CN108176256B - Preparation method of high-temperature-resistant composite nanofiber filtering membrane - Google Patents
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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
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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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
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- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- 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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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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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
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
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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
- B01D71/06—Organic material
- B01D71/26—Polyalkenes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
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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
- B01D71/06—Organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2323/00—Details relating to membrane preparation
- B01D2323/39—Electrospinning
Abstract
A preparation method of a high-temperature-resistant composite nanofiber filtering membrane relates to the field of air filtration. The method comprises the following steps: 1) preparing a high molecular polymer solution; 2) preparing a high-molecular polymer fiber base material; 3) preparation of Al2O3A fiber precursor solution; 4) al preparation by electrostatic spinning device2O3A fibrous layer; 5) preparing a SiC fiber precursor solution; 6) preparing a SiC fiber layer; 7) repeating the step 3) and the step 4) to prepare upper Al layer2O3A high temperature resistant fiber layer; 8) repeating the step 1) and the step 2) to prepare an upper-layer high-molecular polymer substrate; 9) preparing the high-temperature resistant composite nanofiber filtering membrane. The mechanical property of the filtering membrane is improved through the composite three-dimensional forming of the organic high-temperature-resistant nanofiber membrane and the inorganic ceramic nanofiber membrane, the service life is prolonged, the high-temperature-resistant property of the fiber membrane is effectively enhanced, and the application of the electrostatic spinning technology in the field of high-temperature flue gas purification and filtration is promoted.
Description
Technical Field
The invention relates to the field of air filtration, in particular to a preparation method of a high-temperature-resistant composite nanofiber filtering membrane.
Background
With the rapid development of industrial technology, a large amount of high-temperature flue gas is generated in the heavy industrial fields of materials, metallurgy, chemical industry, electric power and the like, a large amount of micro particles suspended in air are formed, the main source of air pollution is provided, and the life quality of people is seriously influenced. The development of an air filtering membrane suitable for high-temperature flue gas is the key point of research in the field of air pollution treatment at present.
Electrostatic spinning is a simple micro-nano structure jet manufacturing technology, and becomes a mainstream nanofiber manufacturing technology due to the advantages of simple process, convenience in operation, good material compatibility and the like. The electrostatic spinning nanofiber material has wide sources, is easy to carry out surface modification, has good permeability, small pore diameter and good pore connectivity, is easier to combine with organic gas and submicron particles, and plays a good role in adsorption and separation. At present, electrostatic spinning nanofiber filtering materials have been successfully applied to the field of efficient air purification, and experiments of a plurality of research institutions and research teams prove that nanofibers have good purification effects on organic gases and micro-nano dust (Liu C, Hsu P C, Lee H W, et al.
As a new material, inorganic ceramic fibers such as Al2O3Fibers, SiC fibers and the like are widely applied to the field of high-temperature flue gas purification. Compared with the traditional filter material, the fiber filter material has the advantages of large specific surface, small aperture, high porosity and better interception effect on small-particle-size pollutant particles. The inorganic ceramic has good mechanical strength, excellent chemical stability and good high temperature resistance (Liuwei, Trueyuanshan, Jinjiang, preparation and performance of ceramic fiber tube for high temperature flue gas purification [ J)]The journal of environmental engineering, 2012,6(9): 3248-. At present, the preparation method of inorganic ceramic fiber mainly comprises a solvent thermal synthesis method, a chemical vapor deposition method, an extrusion method, an ultrafine powder sintering method, a sol-gel method and the like, but the methods have the problems of complex equipment, high cost and the like, and the prepared fiber has the problems of large diameter, easy mutual adhesion, poor uniformity and the like, so the application of the prepared fiber in the filtration of high-temperature smoke tiny particles is limited.
The inorganic ceramic nanofiber membrane prepared by the electrostatic spinning technology becomes a novel means of a novel high-temperature-resistant air filtering membrane, but the single inorganic ceramic fiber membrane has the defect of poor mechanical performance of membrane formation, and the raw material cost of the material with good high-temperature resistance, such as SiC fiber, is higher.
Disclosure of Invention
The invention aims to provide a preparation method of a high-temperature-resistant composite nanofiber filtering membrane, which can improve the mechanical property of the filtering membrane, prolong the service life and enhance the high-temperature resistance of the fiber membrane.
