CN113354953A - Flexible conductive biopolymer material and preparation method and application thereof - Google Patents
Flexible conductive biopolymer material and preparation method and application thereof Download PDFInfo
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- CN113354953A CN113354953A CN202110689116.0A CN202110689116A CN113354953A CN 113354953 A CN113354953 A CN 113354953A CN 202110689116 A CN202110689116 A CN 202110689116A CN 113354953 A CN113354953 A CN 113354953A
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- biopolymer
- eutectic solvent
- deep eutectic
- flexible conductive
- aqueous solution
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- 229920001222 biopolymer Polymers 0.000 title claims abstract description 196
- 239000000463 material Substances 0.000 title claims abstract description 127
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 79
- 230000005496 eutectics Effects 0.000 claims abstract description 77
- 239000007864 aqueous solution Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000010297 mechanical methods and process Methods 0.000 claims abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 38
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
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- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 6
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- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 3
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- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
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- 239000000811 xylitol Substances 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- 235000010643 Leucaena leucocephala Nutrition 0.000 claims description 2
- 241000220479 Acacia Species 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 21
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 4
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- 230000008439 repair process Effects 0.000 description 3
- -1 silk Polymers 0.000 description 3
- 244000215068 Acacia senegal Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920000084 Gum arabic Polymers 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000205 acacia gum Substances 0.000 description 2
- 239000001785 acacia senegal l. willd gum Substances 0.000 description 2
- 238000003490 calendering Methods 0.000 description 2
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- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/12—Agar-agar; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/19—Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/21—Urea; Derivatives thereof, e.g. biuret
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a flexible conductive biopolymer material and a preparation method and application thereof, wherein the preparation method comprises the following steps: dissolving a biopolymer in water to obtain a biopolymer aqueous solution; adding a deep eutectic solvent into the biopolymer aqueous solution, and stirring to obtain an aqueous solution containing the deep eutectic solvent and the biopolymer; and forming the aqueous solution containing the deep eutectic solvent and the biopolymer by a mechanical method, and drying to obtain the flexible conductive biopolymer material. The deep eutectic solvent and the biopolymer have good intermiscibility, and a large number of hydrogen bonds in the deep eutectic solvent and hydrogen bonds in a biopolymer chain form interaction to form new hydrogen bonds, so that intermolecular interaction in the biopolymer chain is reduced, the mobility of a biopolymer molecular chain is increased, the tensile strength of a biopolymer material is reduced, and the ductility of the biopolymer material is improved.
Description
Technical Field
The invention relates to the field of biological materials, in particular to a flexible conductive biological polymer material and a preparation method and application thereof.
Background
The biological polymer (including silk, gelatin, starch, cellulose, sodium alginate, chitosan and the like) is a green high molecular material with good biocompatibility and degradability, can be used as an additive and an encapsulating agent of food or medicines, and can also be used as wound dressing and tissue repair materials. However, biopolymers generally form hard and brittle films with poor mechanical properties and poor stability. The addition of plasticizers is an effective means for solving the above problems, and common plasticizers include polyhydric alcohols such as glycerin, mannitol, sorbitol, polyethylene glycol and ethylene glycol, or other solvent-based molecules. However, the biopolymer materials obtained based on the current technology have high tensile strength (MPa grade) and poor ductility (ductility less than 50%).
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a flexible conductive biopolymer material, a preparation method and application thereof, and aims to solve the problems of high tensile strength and poor ductility of the conventional biopolymer material.
The technical scheme of the invention is as follows:
in a first aspect of the present invention, there is provided a method for preparing a flexible conductive biopolymer material, comprising the steps of:
dissolving a biopolymer in water to obtain a biopolymer aqueous solution;
adding a deep eutectic solvent into the biopolymer aqueous solution, and stirring to obtain an aqueous solution containing the deep eutectic solvent and the biopolymer;
and forming the aqueous solution containing the deep eutectic solvent and the biopolymer by a mechanical method, and drying to obtain the flexible conductive biopolymer material.
Optionally, the biopolymer is selected from one or more of cellulose, gelatin, chitosan, sodium alginate, carrageenan, agar, acacia, silk, and starch.
