CN114773533A - Hydrogel with temperature control light filtering function and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of intelligent materials, in particular to hydrogel with a temperature control light filtering function and a preparation method thereof. Comprises a polymer hydrogel and a temperature-sensitive polymer dispersed in the polymer hydrogel; the polymer hydrogel is composed of a water-soluble polymer, a cross-linking agent and water. The invention realizes the responsiveness of the filtering function to the change of the external temperature, and the hydrogel material can present different filtering functions through the change of the temperature. When the hydrogel is at low temperature, light of all wavebands above the visible light wavelength can penetrate through the hydrogel, and the light can not selectively penetrate through a specific waveband; when the temperature is raised to a specific temperature, light with the wavelength lower than a certain critical wavelength is attenuated, and light with the wavelength higher than the specific wavelength passes through the optical filter to show selective transmission of high-wavelength light, so that the optical filter material can change the optical filter band along with the change of environmental factors, and meets specific use requirements.
Description
Technical Field
The invention relates to the technical field of intelligent materials, in particular to hydrogel with a temperature control light filtering function and a preparation method thereof.
Background
Filter material refers to an optical device that selectively transmits light in different wavelength bands to select a desired wavelength band of radiation from the incident light. The filter material (sheet) has important application value in various optical equipment settings such as photography, optical sensing, optical fiber communication and the like and optical engineering. At present, the preparation principle of the optical filter material is mainly divided into two categories, wherein one category is absorption type optical filter material, which is mainly characterized in that various organic or inorganic substances with specific absorption wave bands are doped into a base material (bottom), and the second category is interference type optical filter material, which is mainly characterized in that two substances with different refractive indexes are alternately evaporated on the base material with specific thicknesses. The absorption type filter material has better durability in use, but the filter wavelength band is determined by the filter substance and cannot be accurately regulated and controlled. The interference type filtering material can accurately regulate and control the filtering wave band through the relation of the refractive index and the evaporation thickness of the evaporation material, but the preparation process is more complicated and expensive.
It is worth emphasizing that the filtering wave bands of the two types of filtering materials are completely fixed after the materials are prepared, that is, the filtering wave bands of the current filtering materials do not change with the change of environmental factors, and the filtering function of the current filtering materials is not influenced by the change of external factors such as temperature.
Disclosure of Invention
The invention aims to provide hydrogel with a temperature control light filtering function and a preparation method thereof, which are used for solving the following problems: the filtering wave band of the current filtering material can not change along with the change of environmental factors, and the change of external factors can not influence the filtering function of the current filtering material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a hydrogel with a temperature-controlled light filtering function, wherein the hydrogel comprises a polymer hydrogel and a temperature-sensitive polymer dispersed in the polymer hydrogel;
the polymer hydrogel is composed of a water-soluble polymer, a cross-linking agent and water.
Further preferably, the water-soluble polymer includes, but is not limited to, at least one of:
polyacrylamide and its copolymers, polyvinyl alcohol, polyethylene glycol and its copolymers, polyethylene oxide, polyacrylic acid and its copolymers, gelatin, xanthan gum, guar gum, starch and its derivatives, chitosan, polyvinylpyrrolidone.
Further preferably, the water content in the polymer hydrogel is 20% to 99%.
Further preferably, the temperature-sensitive polymer refers to a polymer whose solubility in water changes significantly with temperature, including but not limited to at least one of the following:
a homopolymer or copolymer of polyisopropylacrylamide, a homopolymer or copolymer of polyethylene glycol, a copolymer of diacetone acrylamide and other monomers, and hydroxypropyl cellulose.
Further preferably, the cross-linking agent includes, but is not limited to, at least one of:
methacrylate glycidyl ether, methylene bisacrylamide, ethylene glycol diacrylate, boric acid, glutaraldehyde, divinylbenzene, formaldehyde.
A preparation method of hydrogel with temperature control light filtering function is a monomer polymerization method or a polymer crosslinking method.
Further preferably, when the preparation method is a monomer polymerization method, the method comprises the following steps:
s1, dissolving a polymer monomer in water to form a solution;
s2, dissolving the temperature-sensitive polymer and the cross-linking agent in the solution according to the mass ratio
And S3, adding a free radical initiator into the solution, and initiating a system to polymerize to form the hydrogel with the temperature control light filtering function.
Further preferably, the polymer monomers include, but are not limited to, at least one of: acrylic, acrylamide, methacrylate, acrylate monomers;
the mass ratio of the polymer monomer to the cross-linking agent is 1: 0.0001-0.1;
the temperature-sensitive polymer accounts for 0.1-1.6% of the mass of the solution;
the hydrogel contains 20-99% of water by mass.
