CN115651228A - Preparation method and application of cellulose-based ionic gel - Google Patents
Preparation method and application of cellulose-based ionic gel Download PDFInfo
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Abstract
The invention relates to a preparation method and application of cellulose-based ionic gel with high ionic conductivity, self-adhesion, self-repair, frost resistance and excellent mechanical strength. The preparation method comprises the steps of taking imidazole type ionic liquid as a raw material, mixing the imidazole type ionic liquid with acrylamide, heating and stirring to obtain a novel eutectic solvent, dissolving cellulose in the imidazole type ionic liquid by a stepwise dissolution method, fully mixing the obtained mixture with the prepared eutectic solvent, and carrying out photoreaction, crosslinking and curing by using a photoinitiator under the irradiation of ultraviolet light to obtain the cellulose-based ionic gel. The ionic gel prepared by the invention has good mechanical property (tensile stress is up to 1.02 MPa), good toughness and self-repairability, and meanwhile, the eutectic solvent is used as a dispersion medium, so that the gel has excellent conductivity (the conductivity can reach 0.41mS/cm at room temperature), frost resistance (the stability can be kept at-20 ℃), self-adhesion and excellent strain sensitivity, and has wide application prospect in the field of flexible electronic devices.
Description
Technical Field
The invention belongs to the technical field of ionic gel, and relates to a preparation method and application of cellulose-based ionic gel with high ionic conductivity, self-adhesion, self-repair, frost resistance and excellent mechanical strength.
Background
The ionic liquid is a room temperature molten salt with good conductivity and thermal stability, which can be used as a green solvent for the synthesis of organic polymer materials, for example, in the field of gels, the ionic liquid is used as an excellent conductive dispersion medium, and can be synthesized by dispersing a polymerization monomer in the ionic liquid or polymerizing polyionic liquid by itself, and compared with traditional hydrogels, the ionic gel has excellent conductivity, viscoelasticity, thermal stability, mechanical properties and fatigue resistance, and is receiving more and more attention and research in recent years. Ionic liquids also have certain drawbacks as solvents, since most ionic liquids have high viscosity and poor flowability, and are solid even at room temperature, which causes difficulties in the dissolution of polymers and application at low temperatures after gelling. The problems are well solved by the occurrence of the Eutectic Solvent, the Eutectic Solvent (DES) is a novel ionic liquid, is a Eutectic mixture prepared by mixing a Hydrogen Bond Acceptor (HBA) and a Hydrogen Bond Donor (HBD) at a higher temperature, has the properties of the ionic liquid such as low steam pressure, good solubility, wide electrochemical stability window and the like, and also has the unique properties of simple preparation, no toxicity, low melting point, biodegradability and the like, so that a good Solvent selection is provided for synthesizing gel. The eutectic solvent is dispersed in a three-dimensional network structure of a high molecular polymer as a dispersion medium in the synthesis of the gel, so that a hydrogen bond binding system can be constructed between the eutectic solvent and the polymer, the stability and the adhesiveness of the gel are improved, and the melting point of the gel can be greatly reduced, so that the frost resistance of the gel is improved, the practical applicability of the gel in an extreme environment is enriched, and the eutectic solvent can be used as an excellent solvent for synthesizing the gel.
At present, with the pollution of petroleum-based materials and the increasing exhaustion of petroleum resources, biomass resources are concerned, and the combination of the biomass materials and the gel is a bright spot. Cellulose is one of the most abundant natural resources in nature, has the characteristics of wide source, good biocompatibility, reproducibility and degradability, and has a wide application prospect in many fields. In the field of gels, cellulose-based functional gels are more and more emphasized, and compared with gels synthesized by taking petroleum processed products as raw materials, cellulose-based gels are more green, economic and environment-friendly and accord with the concept of sustainable development. However, most of the eutectic solvents or poly-eutectic solvents (PDES) synthesized by taking choline chloride as a hydrogen bond acceptor have poor dissolving effect on biomass materials, and the method adopts a two-step method to dissolve cellulose, namely, imidazole type ionic liquid is used as the hydrogen bond acceptor, acrylamide is used as a hydrogen bond donor to synthesize the eutectic solvent, the imidazole type ionic liquid is used to dissolve the cellulose, and then the dissolved cellulose solution is fully mixed with the eutectic solvent, so that the cellulose is dissolved in the eutectic solvent. As the cellulose molecular structure contains a large amount of hydroxyl, the cellulose molecular structure can form rich hydrogen bonds with polar groups in the ionic liquid used as a solvent, so that a firm gel system is constructed, the mechanical property, toughness and self-repairing performance of the gel are improved, and the performance of the prepared ionic gel is obviously improved.