Optionally, the mass content of the biopolymer in the biopolymer aqueous solution is 0.1% -30%.
Optionally, the deep eutectic solvent is prepared by mixing a first component and a second component, wherein the first component is selected from one or more of urea, glycerol, glycol, thiourea, gluconic acid, citric acid, fructose, sorbitol, xylitol and malic acid, and the second component is selected from one or two of amino acid and quaternary ammonium salt.
Optionally, the mass content of the first component in the deep eutectic solvent is 25% to 75%.
Optionally, the amino acid is selected from one or more of glycine, alanine and proline, and/or the quaternary ammonium salt is selected from one or two of betaine and choline chloride.
Optionally, in the step of adding the deep eutectic solvent into the aqueous biopolymer solution, the mass of the deep eutectic solvent is 20% to 95% of the mass sum of the deep eutectic solvent and the biopolymer in the aqueous biopolymer solution.
Optionally, the step of adding a deep eutectic solvent to the aqueous biopolymer solution further comprises adding one or more of a cross-linking agent, an electrolyte, a surfactant, and conductive nanoparticles to the aqueous biopolymer solution.
In a second aspect of the present invention, a flexible conductive biopolymer material is provided, wherein the flexible conductive biopolymer material is prepared by the preparation method of the flexible conductive biopolymer material of the present invention.
In a third aspect of the invention, there is provided a use of the flexible conductive biopolymer material of the invention in the preparation of flexible electronic devices.
Has the advantages that: the invention provides a flexible conductive biopolymer material and a preparation method and application thereof, wherein a deep eutectic solvent is used as a plasticizer of a biopolymer, the deep eutectic solvent has good intermiscibility with the biopolymer, and a large number of hydrogen bonds exist in the deep eutectic solvent, and the deep eutectic solvent and the hydrogen bonds in a biopolymer chain form interaction to form new hydrogen bonds, so that the hydrogen bonds in the biopolymer chain are broken, the intermolecular interaction in the biopolymer chain is reduced, the mobility of a biopolymer molecular chain is increased, the mechanical property of the biopolymer material is improved, the tensile strength of the biopolymer material is reduced, the ductility of the biopolymer material is improved, the efficient plasticization of the biopolymer material is realized, in addition, the deep eutectic solvent contains ionic electrolyte, so that the flexible conductive biopolymer material has conductivity, thereby realizing the preparation of the flexible conductive biopolymer material.
Drawings
Fig. 1 is a flow chart of the preparation of a flexible conductive biopolymer material in an embodiment of the invention.
Fig. 2 is a graph showing the stress-strain test result of the flexible thin film material in example 1 of the present invention.
Fig. 3 is a graph showing the stress-strain test result of the flexible thin film material in example 2 of the present invention.
Fig. 4 is a graph showing the stress-strain test results of the flexible thin film materials in examples 1, 3, 4, and 5 of the present invention.
FIG. 5 is a schematic diagram of the raw materials, processes, results and applications of the flexible conductive biopolymer material in the embodiment of the invention.
Detailed Description
The invention provides a flexible conductive biopolymer material and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear and definite. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a flexible conductive biopolymer material, which comprises the following steps:
s1, dissolving the biopolymer in water to obtain a biopolymer aqueous solution;
s2, adding a deep eutectic solvent into the biopolymer aqueous solution, and stirring to obtain an aqueous solution containing the deep eutectic solvent and the biopolymer;
s3, forming the aqueous solution containing the deep eutectic solvent and the biopolymer by a mechanical method, and drying to obtain the flexible conductive biopolymer material.