Further preferably, when the preparation method is a polymer crosslinking method, the method comprises the following steps:
s1, dissolving a water-soluble polymer and a temperature-sensitive polymer in water;
s2, adding a cross-linking agent into the solution;
and S3, forming the hydrogel with the temperature control filtering function through the occurrence of a crosslinking reaction.
Further preferably, the water-soluble polymer accounts for 5-20% of the total mass of all the components;
the temperature-sensitive polymer accounts for 0.0001-30% of the mass of all the components;
the content of the cross-linking agent is 0.0001-10%.
The invention has at least the following beneficial effects:
the invention realizes the responsiveness of the filtering function to the change of the external temperature, and the hydrogel material can present different filtering functions through the change of the temperature. When the hydrogel is at low temperature, light of all wavebands above the visible light wavelength can penetrate through the hydrogel, and the light can not selectively penetrate through a specific waveband; when the temperature is raised to a certain temperature, light with a wavelength below a certain critical wavelength is attenuated, while light with a wavelength above the certain wavelength passes through, exhibiting selective transmission of light with a high wavelength, so-called long-pass filtering. Therefore, the filter wavelength band of the filter material can be changed along with the change of environmental factors, and the specific use requirement is met.Drawings
FIG. 1 is a schematic diagram of temperature controlled filtering according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
According to a first aspect of the invention, the present disclosure provides a hydrogel capable of regulating visible light transmittance by changing temperature, having no filtering function at low temperature, and exhibiting a long-pass filtering function at high temperature.
In the invention, a typical embodiment of the hydrogel with the temperature-controlled light-filtering function is provided, and is a monomer polymerization method. The monomer polymerization method is to dissolve a polymer monomer, a temperature-sensitive polymer and a cross-linking agent in a solvent, and then add a free radical initiator to initiate polymerization, wherein the polymer monomer is acrylamide, the temperature-sensitive polymer is a copolymer of diacetone acrylamide and acrylamide, the cross-linking agent is methylene bisacrylamide, and the free radical initiator is a ceric ammonium nitrate/sodium bisulfite redox system.
First, the present invention discloses that a crosslinked polymer hydrogel has a transparent property. The invention discloses a method for preparing hydrogel, which comprises the steps of adding a temperature-sensitive polymer in the synthesis process, wherein the solubility of the temperature-sensitive polymer in water is obviously changed along with the change of temperature, compounding a conventional hydrogel and the temperature-sensitive polymer to change the skeleton property of the hydrogel, wherein when the temperature is lower than the Lowest Critical Solution Temperature (LCST) of the polymer, the polymer can be well dissolved in the water in a molecular form, the hydrogel is in a transparent state on a macroscopic scale, and when the temperature is higher than the LCST, the polymer is insoluble in water, molecular chains collapse and are dispersed in the hydrogel in a microsphere form, and the hydrogel is white and poor in transparency on the macroscopic scale due to the strong light scattering phenomenon of microspheres in the hydrogel. Third, the present invention discloses that the volume shrinkage before and after the phase transition of the hydrogel can be effectively suppressed.
In one or more embodiments of this embodiment, the mass ratio of the polymer monomer acrylamide to the crosslinking agent is 1: 0.001 to 0.02.
In one or more embodiments of the present disclosure, the content (mass content) of the temperature-sensitive polymer in the system is 0.1% to 1.6%.
In one or more examples of this embodiment, the water content (mass content) of the polymer hydrogel is 80% to 95%.
In one or more embodiments of this embodiment, the initiator in the polymer hydrogel is a cerium ammonium nitrate/sodium bisulfite redox system.
In one or more embodiments of this embodiment, the mass ratio of the polymer monomer acrylamide to the initiator is 1: 0.001 to 0.015.
Another embodiment disclosed herein is a method of crosslinking a polymer. The polymer crosslinking method is to dissolve a water-soluble polymer, a temperature-sensitive polymer and a crosslinking agent in a solvent for crosslinking, wherein the water-soluble polymer is guar gum, the temperature-sensitive polymer is a copolymer of diacetone acrylamide and acrylamide, and the crosslinking agent is boric acid.
In one or more examples of this embodiment, the water soluble polymer guar is present in the system at a level (mass fraction) of 5% to 20%.
In one or more embodiments of this embodiment, the content (mass content) of the temperature-sensitive polymer in the system is 0.1% to 1.6%.
In one or more embodiments of this embodiment, the boric acid is present in the system at a level of 0.01% to 1%.
In order to make the technical solutions of the present disclosure more clearly understood by those skilled in the art, the technical solutions of the present disclosure will be described in detail below with reference to specific examples and comparative examples.
Example 1
1. 1.11g of acrylamide is weighed and added into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), and the solution is promoted to be dissolved by ultrasonic oscillation for 5min in an ultrasonic cleaner at the power of 40KHz at room temperature.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-control light-filtering hydrogel which is marked as FDAM-0.001-AM-10% -MBA-0.
