CN112920440B - Nano cellulose base composite membrane and preparation method and application thereof - Google Patents
Nano cellulose base composite membrane and preparation method and application thereof Download PDFInfo
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- C08J2301/04—Oxycellulose; Hydrocellulose
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
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- 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
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
Abstract
A nano cellulose-based composite membrane comprises nano cellosilk, michael nanosheets and polyphenol compounds, is combined through hydrogen bonds to form a uniform membrane structure, and is prepared through the following steps: 1) preparing nano-cellosilk, michaene nanosheets and polyphenol compounds into nano-cellosilk dispersion liquid, michaene nanosheet dispersion liquid and polyphenol compound dispersion liquid respectively; 2) mixing the nano-cellosilk dispersion liquid and the michael nanosheet dispersion liquid to obtain a mixed solution; 3) dropwise adding the polyphenol compound dispersion liquid into the mixed solution obtained in the step 2), and stirring for 6-12h to obtain a uniform mixed solution; 4) and (3) carrying out suction filtration on the uniform mixed solution, and drying a filter cake for 6-8h to obtain the nano cellulose base composite membrane with the thickness of 10-30 mu m. The nano cellulose-based composite membrane prepared by the method has high mechanical strength and excellent joule heat and antibacterial performance.
Description
Technical Field
The invention relates to the field of materials, in particular to a nano cellulose-based composite membrane and a preparation method and application thereof.
Background
In the current society pursuing green energy conservation and intellectualization, researchers have successfully designed and developed various intelligent drivers capable of reversibly deforming in response to external stimuli (such as humidity, electricity, light, temperature and magnetism) inspired by biological behaviors (that chameleon autonomously changes body color to resist external enemies, forages and forages, and catches food by controlling opening and closing of leaves by catching flies). In particular, humidity responsive actuators are of great interest due to environmental friendliness and humidity availability, and have great potential for development in many sophisticated areas, including smart wearable devices, soft robots, artificial muscles, energy converters, and the like. There are two general strategies for designing humidity responsive actuators: 1. the double-layer/multi-layer structure is constructed according to the obvious difference of the hydrophilicity among the materials, and the self-driving behavior is realized by responding to the uniform humidity stimulation. 2. A uniform unitary structure comprised of one or more hydrophilic materials that is self-actuating in response to localized moisture stimuli. Unfortunately, the bi-or multi-layer humidity responsive actuator of the first case described above is generally complicated to manufacture, has poor mechanical properties, and has poor interface stability due to strain mismatch between materials. Therefore, in order to overcome these problems, designing a single-layer humidity-responsive actuator has been the focus of attention. Despite the remarkable progress made by the single-layer humidity-responsive actuator, most of the single-layer humidity-responsive actuators reported are based on synthetic materials and mainly focus on improving the humidity-responsive performance of the actuator, while neglecting the development of mechanical strength and multifunctional performance, which hinders its wider application.
The nano-cellulose is the most promising candidate raw material for constructing the humidity response driver due to the advantages of wide sources, renewability, degradability, biocompatibility, abundant moisture absorption functional groups and the like. However, the pure nano cellulose membrane has the limitations of low strength and single function, and the development of nano cellulose in the field of emerging intelligent materials is limited. How to introduce functional materials into the nanocellulose has great challenge on endowing the body with high mechanical properties and versatility on the premise of not influencing humidity response.
Disclosure of Invention
One of the objects of the present invention is to provide a nanocellulose-based composite membrane having high mechanical strength and excellent joule heat and antibacterial properties, in view of the shortcomings of the prior art.
The invention also aims to provide a preparation method of the nano cellulose-based composite membrane, which has the advantages of simple preparation process, green and environment-friendly raw materials and easy implementation.
The technical scheme for realizing one purpose of the invention is as follows: a nano cellulose base composite film comprises nano cellosilk, Michelene nano-sheets and a polyphenol compound, and a uniform film structure is formed by hydrogen bonding.
Further, the diameter of the nanofiber is 3-5nm, the length-diameter ratio is greater than 1000, preferably, the length of the nanofiber is 3-10um, the average size of the michael nanosheet is greater than or equal to 300nm, the thickness of the michael nanosheet is 1-3nm, preferably, the average size of the michael nanosheet is 300-500nm, and the thickness of the michael nanosheet is 1-2 nm.
