CN112831061A - Preparation method of copper nanowire composite organic hydrogel - Google Patents
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Abstract
The invention discloses a preparation method of copper nanowire composite organic hydrogel, which is characterized in that a nano material forms the nano composite hydrogel through free radical polymerization reaction, dynamic cross-linking between ions and supermolecule action between the nano material and a polymer in the presence of a polymerizable monomer, and then is soaked in an organic solvent for solvent replacement to finally obtain the nano composite organic hydrogel so as to obtain the composite organic hydrogel with low temperature resistance, excellent mechanical property and excellent electrical property.
Description
Technical Field
The invention relates to a preparation method of copper nanowire composite organic hydrogel, belonging to the technical field of nano materials.
Background
Stretchable elastic conductor materials are a new class of advanced materials, which can be applied in a variety of fields. Over the past few years, significant advances have been made in designing flexible conductors from different materials, including carbon nanotubes, metal nanoparticles, semiconductor nanostructures, graphene, conductive polymers, metal oxides, metal nanowires, and the like. Despite the significant advances, in downstream applications, certain of the materials described above will inevitably face cost or quantity deficiencies. For example, the success of flexible conductors based on metallic nanomaterials is mainly limited to precious gold or silver nanowires. Copper nanowires (CuNWs) not only have excellent performance, but also can provide cost advantages for commercial applications of flexible conductors due to the high copper content on earth. The superior electrical properties of CuNWs result due to the high intrinsic bulk conductivity of copper as compared to the less expensive commercial conductive fillers (e.g., carbon black).
The concept of nanocomposite hydrogel was first proposed by the 2002 japanese scientist t.takehisa, and the mechanical properties of the hydrogel formed by the method using clay plate nano-material as a crosslinking agent are further improved. Conductive hydrogels have attracted great interest in the field of flexible and wearable soft strain sensors due to their great potential in electronic skin and personalized healthcare. However, the conventional conductive hydrogel using pure water as a dispersion medium inevitably freezes at a temperature lower than zero, resulting in a decrease in its electrical conductivity and mechanical properties. Meanwhile, even at room temperature, such hydrogels inevitably lose moisture due to evaporation, resulting in poor shelf life, and these characteristics of the conventional conductive hydrogels severely limit their applications in extreme environments.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of copper nanowire composite organic hydrogel, which achieves the aim of preventing freezing by replacing part of water molecules with glycol solvent so as to obtain the composite organic hydrogel which is anti-freezing and has excellent mechanical property and electrical property.
The preparation method of the copper nanowire composite organic hydrogel comprises the steps of forming the nano composite hydrogel through free radical polymerization reaction, dynamic cross-linking between ions and supermolecule action between the nano material and a polymer under the condition that a polymerizable monomer exists in the nano material, and then soaking the nano composite hydrogel in an organic solvent for solvent replacement to finally obtain the nano composite organic hydrogel.
The preparation method of the copper nanowire composite organic hydrogel comprises the following steps:
step 1: firstly, sequentially adding 0.84g of copper chloride dihydrate and 0.99g of glucose into 400mL of deionized water solution, adding 5.4g of hexadecylamine into the mixture under the stirring of a magnetic stirrer at 600rpm, and finally stirring the mixture to a homogeneous light blue emulsion state; and then pouring the mixture into a polytetrafluoroethylene container, reacting at the high temperature of 120 ℃ for 8 hours, cooling to room temperature, sequentially carrying out centrifugal washing by using normal-temperature water and hot water at the temperature of 65 ℃, wherein the centrifugal rotating speed and the centrifugal time are 9000rpm and 6min respectively, and finally obtaining a reddish-brown copper nanowire solution with the concentration of 20 mg/mL.
In step 1, the length of the synthesized copper nanowire is 60-70 μm, and the diameter is 70-90 nm.
Step 2: sequentially adding a monomer, a polymer, a cross-linking agent and an initiator into the copper nanowire solution prepared in the step (1) under the protection of nitrogen, ultrasonically mixing, then placing in a vacuum drying oven to remove bubbles contained in the dispersion liquid, controlling the pH value and optimizing the pH value to be 8-10, and dropwise adding a sodium tetraborate aqueous solution under magnetic stirring until gel is obtained; in-situ polymerizing at 60 deg.c for 5 hr, and cooling to room temperature to obtain the hydrogel substrate.