Example 2
1. Weighing 1.11g of acrylamide, adding the acrylamide into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), adding 0.0045g of cross-linking agent methylene bisacrylamide, and ultrasonically oscillating for 5min at 40KHz power in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-control light-filtering hydrogel which is marked as FDAM-0.001-AM-10% -MBA-0.0045.
Example 3
1. Weighing 1.11g of acrylamide, adding the acrylamide into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), adding 0.0100g of cross-linking agent methylene bisacrylamide, and ultrasonically oscillating for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-controlled light-filtering hydrogel which is marked as FDAM-0.001-AM-10% -MBA-0.0100.
Example 4
1. 1.11g of acrylamide is weighed and added into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), 0.0156g of cross-linking agent methylene bisacrylamide is added, and the solution is accelerated to dissolve by ultrasonic oscillation for 5min in an ultrasonic cleaner at the power of 40KHz at room temperature.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the prepolymerized solution into a mold, and reacting completely to obtain the temperature-controlled light-filtering hydrogel which is marked as FDAM-0.001-AM-10% -MBA-0.0156.
Example 5
1. Weighing 1.11g of acrylamide, adding the acrylamide into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), adding 0.0222g of cross-linking agent methylene bisacrylamide, and ultrasonically oscillating for 5min at 40KHz power in an ultrasonic cleaner at room temperature to promote dissolution.
2. And after the solutions are uniformly mixed, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-controlled light-filtering hydrogel which is marked as FDAM-0.001-AM-10% -MBA-0.0222.
Example 6
1. Weighing 0.53g of acrylamide, adding the acrylamide into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), adding 0.0100g of cross-linking agent methylene bisacrylamide, and ultrasonically oscillating for 5min at the power of 40KHz in an ultrasonic cleaning machine at room temperature to promote dissolution.
2. After the above solutions were mixed uniformly, 0.0005g of ammonium cerium nitrate and 0.0010g of sodium hydrogen sulfite as initiators were added, and prepolymerization was carried out after uniform mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-controlled light-filtering hydrogel which is marked as FDAM-0.001-MBA-0.0100-AM-5%.
Example 7
1. 2.00g of acrylamide is weighed and added into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), 0.0100g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solution is mixed evenly, 0.0020g of initiator ammonium ceric nitrate and 0.0040g of initiator sodium bisulfite are added, and prepolymerization is carried out after even mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-controlled light-filtering hydrogel which is marked as FDAM-0.001-MBA-0.0100-AM-15%.
Example 8
1. 2.50g of acrylamide is weighed and added into 10mL of temperature-sensitive polymer solution (the mass fraction is 0.001), 0.0100g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solution is mixed evenly, 0.0025g of initiator ammonium ceric nitrate and 0.0050g of initiator sodium bisulfite are added, and prepolymerization is carried out after even mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-controlled light-filtering hydrogel which is marked as FDAM-0.001-MBA-0.0100-AM-20%.
Example 9
1. 1.11g of acrylamide and 0.02g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the hydrogel with the temperature control light filtering function, which is marked as AM-10% -MBA-0.0150-FDAM-0.02.
Example 10
1. 1.11g of acrylamide and 0.04g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. And after the solutions are uniformly mixed, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the prepolymerized solution into a mold, and reacting completely to obtain the hydrogel with the temperature-controlled light-filtering function, which is marked as AM-10% -MBA-0.0150-FDAM-0.04.
Example 11
1. 1.11g of acrylamide and 0.08g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the prepolymerized solution into a mold, and reacting completely to obtain the hydrogel with the temperature-controlled light-filtering function, which is marked as AM-10% -MBA-0.0150-FDAM-0.08.
Example 12
1. 1.11g of acrylamide and 0.16g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the prepolymerized solution into a mold, and reacting completely to obtain the hydrogel with the temperature-controlled light-filtering function, which is marked as AM-10% -MBA-0.0150-FDAM-0.16.
Example 13
1. 1.11g of acrylamide and 0.04g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the solutions are mixed uniformly, 0.0011g of initiator ammonium ceric nitrate and 0.0022g of initiator sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the prepolymerized solution into a mold, and reacting completely to obtain the hydrogel with the temperature-control light-filtering function, wherein the hydrogel is marked as AM-10% -MBA-0.0150-FDAM-0.04-initiator-0.0030.
Example 14
1. 1.11g of acrylamide and 0.04g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. After the above solutions were mixed well, 0.0017g of ammonium ceric nitrate and 0.0034g of sodium bisulfite as initiators were added, and prepolymerization was carried out after mixing well.
3. And transferring the pre-polymerized solution into a mold, and reacting completely to obtain the temperature-control light-filtering hydrogel which is marked as AM-10% -MBA-0.0150-FDAM-0.04-initiator-0.0046.