The invention comprises the following steps:
1) preparing a high molecular polymer solution;
in step 1), the specific method for preparing the high molecular polymer solution may be: dissolving high-temperature-resistant high-molecular polymer powder in an organic solvent, and stirring to obtain a high-molecular polymer solution; the high polymer powder includes but is not limited to PVDF, PPS, PES, PTFE and other high temperature resistant high polymer.
2) Preparing a high-molecular polymer fiber base material;
in step 2), an electrostatic spinning device can be adopted for preparing the high molecular polymer fiber base material, and the specific method comprises the following steps: a high-voltage electric field is formed between the spinning spray head and the collecting plate by using a high-voltage power supply, the anode of the high-voltage power supply is connected with the spinning spray head, and the cathode of the high-voltage power supply is connected with the collecting plate and is grounded; injecting a high molecular polymer solution into a spinning nozzle, after the liquid supply speed is stable, turning on a high-voltage power supply to generate a stretching effect on the polymer solution to form jet flow injection, volatilizing a solvent and solidifying the jet flow to obtain a high molecular polymer nanofiber membrane on a collecting plate, wherein the high molecular polymer nanofiber membrane is used as a base material of the composite filtering membrane;
the spinning nozzle in the electrostatic spinning device can adopt a single nozzle, multiple nozzles and a needle-free nozzle, and the needle-free nozzle can adopt needle-free nozzles such as a line electrode, a roller electrode, a screw electrode and the like; the high-voltage power supply can be a direct-current power supply or an alternating-current power supply; the distance between the spray head and the collecting plate is 10-30 cm adjustable;
the method for preparing the high molecular polymer fiber substrate can be a fiber preparation method such as solution electrospinning or melt electrospinning.
3) Preparation of Al2O3A fiber precursor solution;
in step 3), the preparation of Al2O3The specific method of the fiber precursor solution may be: dissolving aluminum salt in acetone to obtain precursor solution of aluminum, adding ethanol solution containing PVP, and preparing Al from the mixed solution2O3Precursor solution of nano-fiberLiquid; the aluminum salts include, but are not limited to, aluminum acetylacetonate, aluminum acetate, aluminum nitrate, and the like;
4) al preparation by electrostatic spinning device2O3A fibrous layer;
in the step 4), Al is prepared by adopting an electrostatic spinning device2O3The specific method of the fiber layer may be: preparing a nanofiber membrane by the electrostatic spinning method in the step 2), carrying out heat treatment for 1-6 h at 1000-1500 ℃, decomposing a polymer, and carrying out high-temperature oxidation to form Al2O3A fibrous layer;
5) preparing a SiC fiber precursor solution;
in step 5), the specific method for preparing the SiC fiber precursor solution may be: dissolving Polycarbosilane (PCS), polynitrosilane or tetraethoxysilane in toluene to form hydrophobic colloidal particles, dissolving PVP in water, mixing the two solutions to prepare high-temperature-resistant Al2O3Precursor solution of nano fiber;
6) preparing a SiC fiber layer;
in step 6), the SiC fiber layer may be prepared by using an electrostatic spinning device, and the specific method for preparing the SiC fiber layer may be: preparing a nanofiber membrane by the electrostatic spinning method in the step 2), oxidizing for 6 hours at 190 ℃ for non-melting treatment, then performing heat treatment for 1-6 hours at 1000-1500 ℃, decomposing by PCS (process control system) to obtain SiC nanofibers, and obtaining a super-high temperature resistant SiC nanofiber layer;
7) repeating the step 3) and the step 4) to prepare upper Al layer2O3A high temperature resistant fiber layer;
8) repeating the step 1) and the step 2) to prepare an upper-layer high-molecular polymer substrate;
9) preparing the high-temperature resistant composite nanofiber filtering membrane.
In step 9), the specific method for preparing the high-temperature resistant composite nanofiber filtering membrane may be: standing the nanofiber membrane obtained in the steps 2), 4), 6), 7) and 8) at room temperature for 24 hours, and then carrying out hot pressing treatment at 100-150 ℃ to improve the composite strength, so as to obtain a high-temperature-resistant composite nanofiber filtering membrane; the thickness of each layer of the composite nanofiber filtering membrane can be adjusted according to the actual high temperature resistance requirement.
