CN107952376B - Ceramic nanofiber-based composite purification membrane and preparation method and application thereof - Google Patents
Ceramic nanofiber-based composite purification membrane and preparation method and application thereof Download PDFInfo
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- CN107952376B CN107952376B CN201711171538.9A CN201711171538A CN107952376B CN 107952376 B CN107952376 B CN 107952376B CN 201711171538 A CN201711171538 A CN 201711171538A CN 107952376 B CN107952376 B CN 107952376B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0036—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions by adsorption or absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—Metals
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/06—Organic material
- B01D71/74—Natural macromolecular material or derivatives thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The preparation method comprises dissolving polyvinylpyrrolidone in ethanol to obtain an electrospinning precursor solution; adding a substance source of a ceramic material, a corresponding solvent and an auxiliary agent into the precursor liquid to form a uniform electro-discharge solution, and collecting fibers obtained by electro-spinning by taking the grounded metal net as a receiver under the conditions of 10kV-20kV, 10-15cm of distance between a metal needle head and a wire collector and 0.3-1.0mL/h of flow speed. And roasting in air at 750 ℃ to obtain loose and porous ceramic nano-fibers which are used as adsorption active layers. The non-woven fabric is used as an encapsulating material to effectively encapsulate the ceramic nanofiber/metal mesh to form the complete purification membrane. The obtained composite purification membrane has excellent PM2.5 purification capacity and mechanical property.
Description
Technical Field
The invention belongs to a preparation technology of a nano material composite membrane, and particularly relates to a ceramic nanofiber/metal mesh/non-woven fabric PM2.5 composite purification membrane, and a preparation method and application thereof.
Background
The prior art is as follows: the ceramic nanofiber prepared by the electrostatic spinning method has a series of unique characteristics and properties, such as a unique one-dimensional structure, a large length-diameter ratio, a high specific surface area, a porous structure and a graded structure. In addition, another significant feature is that these nanofibers can be conveniently fabricated into a film shape, making them well suited for some membrane-based applications, including filtration membranes, separations. However, the inherently weak mechanical strength of ceramic materials greatly limits their range of applications. Therefore, creatively using the high-strength substrate can become a convenient way for effectively improving the mechanical property of the ceramic nanofiber material.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides a ceramic nanofiber-based composite purification membrane and a preparation method and application thereof, and composite materials with different adsorption capacities can be obtained by regulating and controlling parameters such as flow speed, distance, voltage, time, aperture of a metal mesh, component ratio of spinning solution and the like in the electrostatic spinning process; by utilizing electrostatic spinning, the ceramic nanofiber adsorption layer can be rapidly and uniformly prepared; by utilizing the special structure of the metal net, the adsorption area can be enlarged to 1.5 times of the membrane area; the adsorbing material obtained by packaging has higher mechanical strength.
The technical scheme is as follows: the preparation method of the ceramic nanofiber-based composite purification membrane comprises the following preparation steps: a. preparing a ceramic nanofiber/metal mesh composite material by adopting an electrostatic spinning method: dissolving polyvinylpyrrolidone (PVP) with the molecular weight of 1300000 in ethanol, stirring overnight to obtain a uniform and transparent solution with the mass fraction of 10-20 wt.%, 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 a uniform precursor solution; b. setting the voltage to be 10kV-20kV, setting the distance between a metal needle and a filament collector to be 10-15cm, setting the flow rate to be 0.3-1.0mL/h, and collecting fibers by taking a grounded metal net as a receiver by using an electrostatic spinning device, wherein the spinning environment temperature is 25 ℃ and the humidity is not more than 40 percent to obtain nano fibers/metal nets; c. roasting the electrospun nanofiber/metal mesh in a muffle furnace at 750 ℃ for 270min, wherein the heating rate is 2.8 ℃/min, so as to obtain the ceramic nanofiber/metal mesh; d. and fixing the non-woven fabric with the gram weight of 60g on the metal mesh surface of the ceramic nanofiber/metal mesh material, and packaging to obtain the ceramic nanofiber-based composite purification membrane.
Preferably, the ceramic material source is isopropyl titanate or aluminum acetylacetonate.