The flexible strain sensor has the working principle that an external stimulation signal is converted into a recognizable electric signal, and the ionic gel serving as a flexible material has excellent ionic conductivity, strain sensitivity and flexibility and can be easily adhered to the epidermis of a human body without external force, so that the flexible strain sensor can be used as a wearable strain sensor for monitoring slight changes of body movement of a wearer, and has wide application prospects in the fields of intelligent robots, electronic skins, medical health monitoring, wearable electronics and the like. As a flexible functional polymer material, the cellulose-based ionic gel has good flexibility, adhesiveness, biocompatibility, fatigue resistance, working stability, response speed, self-healing property and self-recovery property, and the properties make the cellulose-based ionic gel an ideal material for a flexible strain sensor.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of cellulose-based ionic gel. The ionic gel prepared by the invention has good conductivity, self-adhesion, self-repair, frost resistance, biocompatibility and the like, shows good stretchability, flexibility and sensitivity when monitoring human body movement, can be easily adhered to the skin of a human body joint, and realizes real-time monitoring of human body movement with large strain and small strain at the human body joint.
The second purpose of the invention is to provide the cellulose-based ionic gel prepared by the preparation method.
The invention also aims to provide application of the cellulose-based ionic gel as a strain sensor in human motion monitoring. The human motion signal monitoring comprises swallowing, coughing, sounding and the like at the throat; bending and straightening finger joints; the upper and lower bending of the wrist joint; flexion, extension of the knee and elbow joints; the neck articulation during head up and head down, etc., but not limited to the above monitoring features.
The technical scheme is as follows:
step 1: preparing a eutectic solvent: mixing the hydrogen bond acceptor imidazole type ionic liquid and the hydrogen bond donor acrylamide according to a certain proportion, stirring the mixture under a heating condition until the solution is transparent and uniform to obtain a eutectic solvent, and cooling the eutectic solvent to room temperature for later use;
step 2: dissolving cellulose: dissolving a certain mass of cellulose in the imidazole ionic liquid used in the step 1 under the heating condition to form a transparent and uniform cellulose solution for later use;
and step 3: preparing cellulose-based ionic gel: adding the eutectic solvent obtained in the step 1 into the cellulose solution obtained in the step 2 according to a certain proportion, fully stirring until the solution is in a uniform state, sequentially adding a certain amount of cross-linking agent and photoinitiator, uniformly mixing to obtain a prepolymer solution, pouring the prepolymer solution into an oxygen-isolated closed die, and performing ultraviolet irradiation crosslinking and curing to obtain cellulose-based ionic gel;
and 4, step 4: preparing a strain sensor: cutting cellulose-based ionic gel into long strips, connecting the two ends of the gel in a wire extending mode, and assembling the strain sensor based on the ionic gel;
and 5: attaching cellulose-based ionic gel to joints of a human body, connecting a Keithley 2450 digital source meter to the extension end of a lead, setting parameters of the instrument, and moving the joints of the human body regularly: the finger, wrist, elbow, neck, knee and throat, from the instrument screen, a graph of the relative resistance change of the gel during the movement of the human joint can be obtained.
Preferably, in step 1, the hydrogen bond acceptor and the hydrogen bond donor of the eutectic solvent are 1-butyl-3-methylimidazolium chloride and acrylamide, respectively, and the molar ratio is 1.
Preferably, in step 1, the heating temperature for preparing the eutectic solvent is 70 ℃.
Preferably, in step 2, the dissolution temperature of the cellulose in the imidazole type ionic liquid is 80 ℃.
Preferably, in the step 2, the mass fraction of the cellulose dissolved in the imidazole type ionic liquid is 0wt% to 4wt%.
Preferably, in step 3, the molar ratio of the imidazole-type ionic liquid to acrylamide in the uniform solution obtained by mixing the eutectic solvent and the cellulose solution and sufficiently stirring the mixture is 1.3.
Preferably, in step 3, the amount of the crosslinking agent polyethylene glycol diacrylate is 0.1% of the amount of the acrylamide monomer material.
Preferably, in step 3, the photoinitiator 2-hydroxy-2-methyl-1-phenylpropanone is used in an amount of 1% of the amount of the acrylamide monomer material.
Preferably, in step 3, the closed mold is a square mold, and is composed of two square full-transparent glass sheets, wherein a rubber sheet with the thickness of 2mm is sandwiched between the two square full-transparent glass sheets, the rubber sheet is hollow, and the hollow part is a square with the size of 6cm × 6 cm.
