CN110064347B - Porous aerogel based on biomimetic vascular bundle microstructure and its preparation method and application - Google Patents
Porous aerogel based on biomimetic vascular bundle microstructure and its preparation method and application Download PDFInfo
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- CN110064347B CN110064347B CN201910435537.3A CN201910435537A CN110064347B CN 110064347 B CN110064347 B CN 110064347B CN 201910435537 A CN201910435537 A CN 201910435537A CN 110064347 B CN110064347 B CN 110064347B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明涉及气凝胶材料技术领域，具体涉及一种基于仿生维管束微结构的多孔气凝胶及其制备方法和应用。本发明提供的基于仿生维管束微结构的多孔气凝胶的制备方法，利用冷冻铸造成型法将无机纳米纤维、有机高分子聚合物制备成多孔气凝胶，其具有由纤维栈架和相容包埋层组装而成的“层‑栈架‑层”结构，所述“层‑栈架‑层”结构为有序三维多孔网络结构，包含维管束横、纵截面仿生结构，可提供高通透性微米通道，具有优异的仿生疏水性能和高吸油能力，能够应用于油水混合物中油品的吸附分离；同时，所述多孔气凝胶还具有优异的抗机械挤压疲劳性能，且在移除驱使变形载荷后，可以自动恢复至初始形态，能够作为弹性材料使用。
The invention relates to the technical field of aerogel materials, in particular to a porous aerogel based on a bionic vascular bundle microstructure and a preparation method and application thereof. The preparation method of the porous aerogel based on the biomimetic vascular bundle microstructure provided by the present invention is to prepare the porous aerogel from the inorganic nanofibers and the organic macromolecular polymer by the freezing casting method. The "layer-stack-layer" structure assembled by the embedding layer, the "layer-stack-layer" structure is an ordered three-dimensional porous network structure, including the vascular bundle transverse and longitudinal cross-section bionic structure, which can provide high-pass Permeable micro-channels have excellent biomimetic hydrophobic properties and high oil absorption capacity, which can be applied to the adsorption and separation of oil products in oil-water mixtures; at the same time, the porous aerogel also has excellent resistance to mechanical extrusion fatigue, and can be removed after removal. After driving the deformation load, it can automatically return to the original shape and can be used as an elastic material.
Description
Technical Field
The invention relates to the technical field of aerogel materials, in particular to a porous aerogel based on a bionic vascular bundle microstructure and a preparation method and application thereof.
Background
After a long time of evolution, biomaterials often show an optimized multi-scale structure and a plurality of excellent performances in the aspects of light, electricity, magnetism, heat, force and the like, such as light weight, high strength, self-cleaning, intelligent response, environmental adaptability, self-healing and self-replication functions and the like, which are all the excellent performances required by people in designing and preparing new materials. Therefore, researchers have attracted extensive attention to develop biomimetic materials by simulating the structural features and functional characteristics of biomaterials. However, the development of biomimetic materials needs to simulate not only the structural features of biomaterials, but also their specific functions.
In the field of emerging nano materials, an aerogel material is used as a hierarchical porous integral solid substance constructed based on a cross-scale and bionic design idea, and has an excellent extensible buckling mechanical structure, and the unique high-permeability nano porous network structure formed by solid framework support and gaseous medium heterogeneous filling enables the aerogel material to have high porosity and flexibility. However, most of the pore structures of the existing aerogel materials are disordered, and compared with the ordered structure, the adsorption and mechanical extrusion resistance of the disordered structure assembly have uncontrollable performance to a greater extent. Therefore, the inspiration needs to be acquired from the natural biological system, so that the bionic porous aerogel with an ordered structure and a controllable structure is designed.
Disclosure of Invention
The porous aerogel provided by the invention has a layer-stack-layer structure, and has excellent bionic hydrophobic property, high oil absorption capacity and excellent mechanical extrusion fatigue resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of porous aerogel based on a bionic vascular bundle microstructure, which comprises the following steps:
mixing inorganic nano-fibers, an organic high-molecular polymer and a solvent to obtain mixed slurry;
and placing the mixed slurry into a mold, placing the mold containing the mixed slurry on a substrate, and then performing freeze casting molding to obtain the porous aerogel based on the bionic vascular bundle microstructure.
Preferably, the diameter of the inorganic nanofiber is 10-120 nm, and the length of the inorganic nanofiber is 50 nm-500 μm.