Further, the thickness of the film-like structure is 10 to 30 μm, preferably 15 μm.
Further, the mass ratio of the nano-cellosilk to the michael nanosheets to the polyphenol compound is 100: 25-100: 2.5-15.
Preferably, the polyphenol compound is any one or a mixture of several of tannic acid, dopamine, gallic acid and lignin.
The second technical scheme for realizing the aim of the invention is as follows: the preparation method of any one of the above nanocellulose-based composite membranes, comprising the steps of:
1) preparing nano-cellosilk, michaene nanosheets and polyphenol compounds into nano-cellosilk dispersion liquid, michaene nanosheet dispersion liquid and polyphenol compound dispersion liquid respectively;
2) mixing the nano-cellosilk dispersion liquid and the michael nanosheet dispersion liquid to obtain a mixed solution;
3) dropwise adding the polyphenol compound dispersion liquid into the mixed solution obtained in the step 2), and stirring for 6-12h to obtain a uniform mixed solution;
4) and (3) carrying out suction filtration on the uniform mixed solution, and drying a filter cake for 6-8h to obtain the nano cellulose composite membrane with the thickness of 10-30 mu m.
Preferably, the concentration of the nanofiber silk dispersion liquid and the michael nanosheet dispersion liquid in the step 1) is 0.3-0.5 wt%.
Further, the nano-fiber in the step 1) is prepared by a TEMPO oxidation method, and the Michael alkene nano-sheet is etched by using LiF/HCl solution to obtain Ti3AlC2MAX phase is prepared.
Preferably, the suction filtration in the step 4) is vacuum filtration in a suction filtration cup, and the drying is natural drying.
The invention also provides the use of any one of the above nanocellulose-based composite membranes in the preparation of a humidity-responsive actuator.
Further, humidity response driver is two semilunar valve shapes, opens or closes through responding to humidity, and is preferred, humidity response driver is applied to intelligent clothes, opens or closes through responding to humidity, realizes automatic heat dissipation, falls wet, keeps warm.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the nano-cellulose composite membrane prepared by the method is composed of one-dimensional nano-fiber filaments, two-dimensional michael nano-sheets and a biological macromolecular polyphenol compound, and integrates excellent humidity response, mechanical strength, Joule heat and antibacterial performance. The michael nanosheet is rich in oxygen-containing functional groups on the surface, and the polyphenol compounds contain a large amount of phenolic hydroxyl groups and respectively form multiple hydrogen bonds with the nano-fiber filaments, so that the mechanical property of the prepared nano-cellulose composite membrane can be effectively improved, and the application range of the nano-cellulose composite membrane is expanded. Based on the hydrophilic nature of the nano-fiber filaments and the behavior that the layer distance of the Michelene nano-sheet can change along with the induction of water molecules, the nano-cellulose composite membrane has excellent humidity response capability. In addition, the michael nano sheet has unique conductivity, endows the nano cellulose composite membrane with excellent joule heat performance, and the biological macromolecular polyphenol compound has natural antibacterial capability and also endows the nano cellulose composite membrane with an antibacterial function.
2. The raw material used for preparing the nano-cellulose composite membrane is the nano-cellulose filaments, so that the nano-cellulose composite membrane is green and environment-friendly, has low cost and realizes high-value utilization of cellulose.
3. The invention prepares the raw materials into dispersion, completes bond bonding in a solution system, and then obtains a uniform composite film by adopting the modes of suction filtration and drying, thereby avoiding the problem that the traditional double-layer or multi-layer composite material is easy to strip, and having beneficial bending-unbending stability (more than 1000 times). Meanwhile, the method is simple in process, environment-friendly and safe, and is beneficial to industrial production.
4. The invention utilizes one-dimensional nano-fiber filaments, two-dimensional michael nano-sheets and biomacromolecule polyphenol compounds as raw materials, and the prepared nano-cellulose composite membrane presents a unique 'brick-bridge-mud' shell-like structure. Wherein, the nanometer fiber silk is used as a reinforcement to play the role of cement; the michael nano sheet is used as a two-dimensional conductive material, plays the role of a shell brick, and the polyphenol compound is used as a binder to form an effective bridge between the nanofiber silk and the michael nano sheet. The three components form multiple hydrogen bonds, so that the prepared nano cellulose-based composite membrane has excellent mechanical strength which can reach 275.4 MPa.
