CN113354861A - Universal method for preparing functional nano material/cellulose composite aerogel by using paper folding principle - Google Patents

Universal method for preparing functional nano material/cellulose composite aerogel by using paper folding principle Download PDF

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CN113354861A
CN113354861A CN202110570835.0A CN202110570835A CN113354861A CN 113354861 A CN113354861 A CN 113354861A CN 202110570835 A CN202110570835 A CN 202110570835A CN 113354861 A CN113354861 A CN 113354861A
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composite aerogel
nano material
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姜越
梁靖雨
程嫣然
彭建
林思劼
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Tongji University
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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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C53/00—Shaping by bending, folding, twisting, straightening or flattening; Apparatus therefor
    • B29C53/02—Bending or folding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C53/00—Shaping by bending, folding, twisting, straightening or flattening; Apparatus therefor
    • B29C53/80—Component parts, details or accessories; Auxiliary operations
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
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    • C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02—Cellulose; Modified cellulose
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls

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Abstract

The invention relates to a method for preparing functional nano material/cellulose composite aerogel, which comprises the following steps: (1) preparing or preparing functional nano materials; (2) dispersing the cellulose into ultrapure water, shaking up by shaking, adding a cellulose solution into the dispersion liquid, fully stirring, and standing; (3) adding a tert-butyl alcohol solution into the mixed solution, uniformly stirring, transferring into a mold for freezing, and performing freeze drying treatment to obtain the functional nano material/cellulose composite aerogel; (4) after being compacted, the paper is folded based on the paper folding principle and then is packaged and stored in vacuum. The invention fully utilizes the soft and foldable performance of aerogel materials, adopts a three-pump paper folding method to easily realize the folding and unfolding of the materials, better solves the technical bottleneck that the aerogel materials are large in volume and difficult to transport, realizes the maximum utilization of the materials, can obtain the composite aerogels with different functional types by replacing functional materials, and has stronger universality.

Description

Universal method for preparing functional nano material/cellulose composite aerogel by using paper folding principle
Technical Field
The invention relates to the technical field of functional nano composite material preparation, in particular to a universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle and application thereof.
Background
Nowadays, the society is developed vigorously, and various novel nano materials and structures thereof emerge in various research reports at home and abroad. Superior performance, application prospect and commercial value of nano-scale materials in energy conversion (such as CO)2Reduction), environmental protection (e.g., degradation of organic pollutants), biological therapy (e.g., drug loading). However, in the current material synthesis and use process, the secondary stacking agglomeration of the material is often caused by strong van der waals acting force in the material, so that the specific surface area of the material is greatly reduced, active sites are masked, and the full capability of the material cannot be released. There are two main methods of improvement: one is to reduce the material consumption, but too little functional material often cannot achieve better effect; another approach is to incorporate various nanomaterial "spacers" (spacers) such as polymers (polyvinyl alcohol and polypropylene), carbon materials (carbon nanotubes and graphene), metal oxides, hydroxides (MnO)2And Fe (OH)3) However, these materials are generally expensive and are prone to secondary pollution during the preparation process, which creates new environmental risks. Therefore, the agglomeration of functional materials and the development of environment-friendly composite materials are problems which need to be solved in the crossing fields of materials and environment.
The aerogel is a material with quite high specific surface area, ultrahigh porosity, controllable open pore structure, easily chemically modified surface and diversified types and forms, and has wide application prospects in the field of environmental purification such as gas adsorption purification, water body purification and the like. Traditional aerogels often require harsh conditions of high temperature, high pressure or no oxygen during the preparation process, and therefore cannot be mass produced in general. In addition, the high-temperature pyrolysis treatment often shows lower mechanical properties and greater brittleness, and cannot meet the requirements of the material on longer cycle period and service life in the use process. Therefore, on the basis of fully utilizing the advantages of the functional nano material, the development of a simple, convenient, easy and environment-friendly synthetic method has very important significance.