Preferably, the good solvent is ethanol or copper propionate.
Preferably, the auxiliary is acetic acid.
Preferably, the pore diameter of the metal mesh is 3mm or 1 mm.
The ceramic nanofiber-based composite purification membrane prepared by the preparation method.
The ceramic nanofiber-based composite purification membrane is applied to adsorption of pollutant molecules in gas.
The ceramic nanofiber-based composite purification membrane is applied to adsorbing PM2.5 in gas.
Has the advantages that: the ceramic nano-fiber prepared by the invention has a loose and porous fine structure after being roasted, thereby providing a great specific surface area and a great amount of adsorption active sites, and further leading the composite material to have excellent adsorption performance. The metal mesh plays a supporting role, so that the composite adsorbing material has higher mechanical strength and is suitable for treating the gas containing PM2.5 within a certain flow rate range. In addition, the net structure of the metal net enables collected fibers to present corresponding net distribution in the electrostatic spinning process, as shown in fig. 2, the nanofibers at the pores of the metal net layer are slightly thinner than the fibers at the non-pores due to the lack of adhesion, the filtration resistance is relatively smaller when gas flows through, and the PM2.5 adsorbed at the early stage of purification is also more. As filtration proceeds, the filtration resistance increases more rapidly at the pores than at the non-pores, and after a certain amount of accumulation the filtration resistance at the pores will reach and have a level of membrane layer attached, and overall the amount of adsorption can be nearly 1.5 times that of a purification membrane without pore design.
Drawings
FIG. 1 is a schematic view of an electrospinning apparatus.
Fig. 2 is a schematic view of a ceramic nanofiber/metal mesh/non-woven fabric structure.
FIG. 3 is a schematic cross-sectional adsorption diagram of ceramic nanofibers.
Fig. 4 is an SEM image of a titania ceramic fiber membrane.
Fig. 5 is an SEM image of an alumina ceramic fiber membrane.
Fig. 6 is an SEM image of the titanium-aluminum composite fiber membrane (titanium-aluminum molar ratio is 10: 1).
FIG. 7 is an SEM image of a titanium-aluminum composite fiber membrane (molar ratio of titanium to aluminum is 5: 1).
Fig. 8 is a schematic view of a PM2.5 adsorption effect detection apparatus.
Detailed Description
Example 1:
a. preparing a titanium dioxide/metal mesh/non-woven fabric composite adsorbing material by adopting an electrostatic spinning method:
first, an electrospinning precursor solution was prepared. 0.4g of PVP powder and 4.5mL of ethanol are mixed, stirred overnight to obtain a uniform and transparent solution, 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 to obtain a yellow and transparent precursor solution.
Secondly, under the conditions that the voltage is 15kV-20kV, the distance between the metal needle head and the metal net is 12.5cm, and the flow rate is 0.5mL/h, the grounded metal net with the aperture of 3mm and the thickness of 0.5mm is used as a receiver for collecting fibers, and the spinning environment temperature is required to be 25 ℃ and the humidity is required to be below 40%.
And roasting the PVP/isopropyl titanate/metal mesh obtained by electrospinning at 750 ℃ for 270min in a muffle furnace at the heating rate of 2.8 ℃/min, and decomposing the PVP in the heating process to obtain the titanium dioxide/metal mesh. And fixing the non-woven fabric with the gram weight of 60g on the metal mesh surface of the titanium dioxide/metal mesh material, and packaging to form the complete titanium dioxide/metal mesh/non-woven fabric composite adsorption mesh.
PM2.5 adsorption Performance test:
the test sample was cut into a circular filter membrane with a diameter of 90 ± 2mm, and placed on the test table shown in fig. 8, with a flow rate of 85L/min, and the results of the experiment showed that the removal rate of PM2.5 by the titanium dioxide/metal mesh/nonwoven fabric composite adsorption net was as shown in the following table.