Preferably, the weight average molecular weight of the organic high molecular polymer is 1200 to 500000, and the polymerization degree is 10 to 1000000.
Preferably, the concentration of the inorganic nano-fibers in the mixed slurry is 5-30 mg/mL, and the concentration of the organic high molecular polymer is 5-50 mg/mL.
Preferably, the material of the mould comprises metal, quartz glass or organic silicon rubber; the wall thickness of the die is 0.1-0.8 cm.
Preferably, the material of the substrate comprises polydimethylsiloxane, cyclomethicone, aminosilicone, polymethylphenylsiloxane, polyether polysiloxane copolymer or polystyrene; the thickness of the substrate is 10 mu m-10 cm.
Preferably, the temperature of the freezing casting molding is-20 to-50 ℃, and the time is 30s to 0.5 h.
The porous aerogel based on the bionic vascular bundle microstructure prepared by the preparation method provided by the technical scheme provided by the invention has a layer-stack-layer structure formed by assembling a fiber stack frame and a compatible embedding layer, wherein the fiber stack frame is formed by inorganic nano fibers, and the compatible embedding layer is formed by organic high molecular polymers.
Preferably, the density of the porous aerogel based on the bionic vascular bundle microstructure is 14.21-35.58 mg/cm3。
The invention provides application of the porous aerogel based on the bionic vascular bundle microstructure as an adsorption separation material or an elastic material.
The invention provides a preparation method of porous aerogel based on a bionic vascular bundle microstructure, which comprises the following steps: mixing inorganic nano-fibers, an organic high-molecular polymer and a solvent to obtain mixed slurry; and placing the mixed slurry into a mold, placing the mold containing the mixed slurry on a substrate, and then performing freeze casting molding to obtain the porous aerogel based on the bionic vascular bundle microstructure. According to the invention, inorganic nanofibers and organic high molecular polymers are prepared into porous aerogel by a freeze casting forming method, the porous aerogel has a layer-stack-layer structure formed by assembling a fiber stack frame and a compatible embedding layer (wherein the fiber stack frame is formed by the inorganic nanofibers, and the compatible embedding layer is formed by the organic high molecular polymers), the layer-stack-layer structure is an ordered three-dimensional porous network structure and comprises bionic structures of transverse and longitudinal sections of a vascular bundle, so that a high-permeability micro channel can be provided, and the porous aerogel has excellent bionic hydrophobic property and high oil absorption capacity and can be applied to adsorption separation of oil products in an oil-water mixture; meanwhile, the porous aerogel also has excellent mechanical extrusion fatigue resistance, can automatically recover to an initial form after a driving deformation load is removed, and can be used as an elastic material. The experimental results of the embodiment show that the adsorption capacity of the porous aerogel provided by the invention on different oil products is 74.2-99.9 g/g, the bearable compressive strain is 30% -90%, the elastic modulus is 0.1425-0.5921 kPa, and the contact angle of the porous aerogel with the interface of a water drop is larger than 90 degrees.
In addition, the preparation method of the porous aerogel provided by the invention has the advantages of easily available raw materials, simple process, low production cost and strong controllability; by controlling the characteristics of the material, the size and the like of the mold and the substrate, the pore-forming mode in the freezing casting process can be regulated, and the controllable regulation of the micro-scale bionic pore structure and the adjustable denaturation of the macro-scale morphology in the finally obtained porous aerogel are realized.
Drawings
FIG. 1 is a flow chart of the present invention for preparing a porous aerogel based on a biomimetic vascular bundle microstructure;
FIG. 2 is a scanning electron microscope photograph of the porous aerogel prepared in example 1;
FIG. 3 is a scanning electron microscope image of a porous aerogel prepared in example 3;
FIG. 4 is a scanning electron microscope image of the porous aerogel prepared in example 3 after one 50% strain compression;
FIG. 5 is a graph of the static surface contact angle of the porous aerogel prepared in example 1;
FIG. 6 is a graph of the static surface contact angle of the porous aerogel prepared in example 2;
FIG. 7 is a graph of the static surface contact angle of the porous aerogel prepared in example 3;
fig. 8 is a compressive stress-strain curve of the copper nanowire-polyvinyl alcohol porous aerogel prepared in example 3.