Preferably, in step 3, the irradiation time of the ultraviolet light is 1 to 10min, more preferably 6min.
Preferably, in step 4, the gel has a long strip size of 4cm × 1cm.
The invention has the beneficial effects that:
according to the invention, the eutectic solvent is used as a dispersion medium, a gel three-dimensional network is formed by polymerization of acrylamide monomers, and compared with the traditional hydrogel, the hydrogel has excellent conductivity, freezing resistance, stimulation response and working stability. The addition of the natural cellulose obviously improves the mechanical property of the gel, compared with the prior reports that the nano cellulose and the microcrystalline cellulose are used as reinforcing materials of the gel, the natural cellulose is more environment-friendly, the acquisition channel is more convenient, the cost is lower, industrial waste is not generated, the carbon neutralization is favorably realized, and the concept of sustainable development is more met.
Drawings
FIG. 1: the photo of hydrogen bond acceptor chloridized 1-butyl-3-methylimidazole and hydrogen bond donor acrylamide and prepared eutectic solvent at normal temperature;
FIG. 2: the chemical reaction formula is that hydrogen bond acceptor 1-butyl-3-methylimidazole chloride reacts with hydrogen bond donor acrylamide to obtain eutectic solvent;
FIG. 3: is a Fourier transform infrared spectrogram of hydrogen bond acceptor 1-butyl-3-methylimidazole chlorine salt, hydrogen bond donor acrylamide and prepared eutectic solvent;
FIG. 4: differential scanning thermal performance analysis chart of prepared eutectic solvent;
FIG. 5: the photos are the initial state of the cellulose base ionic gel and the stretching and knotting states at normal temperature;
FIG. 6: a graph of ionic gel conductivity for different cellulose contents;
FIG. 7 is a schematic view of: ionic gel stress-strain curves for different cellulose contents;
FIG. 8: optical microscope pictures of the cuts of 8h, 16h and 24h after the cellulose-based ionic gel is cut and self-healed;
FIG. 9: is a sensing curve graph of regular motion of cellulose-based ionic gel attached to the wrist of a human body.
Detailed Description
Embodiments of the present invention will be described in detail with reference to examples.
Example 1
This example provides an ionic gel prepared as follows:
step 1: preparing a eutectic solvent: mixing hydrogen bond acceptor 1-butyl-3-methylimidazole chloride salt and hydrogen bond donor acrylamide according to a molar ratio of 1 to 2, stirring the mixture under the heating condition of 70 ℃ until the solution is in a transparent and uniform state, taking the solution out, and placing the solution in a room temperature environment for later use;
and 2, step: dissolving cellulose: dissolving cellulose in 1-butyl-3-methylimidazole chloride salt under the heating condition of 80 ℃ to form a transparent and clear cellulose solution, wherein the mass fraction of the cellulose is 2wt%;
and step 3: preparing cellulose-based ionic gel: and 3g of the eutectic solvent in the step 1 is added into 2.64g of the cellulose solution prepared in the step 2 and fully stirred to obtain a uniform solution, wherein the molar ratio of the 1-butyl-3-methylimidazolium chloride to the acrylamide in the solution is 1.3. Then 3 microliters of cross-linking agent polyethylene glycol diacrylate and 30 microliters of photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone are sequentially added and fully stirred, the obtained prepolymer solution is poured into an airtight mold isolated from oxygen, the airtight mold is a square mold, the composition of the airtight mold is that two square full-transparent glass sheets sandwich a rubber sheet with the thickness of 2mm, the rubber sheet is hollow, and the size of the hollow part is a square of 6cm multiplied by 6 cm. Then irradiating for 6min by ultraviolet light to obtain the cellulose-based ionic gel.
Example 2
This example provides an ionic gel which was prepared in a manner different from that of example 1 in that the mass fraction of cellulose in the cellulose solution obtained in step 2 was 0wt%.
Example 3
This example provides an ionic gel which was prepared in a manner different from that of example 1 in that the mass fraction of cellulose in the cellulose solution obtained in step 2 was 1wt%.
Example 4
This example provides an ionic gel which was prepared in a manner different from that of example 1 in that the cellulose solution obtained in step 2 had a mass fraction of cellulose of 3wt%.
Example 5
This example provides an ionic gel which was prepared in a manner different from that of example 1 in that the cellulose solution obtained in step 2 had a mass fraction of cellulose of 4wt%.