In the step 2, the monomer is acrylamide, and the addition mass of the monomer is 5-20% of the mass of the copper nanowire solution obtained in the step 1.
In the step 2, the cross-linking agent is methylene bisacrylamide, and the addition mass of the cross-linking agent is 0.02-0.06% of the mass of the copper nanowire solution obtained in the step 1.
In the step 2, the initiator is 2,2' -azobis [2- (2-imidazoline-2-yl) propane ] dihydrochloride, and the addition mass of the initiator is 0.2-0.6% of the mass of the copper nanowire solution obtained in the step 1.
In the step 2, the polymer is polyvinyl alcohol aqueous solution, the mass concentration is 10 wt%, and the adding mass of the polymer is 3-8% of the mass of the copper nanowire solution obtained in the step 1.
In the step 2, the adding mass of the sodium tetraborate is 0.3-0.6% of the mass of the copper nanowire solution obtained in the step 1.
And step 3: and (3) soaking the hydrogel substrate obtained in the step (2) in an organic solvent for 4 hours, and removing the surface solvent by using filter paper to obtain the final organic hydrogel.
In step 3, the organic solvent is ethylene glycol.
Different copper wire concentrations have different conductivities, and as a nano material, within a certain range, along with the increase of the copper nanowire concentration, the mechanical property of the composite gel can be relatively improved, so that the composite gel has more excellent mechanical and electrical properties.
The invention has the beneficial effects that:
the invention adopts a preparation method of double-network cooperative strengthening hydrogel when preparing the nano-composite organic hydrogel, firstly, the dynamic crosslinking between polyvinyl alcohol and tetrahydroxy borate ions forms a double-network structure with a polyacrylamide network, and then the double-network structure is soaked in ethylene glycol solution, so that supermolecule action exists among ethylene glycol, polyvinyl alcohol and copper nanowires. Therefore, through the synergistic effect of the double networks, the organic hydrogel has excellent mechanical properties and electrical stability at a lower temperature.
In conclusion, the invention provides a brand-new preparation method of the copper nanowire composite double-network organic hydrogel. The invention provides a brand new thought and theoretical basis for the nano material composite organic hydrogel. Meanwhile, due to a network formed by the copper nano material, the organic hydrogel prepared by the invention has good application prospect in the fields of elastic problems and the like.
Drawings
Fig. 1 is a scanning electron micrograph of copper nanowires prepared according to the present invention. It can be seen from fig. 1 that the copper nanowire solution prepared by the present invention is uniformly dispersed.
FIG. 2 is a drawing of a nanocomposite hydrogel prepared according to the present invention and an optical photograph during the drawing. It can be seen from FIG. 2 that the hydrogel prepared by the present invention has good extensibility, i.e., has good elasticity.
FIG. 3 is a graph of a drawing cycle for a nanocomposite hydrogel prepared according to the present invention. It can be seen from fig. 3 that the nanocomposite hydrogel prepared by the present invention has a low modulus loss during the stretching process, i.e., has good mechanical stability.
FIG. 4 is a graph of the change in resistance during the stretching cycle of the nanocomposite hydrogel prepared in accordance with the present invention. It can be seen from fig. 4 that the nanocomposite hydrogel prepared according to the present invention has stable resistance change during the stretching cycle, i.e., has excellent electrical stability.
FIG. 5 is a circuit diagram of a nanocomposite hydrogel and a nanocomposite organic hydrogel prepared by the present invention, respectively, in series with an LED indicator at low temperature. It can be seen from fig. 4 that the nanocomposite organic hydrogel prepared by the present invention maintains conductivity at low temperature.
Detailed Description
The following examples illustrate the invention in detail. The reagent raw materials and equipment used in the invention are all commercially available products and can be purchased in the market.
Example 1:
1. and synthesizing a copper nanowire solution with the concentration of 20 mg/mL. Firstly, sequentially adding 0.84g of copper chloride dihydrate and 0.99g of glucose into 400mL of deionized water solution, adding 5.4g of hexadecylamine into the mixture under the stirring of a magnetic stirrer at 600rpm, and finally stirring the mixture to a homogeneous light blue emulsion state; and then pouring the mixture into a polytetrafluoroethylene container, reacting for 8 hours at a high temperature of 120 ℃, cooling to room temperature, and sequentially carrying out centrifugal washing by using water and hot water at a temperature of 65 ℃, wherein the centrifugal rotation speed and the centrifugal time are 9000rpm and 6min respectively, so as to finally obtain the reddish-brown copper nanowire solution.