Detailed Description
The invention provides a preparation method of porous aerogel based on a bionic vascular bundle microstructure, which comprises the following steps:
mixing inorganic nano-fibers, an organic high-molecular polymer and a solvent to obtain mixed slurry;
and placing the mixed slurry into a mold, placing the mold containing the mixed slurry on a substrate, and then performing freeze casting molding to obtain the porous aerogel based on the bionic vascular bundle microstructure.
According to the invention, inorganic nanofibers and organic high molecular polymers are prepared into porous aerogel by a freeze casting forming method, the porous aerogel has a layer-stack-layer structure formed by assembling a fiber stack frame and a compatible embedding layer (wherein the fiber stack frame is formed by the inorganic nanofibers, and the compatible embedding layer is formed by the organic high molecular polymers), the layer-stack-layer structure is an ordered three-dimensional porous network structure and comprises bionic structures of transverse and longitudinal sections of a vascular bundle, so that a high-permeability micro channel can be provided, and the porous aerogel has excellent bionic hydrophobic property and high oil absorption capacity and can be applied to adsorption separation of oil products in an oil-water mixture; meanwhile, the porous aerogel also has excellent mechanical extrusion fatigue resistance, can automatically recover to an initial form after a driving deformation load is removed, and can be used as an elastic material.
The invention mixes inorganic nano-fiber, organic high molecular polymer and solvent to obtain mixed slurry.
In the invention, the diameter of the inorganic nano-fiber is preferably 10-120 nm, and more preferably 20-80 nm; the length is preferably 50nm to 500 μm, and more preferably 10 to 100 μm. In the present invention, the inorganic nanofibers preferably include one or more of copper nanowires, silver nanowires, tin nanowires, niobium nanowires, indium nanowires, silicon nanowires, copper oxide nanowires, silver oxide nanowires, tin oxide nanowires, niobium oxide nanowires, indium oxide nanowires, silicon carbide nanowires, platinum-cobalt nanowires, and platinum-nickel nanowires, and more preferably copper nanowires or silver nanowires.
In the invention, the weight average molecular weight of the organic high molecular polymer is preferably 1200-500000, and more preferably 10000-100000; the polymerization degree is preferably 10 to 1000000, more preferably 5000 to 30000. In the present invention, the organic high molecular polymer preferably includes one or more of polyvinyl alcohol, polyethylene glycol, chitosan, sodium alginate, chitin (i.e., chitin), chondroitin sulfate, polyacrylamide, polymethyl methacrylate, a polypropylene-acrylonitrile copolymer, and a polybutadiene-acrylonitrile copolymer, and more preferably sodium alginate or polyvinyl alcohol.
The specific combination of the inorganic nanofibers and the organic high molecular polymer required in the preparation of the porous aerogel is not particularly limited, and specifically, the porous aerogel is prepared by using the copper nanowires and the sodium alginate as raw materials, the porous aerogel is prepared by using the copper nanowires and the polyvinyl alcohol as raw materials, the porous aerogel is prepared by using the silver nanowires and the sodium alginate as raw materials, or the porous aerogel is prepared by using the silver nanowires and the polyvinyl alcohol as raw materials.
In the present invention, the solvent preferably includes water and an organic solvent; the organic solvent preferably comprises one or more of benzene, toluene, dichloromethane, N-dimethylformamide and dimethyl sulfoxide, and more preferably N, N-dimethylformamide. In the invention, the volume ratio of the water to the organic solvent is preferably (3-10): (0.5-4), and more preferably (5-8): 1-3.
In the invention, the concentration of the inorganic nano-fibers in the mixed slurry is preferably 5-30 mg/mL, and more preferably 5-22.1 mg/mL; the concentration of the organic high molecular polymer is preferably 5 to 50mg/mL, more preferably 5 to 38.9 mg/mL. According to the invention, the usage amount of the inorganic nano-fiber and the organic high molecular polymer is controlled to ensure that the obtained porous aerogel has a layer-trestle-layer structure; if the consumption of the organic high molecular polymer is too low, the aerogel can not be obtained by subsequent freezing casting molding; if the amount of the organic high molecular polymer is too much, although the aerogel can be obtained, the inner pore channel of the aerogel is closed and does not have a layer-stack-layer structure.
