CN116478427A - All-natural cellulose-based ionic gel material and preparation method and application thereof - Google Patents

All-natural cellulose-based ionic gel material and preparation method and application thereof Download PDF

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Publication number
CN116478427A
CN116478427A CN202310390176.1A CN202310390176A CN116478427A CN 116478427 A CN116478427 A CN 116478427A CN 202310390176 A CN202310390176 A CN 202310390176A CN 116478427 A CN116478427 A CN 116478427A
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cellulose
gel material
ionic gel
natural cellulose
preparation
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吴栋
张嘉恒
王密
喻文
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Shenzhen Graduate School Harbin Institute of Technology
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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
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/11—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids from solid polymers
    • 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
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
    • C08J3/096—Nitrogen containing compounds
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
    • G01D21/00—Measuring or testing not otherwise provided for
    • G01D21/02—Measuring two or more variables by means not covered by a single other subclass
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/02—Cellulose; Modified cellulose

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  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
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  • Polymers & Plastics (AREA)
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Abstract

The invention relates to the technical field of ionic gel, in particular to an all-natural cellulose-based ionic gel material and a preparation method and application thereof. The preparation method of the invention comprises the following steps: heating biomass material in sodium chlorite water solution to obtain cellulose; and (3) coating the cellulose with the ionic liquid, heating at a preset temperature to enable the cellulose to be dissolved in situ, and then cooling to room temperature to enable the cellulose to self-assemble, so as to obtain the all-natural cellulose-based ionic gel material. The preparation method provided by the invention has simple process and does not need toxic or harmful organic solvents. The all-natural cellulose-based ionic gel material prepared by the preparation method provided by the invention has the advantages of flexibility, high transparency and high ionic conductivity, can realize detection of various motions of a human body and detection of environmental temperature and humidity, and is expected to be applied to various flexible electronic devices including super capacitors, flexible batteries, friction nano generators, flexible thermoelectric devices and the like.