Cellulose is the most abundant natural polymer on earth, and among them, Bacterial Cellulose (BC) has been receiving much attention as a novel eco-friendly nano biomaterial discovered in recent years due to its unique interconnected network structure and strong physical properties such as high water holding capacity, large specific surface area, good chemical stability, environmental friendliness and excellent biodegradability. Bacterial cellulose has a more attractive microstructure and unique properties compared to conventional cellulose fibers. First, bacterial cellulose possesses an ultrafine nano-scale three-dimensional (3D) fiber network structure, the diameter of which is in the range of 10 to 100nm, which is about 2 orders of magnitude smaller than plant cellulose, and thus can have a higher specific surface area and porous structure. Meanwhile, it can be mass-produced by a low-cost microbial fermentation process, and the yield is still growing year by year. More importantly, compared with other polymers, the bacterial cellulose has a one-dimensional (1D) nanofiber structure, so that the insulating contact between nano-functional materials is less, and the stacking problem of the materials can be well solved to a certain extent. In addition, only simple physical stirring and freeze drying processes are needed, the bacterial cellulose serving as a nano binder (nano binder) can be easily intertwined with the functional nano material and connected into a layered macroscopic structure, and the composite aerogel with extremely high stability and functionality is prepared. The preparation method has strong universality and has potential application values in the fields of environmental remediation, electromagnetic shielding, photo-thermal conversion devices, new energy and the like.
Patent CN109679146A discloses a preparation method of MXene/cellulose composite aerogel, which comprises the steps of firstly obtaining MXene nano powder, adding cellulose powder into a mixed aqueous solution of sodium hydroxide and urea in a certain proportion by adopting a cellulose sol method, cooling to-12 ℃ to prepare a transparent cellulose mixed solution, keeping the temperature, adding the MXene nano powder into the cellulose mixed solution, then adding a proper amount of epoxy chloropropane, fully stirring for chemical crosslinking, increasing the temperature, carrying out gel reaction on the obtained uniform mixture, carrying out directional freezing on a gel product, and carrying out freeze-drying treatment to obtain the MXene/cellulose composite aerogel. However, this patent has the following drawbacks: 1) the reaction condition of minus 12 ℃ is required to be kept all the time, so that the control is difficult, the operation is complex, and the energy consumption is high; 2) epichlorohydrin belongs to a medium-toxicity chemical, and animal experiments prove that the epichlorohydrin has a potential carcinogenic effect.
In addition, the aerogel has low density, so that the volume is large, and the transportation is difficult, and therefore, how to solve the problem of portable transportation of the composite aerogel is one of the research hotspots in the field.
Disclosure of Invention
The invention aims to overcome the defects of complicated stacking and preparation methods of functional materials, environmental risks and the like in the prior art, and further provides a universal method for preparing a functional nano material/cellulose composite aerogel by using the three-pump paper folding principle and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) preparing or preparing functional nano materials;
(2) dispersing the functional nano material into ultrapure water, shaking uniformly, adding a cellulose solution into the dispersion liquid, fully stirring, and standing;
(3) adding a tert-butyl alcohol solution into the reacted solution, uniformly stirring, transferring the solution into a mold for freezing, and performing freeze drying treatment to obtain the functional nano material/cellulose composite aerogel;
(4) after the composite aerogel is compacted, the composite aerogel is folded based on a paper folding principle, and finally, a finished product is packaged and stored in vacuum.
The invention utilizes the paper folding principle, such as the three-pump folding technology, utilizes the flexibility of the aerogel, compacts the composite aerogel, firstly folds the composite aerogel into an accordion shape along the short edge, then turns over the long edge along a certain angle, laminates well along the transverse crease layer after unfolding, completes the folding process based on the three-pump paper folding principle, packages and stores in vacuum, the specific surface area of the final product is only 1/25 of the original area, easily realizes the folding and unfolding of the material, solves the technical bottleneck that the aerogel material has large volume and is difficult to transport to a great extent, realizes the maximum utilization of the material, and has the advantages of low cost, simple and convenient operation, good repeatability, easy conversion of the result and the like.