The invention has no special limitation on the mixing of the inorganic nano-fiber, the organic high molecular polymer and the solvent, and can fully dissolve and disperse all the components. In the invention, the inorganic nanofibers, the organic high molecular polymer and the solvent are preferably mixed under a stirring condition, and the stirring speed is preferably 300-500 rpm. In the embodiment of the invention, specifically, an organic high molecular polymer solution is mixed with an inorganic nanofiber aqueous dispersion; the solvent in the organic high molecular polymer solution is preferably water and an organic solvent, the concentrations of the organic high molecular polymer solution and the inorganic nanofiber aqueous dispersion and the proportion of the organic high molecular polymer solution and the inorganic nanofiber aqueous dispersion are not specially limited, and the concentrations of the organic high molecular polymer and the inorganic nanofiber in the mixed slurry obtained by mixing the organic high molecular polymer solution and the inorganic nanofiber can meet the requirements.
After the mixed slurry is obtained, the mixed slurry is placed in a mold, the mold containing the mixed slurry is placed on a substrate, and then the porous aerogel based on the bionic vascular bundle microstructure is obtained by performing freeze casting molding.
In the present invention, the material of the mold preferably includes metal, quartz glass, or silicone rubber, and the metal preferably includes aluminum, copper, or iron; the wall thickness of the die is preferably 0.1-0.8 cm, and more preferably 0.2-0.4 cm. The shape of the die is not specially limited, and a proper shape is selected according to actual needs; in the present invention, the mold is preferably a hollow cube, a hollow cuboid or a hollow cylinder. According to the invention, by controlling the characteristics of the material, size, shape and the like of the mold, the pore-forming mode in the freeze casting process can be regulated, and the controllable regulation of the micro-scale bionic pore structure and the adjustable denaturation of the macro-scale morphology in the finally obtained porous aerogel can be realized.
In the present invention, the material of the substrate preferably includes polydimethylsiloxane, cyclomethicone, aminosiloxane, polymethylphenylsiloxane, polyether polysiloxane copolymer, or polystyrene; the thickness of the substrate is preferably 10 μm to 10cm, more preferably 10 μm to 1cm, and further preferably 10 to 30 μm. According to the invention, by controlling the material and the thickness of the substrate, the pore-forming mode and the pore-forming speed in the freeze casting process can be regulated, and the controllable regulation of the micro-scale bionic pore structure in the finally obtained porous aerogel is realized.
In the invention, the temperature of the freezing casting molding is preferably-20 to-50 ℃, and the time is preferably 30s to 0.5 h. The temperature of the freeze casting molding is preferably provided by liquid nitrogen, as shown in fig. 1, specifically, a substrate is placed on a metal plate, a mold is placed on the substrate, the mixed slurry is poured into the mold, then the liquid nitrogen is placed under the metal plate, the temperature of the metal plate (namely the temperature of the freeze casting molding, and the set temperature is detected by an armored temperature sensor) is controlled by the liquid nitrogen, and the freeze casting molding of the mixed slurry in the mold is realized; in the process of freezing, casting and molding, high molecular polymer is extruded into layers in the process of ice crystal production, inorganic nano fibers are lapped between layers to form a trestle, and finally the layers are assembled into a layer-trestle-layer structure to obtain the porous aerogel with the bionic vascular bundle microstructure. The invention has no special limitation on the specific type of the metal plate, and in the embodiment of the invention, a copper plate is specifically adopted; in the invention, the thickness of the metal plate is preferably 0.1-1 cm, and more preferably 0.25-0.6 cm.
After the freezing casting molding is completed, the obtained molded frozen entity is preferably separated from the mold, and after drying, the porous aerogel based on the bionic vascular bundle microstructure is obtained. In the present invention, the drying is preferably freeze-drying; the temperature of the freeze drying is preferably-50 ℃, and the time is preferably 48 h.
The porous aerogel based on the bionic vascular bundle microstructure prepared by the preparation method provided by the technical scheme has a layer-stack-layer structure formed by assembling a fiber stack and a compatible embedding layer, wherein the fiber stack is formed by inorganic nano fibers, and the length of a fiber bridge is preferably 10-150 mu m; the compatible buried layer is formed by organic high molecular polymer, and the thickness of the compatible buried layer is preferably 0.5-12 mu m. In the invention, the contents of the inorganic nanofibers and the organic high molecular polymer in the porous aerogel can be controlled according to the adding amount of the corresponding raw materials.
