CN114044924A - Temperature-sensitive color-changing hydrogel and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of temperature-sensitive color-changing materials, and particularly relates to a temperature-sensitive color-changing hydrogel and a preparation method thereof. The preparation method comprises the following steps of preparing a solution A: dissolving a color-changing agent and a polymer in water to obtain a solution A; preparation of solution B: dissolving a cross-linking agent in water to obtain a solution B; preparing a hydrogel: and mixing and crosslinking the solution A and the solution B to obtain the hydrogel. The invention adopts the polymer, the cross-linking agent and the color-changing agent as raw materials, and prepares the temperature-sensitive color-changing hydrogel through chemical cross-linking, so that the preparation method is simpler and more convenient. The solubility of the color-changing agent in water changes along with the change of temperature, crystals are separated out at low temperature, and the hydrogel integrally presents opaque white; the color-changing agent is completely dissolved in water at high temperature, the hydrogel is transparent and the process is reversible. In addition, the temperature range and speed of the hydrogel color change can be conveniently controlled by adjusting the content of the color change agent.
Description
Technical Field
The invention belongs to the technical field of temperature-sensitive color-changing materials, and particularly relates to a temperature-sensitive color-changing hydrogel and a preparation method thereof.
Background
The hydrogel is a hydrophilic material with a three-dimensional network structure, can rapidly swell in water and store a large amount of water, and is widely applied to the fields of agriculture, medical treatment, buildings and the like. According to the response condition of the hydrogel to external stimuli, the hydrogel can be divided into two categories of traditional hydrogel and environment-sensitive hydrogel. Among them, the hydrogel sensitive to the environment generally has a specific change with the environmental temperature, pH, humidity, etc., and has important applications in many fields.
The temperature-sensitive hydrogel is a common and very important functional hydrogel, can generate reversible changes such as color and form along with the change of the environmental temperature, and has good application prospect in the aspects of temperature detection, glass production, brakes and the like.
The temperature-sensitive allochroic hydrogel comprises 0.1-2% of sodium alginate by mass, 1-20% of a polymerization monomer by mass, 0.1-1% of a cross-linking agent by mass, 0.1-1% of an initiator by mass, 0.1-3% of a divalent metal salt by mass, 0.1-3% of a temperature-sensitive block material by mass, 0.1-3% of a surfactant by mass and the balance of deionized water.
However, the preparation process of the method is complex, and the color-changing agent is an organic raw material, so that the method is high in price and is not environment-friendly.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the preparation method in the prior art is complicated, and the color-changing agent is organic and is not environment-friendly, thereby providing the temperature-sensitive color-changing hydrogel and the preparation method thereof.
Therefore, the invention provides the following technical scheme.
The invention provides a preparation method of temperature-sensitive color-changing hydrogel, which comprises the following steps:
preparation of solution a: dissolving a color-changing agent and a polymer in water to obtain a solution A;
preparation of solution B: dissolving a cross-linking agent in water to obtain a solution B;
preparing a hydrogel: and mixing and crosslinking the solution A and the solution B to obtain the hydrogel.
Optionally, the mixing and crosslinking are performed under stirring conditions, and the stirring time is 1-30 s.
Optionally, the hybrid crosslinking step is followed by a degassing step;
optionally, the temperature of the degassing step is 90-100 ℃, and the degassing time is 1-5 h.
Optionally, the mass ratio of the toner, the polymer and the water in the solution A is (0.1-1.5): (3-6): (80-100); the mass ratio of the cross-linking agent to the water in the solution B is (1-10): (90-100).
Optionally, the mass ratio of the polymer to the cross-linking agent is (3-6): (0.1-1).
Optionally, the color-changing agent is one of sodium chloride, potassium chloride and ammonium chloride. It can also be selected to meet the condition of inorganic salt which has certain solubility in water, has larger change of solubility along with temperature and does not react with the polymer and the crosslinking agent.
The polymer is typically, but not limited to, one of polyvinyl alcohol and polyethyleneimine; it can also select polyfunctional group organic matter which can react with a certain cross-linking agent to form a three-dimensional grid structure.
For example, the polyvinyl alcohol may be type 1799. The weight average molecular weight of the water solution with the mass fraction of 50% of polyethyleneimine is as follows: 50000-70000.