As shown in fig. 7, the stress-strain curves for the ionic gels with different cellulose contents are shown. It can be seen that the gel stress gradually increased with the increase in the cellulose content, and the stress hardly increased any more after the cellulose content reached 3wt%.
Example 6
This example provides an ionic gel prepared as follows:
step 1: preparing a eutectic solvent: mixing hydrogen bond acceptor 1-allyl-3-methylimidazole chloride and hydrogen bond donor acrylamide according to a molar ratio of 1 to 2, stirring under a heating condition of 70 ℃ until the solution is transparent and uniform, taking out and placing in a room temperature environment for later use;
and 2, step: dissolving cellulose: dissolving cellulose in 1-allyl-3-methylimidazole chloride salt under the heating condition of 80 ℃ to form a transparent and clear cellulose solution, wherein the mass fraction of the cellulose is 2wt%;
and 3, step 3: preparing cellulose-based ionic gel: 3g of the eutectic solvent in the step 1 is added into 2.53g of the cellulose solution prepared in the step 2 and fully stirred to obtain a uniform solution, wherein the molar ratio of the 1-allyl-3-methylimidazole chloride salt to the acrylamide in the solution is 1.3. Then, 2.7 microliters of cross-linking agent polyethylene glycol diacrylate and 39 microliters of photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone are sequentially added and fully stirred, and the obtained prepolymer solution is poured into an oxygen-isolated closed mold which is a square mold and consists of two square full-transparent glass sheets, wherein a rubber sheet with the thickness of 2mm is clamped between the two square full-transparent glass sheets, the rubber sheet is hollow, and the hollow part is a square with the size of 6cm multiplied by 6 cm. Then irradiating for 6min by ultraviolet light to obtain the cellulose-based ionic gel.
Example 7
The embodiment provides a cellulose-based ionic gel sensor, which is prepared according to the following steps:
step 1: preparing a eutectic solvent: mixing hydrogen bond acceptor 1-butyl-3-methylimidazole chloride salt and hydrogen bond donor acrylamide according to a molar ratio of 1;
step 2: dissolving cellulose: dissolving cellulose in 1-butyl-3-methylimidazole chloride salt under the heating condition of 80 ℃ to form a transparent and clear cellulose solution, wherein the mass fraction of the cellulose is 2wt%;
and step 3: preparing cellulose-based ionic gel: and 3g of the eutectic solvent in the step 1 is added into 2.64g of the cellulose solution prepared in the step 2 and fully stirred to obtain a uniform solution, wherein the molar ratio of the 1-butyl-3-methylimidazole chloride salt to the acrylamide in the solution is 1.3. Then 3 microliters of cross-linking agent polyethylene glycol diacrylate and 30 microliters of photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone are sequentially added and fully stirred, the obtained prepolymer solution is poured into an airtight mold isolated from oxygen, the airtight mold is a square mold, the composition of the airtight mold is that two square full-transparent glass sheets sandwich a rubber sheet with the thickness of 2mm, the rubber sheet is hollow, and the size of the hollow part is a square of 6cm multiplied by 6 cm. Then irradiating for 6min by ultraviolet light to obtain cellulose-based ionic gel;
and 4, step 4: preparing a strain sensor: the cellulose-based ionic gel is cut into a long strip-shaped structure, the two ends of the gel are connected in a wire extending mode, and the strain sensor based on the ionic gel is assembled. The cellulose-based ionic gel is attached to a human body joint, the extension end of the lead is connected with a Keithley 2450 digital source meter, parameters of the instrument are set, the wrist is bent up and down regularly, and a curve graph of relative resistance change of the gel during wrist joint movement is obtained from a screen of the instrument.
Fig. 9 shows a sensing curve of regular motion of cellulose-based ionic gel attached to a wrist of a human body. It can be seen from the figure that the cellulose-based ionic gel can rapidly monitor the movement of the human body joints as the wrist is bent regularly upwards and downwards, and converts the physical signals into electric signals, so that the relative resistance change curve of the gel can be clearly seen in the graph, which shows that the sensor has good sensitivity to applied strain.