Description

All-natural cellulose-based ionic gel material and preparation method and application thereof
Technical Field
The invention relates to the technical field of ionic gel, in particular to an all-natural cellulose-based ionic gel material and a preparation method and application thereof.
Background
With the development of human society, the use of large amounts of non-renewable fossil fuels and derivatives thereof raises various environmental issues, and the use of sustainable renewable biomass materials to replace fossil products is the best countermeasure. At present, ionic gel materials with high mechanical strength and flexibility are widely applied to the preparation and research of high-performance flexible electronic devices, but the most used polymer materials are synthesized artificially (most common polymer materials comprise acrylic acid and acrylamide). If natural polymer materials are used as framework materials of the gel, the gel is used for replacing artificially synthesized materials, and environmental problems caused by the use of non-renewable materials can be reduced. Cellulose has long been an important research object for domestic and foreign specialists as a natural polymer material with the largest reserves in nature, but nano cellulose is mainly used as a research object. The preparation process of the nanocellulose is complex, and reagents required in the preparation process are toxic and expensive, so that the mass production is not facilitated.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide an all-natural cellulose-based ionic gel material, and a preparation method and application thereof, and aims to solve the environmental problem caused by the fact that the existing ionic gel material adopts an artificially synthesized polymer material as a framework material of gel.
The technical scheme of the invention is as follows:
in a first aspect of the present invention, there is provided a method for preparing an all-natural cellulose-based ionic gel material, comprising the steps of:
heating biomass material in sodium chlorite water solution to obtain cellulose;
and (3) coating the ionic liquid on the cellulose, heating to enable the cellulose to be dissolved in situ, and then cooling to room temperature to enable the cellulose to self-assemble, so as to obtain the all-natural cellulose-based ionic gel material.
Optionally, the biomass material is selected from one or more of waste wood, bamboo and straw.
Optionally, the biomass material is waste wood.
Optionally, the mass ratio of the biomass material to sodium chlorite is 1: (1-10).
Optionally, the sodium chlorite aqueous solution is a sodium chlorite aqueous solution with the pH adjusted, and the pH of the sodium chlorite aqueous solution is 2-6.
Optionally, the temperature of the heating treatment is 50-150 ℃, and the time of the heating treatment is 1-100h.
Optionally, in the step of coating the cellulose with an ionic liquid, the mass ratio of the ionic liquid to the cellulose is (8-10): 1.
Optionally, in the step of heating to dissolve the cellulose in situ, the heating is performed at a temperature of 50-100 ℃ for a time of 1-100h.
In a second aspect of the present invention, there is provided an all-natural cellulose-based ionic gel material, wherein the all-natural cellulose-based ionic gel material is mainly composed of a cellulose skeleton and an ionic liquid capable of ionic conduction;
the all-natural cellulose-based ionic gel material is prepared by adopting the preparation method disclosed by the invention.
In a third aspect, the invention provides an application of the all-natural cellulose-based ionic gel material as a sensing material in the aspects of ambient temperature and humidity detection.
The beneficial effects are that: the invention provides an all-natural cellulose-based ionic gel material, and a preparation method and application thereof. In the prior art, when the ionic gel material is prepared, non-renewable synthetic polymer materials are mainly used, and the polymer materials are mainly derived from petrochemical materials, so that a series of environmental problems can be caused. However, the invention converts biomass materials (such as waste wood) into the ionic gel materials with high added value through the processes of delignification, in-situ dissolution, self-assembly and the like, thereby not only realizing the high added value utilization of the biomass materials such as wood waste and the like, but also solving the problems of space occupation and resource waste caused by the biomass materials and being more in line with the concept of green sustainable development. Compared with the prior art, the preparation method provided by the invention has the advantages of simple process and no need of toxic or harmful organic solvents. In addition, the preparation method provided by the invention has the advantages of low cost, no need of complex equipment, mild condition, good stability, environment friendliness and mass production.
Drawings
FIG. 1 is a flow chart showing the preparation of the all-natural cellulose-based ionic gel material according to example 1 of the present invention.
FIG. 2 is an optical photograph of a balsa board in example 1 of the present invention.
FIG. 3 is an optical photograph of delignified balsa wood board in example 1 of the present invention.
FIG. 4 is an optical photograph of an all-natural cellulose-based ionic gel material according to example 1 of the present invention.
FIG. 5 shows the use of an all-natural cellulose-based ionic gel material as an ambient temperature sensor in example 2 of the present invention.
FIG. 6 shows the use of an all-natural cellulose-based ionic gel material as an ambient humidity sensor in example 2 of the present invention.
Detailed Description
The invention provides an all-natural cellulose-based ionic gel material, a preparation method and application thereof, and the invention is further described in detail below in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The embodiment of the invention provides a preparation method of an all-natural cellulose-based ionic gel material, which comprises the following steps:
s1, heating a biomass material in a sodium chlorite aqueous solution to obtain cellulose;
s2, coating the ionic liquid on the cellulose, heating at a preset temperature to enable the cellulose to be dissolved in situ, and then cooling to room temperature to enable the cellulose to self-assemble, so that the all-natural cellulose-based ionic gel material is obtained.