The cross-linking agent is typically, but not limited to, one of borax, magnesium chloride, and glutaraldehyde. It can also select the polyfunctional group organic matter condition which can make the polymer produce cross-linking reaction to form three-dimensional grid structure.
Optionally, the heating temperature in the step of preparing the solution A is 85-95 ℃; the stirring time is 1-3 h.
Optionally, the heating temperature in the step of preparing the solution B is 50-70 ℃; the stirring time is 0.5-1 h.
The invention also provides the temperature-sensitive color-changing hydrogel prepared by the preparation method.
The technical scheme of the invention has the following characteristics:
1. the preparation method of the temperature-sensitive color-changing hydrogel provided by the invention comprises the following steps of: dissolving a color-changing agent and a polymer in water to obtain a solution A; preparation of solution B: dissolving a cross-linking agent in water to obtain a solution B; preparing a hydrogel: and mixing and crosslinking the solution A and the solution B to obtain the hydrogel. The invention adopts the polymer, the cross-linking agent and the color-changing agent as raw materials, and prepares the temperature-sensitive color-changing hydrogel through chemical cross-linking, so that the preparation method is simpler and more convenient. Wherein the polymer and the cross-linking agent are cross-linked to form a three-dimensional network structure having a network of voids, and a substantial amount of water and color-changing agent are present in the network. The solubility of the color-changing agent in water changes along with the change of temperature, crystals are separated out at low temperature, and the hydrogel integrally presents opaque color; the color-changing agent is completely dissolved in water at high temperature, and the hydrogel is transparent. The process is reversible, the contents of the color-changing agents are different, the color-changing temperature and speed are different, and the temperature range and speed of the hydrogel color change can be conveniently controlled by adjusting the contents of the color-changing agents.
2. According to the preparation method of the temperature-sensitive color-changing hydrogel, a degassing step is further included after the mixing and crosslinking step; optionally, the temperature of the degassing step is 90-100 ℃, and the degassing time is 1-5 h. Wherein, the stirring process can make A, B solution misce bene, and each part of product discolour the effect unanimously, avoids because of the cross-linking reaction is too fast, and the unable even diffusion of discolour agent gets into the cross-linking net to each part of product is inhomogeneous. The bubbles mixed in the product can be removed by high-temperature heating, so that the good quality and the transparent color of the product are ensured.
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, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a picture at 90 degrees Celsius of the product prepared in example 2;
FIG. 2 is a picture at 25 degrees Celsius of the product prepared in example 2;
FIG. 3 is a graph of light transmittance at 25 degrees Celsius for the product prepared in example 8;
FIG. 4 is a graph of light transmittance at 90 degrees Celsius for the product prepared in example 8;
figure 5 is a picture at 90 degrees celsius of the product prepared in example 7.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
To facilitate comparison of the data, the polyvinyl alcohol and polyethyleneimine used in the following examples of the present invention were of the same specifications as follows:
the polyvinyl alcohol is 1799 type, offered by Shanghai Allantin Biotechnology Co., Ltd;
the polyethyleneimine is 50% aqueous solution by mass and is provided by Shanghai Allantin Biotechnology Co., Ltd.
Example 1
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.1g of sodium chloride, 6g of polyvinyl alcohol and 100g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 90 ℃, stirring for 3 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 10g of borax and 90g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating to 60 ℃, stirring for 0.5h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into the beaker A, stirring for 10s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 2 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 30 ℃ and white below 30 ℃.
Example 2
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.5g of sodium chloride, 5g of polyvinyl alcohol and 100g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 95 ℃, stirring for 2 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 5g of borax and 95g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating to 70 ℃, stirring for 0.5h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into a beaker A, stirring for 30s, and then putting the beaker A into a water bath kettle for heating at 90 ℃ for 3 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 60 ℃ and white below 60 ℃.
Example 3
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.5g of sodium chloride, 5g of polyvinyl alcohol and 90g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 95 ℃, stirring for 3 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 5g of borax and 90g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating to 70 ℃, stirring for 0.5h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into a beaker A, stirring for 2s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 4 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 60 ℃ and white below 60 ℃.