Example 2:
a. preparing an alumina/metal mesh/non-woven fabric composite adsorbing material by adopting an electrostatic spinning method:
first, an electrospinning precursor solution was prepared. Mixing 0.3g PVP powder with 2mL of ethanol, stirring overnight to obtain a uniform and transparent solution, sequentially adding 3mL of acetone and 0.3g of aluminum acetylacetonate into the solution, and stirring at room temperature to completely dissolve the mixture to obtain a colorless and transparent precursor solution.
Secondly, under the conditions that the voltage is 15kV-20kV, the distance between the metal needle head and the metal net is 12.5cm, and the flow rate is 0.5mL/h, the grounded metal net with the aperture of 3mm and the thickness of 0.5mm is used as a receiver for collecting fibers, and the spinning environment temperature is required to be 25 ℃ and the humidity is required to be below 40%.
And roasting the PVP/aluminum acetylacetonate/metal mesh obtained by electrospinning at 750 ℃ for 270min in a muffle furnace, wherein the heating rate is 2.8 ℃/min, and the PVP and the aluminum acetylacetonate are decomposed in the heating process to obtain the aluminum oxide/metal mesh. And fixing the non-woven fabric with the gram weight of 60g on the metal mesh surface of the alumina/metal mesh material, and packaging to form the complete alumina/metal mesh/non-woven fabric composite adsorption mesh.
PM2.5 adsorption Performance test:
the experimental test sample was cut into a circular filter membrane with a diameter of 90 ± 2mm, and placed on the test table shown in fig. 8, with a flow rate of 85L/min, and the experimental results showed that the removal rate of PM2.5 by the alumina/metal mesh/nonwoven composite adsorption mesh is shown in the following table.
Example 3:
a. preparing a Ti/Al molar ratio of 10 by adopting an electrostatic spinning method: 1, alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorbing material:
first, an electrospinning precursor solution was prepared. 1g of PVP powder and 4.5mL of ethanol are mixed, stirred overnight to obtain a uniform and transparent solution, 4.6mL of acetone, 0.27g 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 to obtain a yellow and transparent precursor solution.
Secondly, under the conditions that the voltage is 15kV-20kV, the distance between the metal needle head and the metal net is 12.5cm, and the flow rate is 0.5mL/h, the grounded metal net with the aperture of 3mm and the thickness of 0.5mm is used as a receiver for collecting fibers, and the spinning environment temperature is required to be 25 ℃ and the humidity is required to be below 40%.
And roasting the PVP/aluminum acetylacetonate/titanium dioxide/metal mesh obtained by electrospinning in a muffle furnace at 750 ℃ for 270min, wherein the heating rate is 2.8 ℃/min, and the PVP and the aluminum acetylacetonate are decomposed in the heating process to obtain the aluminum oxide/titanium dioxide/metal mesh. And fixing the non-woven fabric with the gram weight of 60g on the metal mesh surface of the alumina/titanium dioxide/metal mesh material, and packaging to form the complete alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorption mesh.
PM2.5 adsorption Performance test:
the experimental test sample is cut into a circular filter membrane with the diameter of 90 +/-2 mm, the circular filter membrane is placed on a detection table shown in figure 8, the set flow rate is 85L/min, and the experimental result shows that the removal rate of the alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorption net to PM2.5 is shown in the following table.
Example 4:
a. preparing a Ti/Al molar ratio of 5:1, alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorbing material:
first, an electrospinning precursor solution was prepared. 1g of PVP powder and 4.5mL of ethanol are mixed, stirred overnight to obtain a uniform and transparent solution, 4.6mL of acetone, 0.53g 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 to obtain a yellow and transparent precursor solution.
Secondly, under the conditions that the voltage is 15kV-20kV, the distance between the metal needle head and the metal net is 12.5cm, and the flow rate is 0.5mL/h, the grounded metal net with the aperture of 3mm and the thickness of 0.5mm is used as a receiver for collecting fibers, and the spinning environment temperature is required to be 25 ℃ and the humidity is required to be below 40%. And roasting the PVP/aluminum acetylacetonate/titanium dioxide/metal mesh obtained by electrospinning in a muffle furnace at 750 ℃ for 270min, wherein the heating rate is 2.8 ℃/min, and the PVP and the aluminum acetylacetonate are decomposed in the heating process to obtain the aluminum oxide/titanium dioxide/metal mesh. And fixing the non-woven fabric with the gram weight of 60g on the metal mesh surface of the alumina/titanium dioxide/metal mesh material, and packaging to form the complete alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorption mesh.
