WO2022048165A1 - Conducteur d'ions nanofluide à base de cellulose structurée à motifs et son procédé de préparation et son application - Google Patents

Conducteur d'ions nanofluide à base de cellulose structurée à motifs et son procédé de préparation et son application Download PDF

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WO2022048165A1
WO2022048165A1 PCT/CN2021/089394 CN2021089394W WO2022048165A1 WO 2022048165 A1 WO2022048165 A1 WO 2022048165A1 CN 2021089394 W CN2021089394 W CN 2021089394W WO 2022048165 A1 WO2022048165 A1 WO 2022048165A1
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cellulose
parts
conductor material
ionic conductor
nanofluidic
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叶冬冬
邹捷
李琦华
郑格格
郑双
林泽婉
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五邑大学
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    • F03G7/04—Mechanical-power-producing mechanisms, not otherwise provided for or using energy sources not otherwise provided for using pressure differences or thermal differences occurring in nature
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
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    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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Definitions

  • the present invention relates to the field of nanofluid, in particular to a cellulose-based nanofluid ion conductor material of elementary order structure, a preparation method and application thereof.
  • Li Tian et al. (Sci. Adv. 2019, 5, u4238) used the natural oriented nano-microstructure of wood to prepare a wood film with nanofluid effect from top to bottom; Hu Liangbing of the University of Maryland et al. designed a class based on wood. Nanofluidic wood membrane realizes low heat recovery (Nat. Mater. 2019, 18, 608), osmotic power generation with salt concentration gradient (Adv. Energy Mater. 2019, 1902590).
  • the invention is based on the wide application of nanomaterials in the fields of energy conversion materials, energy storage materials, conductive materials, biomedical materials and the like.
  • a “top-down” strategy that is, from the molecular chain level of cellulose, prepared by dissolving cotton, chemical modification, etc.
  • An environmentally friendly, renewable, and degradable functional cellulose-based nanofluid ion conductor material, and its application in the field of salt gradient concentration osmotic power generation is realized.
  • An object of the present invention is to provide a cellulose-based nanofluidic ionic conductor material of elementary ordered structure, which can be realized by the following technical means:
  • a cellulose-based nano fluid ionic conductor material which is prepared from the following raw materials in parts by mass:
  • the cellulose solvent contains alkali, urea and water
  • the first functional nanofiller includes one or both of carbon nanotubes or carboxylated carbon nanotubes
  • the second functional nanofiller includes one or more of graphene, graphene oxide, MXene, boron nitride nanosheets or hydroxylated boron nitride nanosheets.
  • the cellulose solvent includes the following components in parts by mass:
  • the first functional nanofiller includes the following components in parts by mass:
  • the second functional nanofiller includes the following components in parts by mass:
  • Another object of the present invention is to provide a method for preparing the above-mentioned elementary ordered cellulose-based nanofluidic ionic conductor material, which can be achieved by the following technical means:
  • a method for preparing a cellulose-based nanofluidic ionic conductor material with a primitive order structure comprising the following steps:
  • the stirring temperature is -20--10°C
  • the stirring speed is 1000-5000 rpm.
  • the stirring time is 2-10min.
  • the chemical crosslinking agent is selected from one or more of epichlorohydrin, epichlorobutane, glutaraldehyde or polyethylene glycol glycidyl ether.
  • the coagulation bath is selected from one or more of sulfuric acid, hydrochloric acid, citric acid, phytic acid, acetic acid, methanol, ethanol or water.
  • Another object of the present invention is to provide the application of the above-mentioned elementary ordered cellulose-based nanofluid ionic conductor material in a cellulose-based nanofluid osmotic energy generator.
  • the invention discloses a cellulose-based nano-fluid ion conductor material of elementary order structure. Due to the addition of functional nano-fillers, the material has excellent electrochemical properties and strong mechanical stability.
  • the invention also discloses a preparation method of the above-mentioned elementary-order structured cellulose-based nano-fluid ion conductor material, which has the characteristics of low cost, simple process and environmental protection.
  • the invention also discloses the application of the elementary ordered cellulose-based nanofluid ion conductor material in the cellulose-based nanofluid osmotic energy generator, which expands the application of natural polymer materials in optics, electricity, energy storage and special Application in the field of functionalized biomedical materials.
  • Example 1 is a schematic diagram of the preparation of a cellulose nanofluidic ionic conductor material with a primitive ordered structure in Example 1 of the present invention
  • Fig. 2 is a picture of cellulose/nano-element composite solution in Example 1 of the present invention.
  • Fig. 3 is the SEM image of the cellulose-based nanofluidic ionic conductor material of elementary ordered structure in Example 1 of the present invention
  • Fig. 4 is the AFM image of the cellulose-based nanofluidic ionic conductor material of the elementary ordered structure in Example 2 of the present invention.