Further, in the step (1), the functional nanomaterial may be a zero-dimensional nanomaterial (carbon quantum dots, etc.), a one-dimensional nanomaterial (carbon nanotubes, etc.), a two-dimensional nanomaterial (transition metal oxyhalide, hexagonal boron nitride, graphitic carbon nitride, graphene, TMDs, MXenes, black phosphorus, LDH, etc.), and a three-dimensional nanomaterial (MOF, perovskite, commercial nanomaterial, etc.). For example, the functional nano material TiO disclosed in the patent CN111715250A can be adopted1.47/C。
Further, in the step (2), the mass-to-volume ratio of the functional nano material to the ultrapure water is 10-100 mg: 10-50 mL, excessive ultrapure water can form a large amount of icicles in the subsequent freezing process, the pore structure of the material is increased, and the mechanical property of the material is reduced; the invention selects and adds a certain amount of tert-butyl alcohol, and the main reason is that the tert-butyl alcohol is frozen into acicular ice crystals, thereby effectively relieving the cracking problem caused by the freezing of a large amount of water and adjusting the pore structure.
Further, in the step (2), the ultrapure water has a resistivity of 18.20M Ω & cm-1The water of (2).
Further, in the step (2), the cellulose mainly includes cellulose nanofibers, cellulose nanowhiskers, microfibrillated nanocellulose, bacterial cellulose, and the like.
Further, in the step (2), the mass concentration of the cellulose solution is 0.5-1%, and the volume of the cellulose solution is 5-50 mL.
Further, in the step (2), the stirring time is 1-2 h.
Further, in the step (2), the gel reaction time is 8-10 h.
Further, in the step (3), the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20 to 60.
Further, in the step (3), the freezing temperature is-20 ℃, and the freezing time is 12-16 h. The freezing temperature selected in the invention is-20 ℃ rather than-80 ℃, because the rapid freezing can lead the ice crystal to grow rapidly, the partial structure of the material is convex or concave, and the gradient freezing or the freezing time prolonged by-20 ℃ is more beneficial to the stability of the material.
Further, in the step (3), the freeze drying condition is that the freeze drying is carried out for 36-48 h at-60 ℃, and the damage to the material is smaller than that of the vacuum heating drying.
Further, in the step (4), the compacting time is 12-24 hours.
Further, in step (4), in addition to the three-fold method, a Z-fold method, an accordion-fold method, or the like can be applied.
The functional nano material/cellulose composite aerogel prepared by the method of the invention can easily realize the folding and unfolding of the material by utilizing the three-pump paper folding principle and the special advantages of aerogel materials. The technical bottleneck that aerogel materials are large in size and difficult to transport is solved to a certain extent, and the maximum utilization of the materials is realized.
The functional nano material/cellulose composite aerogel prepared by the method can be used for obtaining different types of composite aerogels through replacement of functional materials, has strong universality and has potential application value in the fields of environmental remediation, electromagnetic shielding, photo-thermal conversion devices, new energy and the like.
In the preparation process, the mass-volume ratio of the selected functional nano material to the ultrapure water is 10-100 mg: 10-50 mL, excessive ultrapure water can form a large amount of icicles in the subsequent freezing process, the pore structure of the material is increased, and the mechanical property of the material is reduced; according to the invention, a certain amount of tert-butyl alcohol is added, and the main reason is that the tert-butyl alcohol is frozen into needle-shaped ice crystals, so that the cracking problem caused by freezing of a large amount of water can be effectively relieved, and the pore structure is adjusted; the freezing temperature selected in the invention is-20 ℃ rather than-80 ℃, because the rapid freezing can lead the ice crystal to rapidly grow, the partial structure of the material is convex or concave, and the gradient freezing or the freezing time prolonged by-20 ℃ is more beneficial to the stability of the material; the drying process of the invention is freeze drying, which has less damage to the material than vacuum heating drying.
The method has the advantages that the folding and unfolding of the material are easily realized by utilizing the three-pump paper folding principle (Z-shaped or organ method) and the special advantages of the aerogel material, the technical bottleneck that the aerogel material is large in size and difficult to transport is solved to a certain extent, the maximum utilization of the material is realized, and meanwhile, the method has strong universality and has potential application value in the fields of environmental remediation, electromagnetic shielding, photo-thermal conversion devices, new energy sources and the like through the replacement of functional materials.