In the invention, the density of the porous aerogel based on the bionic vascular bundle microstructure is 14.21-35.58 mg/cm3. According to the invention, the density of the porous aerogel is regulated and controlled by controlling the use amounts of the inorganic nano-fibers and the organic high molecular polymer, and the material and the size of the die and the substrate, so that the porous aerogel has excellent bionic hydrophobic property, high oil absorption capacity and excellent mechanical extrusion fatigue resistance.
The invention provides application of the porous aerogel based on the bionic vascular bundle microstructure as an adsorption separation material or an elastic material. The porous aerogel based on the bionic vascular bundle microstructure provided by the invention has excellent mechanical extrusion fatigue resistance, can automatically recover to an initial form after a deformation driving load is removed, and can be used as an elastic material; meanwhile, the oil-water composite material also has excellent bionic hydrophobic property and high oil absorption capacity, and can be applied to adsorption separation of oil products in oil-water mixtures. In the invention, when the porous aerogel based on the bionic vascular bundle microstructure is used as an adsorption separation material, the application method preferably comprises the following steps: placing the porous aerogel based on the bionic vascular bundle microstructure in an oil-water mixture, wherein the porous aerogel based on the bionic vascular bundle microstructure can adsorb an oil product, so that the separation of the oil product and a water phase is realized; in the present invention, the oil preferably comprises one or more of gasoline, kerosene, diesel oil, olive oil and peanut oil.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the copper nanowire-sodium alginate porous aerogel based on the bionic vascular bundle microstructure comprises the following steps as shown in figure 1:
weighing 0.49g of sodium alginate (weight-average molecular weight of 15000 and polymerization degree of 5000) solid particles in a 30mL beaker, adding 10mL of N-dimethylformamide, then adding 10mL of deionized water, and mechanically stirring for 12h at the rotating speed of 500rpm to obtain a uniform sodium alginate solution;
taking 5mL of 45mg/mL copper nanowire water dispersion (wherein the diameter of the copper nanowire is 20nm, and the length of the copper nanowire is 100 microns), slowly adding 7.5mL of the sodium alginate solution into the copper nanowire water dispersion, and magnetically stirring for 8 hours at the rotating speed of 300rpm to obtain mixed slurry;
placing a polydimethylsiloxane substrate (with the thickness of 0.01cm) on a clean copper plate (with the thickness of 0.5cm), then placing a mold (made of quartz glass, shaped like a hollow cube and with the wall thickness of 0.2cm) on the polydimethylsiloxane substrate, and pouring the mixed slurry into the mold; and (3) placing liquid nitrogen below the surface of the copper plate, controlling the copper plate to reach-20 ℃ (the set temperature is detected by an armored temperature sensor) by using the liquid nitrogen, separating the obtained formed frozen entity from the mold after 5min of freeze casting forming, and freeze-drying (the temperature is-50 ℃ and the time is 48h) to obtain the copper nanowire-sodium alginate porous aerogel based on the bionic vascular bundle microstructure.
Example 2
The preparation method of the silver nanowire-sodium alginate porous aerogel based on the bionic vascular bundle microstructure comprises the following steps:
weighing 1.4g of sodium alginate (with the weight-average molecular weight of 25000 and the polymerization degree of 10000) solid particles in a 30mL beaker, adding 10mL of N-dimethylformamide, then adding 10mL of deionized water, and mechanically stirring for 12h at the rotating speed of 500rpm to obtain a uniform sodium alginate solution;
taking 5mL of silver nanowire water dispersion with the concentration of 11mg/mL (wherein the diameter of the silver nanowire is 30nm, and the length of the silver nanowire is 100 micrometers), slowly adding 5mL of the sodium alginate solution into the silver nanowire water dispersion, and magnetically stirring for 8 hours at the rotating speed of 300rpm to obtain mixed slurry;
placing a polydimethylsiloxane substrate (with the thickness of 0.01cm) on a clean copper plate (with the thickness of 0.5cm), then placing a mold (made of quartz glass, shaped like a hollow cube and with the wall thickness of 0.2cm) on the polydimethylsiloxane substrate, and pouring the mixed slurry into the mold; and (2) placing liquid nitrogen below the surface of the copper plate, controlling the copper plate to reach-30 ℃ (the set temperature is detected by an armored temperature sensor) by using the liquid nitrogen, separating the obtained formed frozen entity from the mold after 2min of freeze casting forming, and freeze-drying (the temperature is-50 ℃ and the time is 48h) to obtain the silver nanowire-sodium alginate porous aerogel based on the bionic vascular bundle microstructure.