In the embodiment, the biomass material is heated in sodium chlorite aqueous solution to obtain a completely delignified biomass material (i.e. cellulose); and then coating a certain amount of ionic liquid (in a uniform dripping mode) on the biomass material completely removing lignin, heating at a certain temperature to realize in-situ dissolution of cellulose, and cooling the cellulose to room temperature under a certain humidity condition (generally RH 50 wt%) to realize self-assembly of cellulose molecules, so as to obtain the all-natural cellulose-based ionic gel material. Under the condition of a certain humidity, water molecules enter a cellulose-ionic liquid system to form hydrogen bonds with cellulose molecules, so that self-assembly of cellulose chains is promoted, and a gel material is formed.
In this example, in situ dissolution of cellulose was achieved by coating an ionic liquid onto a fully delignified biomass material. However, in the prior art, cellulose is usually directly dissolved in an ionic liquid, a large amount of bubbles are formed in the stirring and dissolving process, high-temperature vacuumizing is needed for removal, and the formed cellulose solution has high viscosity and poor operability at normal temperature. The embodiment adopts an in-situ dissolution method, so that the defects are effectively avoided.
In this embodiment, the biomass material has the characteristics of being renewable, biodegradable and excellent in mechanical properties, the sodium chlorite aqueous solution can completely remove lignin in the biomass material, the designability and the applicability of the wood are improved, the ionic liquid is a green solvent of cellulose, the in-situ dissolution of cellulose can be realized, meanwhile, the ionic liquid has the ionic conductivity, and the ionic liquid and the cellulose are combined to give the all-natural cellulose-based ionic gel material good transparency, good mechanical strength and ionic conductivity, that is, the all-natural cellulose-based ionic gel material has good transparency, good mechanical strength and good ionic conductivity. In addition, the all-natural cellulose-based ionic gel material has good self-repairing performance and freezing resistance, and the reusability and the practicability of the all-natural cellulose-based ionic gel material under severe environments are further improved. The all-natural cellulose-based ionic gel material can be used as a sensing component of electronic skin, and can realize real-time monitoring of various activities of human bodies and environmental humiture.
In the prior art, when the ionic gel material is prepared, non-renewable synthetic polymer materials are mainly used, and the polymer materials are mainly derived from petrochemical materials, so that a series of environmental problems can be caused. However, the embodiment converts biomass materials (such as waste wood) into the ionic gel materials with high added value through the processes of delignification, in-situ dissolution, self-assembly and the like, so that the high added value utilization of the biomass materials such as wood waste and the like can be realized, the problems of space occupation and resource waste caused by the biomass materials can be solved, and the environment-friendly sustainable development concept is more met.
Compared with the prior art, the preparation method provided by the embodiment has simple process and does not need toxic or harmful organic solvents. In addition, the preparation method provided by the embodiment has the advantages of low cost, no need of complex equipment, mild condition, good stability, environmental protection and mass production.
In one embodiment, before step S1, the method further comprises the steps of:
and ultrasonically cleaning the biomass material with water (preferably ultrapure water), drying, and removing dust on the surface of the biomass material.
In specific implementation, the ultrasonic cleaning time can be 1min-1000min, the drying temperature can be 40-100 ℃ and the ultrasonic cleaning time can be 1h-100h. The ultrasonic cleaning for 1min-1000min can ensure that dust on the surface of the biomass material is removed completely, and is beneficial to the subsequent preparation of all-natural cellulose-based ionic gel materials.
In step S1, in one embodiment, the biomass material is selected from one or more of waste wood, bamboo, and straw, but is not limited thereto.
In one embodiment, the biomass material is waste wood.
In the embodiment, the waste wood is cheap and easy to obtain, and the wood belongs to natural resources and is green.
In one embodiment, the biomass is in the form of one or more of a cake, a flake, and a powder.
In one embodiment, the mass ratio of biomass material to sodium chlorite is 1: (1-10).
Within this ratio range, the formation of all-natural cellulose-based ionic gel materials is favored.
In one embodiment, the aqueous sodium chlorite solution is a pH-adjusted aqueous sodium chlorite solution having a pH of 2-6 (e.g., 4.6). Further, an acid (e.g., acetic acid) is used to adjust the pH of the aqueous sodium chlorite solution.
In one embodiment, the pH adjusted aqueous sodium chlorite solution is formulated by:
dissolving sodium chlorite in water to obtain sodium chlorite water solution;
and adding a small amount of acetic acid into the sodium chlorite aqueous solution to adjust the pH of the solution, thereby obtaining the sodium chlorite aqueous solution after the pH adjustment.
In one embodiment, the mass ratio of biomass material, sodium chlorite to acetic acid is 1: (1-10): (0.01-1).
In one embodiment, the temperature of the heat treatment is 50-150 ℃ (e.g., 90 ℃), and the time of the heat treatment is 1-100 hours, preferably 1-50 hours, and more preferably 1-10 hours (e.g., 6 hours).
In step S2, in one embodiment, in the step of coating the cellulose with an ionic liquid, the mass ratio of the ionic liquid to the cellulose is (8-10): 1. Better in-situ dissolution effect of lignocellulose can be realized at the ratio, and the waste of ionic liquid is avoided.
In one embodiment, the ionic liquid may be selected from one or more of 1-ethyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole hydrochloride, 1-butyl-3-methylimidazole hydrochloride, and the like.
In one embodiment, the heating is performed at a temperature of 50-100deg.C (e.g., 90deg.C) for a period of 1-100 hours, preferably 1-50 hours, and more preferably 1-5 hours (e.g., 1.5 hours) in the step of dissolving the cellulose in situ.