Compared with the prior art, the invention has the following advantages:
(1) the functional nano material/cellulose composite aerogel prepared by the invention can be easily intertwined with the functional nano material by only using the bacterial cellulose as the nano adhesive through simple physical stirring and freeze drying processes, and is connected into a layered macroscopic structure to prepare the composite aerogel with extremely high stability and functionality, so that the problem of material stacking is solved to a certain extent, and the composite aerogel has the advantages of low cost, simplicity and convenience in operation, good repeatability and the like;
(2) the functional nano material/cellulose composite aerogel prepared by the method can obtain different types of composite aerogels only by replacing functional materials, can fully utilize the advantages of the functional materials, has stronger universality, and has potential application values in the fields of environmental remediation, electromagnetic shielding, photo-thermal conversion devices, new energy and the like;
(3) according to the functional nano material/cellulose composite aerogel prepared by the invention, the application scene of the material is greatly improved by utilizing the flexibility of the aerogel and integrating the paper folding technology into the preparation process of the material, and the transportation problem of the functional aerogel is greatly solved for the first public report of the cross application of a plurality of subjects such as the functional nano material, the aerogel, the paper folding technology and the like.
Drawings
FIG. 1 is a photograph of a sample of functional nanomaterial/cellulose composite aerogel prepared using the principles of three-pump origami in the present invention;
FIG. 2 is a photograph of a sample of functional nanomaterial/cellulose composite aerogel folded using the three-pump paper folding principle;
FIG. 3 is a scanning electron microscope photomicrograph of functional nanomaterial/cellulose composite aerogel prepared by using the principles of three-pump origami in the present invention;
FIG. 4 shows the detailed parameters of the three-pump folding method for preparing functional nano material/cellulose composite aerogel by using the three-pump paper folding principle in the present invention;
FIG. 5 is a graph showing the degradation curve of p-nitrophenol in the functional nanomaterial/cellulose composite aerogel prepared by the triple-pump origami principle according to the present invention;
FIG. 6 is an oil absorption curve of functional nanomaterial/cellulose composite aerogel prepared by the principles of three-pump origami to castor oil in accordance with the present invention;
FIG. 7 is a wave-absorbing property curve of the functional nanomaterial/cellulose composite aerogel prepared by using the three-pump origami principle in the present invention;
fig. 8 is a diagram of 8 kinds of functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle in the invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) preparing or preparing functional nano materials;
the functional nano material can be a zero-dimensional nano material (carbon quantum dots and the like), a one-dimensional nano material (carbon nano tubes and the like), a two-dimensional nano material (transition metal oxyhalide, hexagonal boron nitride, graphite carbon nitride, graphene, TMDS, MXenes, black phosphorus, LDH and the like), a three-dimensional nano material (MOF, perovskite, commercial nano material and the like) and the like;
(2) dispersing the 10-100 mg of the functional nano material into a solution with the resistivity of 18.20M omega cm-1Shaking up in 10-50 mL of ultrapure water, adding a cellulose solution with the mass concentration of 0.5-1% and the volume of 5-50 mL into the dispersion liquid, fully stirring for 1-2 h, standing for 8-10 h, and carrying out gel reaction on the obtained uniformly mixed solution;
(3) adding a tert-butyl alcohol solution into the reacted solution, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20-60, uniformly stirring, transferring into a mold, freezing at-20 ℃ for 12-16 h, and freeze-drying for 36-48 h to obtain the functional nano material/cellulose composite aerogel;
(4) compacting the composite aerogel for 12-24 h, then folding by utilizing a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel.
Among them, the folding method is also applicable to a method such as a Z-folding method and an organ-folding method, in addition to the three-pump folding method. By utilizing the three-pump paper folding principle and the unique advantages of the aerogel material, the folding and unfolding of the material are easily realized, the technical bottleneck that the aerogel material is large in size and difficult to transport is solved to a certain extent, and the maximum utilization of the material is realized.
The functional nano material/cellulose composite aerogel obtained by the preparation method can be prepared into different types of composite aerogels only by replacing functional materials, the advantages of the functional materials can be fully utilized, and the preparation method has strong universality and has potential application values in the fields of environmental restoration, electromagnetic shielding, photo-thermal conversion devices, new energy and the like.