In this embodiment, a biopolymer is dissolved in water to obtain a biopolymer aqueous solution, where the water is used as a cosolvent, then a deep eutectic solvent is added to the biopolymer aqueous solution as a plasticizer of the biopolymer to form a uniform mixed solution, and then the mixed solution is mechanically formed and dried to remove moisture, so as to obtain a flexible conductive biopolymer material, where the flexible conductive biopolymer material contains the deep eutectic solvent and the biopolymer. The deep eutectic solvent has low melting point and contains a large amount of hydrogen bonds which can form interaction with the hydrogen bonds in the biopolymer chain to form new hydrogen bonds, so that the hydrogen bonds in the biopolymer chain are broken, the intermolecular interaction in the biopolymer chain is reduced, and the mobility of the biopolymer molecular chain is increased. In addition, compared with plasticizers in the prior art (such as glycerol, mannitol and the like with single components), the deep eutectic solvent has better compatibility with the biopolymer, the content of the deep eutectic solvent in the prepared flexible conductive biopolymer material is up to 95%, that is, the content of the plasticizer in the flexible material prepared by adopting the plasticizer in the prior art is far less than that of the plasticizer (deep eutectic solvent) in the flexible conductive biopolymer material in the embodiment of the invention, on one hand, more deep eutectic solvents can form hydrogen bonds with more molecules in biopolymer chains to reduce intermolecular interaction in the biopolymer chains, on the other hand, more deep eutectic solvents exist in the biopolymer to improve the softness of the polymer, thereby realizing efficient plasticization of the biopolymer material, the mechanical property of the biopolymer material is improved, the tensile strength of the biopolymer material is reduced, the ductility of the biopolymer material is improved, and the preparation of the flexible biopolymer material is further realized. Compared with the prior art, the preparation method can realize the preparation of the ultra-soft polymer material, and the flexible conductive biopolymer material prepared by the preparation method has the breaking tensile strength of less than 10MPa, the elastic modulus of less than 500kPa and the extensibility of more than 300%. In addition, the deep eutectic solvent contains ionic electrolyte, so that the flexible biopolymer material has conductivity, and finally, the preparation of the flexible conductive biopolymer material is realized.
In step S1, in one embodiment, the biopolymer is selected from one or more of cellulose, gelatin, chitosan, sodium alginate, carrageenan, agar, gum arabic, silk, starch, but is not limited thereto.
In the present embodiment, the present inventors have studied and found that a polymer synthesized based on a biopolymer or a partially synthesized polymer is also suitable for the present invention, not only for biopolymers. For example, the polymer synthesized on the basis of a biopolymer may be a cellulose derivative; the synthetic polymer may be one of polyvinylpyrrolidone, polyvinyl alcohol, polyurethane, but is not limited thereto.
In one embodiment, the biopolymer is present in the aqueous biopolymer solution in an amount of 0.1% to 30% by weight. The mass content can fully dissolve the biopolymer to form a solution with a certain viscosity, thereby being beneficial to controlling the size and thickness of the film prepared in the subsequent forming process, reducing the operation complexity, lowering the equipment requirement and facilitating the operation.
The aqueous solution containing the deep eutectic solvent and the biopolymer obtained in step S2 is a uniform mixed solution.
In one embodiment, the deep eutectic solvent is prepared by mixing a first component selected from one or more of urea, glycerol, ethylene glycol, thiourea, gluconic acid, citric acid, fructose, sorbitol, xylitol, malic acid and a second component selected from one or two of amino acid and quaternary ammonium salt. In the embodiment, the deep eutectic solvent is prepared by mixing the first component serving as a hydrogen bond donor and the second component serving as a hydrogen bond acceptor at normal temperature or under heating.
In the prior art, a single-component plasticizer (such as a single-component polyol, a single-component glycerol, mannitol and the like) is generally used, the plasticizing effect on the biopolymer is general, the elongation of the obtained biopolymer material is less than 50%, and the hardness of the biopolymer material is larger. The deep eutectic solvent is used as a plasticizer, and comprises one or more hydrogen bond donors and one or more hydrogen bond donors, and the inventor researches show that compared with the plasticizers in the prior art, the deep eutectic solvent has better compatibility with the biopolymer, has better adaptability with the biopolymer, and is more suitable for being used as the plasticizer of the biopolymer, the deep eutectic solvent is used as the plasticizer to show a plasticizing effect completely different from that of the plasticizer with a single component in the prior art, the deep eutectic solvent in the embodiment can enable the extensibility of the biopolymer material to reach more than 300%, and the minimum modulus of the biopolymer material can be as low as 10 kPa.
In one embodiment, the mass content of the first component in the deep eutectic solvent is 25% to 75%. This ratio enables the two components to form a good mutual solution, which in turn facilitates interaction with the biopolymer.