Example 3
The preparation method of the copper nanowire-polyvinyl alcohol porous aerogel based on the bionic vascular bundle microstructure comprises the following steps:
weighing 1.2g of solid particles of polyvinyl alcohol (weight-average molecular weight of 15000 and polymerization degree of 5000) in a 50mL beaker, adding 20mL of N-dimethylformamide, then adding 20mL of deionized water, and mechanically stirring for 12h at the rotating speed of 500rpm to obtain a uniform polyvinyl alcohol solution;
taking 1.6mL of copper nanowire water dispersion with the concentration of 75mg/mL (wherein the diameter of the copper nanowire is 20nm, and the length of the copper nanowire is 100 micrometers), slowly adding 7.5mL of the polyvinyl alcohol solution into the copper nanowire water dispersion, and magnetically stirring for 8 hours at the rotating speed of 300rpm to obtain mixed slurry;
placing a polydimethylsiloxane substrate (with the thickness of 0.03cm) on a clean copper plate (with the thickness of 0.6cm), then placing a mold (made of silicon rubber, shaped like a hollow cube and with the wall thickness of 0.2cm) on the polydimethylsiloxane substrate, and pouring the mixed slurry into the mold; and (2) placing liquid nitrogen below the surface of the copper plate, controlling the copper plate to reach-50 ℃ (the set temperature is detected by an armored temperature sensor) by using the liquid nitrogen, separating the obtained formed frozen entity from the mold after 30s of freezing casting forming, and carrying out freeze drying (the temperature is-50 ℃ and the time is 48h) to obtain the copper nanowire-polyvinyl alcohol porous aerogel based on the bionic vascular bundle microstructure.
Example 4
The preparation method of the silver nanowire-polyvinyl alcohol porous aerogel based on the bionic vascular bundle microstructure comprises the following steps:
weighing 0.6g of solid particles of polyvinyl alcohol (weight-average molecular weight of 15000 and polymerization degree of 5000) in a 50mL beaker, adding 20mL of N-dimethylformamide, then adding 20mL of deionized water, and mechanically stirring for 12h at the rotating speed of 500rpm to obtain a uniform polyvinyl alcohol solution;
taking 5mL of 56mg/mL silver nanowire water dispersion (wherein the diameter of the silver nanowire is 30nm, and the length of the silver nanowire is 150 micrometers), slowly adding 10mL of the polyvinyl alcohol solution into the silver nanowire water dispersion, and magnetically stirring for 8 hours at the rotating speed of 300rpm to obtain mixed slurry;
placing a polydimethylsiloxane substrate (with the thickness of 0.01cm) on a clean copper plate (with the thickness of 0.25cm), then placing a mold (made of quartz glass, shaped like a hollow cube and with the wall thickness of 0.2cm) on the polydimethylsiloxane substrate, and pouring the mixed slurry into the mold; and (2) placing liquid nitrogen below the surface of the copper plate, controlling the copper plate to reach-50 ℃ (the set temperature is detected by an armored temperature sensor) by using the liquid nitrogen, carrying out 1min freeze casting molding, separating the obtained molded frozen entity from a mold, and carrying out freeze drying (the temperature is-50 ℃ and the time is 48h) to obtain the silver nanowire-polyvinyl alcohol porous aerogel based on the bionic vascular bundle microstructure.
The porous aerogel prepared in the embodiments 1 to 4 is characterized by the following specific steps:
fig. 2 is a scanning electron microscope photograph of the porous aerogel prepared in example 1, and fig. 3 is a scanning electron microscope photograph of the porous aerogel prepared in example 3. As can be seen from FIGS. 2 and 3, the layer-trestle-layer structure is vertically distributed and embedded in the aerogel, sodium alginate or polyvinyl alcohol forms a compatible embedding layer (with a thickness of 0.5-12 μm) in the preparation process, the copper nanowires form a fiber trestle (with a length of 10-30 μm), and the compatible embedding layers are effectively connected to form the porous aerogel with the layer-trestle-layer structure. The scanning electron microscope images of the porous aerogel prepared in example 2 and the porous aerogel prepared in example 4 are similar to those of fig. 2 and 3, and the porous aerogel can be observed to have a structure of "layer-stack-layer".