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
As shown in fig. 1, from the physical diagram of the functional nanomaterial/cellulose composite aerogel, we can observe that the material is a sponge with a length of 12cm, a width of 8.4cm and a height of 0.5cm (the specific parameters can be adjusted by changing the amount of the solution and the size of the mold according to the experimental needs), and the material is uniformly distributed, soft and free of obvious cracks. From the low power scanning electron microscope photograph of fig. 3, it can be observed that cellulose and the functional nanomaterial are cross-linked to each other to form a three-dimensional network structure. And then the composite aerogel is compacted into paper and then folded.
As shown in FIG. 4, a parametric diagram of the three-Pump folding method is detailed, the three-Pump folding is a periodic structure with a Miura-unit consisting of 4 parallelograms, and the parameters are as follows, in each parallelogram, the short side is a, the long side is b, and the actuation angle is β ∈ [0 °, 90 ° ]]The projection angle between two ridges is
Figure BDA0003082636530000071
Figure BDA0003082636530000075
Angle of projection
Figure BDA0003082636530000072
Can be used for characterizing the folding degree of the Miura-unit when
Figure BDA0003082636530000073
When the Miura-unit is in the fully extended planar state, when
Figure BDA0003082636530000074
In this case, the Miura-unit is in a completely folded state. The size of the Miura-unit in the x, y and z directions is l, w and h respectively. The correlation formula of each parameter in the Miura-unit is as follows:
Figure BDA0003082636530000081
Figure BDA0003082636530000082
Figure BDA0003082636530000083
Figure BDA0003082636530000084
Figure BDA0003082636530000085
the dimensions occupied by the entire three-pump folded structure are given by:
Figure BDA0003082636530000086
Figure BDA0003082636530000087
Figure BDA0003082636530000088
the hypothetical volume occupied is:
V＝L×W×H
one of the main advantages of the three-pump folding scheme is that the effect of reducing the maximum curvature of the film is achieved due to the slight angular deviation of the adjacent segments on their vertical folds, thereby reducing the stress to which these folds are subjected during folding.
Fig. 2 is a photograph of a sample of functional nanomaterial/cellulose composite aerogel folded using the three-pump paper folding principle. Example 2
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 50mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up, adding 0.5% mass concentration into the system5mL of bacterial cellulose solution is accumulated, the mixture is stirred for 1h at room temperature after a sealing film is sealed, the rotating speed is 300rpm, then the mixture is kept stand for 8h, and the obtained uniform mixed solution is subjected to gel reaction;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 3
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 100mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 4
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 100mg, the volume of ultrapure water was 50mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 5
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking uniformly, adding a bacterial cellulose solution with the mass concentration of 0.5% and the volume of 50mL into the system, sealing by using a sealing film, stirring at room temperature for 1h at the rotating speed of 300rpm, standing for 8h, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 6
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking uniformly, adding a bacterial cellulose solution with the mass concentration of 1% and the volume of 5mL into the system, sealing by using a sealing film, stirring at room temperature for 1h at the rotating speed of 300rpm, standing for 8h, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 7
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a mass ofDissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking uniformly, adding a bacterial cellulose solution with the mass concentration of 1% and the volume of 50mL into the system, sealing by using a sealing film, stirring at room temperature for 1h at the rotating speed of 300rpm, standing for 8h, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 8
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 60, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 9
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 16h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 10
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking evenly, then adding fine powder with the mass concentration of 0.5 percent and the volume of 5mL into the systemSealing the bacterial cellulose solution with a sealing film, stirring at room temperature for 1h at the rotating speed of 300rpm, standing for 8h, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 60, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at the temperature of-20 ℃ for 16h, and freeze-drying at the temperature of-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 11
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and then, freezing and drying at-60 ℃ for 48h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Example 12
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing a certain mass of functional nano material, and dissolving the functional nano material into ultrapure water, wherein the functional nano material is TiO1.47The mass of/C was 10mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 5mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 8 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and freeze-drying at-60 ℃ for 36h to obtain the functional nano material/cellulose composite aerogel;
(3) compacting the obtained composite aerogel weight for 24 hours, then folding by utilizing a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by utilizing the three-pump paper folding principle.