  • Figure 5 shows the ionic conductivity of the elementary-ordered cellulose-based nanofluidic ionic conductor material in different concentrations of KCl solution in Example 1 of the present invention, and the ordered cellulose/functional elementary composite membrane (Comparative Example 1) , the measurement diagram of the structured cellulose membrane (Comparative Example 2);
  • Example 6 is the graph of the gradient salt concentration diffusion potential and diffusion current in the application of the elementary-ordered cellulose-based nanofluid ionic conductor material in the cellulose-based nanofluid osmotic energy generator in Example 3 of the present invention.
  • MXene refers to a class of two-dimensional inorganic compounds. These materials consist of transition metal carbides, nitrides or carbonitrides several atomic layers thick.
  • the source of cellulose selected from one or more of cotton linter pulp, wood pulp, bamboo pulp and straw pulp;
  • the carbon nanotubes described in the embodiments of the present invention are purchased from NANOCYL TM , and the model is NC7000;
  • carboxylated carbon nanotubes described in the embodiment of the present invention are purchased from Pioneer Nano, and the model is XFM72;
  • the graphene described in the embodiment of the present invention is purchased from Pioneer Nano, and the model is XF001H;
  • the graphene oxide described in the embodiment of the present invention is purchased from Pioneer Nano, and the model is XF002-3;
  • the MXene described in the embodiment of the present invention is purchased from Pioneer Nano, and the model is XFK08;
  • the boron nitride nanosheets described in the embodiment of the present invention are purchased from Pioneer Nano, and the model is XFBN03-1;
  • hydroxylated boron nitride nanosheets described in the embodiments of the present invention are obtained by ultrasonically treating the above boron nitride in isopropanol (300W, 1h).
  • a fundamentally ordered cellulose-based nanofluid ionic conductor material is prepared from the following raw materials in parts by mass:
  • the preparation method of the above-mentioned elementary ordered cellulose nanofluidic ionic conductor membrane material comprises the following steps:
  • the composite alkali gel is drawn by external force (the drawing strain is 160%), and then placed in a 10 wt% sulfuric acid coagulation bath for 1 min to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • Example 1 is a flow chart of the preparation of the nano-element-ordered cellulose nanofluidic ionic conductor membrane material prepared in Example 1 of the present invention, illustrating that the present invention is based on a bottom-up strategy to construct nano-element-ordered fibers
  • the preparation process is simple and controllable, which is different from the cumbersome bottom-up construction methods such as wood-based materials.
  • Example 2 is a photo of the composite solution of the cellulose-based nanofluidic ionic conductor material prepared in Example 1 of the present invention, which shows that the cellulose solution in which the nano-elements are dispersed has good stability and good fluidity.
  • Fig. 3 is the SEM image of the cellulose-based nanofluid ionic conductor material in Example 1 of the present invention, which shows that the structure of the nano-element-ordered cellulose nanofluid ionic conductor film after dehydration and drying is very dense, and the surface is flat, Highly oriented with nanoscale ion channels.
  • Figure 5 illustrates that the cellulose functional membrane with the basic element order structure prepared in Example 1 has higher ionic conductivity than the ordered structure composite membrane without chemical modification and the oriented cellulose membrane, which is more conducive to the selective transport of ions.
  • a fundamentally ordered cellulose-based nanofluid ionic conductor material is prepared from the following raw materials in parts by mass:
  • the preparation method of the above-mentioned elementary ordered cellulose nanofluidic ionic conductor membrane material comprises the following steps:
  • the composite alkali gel is drawn by external force (the drawing strain is 180%), and then placed in a 2wt% phytic acid coagulation bath for 10 minutes to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • Example 4 is an AFM image of the cellulose-based nanofluidic ionic conductor material in Example 2 of the present invention, which shows that there are a large number of long-range ordered nanofibers in the functional cellulose membrane, showing a highly oriented and highly densified structure, which is Ions produce better transport properties in nanoscale channels.
  • a fundamentally ordered cellulose-based nanofluid ionic conductor material is prepared from the following raw materials in parts by mass:
  • a preparation method of a cellulose nanofluid ionic conductor membrane material with a primitive order structure comprising the following steps:
  • the composite alkali gel is drawn by external force (drawing strain is 200%), and then placed in a coagulation bath of absolute ethanol for 20 minutes to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • Figure 6 illustrates the diffusion voltage and diffusion current that the functional cellulose nanofluidic film prepared in Example 3 can generate under 10-fold, 100-fold, 100-fold, and 1000-fold salt concentration gradients. Simulations verify the feasibility of salt concentration gradient power generation.
  • a fundamentally ordered cellulose-based nanofluid ionic conductor material is prepared from the following raw materials in parts by mass:
  • the preparation method of the above-mentioned elementary ordered cellulose nanofluidic ionic conductor membrane material comprises the following steps:
  • the composite alkali gel is drawn by external force (drawing strain is 140%), and then placed in a 10wt% hydrochloric acid coagulation bath for 1 min to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • a fundamentally ordered cellulose-based nanofluid ionic conductor material is prepared from the following raw materials in parts by mass:
  • the preparation method of the above-mentioned elementary ordered cellulose nanofluidic ionic conductor membrane material comprises the following steps:
  • the composite alkali gel is drawn by external force (the drawing strain is 170%), and then placed in a 10 wt% phytic acid coagulation bath for 10 minutes to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • a fundamentally ordered cellulose-based nanofluid ionic conductor material is prepared from the following raw materials in parts by mass:
  • the preparation method of the above-mentioned elementary ordered cellulose nanofluidic ionic conductor membrane material comprises the following steps:
  • the composite alkali gel is drawn by external force (the drawing strain is 160%), and then placed in a 10wt% citric acid coagulation bath for 5 minutes to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • Comparative Example 1 is a regenerated cellulose/functional element composite membrane without chemical modification, while Example 1 is TEMPO oxidized, and the cellulose molecular chain is negatively charged. Structured cellulose/functional motif composite membranes.
  • a preparation method of a structured cellulose/functional element composite membrane material comprising the following steps:
  • the composite alkali gel is drawn by external force (the drawing strain is 160%), and then placed in a 10 wt% sulfuric acid coagulation bath for 1 min to fix the orientation to obtain a highly oriented cellulose/nano-element composite hydrogel;
  • Comparative Example 2 The difference between the components of Comparative Example 2 and Example 1 is that the components in Comparative Example 2 are only regenerated cellulose, while the components in Example 1 contain regenerated cellulose and nano-functional primitives.
  • a preparation method of a sequenced cellulose membrane material comprising the following steps:
  • the alkali gel is drawn by external force (drawing strain is 160%), and then placed in a 10wt% sulfuric acid coagulation bath for 1min to fix the orientation to obtain a highly oriented cellulose hydrogel;
  • Test method prepare six concentrations of potassium chloride solutions of 10 -6 , 10 -5 , 10 -4 , 10 -3 , 10 -2 and 10 -1 M, and test the conductivity values of the bulk solutions of the six concentrations respectively. Next, the conductance of nano-element-structured cellulose nanofluidic ionic conductor membranes immersed in 10 -6 , 10 -5 , 10 -4 , 10 -3 , 10 -2 , and 10 -1 M potassium chloride solution were tested. Rate. Two parallel test probes are placed at both ends of the sample to be tested, then a certain potential is applied to both ends of the probes, and then the current through the sample is measured. An IV image was made with the obtained current and potential, fitted, and the slope was taken as the conductivity.
  • the formula for calculating conductivity ( ⁇ ) is as follows:
  • G is the measured conductance (ie, the slope of the I-V curve)
  • l is the length of the measured composite film
  • h is the measured height of the film
  • w is the measured width of the composite film.
  • Test method Two parallel test probes are placed on both ends of the sample to be tested, and the inside of the sample is immersed in 10 -6 , 10 -5 , 10 -4 , 10 -3 , 10 -2 , 10 -1 M chloride respectively. The potassium solution then applies a certain potential across the probe, and the current through the ordered cellulose/functional motif composite membrane is then measured. An IV image was made with the obtained current and potential, fitted, and the slope was taken as the conductivity.
  • the formula for calculating conductivity ( ⁇ ) is as follows:
  • G is the measured conductance (ie, the slope of the IV curve)
  • l is the length of the sequenced structured cellulose/functional motif composite membrane
  • h is the height of the sequenced structured cellulose/functional motif composite membrane
  • w is The width of the sequenced structured cellulose/functional motif composite membrane.
  • Test method Two parallel test probes are placed on both ends of the sample to be tested, and the inside of the sample is immersed in 10 -6 , 10 -5 , 10 -4 , 10 -3 , 10 -2 , 10 -1 M chloride respectively. The potassium solution then applies a potential across the probe and the current through the structured cellulose membrane is then measured. An IV image was made with the obtained current and potential, fitted, and the slope was taken as the conductivity.
  • the formula for calculating conductivity ( ⁇ ) is as follows:
  • G is the measured conductance (ie, the slope of the I-V curve)
  • l is the length of the sequenced textured cellulose membrane
  • h is the height of the sequenced textured cellulose membrane
  • w is the width of the sequenced textured cellulose membrane.
  • a system of mixing seawater (0.5M NaCl) and river water (0.01M NaCl) is designed, with seawater and river water on both sides, and a highly oriented functional cellulose nanofluid material in the middle, which can obtain a certain voltage and current.
  • the above-mentioned functional film is placed between the two grooves; finally, the two test electrodes of the digital source meter are immersed in the above-mentioned two grooves respectively to test and record the diffusion voltage and diffusion current generated by the functional cellulose film.
  • Example 1 has different degrees of advantages in electrical conductivity at different solution concentrations.