5. The nano cellulose-based composite film adopts the nano cellosilk with high length-diameter ratio and the uniform and mostly single Michelene nano sheets, improves the contact area of the cellosilk and the Michelene nano sheets, and is beneficial to constructing a high-strength composite film.
6. The humidity response mechanism of the nano cellulose-based humidity response composite membrane of the invention is as follows: on one hand, hydrophilic functional groups of michael nanosheets and polyphenol compounds, especially nanofiber filaments in the composite film can adsorb water molecules when exposed to humidity, and hydrogen bond interaction among the nanofiber filaments, the michael nanosheets and the polyphenol compounds is weakened or even destroyed, so that expansion among the michael nanosheets in the composite film is caused. On the other hand, the compact shell-like layered structure of the composite film is used as a barrier and can block the diffusion of water molecules along the vertical direction, so that a water gradient is generated in the thickness direction of the film, and therefore the composite film responds to local humidity and generates asymmetric deformation, and humidity response is realized.
7. The mass ratio of the nano cellosilk, the michael nano sheets and the polyphenol compound used by the nano cellulose-based humidity-driven composite membrane is 100: 25-100: 2.5-15. Too much or too little michael nanosheet or polyphenol compound affects the effect of the combination of mechanical properties, humidity response and joule heating.
8. According to the preparation method, the nano-cellosilk and the michael nanosheet are mixed, and finally the polyphenol compound is dropwise added, so that the functions of the three components can be fully cooperated, and the exertion effect of the composite material is maximized.
The applicant tests and verifies that the nano cellulose-based composite membrane prepared by the invention can be bent by 180 degrees at 3.5s in response to humidity, and has high sensitivity. The temperature can be raised by 17 ℃ by applying 5V voltage, and escherichia coli and staphylococcus aureus can be effectively inhibited.
The following further description is made with reference to the accompanying drawings and detailed description.
Drawings
FIG. 1 is a TEM photograph of example 2 of the present invention;
FIG. 2 is a SEM photograph of example 2 of the present invention;
FIG. 3 shows the mechanical properties of example 2 of the present invention;
FIG. 4 is humidity driving performance of example 2 of the present invention;
FIG. 5 is a Joule thermal performance of example 2 of the present invention;
FIG. 6 shows the antibacterial ability of example 2 of the present invention;
fig. 7 shows the heat and moisture dissipating performance of the intelligent clothes according to embodiment 2 of the present invention.
Detailed Description
In the invention, the raw material of the nano-cellulose is wood pulp (the cellulose content is 90%), and the nano-cellulose is prepared by a TEMPO oxidation method, and certainly, the nano-cellulose can also be directly purchased from the market. The raw material of the michael is Ti3AlC2MAX powder, particle size 40 μm, available from 11 science and technology, Inc., is etched with LiF/HCl solution3AlC2The MAX phase is prepared into a Michael alkene nano-sheet, and can be directly purchased from the market.
Comparative example 1
Mixing 0.3 wt% of a michael nanosheet aqueous solution and 0.3 wt% of a nano-cellosilk aqueous dispersion according to the michael content of 25% to obtain a uniform nano-cellosilk-michael nanosheet mixed solution, putting 12ml of the mixed solution into a suction filtration cup for vacuum suction filtration, naturally drying for 6 hours, and carefully uncovering from a polytetrafluoroethylene filter membrane to obtain a nano-cellosilk-michael nanosheet composite membrane with the thickness of 15 microns; through testing, the mechanical strength of the prepared nanofiber silk-mikkene nanosheet composite membrane is 161.4 MPa.
Comparative example 2
Except that 0.3 wt% of michael nanosheet aqueous solution and 0.3 wt% of nano-cellosilk aqueous dispersion were mixed according to the michael content of 50%, a nano-cellosilk-michael nanosheet composite film was prepared according to the same procedure as in comparative example 1, and through testing, the mechanical strength was up to 199.5 MPa.
Comparative example 3
Except that 0.3 wt% of michael nanosheet aqueous solution and 0.3 wt% of nano-cellosilk aqueous dispersion were mixed according to the michael content of 75%, a nano-cellosilk-michael nanosheet composite film was prepared according to the same procedure as in comparative example 1, and through testing, the mechanical strength was up to 245.5 MPa.