2. Acrylamide accounting for 5-20% of the mass of the copper nanowire solution, polyvinyl alcohol aqueous solution accounting for 3-8% of the mass of the copper nanowire solution, methylene bisacrylamide accounting for 0.02-0.06% of the mass of the copper nanowire solution and 2,2' -azobis [2- (2-imidazoline-2-yl) propane ] dihydrochloride accounting for 0.2-0.6% of the mass of the copper nanowire solution are sequentially added into the copper nanowire solution, and the mixture is uniformly stirred before the next medicine is added each time. The whole process is completed under the protection of nitrogen, and the flow rate of the nitrogen is controlled to be 0.5 mL/s. The mixture was ultrasonically mixed and then placed in a vacuum drying oven to remove air bubbles contained in the dispersion. Controlling the pH value and optimizing the pH value to be 8-10, and dropwise adding a sodium tetraborate aqueous solution with the mass of 0.3-0.6% of that of the copper nanowire solution under magnetic stirring until gel is obtained. In-situ polymerizing at 60 deg.c for 5 hr, and cooling to room temperature to obtain the hydrogel substrate.
3. And (3) soaking the hydrogel substrate obtained in the step (2) in an ethylene glycol solution for 4 hours, and removing the surface solvent by using filter paper to obtain the final organic hydrogel.
Example 2:
1. and synthesizing a copper nanowire solution with the concentration of 25 mg/mL. Firstly, sequentially adding 0.84g of copper chloride dihydrate and 0.99g of glucose into 400mL of deionized water solution, adding 5.4g of hexadecylamine into the mixture under the stirring of a magnetic stirrer at 600rpm, and finally stirring the mixture to a homogeneous light blue emulsion state; and then pouring the mixture into a polytetrafluoroethylene container, reacting for 8 hours at a high temperature of 120 ℃, cooling to room temperature, and sequentially carrying out centrifugal washing by using water and hot water at a temperature of 65 ℃, wherein the centrifugal rotation speed and the centrifugal time are 9000rpm and 6min respectively, so as to finally obtain the reddish-brown copper nanowire solution.
2. Acrylamide accounting for 5-20% of the mass of the copper nanowire solution, polyvinyl alcohol aqueous solution accounting for 3-8% of the mass of the copper nanowire solution, methylene bisacrylamide accounting for 0.02-0.06% of the mass of the copper nanowire solution and 2,2' -azobis [2- (2-imidazoline-2-yl) propane ] dihydrochloride accounting for 0.2-0.6% of the mass of the copper nanowire solution are sequentially added into the copper nanowire solution, and the mixture is uniformly stirred before the next medicine is added each time. The whole process is completed under the protection of nitrogen, and the flow rate of the nitrogen is controlled to be 0.5 mL/s. The mixture was ultrasonically mixed and then placed in a vacuum drying oven to remove air bubbles contained in the dispersion. Controlling the pH value and optimizing the pH value to be 8-10, and dropwise adding a sodium tetraborate aqueous solution with the mass of 0.3-0.6% of that of the copper nanowire solution under magnetic stirring until gel is obtained. In-situ polymerizing at 60 deg.c for 5 hr, and cooling to room temperature to obtain the hydrogel substrate.
3. And (3) soaking the hydrogel substrate obtained in the step (2) in an ethylene glycol solution for 4 hours, and removing the surface solvent by using filter paper to obtain the final organic hydrogel.
Example 3:
1. and synthesizing a copper nanowire solution with the concentration of 30 mg/mL. Firstly, sequentially adding 0.84g of copper chloride dihydrate and 0.99g of glucose into 400mL of deionized water solution, adding 5.4g of hexadecylamine into the mixture under the stirring of a magnetic stirrer at 600rpm, and finally stirring the mixture to a homogeneous light blue emulsion state; and then pouring the mixture into a polytetrafluoroethylene container, reacting for 8 hours at a high temperature of 120 ℃, cooling to room temperature, and sequentially carrying out centrifugal washing by using water and hot water at a temperature of 65 ℃, wherein the centrifugal rotation speed and the centrifugal time are 9000rpm and 6min respectively, so as to finally obtain the reddish-brown copper nanowire solution.