In this embodiment, the mass content of the first component in the deep eutectic solvent is 25% to 75%, that is, the mass content of the hydrogen bond donor in the deep eutectic solvent is 25% to 75%.
In one embodiment, the amino acid is selected from one or more of glycine, alanine, proline.
In one embodiment, the quaternary ammonium salt is selected from one or both of betaine, choline chloride.
In one embodiment, the amino acid is selected from one or more of glycine, alanine, proline, and the quaternary ammonium salt is selected from one or two of betaine and choline chloride.
In one embodiment, in the step of adding a deep eutectic solvent to the aqueous biopolymer solution, the mass of the deep eutectic solvent is 20% to 95% of the mass sum of the deep eutectic solvent and the biopolymer in the aqueous biopolymer solution.
The plasticizing effect of the deep eutectic solvent on the biopolymer is influenced by the dosage proportion of the deep eutectic solvent, the ductility of the prepared flexible conductive biopolymer material is improved and the elastic modulus is reduced along with the increase of the dosage of the deep eutectic solvent in a certain proportion range, and when the mass of the deep eutectic solvent is 20% -95% of the mass sum of the deep eutectic solvent and the biopolymer in the biopolymer aqueous solution, the deep eutectic solvent has a remarkable softening effect on the biopolymer material.
In one embodiment, the deep eutectic solvent is added to the aqueous biopolymer solution and stirred for 0.5-6 hours to obtain an aqueous solution containing the deep eutectic solvent and the biopolymer.
In one embodiment, the step of adding a deep eutectic solvent to the aqueous biopolymer solution further comprises adding one or more of an electrolyte, a surfactant, a cross-linking agent, and conductive nanoparticles to the aqueous biopolymer solution.
In this embodiment, the mechanical properties of the flexible conductive biopolymer material can be further improved by adding a cross-linking agent; other properties of the flexible conductive biopolymer material may also be improved by adding adjuvants including, but not limited to, electrolytes, surfactants, conductive nanoparticles, e.g., the addition of electrolytes may improve the ionic conductivity of the flexible conductive biopolymer material; adding a surfactant to improve the surface lubricating property of the flexible conductive biopolymer material; the addition of conductive nanoparticles can form a flexible electronically conductive composite. One or more of a cross-linking agent, an electrolyte, a surfactant and conductive nanoparticles can be selected according to actual needs to improve the performance of the flexible conductive biopolymer material.
In one embodiment, the cross-linking agent is selected from one or more of glutaraldehyde, epoxy capping compounds, but is not limited thereto.
In one embodiment, the electrolyte is selected from one or more of sodium chloride, potassium chloride, lithium chloride, but is not limited thereto.
In one embodiment, the surfactant is selected from one or more of tween, span, phospholipid, but is not limited thereto.
In one embodiment, the conductive nanoparticles are selected from one or more of silver nanowires, silver nanoplates, carbon nanotubes, graphene, carbon black, liquid metal or other metal nanoparticles, and the like, but are not limited thereto.
In step S3, in one embodiment, the mechanical method includes one of molding, injection, extrusion, calendering, but is not limited thereto.
In this embodiment, the flexible conductive biopolymer material can be obtained by shaping the aqueous solution containing the deep eutectic solvent and the biopolymer by one of the mechanical methods including, but not limited to, molding, injection, extrusion, calendering, and the like, and drying and removing water. The flexible conductive biopolymer material obtained after the aqueous solution containing the deep eutectic solvent and the biopolymer is formed can be in any shape, in other words, the aqueous solution containing the deep eutectic solvent and the biopolymer can be formed according to actual needs to obtain the flexible conductive biopolymer material in any shape. For example, an aqueous solution containing a deep eutectic solvent and a biopolymer is poured into a square mold for molding and drying to obtain a thin film flexible conductive biopolymer material, and an aqueous solution containing a deep eutectic solvent and a biopolymer is poured into a strip-shaped mold for molding and drying to obtain a strip-shaped flexible conductive biopolymer material.
