CN113149615A - Super-elastic flexible three-dimensional composite ceramic nanofiber block and preparation method and application thereof - Google Patents
Super-elastic flexible three-dimensional composite ceramic nanofiber block and preparation method and application thereof Download PDFInfo
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Abstract
A super elastic flexible three-dimensional composite ceramic nano-fiber block and a preparation method and application thereof are disclosed, wherein polyvinylpyrrolidone is dissolved in ethanol to be used as spinning precursor liquid; adding a substance source of a ceramic material, a corresponding solvent and an auxiliary agent into the precursor liquid to form uniform electrospinning liquid, and collecting a fiber membrane obtained by electrospinning, wherein the membrane thickness is 10-30 mu m. Meanwhile, simply superposing the electrospun fiber membranes in the modes of folding, cutting and the like under the condition that the humidity is 40-60 wt.%, adhering by utilizing the volatility of the solvent of the fiber membranes, and then calcining in air or other atmosphere to obtain the three-dimensional ceramic fiber block. The obtained three-dimensional ceramic fiber block has rich pore structures, combines excellent thermal stability and chemical stability of ceramic fibers, and can be applied to the fields of air purification, particularly high-temperature waste gas treatment and the like.
Description
Technical Field
The invention belongs to the technical field of three-dimensional ceramic nanofiber blocks, and particularly relates to a super-elastic flexible three-dimensional composite ceramic nanofiber block as well as a preparation method and application thereof.
Background
Ceramic fiber is a fibrous light refractory material, and has the advantages of light weight, high temperature resistance, good thermal stability, low thermal conductivity, small specific heat, mechanical shock resistance and the like, so the ceramic fiber is widely applied to the industries of machinery, metallurgy, chemical industry, petroleum, ceramics, glass, electronics and the like. In recent years, due to the continuous rise of global energy prices, energy conservation becomes the Chinese national strategy, and under the background, ceramic fibers which can save 10 to 30 percent of energy compared with traditional refractory materials such as heat insulation bricks, castable and the like are more and more widely applied in China, and the development prospect is very good.
At present, most of ceramic fibers obtained by electrostatic spinning are low-dimensional materials, large-size ceramic fiber membranes are difficult to obtain due to inevitable shrinkage in the fiber preparation process, and industrial development in the fields of air filtration and the like is difficult due to the limitation of the mechanical properties of the ceramic fiber membranes. Although the low-dimensional ceramic fibers can be assembled into three-dimensional blocks (such as aerogel and the like) by a sol-gel method and the like, the preparation method is complex, takes a long time and has high cost.
Disclosure of Invention
The technical problem to be solved is as follows: the invention provides a super-elastic flexible three-dimensional composite ceramic nanofiber block and a preparation method and application thereof, wherein the solvent volatility of a fiber membrane is utilized to wet the fiber membrane on a three-dimensional layer for adhesion, and the fiber membrane is self-assembled into the three-dimensional block in situ; meanwhile, the three-dimensional block is less limited by the size of equipment, the mechanical property is further improved compared with that of a membrane material, and beneficial conditions are provided for large-scale production and industrial popularization of ceramic fibers. In addition, the alumina/titanium dioxide three-dimensional composite ceramic fiber block prepared by the method has abundant pore structures, combines excellent thermal stability and chemical stability, and can be applied to the field of air purification, especially high-temperature waste gas treatment.
The technical scheme is as follows: a preparation method of a super-elastic flexible three-dimensional composite ceramic nanofiber block comprises the following steps: a. preparing 10-30 wt.% of ethanol solution of polyvinylpyrrolidone (PVP), sequentially adding a ceramic material source, a good solvent of the ceramic material source and an auxiliary agent into the solution, and stirring at room temperature to completely dissolve the ceramic material source, the good solvent and the auxiliary agent to obtain uniform precursor solution, wherein the volume ratio of the ethanol solution of PVP to the good solvent to the auxiliary agent is (5-15) to (2-10); the ceramic material source is isopropyl titanate and aluminum acetylacetonate, wherein the mass fraction of the aluminum acetylacetonate is 5-50 wt.%, and the volume ratio of the isopropyl titanate to the ethanol is (2-5): 9; b. preparing the precursor solution into an electrospun nanofiber membrane by using an electrostatic spinning device; c. and tearing off the obtained electrospun nanofiber membrane, assembling the electrospun nanofiber membrane in a folding and cutting mode to obtain a three-dimensional fiber block, and roasting the block in a muffle furnace at the temperature of 500-900 ℃ for 1-2h at the heating rate of 2.0 ℃/min to obtain the three-dimensional composite ceramic nanofiber block.
Preferably, the polyvinylpyrrolidone has a molecular weight of 1300000.