Example 4
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.1g of sodium chloride, 3g of polyvinyl alcohol and 90g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 85 ℃, stirring for 3 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 10g of borax and 90g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating at 60 ℃, stirring for 1h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into a beaker A, stirring for 20s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 4 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 30 ℃ and white below 30 ℃.
Example 5
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.25g of sodium chloride, 6g of polyvinyl alcohol and 100g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 95 ℃, stirring for 3 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 1g of borax and 100g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating to 60 ℃, stirring for 0.5h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into a beaker A, stirring for 25s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 4 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 40 ℃ and white below 40 ℃.
Example 6
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 1g of sodium chloride, 6g of polyvinyl alcohol and 100g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 90 ℃, stirring for 2 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 10g of borax and 90g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating at 60 ℃, stirring for 1h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into a beaker A, stirring for 30s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 5 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 80 ℃ and white below 80 ℃.
Example 7
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.1g of sodium chloride, 3g of polyvinyl alcohol and 90g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 85 ℃, stirring for 3 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 10g of borax and 90g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating at 60 ℃, stirring for 1h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
pouring 10g of borax solution into a beaker A, stirring for 20s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 1 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 30 ℃ and white below 30 ℃.
Example 8
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.75g of sodium chloride, 6g of polyvinyl alcohol and 90g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 95 ℃, stirring for 2 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 5g of glutaraldehyde and 100g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating at 80 ℃, stirring for 0.5h, and stopping stirring after the glutaraldehyde is completely dissolved to obtain a glutaraldehyde solution;
pouring 10g of glutaraldehyde solution into a beaker A, stirring for 25s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 5 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 70 ℃ and white below 70 ℃.
Example 9
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.1g of ammonium chloride, 6g of polyethyleneimine and 90g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 95 ℃, stirring for 2 hours, and stopping stirring after the polyethyleneimine is completely dissolved to obtain a polyethyleneimine-sodium chloride solution;
putting 5g of magnesium chloride and 100g of purified water into a beaker B, stirring for 0.5h, and stopping stirring after the magnesium chloride is completely dissolved to obtain a magnesium chloride solution;
pouring 10g of magnesium chloride solution into the beaker A, stirring for 25s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 5 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 30 ℃ and white below 30 ℃.
Example 10
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
putting 0.1g of potassium chloride, 6g of polyethyleneimine and 90g of purified water into a beaker A, putting the beaker A into a water bath kettle for heating, wherein the heating temperature is 95 ℃, stirring for 2 hours, and stopping stirring after the polyethyleneimine is completely dissolved to obtain a polyethyleneimine-sodium chloride solution;
putting 5g of magnesium chloride and 100g of purified water into a beaker B, stirring for 0.5h, and stopping stirring after the magnesium chloride is completely dissolved to obtain a magnesium chloride solution;
pouring 10g of magnesium chloride solution into the beaker A, stirring for 25s, and then putting the beaker A into a water bath kettle for heating at the temperature of 95 ℃ for 5 h. And obtaining the temperature-sensitive color-changing hydrogel after heating. The hydrogel is transparent above 35 ℃ and white below 35 ℃.
Example 11
The embodiment provides a preparation method of a temperature-sensitive color-changing hydrogel, which comprises the following steps:
placing 0.1g of sodium chloride, 6g of polyvinyl alcohol and 100g of purified water in a beaker A, placing the beaker A in a water bath kettle for heating, wherein the heating temperature is 90 ℃, stirring for 3 hours, and stopping stirring after the polyvinyl alcohol is completely dissolved to obtain a polyvinyl alcohol-sodium chloride solution;
putting 10g of borax and 90g of purified water into a beaker B, putting the beaker B into a water bath kettle, heating to 60 ℃, stirring for 0.5h, and stopping stirring after the borax is completely dissolved to obtain a borax solution;
and pouring 10g of borax solution into the beaker A, stirring for 10s, and obtaining the temperature-sensitive color-changing hydrogel after stirring. The hydrogel is transparent above 30 ℃ and white below 30 ℃.
Performance testing
The hydrogel prepared in the embodiments 1 to 11 is subjected to performance tests, and specifically includes the light transmittance of the hydrogel, the temperature-sensitive color-changing effect of the hydrogel, and the bubble content in the hydrogel.