Taking waste wood as a raw material for example, the preparation process of the all-natural cellulose-based ionic gel material of this embodiment is further described. In the embodiment, the waste timber is used as a raw material, the waste timber is heated in sodium chlorite aqueous solution with a certain pH value, the timber is changed from dark brown into white, and the fully delignified waste timber (namely cellulose) is obtained after drying; and uniformly dripping a certain amount of ionic liquid on the waste wood completely removing lignin, performing heating treatment at a certain temperature to realize in-situ dissolution of cellulose, and cooling the cellulose to room temperature under a certain humidity condition to realize self-assembly of cellulose molecules, so as to obtain the all-natural cellulose-based ionic gel material.
In this embodiment, the waste wood has the characteristics of being renewable, biodegradable and excellent in mechanical properties, the sodium chlorite aqueous solution can completely remove lignin in the waste wood, designability and applicability of the wood are improved, the ionic liquid is a green solvent of cellulose, in-situ dissolution of cellulose can be realized, and meanwhile, the ionic liquid has ion conductivity, and the combination of the two effects gives the all-natural cellulose-based ion gel material good transparency, good mechanical strength and ion conductivity, that is, the all-natural cellulose-based ion gel material has good transparency, good mechanical strength and ion conductivity. In addition, the all-natural cellulose-based ionic gel material has good self-repairing performance and freezing resistance, and the reusability and the practicability of the all-natural cellulose-based ionic gel material under severe environments are further improved. The all-natural cellulose-based ionic gel material can be used as a sensing component of electronic skin, and can realize real-time monitoring of various activities of human bodies and environmental humiture.
The embodiment of the invention also provides an all-natural cellulose-based ionic gel material prepared by the preparation method.
The all-natural cellulose-based ionic gel material consists of an all-natural cellulose framework and ionic liquid capable of conducting ions, so that the use of an artificially synthesized high molecular framework material is avoided, and the all-natural cellulose-based ionic gel material can be completely biodegraded, so that the all-natural cellulose-based ionic gel material is more environment-friendly; the cellulose source is waste wood, a new idea is provided for the high added value utilization of the waste wood, and the all-natural cellulose-based ionic gel material has high transparency, self-healing, high strength and high ionic conductivity.
The embodiment of the invention also provides application of the all-natural cellulose-based ionic gel material as a sensing material in the aspects of ambient temperature and humidity detection.
The invention is further illustrated by the following specific examples.
Example 1
The preparation of the all-natural cellulose-based ionic gel material is shown in the figure 1.
1mm thick bar Sha Muban (i.e. FIG. 2) was placed in 5wt% aqueous sodium chlorite solution adjusted to pH 4.6 with acetic acid and heat treated at 90℃for 6 hours.
The heat treated bar Sha Muban was rinsed with ultra pure water to completely remove chemical residues and dried at room temperature to give a fully delignified bar Sha Muban (i.e. fig. 3).
The ionic liquid (1-ethyl-3-methylimidazole acetate) with the mass 9 times that of the fully delignified basha wood board is uniformly dripped on the surface of the fully delignified basha wood board, and the processing is carried out for 1.5 hours at the temperature of 90 ℃ to realize the in-situ dissolution of cellulose.
The cellulose gel is stored for 4 hours under the condition of RH 45wt percent, cellulose molecule self-assembly is realized, and finally the transparent, flexible and ion-conductive all-natural cellulose-based ion gel material (namely, figure 4) is obtained.
Example 2
The all-natural cellulose-based ionic gel material prepared in example 1 was used as a sensing material for the detection of ambient temperature and humidity.
The method comprises the following specific steps:
the all-natural cellulose-based ionic gel material prepared in example 1 was used as a sensing material.
An enameled wire with the diameter of 0.3mm is used as a lead, and the all-natural cellulose-based ionic gel sensor is connected with a DAQ6510 universal meter.
When the sensor is tested to monitor the environment temperature in real time, the full-natural cellulose-based ionic gel sensor is placed on a semiconductor temperature control table, a circulating temperature change program (20-70 ℃) is set, and the real-time resistance change is recorded through a computer (namely, figure 5).
When the sensor is used for monitoring the environment humidity in real time, the all-natural cellulose-based ionic gel sensor is placed in a temperature and humidity control box, a circulating humidity change program (RH 30-60 wt%) is set, and real-time resistance change is recorded through a computer (namely, the temperature and humidity control box is shown in FIG. 6).
In summary, the invention provides an all-natural cellulose-based ionic gel material, and a preparation method and application thereof, wherein the preparation method comprises the following steps: providing a biomass material, sodium chlorite and an ionic liquid; delignification treatment is carried out on the biomass material in a sodium chlorite aqueous solution with a certain pH value, so as to obtain a delignified biomass material; and uniformly dripping a certain amount of ionic liquid on the delignified biomass material, heating to complete in-situ dissolution of cellulose, and then cooling to complete self-assembly of cellulose molecules to obtain the all-natural cellulose-based ionic gel material. The preparation method provided by the invention has the advantages of simple process, no need of toxic or harmful organic solvents, low cost, no need of complex equipment, mild conditions, good stability, environment friendliness and capability of mass production on a large scale. The all-natural cellulose-based ionic gel material prepared by the preparation method provided by the invention has the advantages of flexibility, high mechanical strength, high transparency and high ionic conductivity, can realize detection of various motions of a human body and detection of environmental temperature and humidity, and is expected to be applied to various flexible electronic devices including super capacitors, flexible batteries, friction nano generators, flexible thermoelectric devices and the like.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.