Comparative example 4
Except that 0.3 wt% of michael nanosheet aqueous solution and 0.3 wt% of nano-cellosilk aqueous dispersion were mixed according to 100% of michael content, a nano-cellosilk-michael nanosheet composite film was prepared according to the same procedure as in comparative example 1, and through testing, the mechanical strength was up to 174.6 MPa.
Example 1
Stirring and mixing 0.3 wt% of a michael nanosheet aqueous solution and 0.3 wt% of a nano-cellosilk aqueous dispersion according to the michael content of 75% to obtain a uniform nano-cellosilk-michael nanosheet mixed solution; then, dripping a tannic acid solution into the mixed solution of the nano cellosilk and the michael nanosheets, wherein the mass of the tannic acid is 2.5% of that of the nano cellulose, and stirring for 6-12h at room temperature to obtain a uniform mixed solution; and (3) putting 12ml of the uniformly mixed solution into a suction cup for vacuum suction filtration, naturally drying for 6 hours, and carefully removing the solution from the polytetrafluoroethylene filter membrane to obtain the nano cellulose composite membrane with the thickness of 15 microns. The nano cellulose composite membrane has the mechanical strength of 260MPa, response to humidity stimulation, bending 180 degrees within 6s, and Joule heat and antibacterial capacity. The fabric is applied as intelligent clothes to effectively dissipate moisture in summer or in strenuous exercise, and the temperature is reduced by 1.0 ℃; the voltage supply in winter can realize the heat preservation function.
Example 2
A nanocellulose composite membrane was prepared by the same procedure as in example 1, except that tannic acid was dropped in an amount of 5% by mass based on the nanocellulose. The mechanical strength of the nano cellulose composite membrane can reach 275.4MPa, the nano cellulose composite membrane can be bent for 180 degrees at 3.5s in response to humidity stimulation, 17-DEG C temperature increase can be realized by applying 5V voltage, and the nano cellulose composite membrane can resist escherichia coli and staphylococcus aureus. When the fabric is applied to intelligent clothes, effective moisture dissipation can be realized in summer or during strenuous exercise, and the temperature is reduced by 1.8 ℃; the voltage supply in winter can realize the heat preservation function.
Example 3
A nanocellulose composite membrane was prepared by the same procedure as in example 1, except that tannic acid was dropped in an amount of 10% by mass based on the nanocellulose. The nano cellulose-based composite membrane has the mechanical strength of 248.2MPa, is bent for 180 degrees at 4.5s in response to humidity stimulation, and has joule heat and antibacterial capacity. When the cooling liquid is applied to intelligent clothes, effective moisture dissipation can be realized in summer or during strenuous exercise, and the temperature is reduced by 1.5 ℃; the voltage supply in winter can realize the heat preservation function.
Example 4
Except that the mass of the tannin accounts for 15% of the mass of the nano-cellulose, the nano-cellulose composite membrane is prepared according to the same steps of the embodiment 1, the mechanical strength of the nano-cellulose composite membrane can reach 199.3MPa, the nano-cellulose composite membrane can be bent by 180 degrees at 5.5s in response to humidity stimulation, and the nano-cellulose composite membrane has Joule heat and antibacterial capacity. The intelligent clothes can be used as intelligent clothes to realize effective moisture dissipation and reduce the temperature by 1.2 ℃ in summer or in violent sports; the voltage supply in winter can realize the heat preservation function.
Example 5
Except that another polyphenol compound dopamine solution is dripped into the nanofiber silk-michael nanosheet mixed solution, and the mass of the dripped dopamine accounts for 5% of that of the nanofiber silk, the nano-cellulose composite membrane is prepared according to the same steps of the embodiment 1, has the mechanical strength of 245.8MPa, is bent by 180 degrees at 4s in response to humidity stimulation, and has joule heat and antibacterial capacity. The intelligent clothes can be used as intelligent clothes to realize effective moisture dissipation and reduce the temperature by 1.4 ℃ in summer or in severe sports; the voltage supply in winter can realize the heat preservation function.