Example 13
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing certain mass of photocatalytic nano material (such as C, N-TiO)2Patent No. ZL201710702033.4) in ultrapure water, in which C, N-TiO is dissolved2Has a mass of 30mg, a volume of ultrapure water of 10mL, and a resistivity of 18.20 M.OMEGA.cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 10mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 10 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and then, freezing and drying at-60 ℃ for 48h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
The catalyst is used for catalytically degrading p-nitrophenol mode pollutants, so that the catalytic activity of the catalyst is tested. The specific operation steps are as follows: 1L of 100ppm p-nitrophenol stock solution is prepared and then diluted to 10ppm for standby. Preparation of BC (control), C, N-TiO2Adding the/BC material into 200mL of 10ppm solution, carrying out dark reaction adsorption, and carrying out photocatalytic degradation under visible light after adsorption saturation. Sampling according to a specific time interval, filtering, measuring the absorbance of the solution by an enzyme-labeling instrument, and observing whether the contaminant solution without the material has degradation effect on the contaminant by pure illumination by paying attention to the independent arrangement of the contaminant solution without the material. The test results are shown in FIG. 5, from which we can see that BC alone has little adsorption to nitrophenol and supports C, N-TiO under dark reaction conditions2The composite aerogel reaches the adsorption saturation balance (19 percent) within 90 min; after the light is turned on, no catalyst and no obvious photocatalytic degradation effect exists in the BC alone, and C, N-TiO2The degradation efficiency of the/BC composite aerogel to p-nitrophenol is more than 90% at 180 min.
Example 14
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing certain mass of photothermal conversion nanometer material (such as Ti)3C2) Dissolving in ultrapure water, wherein Ti3C2Has a mass of 30mg, a volume of ultrapure water of 10mL, and a resistivity of 18.20 M.OMEGA.cm-1Shaking up and then adding into the systemAdding bacterial cellulose solution with the mass concentration of 0.5% and the volume of 10mL, sealing by using a sealing film, stirring at room temperature for 1h at the rotating speed of 300rpm, standing for 10h, and carrying out gel reaction on the obtained uniform mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and then, freezing and drying at-60 ℃ for 48h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
Castor oil is selected as model oil to test Ti loaded with photothermal conversion nano material3C2The oil absorption rate of the/BC composite aerogel was varied. The specific operation steps are as follows: selecting BC and Ti3C2Two types of materials,/BC, were tested for oil absorption capacity under dark/visible light illumination (0.514 sun and 1.01 sun), respectively. As can be seen in fig. 6: 1) the single BC has better oil absorption characteristic, and no light has great influence on the oil absorption rate and the adsorption capacity of the BC; 2) carrying Ti3C2The oil absorption rate of the composite aerogel is reduced under the dark condition, mainly because the MXene material has good hydrophilic property, the oil absorption capacity of the single BC is reduced after loading; 3) after addition of light, Ti3C2The oil absorption rate of the/BC composite aerogel is obviously improved, and the stronger the light intensity is, the faster the adsorption rate is, mainly because of Ti3C2The photo-thermal effect of (2) can degrade the viscosity degree of the castor oil, thereby accelerating the adsorption rate.
Example 15
A universal method for preparing functional nano material/cellulose composite aerogel by utilizing the three-pump paper folding principle comprises the following steps:
(1) weighing electromagnetic shielding nanometer material (such as Nb) with certain mass2C) Dissolving in ultrapure water, wherein Nb2The mass of C was 30mg, the volume of ultrapure water was 10mL, and the resistivity was 18.20 M.OMEGA.. cm-1Shaking up the mixture by shaking, adding a bacterial cellulose solution with the mass concentration of 0.5 percent and the volume of 10mL into the system, sealing the sealing film, stirring the mixture for 1 hour at room temperature at the rotating speed of 300rpm, standing the mixture for 10 hours, and carrying out gel reaction on the obtained uniformly mixed solution;
(2) adding a certain volume of tert-butyl alcohol solution into the solution after the gel reaction, wherein the volume ratio of the tert-butyl alcohol solution to the total solution is 1: 20, stirring at room temperature for 5min at the rotating speed of 300rpm, transferring into a mold, freezing at-20 ℃ for 12h, and then, freezing and drying at-60 ℃ for 48h to obtain the functional nano material/cellulose composite aerogel;
(3) and compacting the obtained composite aerogel by using a weight for 12h, folding by using a three-pump paper folding principle, and finally carrying out vacuum packaging to obtain the functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle.