PM2.5 adsorption Performance test:
the experimental test sample is cut into a circular filter membrane with the diameter of 90 +/-2 mm, the circular filter membrane is placed on a detection table shown in fig. 8, the set flow rate is 85L/min, and the experimental result shows that the removal rate of the alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorption material to PM2.5 is shown in the following table.
Claims (1)
1. The application of the ceramic nanofiber-based composite purification membrane in adsorbing PM2.5 in gas is characterized in that the ceramic nanofiber-based composite purification membrane is prepared by the following steps: preparing a Ti/Al molar ratio of 5:1, alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorbing material: firstly, preparing electrostatic spinning precursor solution; mixing 1g of PVP powder with 4.5mL of ethanol, stirring overnight to obtain a uniform and transparent solution, sequentially adding 4.6mL of acetone, 0.53g of aluminum acetylacetonate, 3mL of acetic acid and 2.5mL of isopropyl titanate into the solution, and stirring at room temperature to completely dissolve the mixture to obtain a yellow and transparent precursor solution; secondly, under the conditions that the voltage is 15kV-20kV, the distance between a metal needle head and a metal net is 12.5cm, and the flow rate is 0.5mL/h, a grounded metal net with the aperture of 3mm and the thickness of 0.5mm is used as a receiver for collecting fibers, and the spinning environment temperature is required to be 25 ℃ and the humidity is required to be below 40%; roasting the PVP/aluminum acetylacetonate/titanium dioxide/metal mesh obtained by electrospinning in a muffle furnace at 750 ℃ for 270min, wherein the heating rate is 2.8 ℃/min, and the PVP and the aluminum acetylacetonate are decomposed in the heating process to obtain an aluminum oxide/titanium dioxide/metal mesh; and fixing the non-woven fabric with the gram weight of 60g on the metal mesh surface of the alumina/titanium dioxide/metal mesh material, and packaging to form the complete alumina/titanium dioxide/metal mesh/non-woven fabric composite adsorption mesh.
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| CN110038451A (en) * | 2019-04-23 | 2019-07-23 | 东南大学 | Ceramic nanofibers base compound purifying film and its preparation method and application |
| CN110038452A (en) * | 2019-04-23 | 2019-07-23 | 东南大学 | Load the ceramic nanofibers base compound purifying film and its preparation method and application of silver |
| CN110193337A (en) * | 2019-06-19 | 2019-09-03 | 上海第二工业大学 | A kind of photochemical catalyst fiber felt fixed-bed type Photoreactor and preparation method thereof |
| CN113117434B (en) * | 2019-12-30 | 2022-11-22 | 西安工程大学 | Preparation method of flexible reticular vein structure ceramic nanofiber ultrahigh-temperature filtering membrane |
| CN113005642B (en) * | 2021-03-01 | 2022-11-22 | 南京工业大学 | Preparation method of nano spider web fiber membrane |
| CN115287823B (en) * | 2022-02-14 | 2024-04-30 | 青岛大学 | Preparation method and application of long-acting charged and pore-size graded nano-film |
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| CN101213330A (en) * | 2005-05-31 | 2008-07-02 | 帝人株式会社 | Ceramic fibre and manufacturing method thereof |
| CN106278368A (en) * | 2016-08-15 | 2017-01-04 | 北京大学深圳研究生院 | A kind of composite molecular sieve film and its preparation method and application |
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| CN101982581B (en) * | 2010-11-18 | 2013-01-16 | 东华大学 | Method for preparing aluminum oxide nanofiber by electrostatic spinning |
| CN103451850B (en) * | 2013-08-16 | 2015-12-09 | 西安理工大学 | The preparation method of lotus positive electroceramics micro nanometer fiber film |
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| CN106278368A (en) * | 2016-08-15 | 2017-01-04 | 北京大学深圳研究生院 | A kind of composite molecular sieve film and its preparation method and application |
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