The nanofiber-based composite membrane prepared in example 2 was characterized by a Scanning Electron Microscope (SEM), a Transmission Electron Microscope (TEM), a universal tensile testing machine, a humidity response test, a joule heat test, and a zone of inhibition test, and the results are shown in fig. 1 to 7. The results show that: the SEM results in fig. 1 show that nanocellulose is distributed tightly and uniformly on the michael sheets, indicating strong interfacial bonding of nanocellulose, michael and tannic acid. The SEM results in fig. 2 show that there is a fairly ordered dense lamellar microstructure throughout the membrane, similar to the regular lamellar structure in the nacreous layer. In particular, the MXene nanosheets are highly distributed in the CNF matrix by high magnification and are closely stacked in the planar direction. The test result of FIG. 3 shows that the mechanical strength of the composite film at 5.8% of tensile break can reach 275.4 MPa. The test result of FIG. 4 shows that the composite membrane responds to the humidity stimulation, and the whole bending-unbending process is completed within 10s after the composite membrane is bent for 180 degrees within 3.5 s. Fig. 5 tests results and found that when 5V voltage was applied, the surface temperature of the composite membrane driver increased from 20 ℃ to 37.2 ℃ in 45s, and 60s returned to the original temperature after the voltage was removed. The test result of FIG. 6 shows that the composite membrane driver can resist Escherichia coli and Staphylococcus aureus, and the bacterial rings with different sizes appear. Fig. 7 shows that the humidity can be reduced by 20% and the temperature can be reduced by 1.8 ℃ compared with the common silk fabric when the composite film driving is applied to the intelligent clothes.
Claims (7)
1. The humidity response driver is characterized in that a nanocellulose-based composite membrane is prepared into a double semilunar valve shape, and is opened or closed by responding to humidity, the nanocellulose-based composite membrane comprises nanofiber filaments, michaene nanosheets and tannic acid, a uniform single-layer membrane-shaped structure is formed by hydrogen bond combination, and the mass ratio of the nanofiber filaments to the michaene nanosheets to the tannic acid is 100: 25-100: 2.5-15, prepared by the following steps:
1) preparing nano-fiber filaments, michaene nanosheets and tannic acid into nano-fiber filament dispersion liquid, michaene nanosheet dispersion liquid and tannic acid dispersion liquid respectively;
2) mixing the nano-cellosilk dispersion liquid and the michael nanosheet dispersion liquid to obtain a mixed solution;
3) dropwise adding the tannin dispersion liquid into the mixed solution obtained in the step 2), and stirring for 6-12h to obtain a uniform mixed solution;
4) and (3) carrying out suction filtration on the uniform mixed solution, and drying a filter cake for 6-8h to obtain the nano cellulose composite membrane with the thickness of 10-30 mu m.
2. The humidity responsive actuator of claim 1, wherein the nanofiber filaments have a diameter of 3-5nm, an aspect ratio of > 1000, the michael nanosheets have an average size of > 300nm and a thickness of 1-3 nm.
3. A humidity responsive actuator as claimed in claim 2 wherein the nanofibrous filaments have a length of 3 to 10 μm, the michael nanosheets have an average size of 300-500nm and a thickness of 1 to 2 nm.
4. A humidity responsive actuator as claimed in claim 1 wherein the membrane like structure has a thickness of 15 μm.
5. The humidity responsive actuator of claim 1, wherein step 1) said nanofiber filament dispersion and michael nanosheet dispersion are aqueous solutions, each at a concentration of 0.3 to 0.5wt%, said nanofibers are prepared using TEMPO oxidation, and said michael nanosheets are etched with a LiF/HCl solution to form Ti3AlC2MAX phase is prepared.
6. The humidity responsive actuator of claim 1, wherein said suction in step 4) is vacuum suction in a suction cup, and said drying is natural drying.
7. Use of a humidity responsive actuator according to any of claims 1 to 6 for the manufacture of smart apparel for automatic heat dissipation, humidity reduction and heat retention by opening or closing in response to humidity.
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| CN114534527B (en) * | 2022-04-18 | 2023-07-04 | 重庆文理学院 | Membrane filtration assembly |
| CN114558467A (en) * | 2022-04-18 | 2022-05-31 | 重庆文理学院 | Protein-filtering bacterium-inhibiting hollow fiber membrane and preparation method and application thereof |
| CN115259878B (en) * | 2022-09-01 | 2023-03-28 | 上海大学 | Suction filtration doping process |
| CN115559109A (en) * | 2022-11-18 | 2023-01-03 | 四川大学华西医院 | Breathable antibacterial nano composite fiber material and preparation method and application thereof |
| CN116218378A (en) * | 2023-03-14 | 2023-06-06 | 中国科学技术大学 | High-performance electromagnetic shielding coating material and preparation method thereof |
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