2. Acrylamide accounting for 5-20% of the mass of the copper nanowire solution, polyvinyl alcohol aqueous solution accounting for 3-8% of the mass of the copper nanowire solution, methylene bisacrylamide accounting for 0.02-0.06% of the mass of the copper nanowire solution and 2,2' -azobis [2- (2-imidazoline-2-yl) propane ] dihydrochloride accounting for 0.2-0.6% of the mass of the copper nanowire solution are sequentially added into the copper nanowire solution, and the mixture is uniformly stirred before the next medicine is added each time. The whole process is completed under the protection of nitrogen, and the flow rate of the nitrogen is controlled to be 0.5 mL/s. The mixture was ultrasonically mixed and then placed in a vacuum drying oven to remove air bubbles contained in the dispersion. Controlling the pH value and optimizing the pH value to be 8-10, and dropwise adding a sodium tetraborate aqueous solution with the mass of 0.3-0.6% of that of the copper nanowire solution under magnetic stirring until gel is obtained. In-situ polymerizing at 60 deg.c for 5 hr, and cooling to room temperature to obtain the hydrogel substrate.
3. And (3) soaking the hydrogel substrate obtained in the step (2) in an ethylene glycol solution for 4 hours, and removing the surface solvent by using filter paper to obtain the final organic hydrogel.
Claims (10)
1. A preparation method of copper nanowire composite organic hydrogel is characterized by comprising the following steps:
under the condition that a polymerizable monomer exists, the nano material forms nano composite hydrogel through free radical polymerization reaction, dynamic cross-linking between ions and supermolecule action between the nano material and the polymer, and then the nano composite hydrogel is soaked in an organic solvent for solvent replacement, so that the copper nanowire composite organic hydrogel is finally obtained.
2. The method of claim 1, comprising the steps of:
step 1: synthesizing a copper nanowire solution with the concentration of 20 mg/mL;
step 2: sequentially adding a monomer, a polymer, a cross-linking agent and an initiator into the copper nanowire solution prepared in the step (1) under the protection of nitrogen, ultrasonically mixing, then placing in a vacuum drying oven to remove bubbles contained in the dispersion liquid, controlling the pH value, and dropwise adding a sodium tetraborate aqueous solution under magnetic stirring until a gel is obtained; in-situ polymerizing at 60 deg.c for 5 hr, and cooling to room temperature to obtain hydrogel substrate;
and step 3: and (3) soaking the hydrogel substrate obtained in the step (2) in an organic solvent for 4 hours, and removing the surface solvent to obtain the copper nanowire composite organic hydrogel.
3. The method of claim 2, wherein:
in step 1, the length of the obtained copper nanowire is 60-70 μm, and the diameter is 70-90 nm.
4. The method of claim 2, wherein:
in step 2, the pH value of the system is controlled to be 8-10.
5. The method of claim 2, wherein:
in the step 2, the monomer is acrylamide, and the addition mass of the monomer is 5-20% of the mass of the copper nanowire solution obtained in the step 1.
6. The method of claim 2, wherein:
in the step 2, the cross-linking agent is methylene bisacrylamide, and the addition mass of the cross-linking agent is 0.02-0.06% of the mass of the copper nanowire solution obtained in the step 1.
7. The method of claim 2, wherein:
in the step 2, the initiator is 2,2' -azobis [2- (2-imidazoline-2-yl) propane ] dihydrochloride, and the addition mass of the initiator is 0.2-0.6% of the mass of the copper nanowire solution obtained in the step 1.
8. The method of claim 2, wherein:
in the step 2, the polymer is polyvinyl alcohol aqueous solution, the mass concentration is 10 wt%, and the adding mass of the polymer is 3-8% of the mass of the copper nanowire solution obtained in the step 1.
9. The method of claim 2, wherein:
in the step 2, the adding mass of the sodium tetraborate is 0.3-0.6% of the mass of the copper nanowire solution obtained in the step 1.
10. The method of claim 2, wherein:
in step 3, the organic solvent is ethylene glycol.
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| US20160002457A1 (en) * | 2013-02-20 | 2016-01-07 | Celluforce Inc. | Tunable and responsive photonic hydrogels comprising nanocrystalline cellulose |
| CN104710584A (en) * | 2015-03-16 | 2015-06-17 | 清华大学 | Polymer hydrogel and preparation method thereof |
| CN107501446A (en) * | 2017-09-29 | 2017-12-22 | 合肥工业大学 | A kind of preparation method of multifunctional nano composite aquogel |
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