In one embodiment, the aqueous solution containing the deep eutectic solvent and the biopolymer is mechanically shaped and then dried at a temperature of less than 100 ℃ until the mass is constant, wherein the temperature allows rapid moisture removal without affecting the stability of the biopolymer. The purpose of drying is to remove water from the aqueous solution containing the deep eutectic solvent and the biopolymer.
The embodiment of the invention also provides a flexible conductive biopolymer material prepared by the preparation method of the flexible conductive biopolymer material.
In one embodiment, the flexible conductive biopolymer material includes a deep eutectic solvent and a biopolymer. Wherein the deep eutectic solvent accounts for 20-95% of the mass of the flexible conductive biopolymer material.
In one embodiment, the flexible conductive biopolymer material further comprises one or more of a cross-linking agent, an electrolyte, a surfactant, conductive nanoparticles.
The flexible conductive biopolymer material in the embodiment belongs to an ultra-soft polymer material, and has a breaking tensile strength of less than 10MPa, an elastic modulus of less than 500kPa, and an elongation of more than 300%.
The flexible conductive biopolymer material in the embodiment has a repairing capability, for example, after the strip-shaped flexible biopolymer material is broken, the fracture can be repaired by heating. The heating method comprises direct heating or putting into hot water. For example, the fractured samples are lapped together and then heated to 60-80 ℃ and kept for 1-3min, and then the fracture can be repaired; or, the fractured sample is soaked in hot water at 60-80 ℃ for 30s to 1min, taken out and lapped together, and then dried to repair the fracture.
The flexible conductive biopolymer material in the embodiment can be recycled, the broken flexible conductive biopolymer material can still form a mixed solution after being placed in hot water, and the flexible conductive biopolymer material with a certain shape can be obtained again after the mixed solution is formed and dried. For example, the broken flexible conductive biopolymer material is added into water (water accounts for 30% -70% of the total mass of the water and the flexible conductive biopolymer material), heated to 60-90 ℃, stirred for 30min, then poured into a mold, dried to remove water, and the flexible conductive biopolymer material with a certain shape can be obtained again.
The flexible conductive biopolymer material in this embodiment has electrical conductivity, and since the deep eutectic solvent in the flexible conductive biopolymer material contains ionic electrolyte, the flexible conductive biopolymer material has electrical conductivity and can be used as electrolyte or an electrical connection unit. The conductivity of the flexible conductive biopolymer material can be further improved by adding electrolytes or conductive nanoparticles to the flexible conductive biopolymer material.
The embodiment of the invention also provides application of the flexible conductive biopolymer material in preparation of flexible electronic devices.
In one embodiment, the flexible electronic device is a flexible bioelectronic device.
In the present invention, natural raw materials, such as biopolymer, are mixed with solvent water in a certain ratio to obtain a biopolymer solution, then a plasticizer (deep eutectic solvent) containing two components is added to the biopolymer solution to obtain a mixed solution, and the mixed solution is formed and dried to obtain a flexible conductive biopolymer material (i.e., the flexible material in the figure), and a conductive material can be added according to actual needs to obtain a flexible composite material. The obtained flexible conductive biopolymer material and flexible composite material have flexible and stretchable properties and can be used in the fields of flexible electrodes, bioelectronics and the like.
The invention is further illustrated by the following specific examples.
Example 1
Preparing a gelatin aqueous solution with the gelatin mass fraction of 15%, mixing 2.6g of choline chloride and 3.4g of glycerol, stirring until the mixture is completely uniform, then adding the mixture into 13.3g of the gelatin aqueous solution (the mass ratio of the gelatin to the mass ratio of the choline chloride to the glycerol is 1:3), stirring for 2 hours, uniformly mixing, pouring the mixture into a film mold, and drying for 24 hours at the temperature of 40 ℃ and the humidity of 20% to obtain a flexible film material, wherein the label is P1-1.
The steps are repeated, except that the mass of the gelatin aqueous solution is respectively 20g, 30g, 40g, 60g and 120g, namely the mass ratio of the gelatin to the mass sum of choline chloride and glycerol is respectively 1:2, 3:4, 1:1, 3:2 and 3:1, and the obtained flexible film materials are respectively marked as P1-2, P1-3, P1-4, P1-5 and P1-6.