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Abstract

La présente invention se rapporte à un matériau conducteur d'ions nanofluide à base de cellulose, qui est préparé à partir des matières premières suivantes : de la cellulose, un solvant cellulosique et une première ou une seconde nanocharge fonctionnelle. Le matériau divulgué présente d'excellentes propriétés électrochimiques et une stabilité mécanique élevée. Est en outre divulgué dans la présente invention, un procédé de préparation du matériau conducteur d'ions nanofluide à base de cellulose, et le procédé présente comme caractéristiques un faible coût, un processus simple et le respect de l'environnement. Est en outre divulguée dans la présente invention, une application du matériau conducteur d'ions nanofluide à base de cellulose dans un générateur d'énergie osmotique nanofluide à base de cellulose, et une application d'un matériau polymère naturel dans les domaines de l'optique, de l'électricité, du stockage d'énergie et des matériaux biomédicaux fonctionnalisés spéciaux est développée.
PCT/CN2021/089394 2020-09-04 2021-04-23 Conducteur d'ions nanofluide à base de cellulose structurée à motifs et son procédé de préparation et son application WO2022048165A1 (fr)

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CN114437389A (zh) * 2022-03-02 2022-05-06 五邑大学 一种具有高表面拉曼增强效应有序纳米褶皱纤维素复合膜及其制备方法
CN114605708A (zh) * 2022-03-21 2022-06-10 上海理工大学 一种MXene纳米纤维素碳纳米管复合材料的制备方法

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CN112143041B (zh) * 2020-09-04 2022-04-08 五邑大学 基元序构化纤维素基纳米流体离子导体材料和制备方法及应用
CN114471214A (zh) * 2022-02-11 2022-05-13 中国矿业大学 一种丙三醇石墨烯量子点纳米流体的制备方法及纳米流体
CN114957805B (zh) * 2022-05-24 2023-11-24 南京林业大学 一种二维纤维素纳米流体通道膜及其制备方法与应用

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