles;
(2) Preparation of surfactant modified gold nanoparticles: centrifuging the obtained gold nanoparticle aqueous solution at 15000 r/min for 30min, redispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution with the molar concentration of 1mmol/L, heating and refluxing for reaction for 12h at 120 ℃, centrifuging for 30min at the rotation speed of 15000 r/min after the reaction is finished, washing with water for three times, and redispersing the obtained product into a mixed solution of 5mL of water and 5mL of ethanol to obtain polyvinylpyrrolidone modified gold nanoparticles;
(3) Preparation of humidity-responsive color-changing hydrogel: firstly, dispersing 0.5g of agarose powder into the 10mL of polyvinylpyrrolidone modified gold nanoparticle solution obtained by stirring, stirring and heating to 90 ℃ for reaction for 1h, pouring the obtained solution into a die, standing in a refrigerator at 4 ℃ for 2h to obtain gold nanoparticle modified hydrogel, cutting the gold nanoparticle modified hydrogel to a corresponding size, and finally, freeze-drying the cut gold nanoparticle modified hydrogel at-20 ℃ for 12h to remove excessive water to obtain the humidity response color-changing hydrogel.
Example 2
(1) Preparing gold nano particles by a citrate reduction method: firstly, dispersing 1mL of aqueous solution of chloroauric acid with the mass concentration of 0.5% into 100mL of water, stirring for 30min to uniformly mix, heating to boiling, adding 1mL of aqueous solution of sodium citrate with the molar concentration of 0.05mol/L, continuing to vigorously stir for 30s, and naturally cooling to room temperature after the reaction is finished to obtain gold nanoparticles;
(2) Preparation of surfactant modified gold nanoparticles: centrifuging the obtained gold nanoparticle aqueous solution at 15000 r/min for 30min, redispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution with the molar concentration of 0.5mmol/L, heating and refluxing for reaction for 12h at 120 ℃, centrifuging for 30min at the rotation speed of 15000 r/min after the reaction is finished, washing with water for three times, and redispersing the obtained product into a mixed solution of 5mL of water and 5mL of ethanol to obtain polyvinylpyrrolidone modified gold nanoparticles;
(3) Preparation of humidity-responsive color-changing hydrogel: firstly, dispersing 0.5g of agarose powder into the 10mL of polyvinylpyrrolidone modified gold nanoparticle solution obtained by stirring, stirring and heating to 80 ℃ for reaction for 0.5h, pouring the obtained solution into a die, standing in a refrigerator at 4 ℃ for 2h to obtain gold nanoparticle modified hydrogel, cutting the gold nanoparticle modified hydrogel to a corresponding size, and finally, freeze-drying the cut gold nanoparticle modified hydrogel at-20 ℃ for 12h to remove excessive water to obtain the humidity response color-changing hydrogel.
Example 3
(1) Preparing gold nano particles by a citrate reduction method: firstly, dispersing 1mL of aqueous solution of chloroauric acid with mass concentration of 2% into 100mL of water, stirring for 30min to uniformly mix, heating to boiling, adding 1mL of aqueous solution of sodium citrate with molar concentration of 0.2mol/L, continuing to vigorously stir for 30s, and naturally cooling to room temperature after the reaction is finished to obtain gold nanoparticles;
(2) Preparation of surfactant modified gold nanoparticles: centrifuging the obtained gold nanoparticle aqueous solution at 15000 r/min for 30min, redispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution with the molar concentration of 2mmol/L, heating and refluxing at 120 ℃ for reaction for 12h, centrifuging for 30min at the rotation speed of 15000 r/min after the reaction is finished, washing with water for three times, and redispersing the obtained product into a mixed solution of 5mL of water and 5mL of ethanol to obtain polyvinylpyrrolidone modified gold nanoparticles;
(3) Preparation of humidity-responsive color-changing hydrogel: firstly, dispersing 0.5g of agarose powder into the 10mL of polyvinylpyrrolidone modified gold nanoparticle solution obtained by stirring, stirring and heating to 100 ℃ for reaction for 100h, pouring the obtained solution into a die, standing in a refrigerator at 4 ℃ for 2h to obtain gold nanoparticle modified hydrogel, cutting the gold nanoparticle modified hydrogel to a corresponding size, and finally, freeze-drying the cut gold nanoparticle modified hydrogel at-20 ℃ for 12h to remove excessive water to obtain the humidity response color-changing hydrogel.
It can be seen from fig. 1 that the humidity response color-changing hydrogel changes in color from dark purple to purple after absorbing water; as can be seen from FIG. 2, by comparing the ultraviolet spectra of the hydrogel materials under different humidity conditions, it is found that the absorption peak intensity at about 740nm gradually decreases and the absorption peak intensity at about 525nm gradually increases with the increase of humidity, and only about 740nm absorption peak disappears and only about 525nm absorption peak remains after the hydrogel is saturated with water.