Claims (10)

1. A method for preparing an all-natural cellulose-based ionic gel material, which is characterized by comprising the following steps:
heating biomass material in sodium chlorite water solution to obtain cellulose;
and (3) coating the ionic liquid on the cellulose, heating to enable the cellulose to be dissolved in situ, and then cooling to room temperature to enable the cellulose to self-assemble, so as to obtain the all-natural cellulose-based ionic gel material.
2. The method of claim 1, wherein the biomass material is selected from one or more of waste wood, bamboo, and straw.
3. The method of claim 2, wherein the biomass material is waste wood.
4. The method of claim 1, wherein the mass ratio of biomass material to sodium chlorite is 1: (1-10).
5. The method according to claim 1, wherein the aqueous sodium chlorite solution is a pH-adjusted aqueous sodium chlorite solution having a pH of 2 to 6.
6. The method according to claim 1, wherein the temperature of the heating treatment is 50 to 150 ℃ and the time of the heating treatment is 1 to 100 hours.
7. The method according to claim 1, wherein in the step of coating the cellulose with an ionic liquid, the mass ratio of the ionic liquid to the cellulose is (8-10): 1.
8. The method according to claim 1, wherein in the step of heating to dissolve the cellulose in situ, the heating is performed at a temperature of 50 to 100 ℃ for a time of 1 to 100 hours.
9. The all-natural cellulose-based ionic gel material is characterized by mainly comprising a cellulose skeleton and ionic liquid capable of conducting ions;
the all-natural cellulose-based ionic gel material is prepared by the preparation method of any one of claims 1-8.
10. Use of an all natural cellulose-based ionic gel material according to claim 9 as a sensing material for ambient temperature and humidity detection.
CN202310390176.1A 2023-04-04 2023-04-04 All-natural cellulose-based ionic gel material and preparation method and application thereof Pending CN116478427A (en)

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