Claims (13)
1. The preparation method of the cellulose-based ionic gel is characterized by comprising the following specific steps of:
step 1: preparing a eutectic solvent: mixing the hydrogen bond acceptor imidazole type ionic liquid and the hydrogen bond donor acrylamide according to a certain proportion, stirring the mixture under a heating condition until the solution is transparent and uniform to obtain a eutectic solvent, and cooling the eutectic solvent to room temperature for later use;
and 2, step: dissolving cellulose: dissolving a certain mass of cellulose in the imidazole ionic liquid used in the step 1 under the heating condition to form a transparent and uniform cellulose solution for later use;
and step 3: preparing cellulose-based ionic gel: and (3) adding the eutectic solvent obtained in the step (1) into the cellulose solution obtained in the step (2) according to a certain proportion, fully stirring until the solution is in a uniform state, sequentially adding a certain amount of cross-linking agent and photoinitiator, uniformly mixing to obtain a prepolymer solution, pouring the prepolymer solution into an oxygen-isolated closed die, and performing ultraviolet irradiation crosslinking and curing to obtain the cellulose-based ionic gel.
2. The method of claim 1, wherein the cellulose-based ionic gel is prepared.
3. The preparation method according to claim 1, wherein the hydrogen bond acceptor of the eutectic solvent in step 1 is imidazole type ionic liquid, and comprises one of 1-butyl-3-methylimidazole chloride salt, 1-allyl-3-methylimidazole chloride salt and 1-ethyl-3-methylimidazole acetate, and more preferably 1-butyl-3-methylimidazole chloride salt; the hydrogen bond donor is acrylamide, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 2.
4. The preparation method according to claim 1, wherein the mixing temperature of the hydrogen bond acceptor and the hydrogen bond donor in the eutectic solvent of step 1 is 65 ℃ to 75 ℃, and more preferably 70 ℃; the mixing time of the hydrogen bond acceptor and the hydrogen bond donor is 10min to 40min, and more preferably 15min.
5. The preparation method according to claim 1, wherein the dissolution temperature of the cellulose in the imidazole type ionic liquid in the step 2 is 80 ℃ to 90 ℃.
6. The preparation method according to claim 1, wherein the mass fraction of the cellulose dissolved in the imidazole-type ionic liquid in step 2 is 0wt% to 9wt%, and more preferably 0wt% to 4wt%.
7. The preparation method according to claim 1, wherein the molar ratio of the imidazole-type ionic liquid to acrylamide in the homogeneous solution obtained by mixing the eutectic solvent and the cellulose solution in step 3 and then fully stirring is 1.5.
8. The method according to claim 1, wherein the crosslinking agent in step 3 is polyethylene glycol diacrylate in an amount of 0.1% to 0.5%, more preferably 0.1%, based on the amount of the acrylamide monomer component.
9. The method according to claim 1, wherein the photoinitiator in step 3 is 2-hydroxy-2-methyl-1-phenylpropanone, and the amount of the photoinitiator is 1 to 5 percent, and more preferably 1 percent, of the amount of the acrylamide monomer material.
10. The method according to claim 1, wherein the closed mold in step 3 is a square mold, and is composed of two square transparent glass sheets with a 2mm thick rubber sheet sandwiched therebetween, wherein the rubber sheet is hollow, and the hollow part has a square shape of 6cm x 6 cm.
11. The method according to claim 1, wherein the UV irradiation time in step 3 is 1min to 15min, and more preferably 6min.
12. A cellulose-based ionic gel prepared by the method of any one of claims 1-11.
13. The cellulose-based ionic gel of claim 12, for use as a strain sensor in human motion monitoring.
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| CN116606401A (en) * | 2023-07-06 | 2023-08-18 | 天津永续新材料有限公司 | Cellulose nanocrystalline ion gel temperature sensor and preparation method thereof |
| CN116856193A (en) * | 2023-06-17 | 2023-10-10 | 烟台先进材料与绿色制造山东省实验室 | Lignocellulose-based coating and preparation method thereof |
| CN117344404A (en) * | 2023-10-27 | 2024-01-05 | 安徽工程大学 | Polypeptide ion conductive fiber based on polymerizable deep eutectic solvent, preparation and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116856193A (en) * | 2023-06-17 | 2023-10-10 | 烟台先进材料与绿色制造山东省实验室 | Lignocellulose-based coating and preparation method thereof |
| CN116606401A (en) * | 2023-07-06 | 2023-08-18 | 天津永续新材料有限公司 | Cellulose nanocrystalline ion gel temperature sensor and preparation method thereof |
| CN116606401B (en) * | 2023-07-06 | 2023-09-22 | 天津永续新材料有限公司 | Cellulose nanocrystalline ion gel temperature sensor and preparation method thereof |
| CN117344404A (en) * | 2023-10-27 | 2024-01-05 | 安徽工程大学 | Polypeptide ion conductive fiber based on polymerizable deep eutectic solvent, preparation and application |
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