The flexible thin film material prepared in example 1 was subjected to a stress strain test, and the result is shown in fig. 2. As can be seen from FIG. 2, the elastic modulus of the flexible film material is less than 500kPa, and the extensibility is more than 300%; the ductility of the flexible film material is gradually increased and the elastic modulus is gradually reduced with the gradual increase of the content of the choline chloride and the glycerin mixture, and when the ratio of the mass of the gelatin to the mass sum of the choline chloride and the glycerin is 1:3, namely the flexible film material P1-1 has the highest ductility and the lowest elastic modulus.
The flexible film material prepared in example 1 was subjected to a tensile test and had a tensile strength at break of less than 10 MPa.
Example 2
2.6g of choline chloride and 3.4g of glycerol are mixed and stirred to be completely uniform, then the mixture is added into 20g of agar aqueous solution (the mass fraction of the agar is 2 percent), stirred for 2 hours and uniformly mixed, poured into a film mold and dried for 24 hours under the conditions of 40 ℃ and 20 percent of humidity, and the flexible film material is obtained.
Repeating the steps for 4 times, except replacing the agar aqueous solution (the mass fraction of the agar is 2%) with carrageenan aqueous solution (the mass fraction of the carrageenan is 2%), sodium alginate aqueous solution (the mass fraction of the sodium alginate is 2%), chitosan aqueous solution (the mass fraction of the chitosan is 2%) and Arabic gum aqueous solution (the mass fraction of the Arabic gum is 2%).
The flexible film material prepared in example 2 was subjected to a stress-strain test, and the result is shown in fig. 3, and it can be seen from fig. 3 that the elastic modulus of the flexible film material is less than 500kPa, and a plasticizer composed of a mixture of choline chloride and glycerin has a good plasticizing effect on agar, carrageenan, sodium alginate, chitosan, and gum arabic.
Example 3
Preparing a gelatin aqueous solution with the gelatin mass fraction of 15%, mixing 3.23g of choline chloride and 2.77g of urea, stirring until the mixture is completely uniform, then adding the mixture into 20g of the gelatin aqueous solution, stirring for 2 hours, uniformly mixing, pouring the mixture into a film mold, and drying for 24 hours under the conditions of the temperature of 40 ℃ and the humidity of 20% to obtain a flexible film material, wherein the label is P2.
Example 4
Preparing a gelatin aqueous solution with the gelatin mass fraction of 15%, mixing 3.19g of choline chloride and 2.81g of ethylene glycol, stirring until the mixture is completely mixed, then adding the mixture into 20g of the gelatin aqueous solution, stirring for 2 hours, uniformly mixing, pouring the mixture into a film mold, and drying for 24 hours under the conditions of the temperature of 40 ℃ and the humidity of 20% to obtain a flexible film material, which is marked as P3.
Example 5
Preparing a gelatin aqueous solution with the gelatin mass fraction of 15%, mixing 3g of choline chloride and 3g of sorbitol, stirring uniformly, adding the mixture into 20g of the gelatin solution, stirring for 2 hours, uniformly mixing, pouring the mixture into a film mold, and drying at the temperature of 40 ℃ and the humidity of 20% for 24 hours to obtain a flexible film material, wherein the label is P4.
The flexible film material P1-2 prepared in example 1, the flexible film material P2 prepared in example 3, the flexible film material P3 prepared in example 4, and the flexible film material P4 prepared in example 5 were subjected to a stress-strain test, and as shown in fig. 4, it can be seen from fig. 4 that the elastic modulus of all the flexible film materials was less than 500kPa, the ductility of P2 was superior to that of P1-2, the ductility of P1-2 was superior to that of P3, and the ductility of P3 was superior to that of P4.
Other tests:
and (3) testing the repair capability: the flexible film material P1-1 prepared in the embodiment 1 is cut into two sections, the two sections are immersed in hot water at the temperature of 80 ℃ for 30 seconds, a fracture is spliced into a whole after being taken out, and then the film is dried, and the two sections of film materials can be completely spliced together and have good ductility; the plasticized flexible film material P1-1 prepared in example 1 was cut into two pieces, then the fractures were spliced together, and then the heating table was heated to 70 ℃ for 1min, and the two pieces of film material could be completely spliced together and had good ductility.