Preferably, Al is obtained by pyrolysis of the above-mentioned aluminum acetylacetonate and isopropyl titanate2O3And TiO2The mass ratio of (1-19) to (19).
Preferably, the good solvent is ethanol and acetone, the auxiliary agent is acetic acid, and the volume ratio of the ethanol to the acetone to the acetic acid is 9:10: 6.
Preferably, the electrostatic spinning device obtains the composite ceramic nanofiber membrane under the conditions of 10kV to 20kV, the distance between the metal needle and the filament collector being 10 cm to 20cm, the flow rate being 0.3 mL/h to 1.0mL/h, and the humidity being 40% to 60%, wherein the ambient temperature is 25 ℃, the humidity is 30% to 40% by weight, and the receiving time is 1 h to 4 h.
Preferably, the electrospun nanofiber membrane has a thickness of 10 to 40 μm.
Preferably, the assembly process environment humidity of the three-dimensional block is maintained at 40-60 wt.%.
The three-dimensional composite ceramic nanofiber block prepared by the preparation method.
Application of three-dimensional composite ceramic nanofiber block in air purification, especially high-temperature waste gas treatment
Has the advantages that: according to the invention, the alumina/titanium dioxide three-dimensional composite ceramic nanofiber block prepared by combining the electrostatic spinning technology with in-situ self-assembly is utilized to volatilize the solvent of the electrospun fiber membrane, so that the fiber membrane is adhered on the three-dimensional layer, the preparation cost of the original three-dimensional ceramic nanofiber block is reduced, and the method is expected to be industrialized. The alumina/titanium dioxide three-dimensional composite ceramic nanofiber block prepared by the invention has a loose and porous structure, is large in specific surface area, combines good thermal stability and chemical stability of ceramic fibers, and can be applied to the fields of air purification, particularly high-temperature waste gas treatment and the like.
Drawings
FIG. 1 is a schematic diagram of the principle of preparation of a three-dimensional composite ceramic nanofiber mass;
FIG. 2 is a three-dimensional electrospun nanofiber mass physical map;
FIG. 3 is a diagram of a three-dimensional composite ceramic nanofiber bulk entity;
fig. 4 is a schematic diagram of a PM particle interception test.
Fig. 5 is a schematic diagram of the elasticity of a three-dimensional composite ceramic nanofiber mass.
Detailed Description
Example 1
a. Preparing an alumina/titanium dioxide three-dimensional composite ceramic nanofiber block with 5% of aluminum by adopting an electrostatic spinning method:
first, an electrospinning precursor solution was prepared. 0.6g of PVP powder and 4.5mL of ethanol are mixed and stirred overnight to obtain a uniform and transparent solution, 5mL of acetone, 0.22g of aluminum acetylacetonate, 3mL of acetic acid and 2.5mL of isopropyl titanate are sequentially added into the solution and stirred at room temperature to be completely dissolved, so that a yellow and transparent precursor solution is obtained.
And secondly, under the conditions that the voltage is 15kV-20kV, the distance between a metal needle and a receiver is 12.5cm, the flow rate is 0.5mL/h, collecting the fiber membrane prepared from the precursor solution after 2h, wherein the membrane thickness is 10-30 mu m, the spinning environment temperature is 25 ℃, and the humidity is 30% -40%.
And assembling the fibers obtained by electrospinning into three-dimensional blocks by means of cutting, folding and the like under the condition of 40-60 wt.%. And roasting the three-dimensional block in a muffle furnace at 600 ℃ for 2h, wherein the heating rate is 2.0 ℃/min, and thus obtaining the alumina/titanium dioxide three-dimensional composite ceramic nanofiber block.
b. High-temperature waste gas treatment test:
the experimental test sample was cut into a cylinder having a diameter of 5cm and placed on the processing apparatus shown in fig. 4, and the results of the experiment showed that the removal rates of the alumina/titania three-dimensional composite ceramic nanofiber blocks for PM 0.3, PM 2.5, and PM10 are shown in the following table.
Example 2
a. Preparing an alumina/titanium dioxide three-dimensional composite ceramic nanofiber block with 15% of aluminum by adopting an electrostatic spinning method:
first, an electrospinning precursor solution was prepared. 0.6g of PVP powder and 4.5mL of ethanol are mixed and stirred overnight to obtain a uniform and transparent solution, 5mL of acetone, 0.73g of aluminum acetylacetonate, 3mL of acetic acid and 2.5mL of isopropyl titanate are sequentially added into the solution and stirred at room temperature to be completely dissolved, so that a yellow and transparent precursor solution is obtained.
And secondly, under the conditions that the voltage is 15kV-20kV, the distance between a metal needle and a receiver is 12.5cm, the flow rate is 0.5mL/h, collecting the fiber membrane prepared from the precursor solution after 2h, wherein the membrane thickness is 10-30 mu m, the spinning environment temperature is 25 ℃, and the humidity is 30% -40%.