Fig. 4 is a scanning electron microscope image of the porous aerogel prepared in example 3 after one 60% strain compression. As can be seen from fig. 4, after being subjected to extrusion under the strain condition, the copper nanowire-polyvinyl alcohol porous aerogel can still maintain a unique "layer-stack-layer" structure, indicating that the "layer-stack-layer" structure has excellent mechanical extrusion fatigue resistance. The sem images of the porous aerogels prepared in examples 1, 2 and 4 after one 60% strain pressing are similar to those of fig. 4, and after the pressing under the strain condition, the porous aerogels can be observed to have the structure of "layer-stack-layer".
Fig. 5 is a contact angle graph of the static surface of the porous aerogel prepared in example 1, fig. 6 is a contact angle graph of the static surface of the porous aerogel prepared in example 2, and fig. 7 is a contact angle graph of the static surface of the porous aerogel prepared in example 3 (the contact angle measurement result directly derived by an instrument is data of light gray and small font size in fig. 5 to 7 at present, and for the convenience of more intuitively reading the contact angle data, the corresponding contact angle data of the static surface of the porous aerogel is marked at the upper left corner of fig. 5 to 7). As can be seen from FIGS. 5 to 7, the porous aerogels prepared in examples 1 to 3 all have a good hydrophobic effect, and the contact angles are greater than 90 °.
Table 1 shows the density and Young's modulus data of the porous aerogels prepared in examples 1 to 4, and it can be seen from Table 1 that the density of the porous aerogels prepared in examples 1 to 4 has adjustable property (14.21 to 35.58 mg/cm)3) The Young modulus corresponding to the material is adjustable (0.1425-0.5921 kPa); and the density and Young modulus of the porous aerogel can be regulated and controlled by adjusting the using amount of the inorganic nano-fibers and the organic high molecular polymer, the sizes of the die and the substrate and other characteristics.
TABLE 1 Density and Young's modulus data for porous aerogels prepared in examples 1-4
The performance of the porous aerogel prepared in examples 1 to 4 was determined as follows:
respectively placing 0.01g of the porous aerogel prepared in the embodiments 1 to 4 in 2mL of water containing oil products, wherein the concentration of the oil products in the water is 500mg/mL, after 5nin adsorption, measuring the concentration of the oil products (gasoline, kerosene, diesel oil, olive oil or peanut oil) in the water after adsorption by using an infrared spectrometer, and calculating to obtain the oil product adsorption numerical value of the porous aerogel, wherein the results are shown in a table 2, and the experimental examples 1 to 4 in the table 2 respectively correspond to the performance test experiments of the porous aerogel prepared in the embodiments 1 to 4; the adsorption value (g/g) of oil in Table 2 is calculated as follows:
adsorption number of oil (M)1-M0)/M0；
Wherein M is1Mass (g) of the porous aerogel after the adsorption experiment; m0The mass (g) of the porous aerogel before the adsorption test, i.e., M0＝0.01g。
The calculation formula of the oil separation efficiency (%) in the water body is as follows:
oil separation efficiency in water body [ [ (C)0-C1)/C0]/M0*100％；
Wherein, C1The concentration (mg/mL) of the oil product in the water body after the adsorption experiment; c0The concentration (mg/mL) of oil products in the water body before the adsorption experiment, namely C0＝500mg/mL；M0The mass (g) of the porous aerogel before the adsorption test, i.e., M0＝0.01g。
TABLE 2 adsorption Performance data of porous aerogels prepared in examples 1-4
As can be seen from Table 2, the porous aerogels prepared in examples 1 to 4 all have better adsorption and desorption capabilities for the above oils.
Fig. 8 is a compressive stress-strain curve of the copper nanowire-polyvinyl alcohol porous aerogel prepared in example 3. As can be seen from fig. 8, under the action of strains of 30%, 60% and 90%, the 3 curves are in a closed state as a whole, which indicates that the copper nanowire-polyvinyl alcohol porous aerogel has better mechanical compression fatigue resistance. The compression stress-strain curves of the porous aerogels prepared in example 1, example 2 and example 4 are similar to those of fig. 8, and the 3 curves are closed as a whole under the strain effects of 30%, 60% and 90%, which indicates that the porous aerogels have better mechanical compression fatigue resistance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
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