FIG. 7 is a wave-absorbing property curve, and it can be seen that BC alone has almost no wave-absorbing property in the range of 2-18GHz, but Nb is loaded2The composite aerogel of C shows good wave-absorbing property within the range of 12-15GHz, and the highest wave-absorbing property can reach-52.73 dB.
The invention utilizes the three-pump paper folding principle and the unique advantages of aerogel materials, easily realizes the folding and unfolding of the materials, solves the technical bottleneck that the aerogel materials are large in volume and difficult to transport, and realizes the maximum utilization of the materials.
Furthermore, by replacement of functional materials, composite aerogels of different functional types can be obtained, such as photocatalysis (e.g., TiO)2、g-C3N4) Adsorption (e.g., MOF), Fenton catalytic oxidation (e.g., supported transition metal carbides), photothermal conversion (e.g., Ti)3C2) Electromagnetic shielding (e.g. Nb)2C) Or flexible electrodes (e.g., graphene), etc. Fig. 8 is a diagram of 8 kinds of functional nano material/cellulose composite aerogel prepared by using the three-pump paper folding principle in the invention.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. A universal method for preparing functional nano material/cellulose composite aerogel by using a paper folding principle is characterized by comprising the following steps:
(1) preparing or preparing functional nano materials;
(2) dispersing the functional nano material into ultrapure water, shaking uniformly, adding a cellulose solution into the dispersion liquid, fully stirring, and standing;
(3) adding a tert-butyl alcohol solution into the mixed solution, uniformly stirring, transferring into a mold for freezing, and performing freeze drying treatment to obtain the functional nano material/cellulose composite aerogel;
(4) after the composite aerogel is compacted, the composite aerogel is folded based on a paper folding principle, and finally a finished product is packaged and stored in vacuum.
2. The universal method for preparing functional nano-material/cellulose composite aerogel according to claim 1, wherein in step (1), the functional nano-material comprises zero-dimensional nano-material, one-dimensional nano-material, two-dimensional nano-material, three-dimensional nano-material.
3. The universal method for preparing functional nano material/cellulose composite aerogel by using the paper folding principle as claimed in claim 2, wherein in the step (1), the zero-dimensional nano material is carbon quantum dots; the one-dimensional nano material is a carbon nano tube; the two-dimensional nano material comprises transition metal oxyhalide, hexagonal boron nitride, graphite carbon nitride, graphene, TMDS, MXenes, black phosphorus and LDH; the three-dimensional nano material comprises MOF, perovskite and commercial nano material.
4. The universal method for preparing the functional nano-material/cellulose composite aerogel by using the paper folding principle as claimed in claim 1, wherein in the step (2), the dosage ratio of the functional nano-material to the ultrapure water is 10-100 mg: 10-50 mL.
5. The universal method for preparing functional nano material/cellulose composite aerogel according to claim 1, wherein in step (2), the cellulose comprises nano fiber, nano whisker, microfibrillated nano cellulose and bacterial cellulose.
6. The universal method for preparing the functional nano material/cellulose composite aerogel by using the paper folding principle as claimed in claim 5, wherein the mass concentration of the cellulose solution is 0.5-1%; stirring for 1-2 h, and standing for 8-10 h.
7. The universal method for preparing functional nano material/cellulose composite aerogel by using the paper folding principle as claimed in claim 1, wherein in the step (3), the volume ratio of the tert-butyl alcohol solution to the mixed solution in the step (2) is 1: 20 to 60.
8. The universal method for preparing the functional nano material/cellulose composite aerogel by using the paper folding principle as claimed in claim 1, wherein in the step (3), the freezing temperature is-20 ℃, and the freezing time is 12-16 h; the freeze drying condition is that the freeze drying is carried out for 36-48 h at the temperature of-60 ℃.
9. The universal method for preparing the functional nano material/cellulose composite aerogel by using the paper folding principle as claimed in claim 1, wherein in the step (4), the compacting time is 12-24 h.
10. The general method for preparing functional nano material/cellulose composite aerogel according to any one of claims 1 to 9, wherein in step (4), the obtained composite aerogel is compacted and then folded by three-pump folding method, Z-type folding method or organ folding method.
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