Example 15
1. 1.11g of acrylamide and 0.04g of temperature-sensitive polymer are weighed and added into 10mL of deionized water, 0.0150g of cross-linking agent methylene bisacrylamide is added, and the mixture is ultrasonically vibrated for 5min at the power of 40KHz in an ultrasonic cleaner at room temperature to promote dissolution.
2. And after the solutions are uniformly mixed, 0.0022g of initiator ammonium ceric nitrate and 0.0044g of sodium bisulfite are added, and prepolymerization is carried out after uniform mixing.
3. And transferring the prepolymerized solution into a mold, and reacting completely to obtain the hydrogel with the temperature control light filtering function, which is marked as AM-10% -MBA-0.0150-FDAM-0.04-initiator-0.0060. A (c)
FIG. 1 is a schematic view of temperature-controlled filtering of the material prepared by the present invention in FIG. 1
As can be seen in fig. 1 in conjunction with the above description and the drawings attached to the description:
the invention realizes the responsiveness of the filtering function to the change of the external temperature, and the hydrogel material can present different filtering functions through the change of the temperature; at low temperature, the hydrogel can transmit light of all wave bands above the wavelength of visible light, and can not selectively transmit light of specific wave bands. When the temperature is raised to a certain temperature, light with a wavelength below a certain critical wavelength is attenuated, while light with a wavelength above the certain wavelength passes through, exhibiting selective transmission of light with a high wavelength, so-called long-pass filtering. The critical wavelength can be regulated and controlled between 300nm and 700nm, and the transition temperature can be regulated and controlled between 5 ℃ and 90 ℃.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A hydrogel with a temperature-control light-filtering function is characterized in that the hydrogel comprises a polymer hydrogel and a temperature-sensitive polymer dispersed in the polymer hydrogel;
the polymer hydrogel is composed of a water-soluble polymer, a cross-linking agent and water.
2. The hydrogel according to claim 1, wherein the water-soluble polymer includes but is not limited to at least one of the following:
polyacrylamide and its copolymers, polyvinyl alcohol, polyethylene glycol and its copolymers, polyethylene oxide, polyacrylic acid and its copolymers, gelatin, xanthan gum, guar gum, starch and its derivatives, chitosan, polyvinylpyrrolidone.
3. The hydrogel with temperature-controlled optical filtering function according to claim 1, wherein the hydrogel has a water content of 20% to 99%.
4. The hydrogel with temperature-controlled optical filtering function according to claim 1, wherein the temperature-sensitive polymer is a polymer whose solubility in water changes with temperature, and includes but is not limited to at least one of the following:
a homopolymer or copolymer of polyisopropylacrylamide, a homopolymer or copolymer of polyethylene glycol, a copolymer of diacetone acrylamide and other monomers, and hydroxypropyl cellulose.
5. The hydrogel according to claim 1, wherein the cross-linking agent includes but is not limited to at least one of the following:
methacrylate glycidyl ether, methylene bisacrylamide, ethylene glycol diacrylate, boric acid, glutaraldehyde, divinylbenzene, formaldehyde.
6. A preparation method of hydrogel with temperature control light filtering function is characterized in that the preparation method is a monomer polymerization method or a polymer crosslinking method.
7. The method for preparing the hydrogel with temperature-controlled optical filtering function according to claim 6, wherein when the preparation method is a monomer polymerization method, the method comprises the following steps:
s1, dissolving a polymer monomer in water to form a solution;
s2, dissolving the temperature-sensitive polymer and the cross-linking agent in the solution according to the mass ratio
And S3, adding a free radical initiator into the solution, and initiating a system to polymerize to form the hydrogel with the temperature control light filtering function.
8. The method according to claim 7, wherein the polymer monomers include but are not limited to at least one of the following: acrylic, acrylamide, methacrylate, acrylate monomers;
the mass ratio of the polymer monomer to the cross-linking agent is 1: 0.0001-0.1;
the temperature-sensitive polymer accounts for 0.0001-30% of the solution by mass;
the hydrogel contains 20-99% of water by mass.
9. The method as claimed in claim 6, wherein the method for preparing the hydrogel with temperature-controlled optical filtering function is a polymer crosslinking method, comprising the following steps:
s1, dissolving a water-soluble polymer and a temperature-sensitive polymer in water;
s2, adding a cross-linking agent into the solution;
and S3, forming the hydrogel with the temperature control light filtering function through the occurrence of a crosslinking reaction.
10. The method according to claim 9, wherein the water-soluble polymer is 5-20% of all the components by mass;
the temperature-sensitive polymer accounts for 0.0001-30% of the mass of all the components;
the content of the cross-linking agent is 0.0001-10%.
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