And assembling the fibers obtained by electrospinning into three-dimensional blocks by means of cutting, folding and the like under the condition of 40-60 wt.%. And roasting the three-dimensional block in a muffle furnace at 600 ℃ for 2h, wherein the heating rate is 2.0 ℃/min, and thus obtaining the alumina/titanium dioxide three-dimensional composite ceramic nanofiber block.
b. High-temperature waste gas treatment test:
the experimental test sample was cut into a cylinder having a diameter of 5cm and placed on the processing apparatus shown in fig. 4, and the results of the experiment showed that the removal rates of the alumina/titania three-dimensional composite ceramic nanofiber blocks for PM 0.3, PM 2.5, and PM10 are shown in the following table.
Example 3
a. Preparing an alumina/titanium dioxide three-dimensional composite ceramic nanofiber block with 30% of aluminum by adopting an electrostatic spinning method:
first, an electrospinning precursor solution was prepared. 0.6g of PVP powder and 4.5mL of ethanol are mixed and stirred overnight to obtain a uniform and transparent solution, 5mL of acetone, 1.00g of aluminum acetylacetonate, 3mL of acetic acid and 1.41mL of isopropyl titanate are sequentially added into the solution and stirred at room temperature to be completely dissolved, so that a yellow and transparent precursor solution is obtained.
And secondly, under the conditions that the voltage is 15kV-20kV, the distance between a metal needle and a receiver is 12.5cm, the flow rate is 0.5mL/h, collecting the fiber membrane prepared from the precursor solution after 2h, wherein the membrane thickness is 10-30 mu m, the spinning environment temperature is 25 ℃, and the humidity is 30% -40%.
And assembling the fibers obtained by electrospinning into three-dimensional blocks by means of cutting, folding and the like under the condition of 40-60 wt.%. And roasting the three-dimensional block in a muffle furnace at 600 ℃ for 2h, wherein the heating rate is 2.0 ℃/min, and thus obtaining the alumina/titanium dioxide three-dimensional composite ceramic nanofiber block.
b. High-temperature waste gas treatment test:
the experimental test sample was cut into a cylinder having a diameter of 5cm and placed on the processing apparatus shown in fig. 4, and the results of the experiment showed that the removal rates of the alumina/titania three-dimensional composite ceramic nanofiber blocks for PM 0.3, PM 2.5, and PM10 are shown in the following table.
Example 4
a. Preparing an alumina/titanium dioxide three-dimensional composite ceramic nanofiber block with 30% of aluminum by adopting an electrostatic spinning method:
first, an electrospinning precursor solution was prepared. 0.6g of PVP powder and 4.5mL of ethanol are mixed and stirred overnight to obtain a uniform and transparent solution, 5mL of acetone, 1.00g of aluminum acetylacetonate, 3mL of acetic acid and 1.41mL of isopropyl titanate are sequentially added into the solution and stirred at room temperature to be completely dissolved, so that a yellow and transparent precursor solution is obtained.
And secondly, under the conditions that the voltage is 15kV-20kV, the distance between a metal needle and a receiver is 12.5cm, the flow rate is 0.5mL/h, collecting the fiber membrane prepared from the precursor solution after 2h, wherein the membrane thickness is 10-30 mu m, the spinning environment temperature is 25 ℃, and the humidity is 30% -40%.
And assembling the fibers obtained by electrospinning into three-dimensional blocks by means of cutting, folding and the like under the condition of 40-60 wt.%. And roasting the three-dimensional block in a muffle furnace at 900 ℃ for 2h, wherein the heating rate is 2.8 ℃/min, and thus obtaining the alumina/titanium dioxide three-dimensional composite ceramic nanofiber block.
b. And (3) testing thermal stability:
firstly, placing a three-dimensional composite ceramic nanofiber block in an alcohol lamp outer flame for heating for 30min, wherein the block almost maintains the original shape and is not changed; next, the block was heated in a butane torch (ca. 1300 ℃ C.) for 10min, and the block remained in the intact shape without significant collapse of the structure.
The test sample heated by the alcohol lamp for 30min was cut into a cylinder with a diameter of 5cm, and placed on the processing apparatus shown in fig. 4, and the experimental results showed that the removal rates of the alumina/titania three-dimensional composite ceramic nanofiber blocks for PM 0.3, PM 2.5, and PM10 are shown in the following table.
Test results show that the three-dimensional composite ceramic nanofiber block has good thermal stability.
c. And (3) testing chemical stability:
the three-dimensional composite ceramic nanofiber block is placed in an environment with the pH value of 3 for 24h, the block structure does not collapse obviously, and the original shape is still kept.