And (3) testing the recyclability: the flexible film material P1-1 prepared in example 1 was cut into pieces, 3g of the pieces were added to 3g of water, heated to 80 ℃, stirred for 30 minutes, poured into a film mold, and dried at 40 ℃ and 20% humidity for 24 hours to obtain a flexible film material, which indicates that the flexible material prepared in example 1 was recyclable.
And (3) conductivity test: after the flexible film material P1-1 prepared in example 1 is connected to a circuit as an electrical connection wire, the LED light bulb can work normally and still maintain a normal working state during stretching.
In summary, the invention provides a flexible conductive biopolymer material and a preparation method and application thereof, the invention adds a deep eutectic solvent as a plasticizer of the biopolymer into the biopolymer solution, the deep eutectic solvent has low melting point, and contains a large amount of hydrogen bonds which can form interaction with the hydrogen bonds of the biopolymer to form new hydrogen bonds, so that the hydrogen bonds in the biopolymer chain are broken, the intermolecular interaction in the biopolymer chain is reduced, and the mobility of the biopolymer molecular chain is increased; in addition, compared with plasticizers (such as glycerol, mannitol and the like with single components) in the prior art, the deep eutectic solvent has better compatibility with the biopolymer, the content of the deep eutectic solvent in the prepared flexible conductive biopolymer material is up to 95%, and then intermolecular interaction in a polymer chain is further reduced, so that efficient plasticization of the biopolymer material is realized, the mechanical property of the biopolymer material is improved, the tensile strength of the biopolymer material is reduced, and the ductility of the biopolymer material is improved. The flexible conductive biopolymer material prepared by the invention has the advantages of repair capability, recyclability and conductive performance, and can be used for preparing flexible electronic devices.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing a flexible conductive biopolymer material is characterized by comprising the following steps:
dissolving a biopolymer in water to obtain a biopolymer aqueous solution;
adding a deep eutectic solvent into the biopolymer aqueous solution, and stirring to obtain an aqueous solution containing the deep eutectic solvent and the biopolymer;
and forming the aqueous solution containing the deep eutectic solvent and the biopolymer by a mechanical method, and drying to obtain the flexible conductive biopolymer material.
2. The method for preparing a flexible conductive biopolymer material according to claim 1, wherein the biopolymer is selected from one or more of cellulose, gelatin, chitosan, sodium alginate, carrageenan, agar, acacia, silk, and starch.
3. The method for preparing the flexible conductive biopolymer material of claim 1, wherein the mass content of the biopolymer in the biopolymer aqueous solution is 0.1% -30%.
4. The method for preparing the flexible conductive biopolymer material according to claim 1, wherein the deep eutectic solvent is prepared by mixing a first component and a second component, wherein the first component is selected from one or more of urea, glycerol, ethylene glycol, thiourea, gluconic acid, citric acid, fructose, sorbitol, xylitol and malic acid, and the second component is selected from one or two of amino acid and quaternary ammonium salt.
5. The method for preparing the flexible conductive biopolymer material of claim 4, wherein the mass content of the first component in the deep eutectic solvent is 25% -75%.
6. The method for preparing the flexible conductive biopolymer material of claim 4, wherein the amino acid is selected from one or more of glycine, alanine and proline, and/or the quaternary ammonium salt is selected from one or two of betaine and choline chloride.
7. The method for preparing a flexible conductive biopolymer material according to claim 1, wherein in the step of adding a deep eutectic solvent to the aqueous biopolymer solution, the mass of the deep eutectic solvent is 20% -95% of the mass sum of the deep eutectic solvent and the biopolymer in the aqueous biopolymer solution.
8. The method of claim 1, wherein the step of adding a deep eutectic solvent to the aqueous biopolymer solution further comprises adding one or more of a cross-linking agent, an electrolyte, a surfactant, and conductive nanoparticles to the aqueous biopolymer solution.
9. A flexible conductive biopolymer material prepared by the method of any one of claims 1-8.
10. Use of the flexible conductive biopolymer material according to claim 9 for the preparation of flexible electronic devices.
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