The hydrogel light transmittance test method is to measure the transmittance by using an ultraviolet-visible spectrophotometer, and the test temperature is 25 ℃.
The method for testing the temperature-sensitive color-changing effect of the hydrogel comprises the following steps: the color-changing hydrogel provided by the embodiment of the invention and the comparative example is heated to 90 ℃ from room temperature by an oven, the heating rate is 5 ℃/min, then, the hydrogel is naturally cooled, and the time from the beginning of temperature reduction to the complete whitening is recorded, wherein the color-changing time is slow when more than 60min, the color-changing time is slow when 40-60min, the color-changing time is fast when 10-20min, and the color-changing time is fast when 0-10 min.
The method for testing the bubble content of the hydrogel comprises observing the distribution quantity of bubbles in a unit area through a microscope, wherein the bubble content is 0-2/cm2Is "small", and the content of bubbles is 2/cm2The above is "much".
The test results are given in the following table:
TABLE 1
| Light transmittance (%) | Temperature sensitive time (min) | Bubble content (pieces/cm)-1) | |
| Example 1 | 99 | 160 | 2 |
| Example 2 | 98 | 30 | 1 |
| Example 3 | 99 | 30 | 0 |
| Example 4 | 96 | 150 | 0 |
| Example 5 | 97 | 60 | 0 |
| Example 6 | 99 | 10 | 0 |
| Example 7 | 97 | 160 | 40 |
| Example 8 | 95 | 20 | 0 |
| Example 9 | 99 | 130 | 0 |
| Example 10 | 98 | 100 | 0 |
| Example 11 | 99 | 150 | 60 |
As can be seen from the above table, when the content of the color-changing agent is too low, the color-changing speed of the hydrogel is slow; with the increase of the content of the color-changing agent, the temperature sensitivity of the hydrogel is enhanced, the color-changing speed is accelerated, and the temperature-sensitive color-changing characteristic can be changed by adjusting the content of the color-changing agent; after the hydrogel is crosslinked, a long-time high-temperature bubble removing process is needed, otherwise, a product contains a large number of bubbles, and the appearance is affected.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of temperature-sensitive color-changing hydrogel is characterized by comprising the following steps:
preparation of solution a: dissolving a color-changing agent and a polymer in water to obtain a solution A;
preparation of solution B: dissolving a cross-linking agent in water to obtain a solution B;
preparing a hydrogel: and mixing and crosslinking the solution A and the solution B to obtain the hydrogel.
2. The method of claim 1, wherein the mixing and crosslinking are performed under stirring for 1-30 s.
3. The method for preparing the temperature-sensitive color-changing hydrogel according to claim 1 or 2, wherein the step of mixing and crosslinking is further followed by a step of degassing;
optionally, the temperature of the degassing step is 90-100 ℃, and the degassing time is 1-5 h.
4. The method for preparing the temperature-sensitive color-changing hydrogel according to claim 1, wherein the mass ratio of the toner, the polymer and the water in the solution A is (0.1-1.5): (3-6): (80-100);
the mass ratio of the cross-linking agent to the water in the solution B is (1-10): (90-100).
5. The method for preparing the temperature-sensitive color-changing hydrogel according to claim 1, wherein the mass ratio of the polymer to the cross-linking agent is (3-6): (0.1-1).
6. The method of claim 1, wherein the color-changing agent is one of sodium chloride, potassium chloride and ammonium chloride.
7. The method for preparing the temperature-sensitive color-changing hydrogel according to claim 1, wherein the polymer is one of polyvinyl alcohol and polyethyleneimine;
the cross-linking agent is one of borax, magnesium chloride and glutaraldehyde.
8. The method for preparing the temperature-sensitive color-changing hydrogel according to claim 1, wherein the heating temperature in the step of preparing the solution A is 85-95 ℃; the stirring time is 1-3 h.
9. The method for preparing the temperature-sensitive color-changing hydrogel according to claim 1, wherein the heating temperature in the step of preparing the solution B is 50-70 ℃; the stirring time is 0.5-1 h.
10. A temperature-sensitive color-changing hydrogel prepared by the preparation method according to any one of claims 1 to 9.
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