The test sample after the acid environment treatment was cut into a cylinder having a diameter of 5cm, and placed on the treatment apparatus shown in fig. 4, and the results of the experiment showed that the removal rates of the alumina/titania three-dimensional composite ceramic nanofiber blocks for PM 0.3, PM 2.5, and PM10 are shown in the following table.
In addition, the three-dimensional composite ceramic nanofiber mass is placed in an environment with the pH value of 10 for 24h, and the bulk structure is not obviously collapsed and still maintains the original shape.
The test sample after the alkaline environment treatment was cut into a cylinder having a diameter of 5cm, and placed on the treatment apparatus shown in fig. 4, and the results of the experiment showed that the removal rates of the alumina/titania three-dimensional composite ceramic nanofiber blocks for PM 0.3, PM 2.5, and PM10 are shown in the following table.
Test results show that the three-dimensional composite ceramic nanofiber block has good chemical stability.
Claims (9)
1. A preparation method of a super-elastic flexible three-dimensional composite ceramic nanofiber block is characterized by comprising the following steps: a. preparing 10-30 wt.% of ethanol solution of polyvinylpyrrolidone (PVP), sequentially adding a ceramic material source, a good solvent of the ceramic material source and an auxiliary agent into the solution, and stirring at room temperature to completely dissolve the ceramic material source, the good solvent and the auxiliary agent to obtain uniform precursor solution, wherein the volume ratio of the ethanol solution of PVP to the good solvent to the auxiliary agent is (5-15) to (2-10); the ceramic material source is isopropyl titanate and aluminum acetylacetonate, wherein the mass fraction of the aluminum acetylacetonate is 5-50 wt.%, and the volume ratio of the isopropyl titanate to the ethanol is (2-5): 9; b. preparing the precursor solution into an electrospun nanofiber membrane by using an electrostatic spinning device; c, tearing off the obtained electrospun nanofiber membrane, assembling the electrospun nanofiber membrane in a folding and cutting mode to obtain a three-dimensional fiber block, and then roasting the block in a muffle furnace at the temperature of 500-900 ℃ for 1-2h at the heating rate of 2.0 ℃/min to obtain the three-dimensional composite ceramic nanofiber block.
2. The method for preparing the ultra-elastic flexible three-dimensional composite ceramic nanofiber mass as claimed in claim 1, wherein the molecular weight of the polyvinylpyrrolidone is 1300000.
3. The method for preparing the ultra-elastic flexible three-dimensional composite ceramic nanofiber mass as claimed in claim 1, wherein Al is obtained by pyrolysis of aluminum acetylacetonate and isopropyl titanate2O3And TiO2The mass ratio of (1-19) to (19).
4. The method for preparing the ultra-elastic flexible three-dimensional composite ceramic nanofiber block as claimed in claim 1, wherein the good solvent is ethanol and acetone, the auxiliary agent is acetic acid, and the volume ratio of the ethanol to the acetone to the acetic acid is 9:10: 6.
5. The method for preparing the ultra-elastic flexible three-dimensional composite ceramic nanofiber block as claimed in claim 1, wherein the electrostatic spinning device is used for obtaining the composite ceramic nanofiber membrane under the conditions of 10kV to 20kV, the distance between the metal needle and the filament collector being 10 cm to 20cm, the flow rate being 0.3 mL/h to 1.0mL/h, and the humidity being 40% to 60%, wherein the ambient temperature is 25 ℃, the humidity is 30% to 40% by weight, and the receiving time is 1 h to 4 h.
6. The method for preparing the ultra-elastic flexible three-dimensional composite ceramic nanofiber bulk according to claim 1, wherein the thickness of the electrospun nanofiber membrane is 10-40 μm.
7. The method for preparing the ultra-elastic flexible three-dimensional composite ceramic nanofiber mass as claimed in claim 1, wherein the humidity of the assembling processing environment of the three-dimensional mass is maintained at 40-60 wt.%.
8. The super elastic flexible three-dimensional composite ceramic nanofiber block prepared by the preparation method of any one of claims 1 to 7.
9. Use of the superelastic flexible three-dimensional composite ceramic nanofiber mass according to claim 8 for air purification, especially high temperature exhaust gas treatment.
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| CN114045608A (en) * | 2021-11-10 | 2022-02-15 | 东华大学 | Flexible polycrystalline titanium oxide-aluminum oxide composite nanofiber membrane and preparation method thereof |
| CN114560709A (en) * | 2021-11-19 | 2022-05-31 | 东华大学 | Ceramic nanofiber aerogel with hinged structure and preparation method thereof |
| CN114920549A (en) * | 2022-05-30 | 2022-08-19 | 东南大学 | Method for preparing oxide ceramic nanofiber membrane by using precursor solution as binder |
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Application publication date: 20210723 |