Therefore, the humidity response color-changing hydrogel is successfully prepared by the preparation method, the distance between the gold nanoparticles is regulated and controlled by the hydrogel through the dehydration expansion contraction, so that the reversible color change is realized, and the method can be applied to the field of intelligent sensing.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (18)
1. A method for preparing a humidity-responsive color-changing hydrogel, comprising the steps of:
(1) Preparing gold nanoparticles by adopting a citrate reduction method;
(2) Modifying gold nanoparticles with a surfactant;
(3) Adding a hydrogel precursor into a gold nanoparticle solution modified by a surfactant to prepare humidity response color-changing hydrogel capable of rapidly generating color change;
the preparation method of the gold nanoparticles in the step (1) comprises the following steps: heating chloroauric acid aqueous solution to boiling, adding sodium citrate aqueous solution, and continuing to stir vigorously to obtain gold nanoparticles;
the step of modifying gold nanoparticles by the surfactant in the step (2) is as follows: centrifuging the gold nanoparticle aqueous solution obtained in the step (1), re-dispersing the gold nanoparticles obtained by centrifugation into polyvinylpyrrolidone aqueous solution, heating and refluxing for reaction, and re-dispersing the obtained product into ethanol solution to obtain polyvinylpyrrolidone-modified gold nanoparticles;
the hydrogel precursor in the step (3) is selected from agarose;
the mass concentration of the chloroauric acid aqueous solution is 0.5% -2%;
the molar concentration of the sodium citrate aqueous solution is 0.05-0.2 mol/L;
the volume ratio of the chloroauric acid aqueous solution to the sodium citrate aqueous solution is 90-110:1;
the mass ratio of agarose to chloroauric acid is 40-60: 1, a step of;
the concentration of the surfactant aqueous solution is 0.5-2 mmol/L.
2. The method for producing a humidity-responsive color-changing hydrogel according to claim 1, wherein the mass concentration of the aqueous chloroauric acid solution is 1%.
3. The method for preparing a humidity responsive color changing hydrogel according to claim 1, wherein the molar concentration of the aqueous sodium citrate solution is 0.1 mol/L.
4. The method for preparing a humidity responsive color changing hydrogel according to claim 1, wherein the volume ratio of aqueous chloroauric acid solution to aqueous sodium citrate solution is 100:1.
5. The method for producing a humidity-responsive color-changing hydrogel according to claim 1, wherein the concentration of the polyvinylpyrrolidone aqueous solution is 1 mmol/L.
6. The method for preparing the humidity-responsive color-changing hydrogel according to claim 1, wherein the temperature of the heating reflux reaction is 110-130 ℃ and the reaction time is 11-13 h.
7. The method for preparing a humidity responsive color changing hydrogel according to claim 1, wherein the temperature of the heat reflow reaction is 120 ℃ and the reaction time is 12 h.
8. The method for preparing a humidity-responsive color-changing hydrogel according to claim 1, wherein the centrifugation is performed for 20 to 40 minutes at 14000 to 16000 rpm.
9. The method for preparing a humidity responsive color changing hydrogel according to claim 1, wherein the centrifugation condition is 15000 rpm for 30 min.
10. The method for preparing the humidity-responsive color-changing hydrogel according to claim 1, wherein the volume fraction of the ethanol solution is 40-60%.
11. The method of preparing a humidity responsive color changing hydrogel according to claim 1, wherein the volume fraction of the ethanol solution is 50%.
12. The method for preparing the humidity-responsive color-changing hydrogel according to claim 1, wherein in the step (3), agarose powder is dispersed into the obtained polyvinylpyrrolidone-modified gold nanoparticle solution under stirring, the gold nanoparticle-modified hydrogel is obtained by stirring and heating for reaction, and the humidity-responsive color-changing hydrogel is obtained after drying.
13. The method of preparing a humidity responsive color changing hydrogel according to claim 12, wherein the agarose is present in an amount of: the mass ratio of agarose to chloroauric acid is 50:1.
14. the method for preparing the humidity-responsive color-changing hydrogel according to claim 12, wherein the temperature of the stirring and heating reaction is 80-100 ℃ and the reaction time is 0.5-1.5 h.
15. The method for preparing a humidity responsive color changing hydrogel according to claim 12, wherein the temperature of the stirring and heating reaction is 90 ℃ and the reaction time is 1 h.
16. The method for preparing the humidity response color-changing hydrogel according to claim 12, wherein the gold nanoparticle modified hydrogel is cut to a corresponding size after the gold nanoparticle modified hydrogel is obtained, and finally the cut gold nanoparticle modified hydrogel is freeze-dried.
17. A humidity-responsive color-changing hydrogel prepared by the method of preparing a humidity-responsive color-changing hydrogel according to any one of claims 1-16.
18. Use of the humidity responsive color changing hydrogel of claim 17 in the field of smart sensing.
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