The compound mode of the filtering membrane can adopt hot-pressing compounding after 5 layers of fiber membranes are respectively formed into membranes, and can also adopt Al2O3Firstly carrying out composite heat treatment on the/SiC precursor fiber to obtain a high-temperature resistant fiber layer, and then carrying out hot-pressing composite on the high-temperature resistant fiber layer and the organic polymer substrate; the composite film may be PVDF-Al2O3-SiC-Al2O3PVDF structure, also PVDF-SiC-Al2O3-SiC-PVDF structure, and the thickness of the different fiber layers can be adjusted according to the high temperature resistance requirement.
The invention provides a high molecular polymer based material, Al2O3Preparation method of high temperature resistant composite nanofiber filtering membrane of high temperature resistant fiber layer and SiC super high temperature resistant fiber layer, wherein Al2O3As a main material of the high-temperature-resistant filtering membrane, the introduction of the SiC super high-temperature-resistant fiber layer can further improve the high-temperature-resistant effect of the filtering membrane, and the application field of the electrostatic spinning nanofiber filtering membrane can be expanded to the fields of high-temperature flue gas purification and the like.
According to the invention, the mechanical property of the filtering membrane is improved through the composite three-dimensional forming of the organic high-temperature-resistant nanofiber membrane and the inorganic ceramic nanofiber membrane, the service life is prolonged, the high-temperature-resistant property of the fiber membrane is effectively enhanced, and the application of the electrostatic spinning technology in the field of high-temperature flue gas purification and filtration is promoted.
Drawings
FIG. 1 is PVDF-Al2O3-SiC-Al2O3Schematic representation of PVDF composite nanofiber membranes.
FIG. 2 is Al2O3-SiC-Al2O3Schematic diagram of the composite high-temperature-resistant nanofiber layer.
FIG. 3 is PVDF-SiC-Al2O3Schematic diagram of-SiC-PVDF composite nanofiber membrane.
FIG. 4 shows SiC-Al2O3Schematic diagram of-SiC composite high-temperature-resistant nanofiber layer.
FIG. 5 is an SEM image of a PVDF high molecular polymer substrate prepared by electrostatic spinning.
FIG. 6 is electrospinningPrepared Al2O3SEM image of the high temperature resistant fiber layer.
FIG. 7 is an SEM image of a SiC ultra-high temperature resistant fiber layer prepared by electrostatic spinning.
FIG. 1 is a PVDF high molecular polymer substrate; al (2)2O3A high temperature resistant fiber layer; 3, SiC ultrahigh temperature resistant fiber layer; al (1)2O3A high temperature resistant fiber layer; 5, PVDF high molecular polymer substrate; 6, PVDF high molecular polymer substrate; 7, SiC ultrahigh temperature resistant fiber layer; al (8)2O3A high temperature resistant fiber layer; 9, SiC ultrahigh temperature resistant fiber layer; a PVDF high molecular polymer substrate.
Detailed Description
The present invention will be further explained with reference to the drawings and examples.
Example 1
1. Preparing a PVDF high molecular polymer nanofiber membrane 1 as a base material of the composite filtering membrane as shown in FIG. 5;
2. mixing Al2O3The precursor fiber is subjected to heat treatment for 1-6 h at 1000-1500 ℃, the polymer is decomposed, and Al is formed by high-temperature oxidation2O3A fibrous layer 2, as shown in fig. 6;
3. oxidizing the SiC precursor fiber at 190 ℃ for 6h for non-melting treatment, then performing heat treatment at 1000-1500 ℃ for 1-6 h, decomposing PCS to obtain SiC nanofiber and obtain a super high temperature resistant SiC nanofiber layer 3, as shown in figure 7;
4. mixing Al2O3The precursor fiber is subjected to heat treatment for 1-6 h at 1000-1500 ℃, the polymer is decomposed, and Al is formed by high-temperature oxidation2O3 A fiber layer 4;
5. preparing a PVDF high molecular polymer nanofiber membrane 5 as a base material of the composite filtering membrane;
6. and (3) standing the 5 layers of nanofiber membranes obtained in the previous step at room temperature for 24 hours, and then carrying out hot pressing treatment at 100-150 ℃ to improve the composite strength, so as to obtain the composite nanofiber membrane, as shown in figure 1.
Example 2
1. Preparing a PVDF high molecular polymer nanofiber membrane 1 as a base material of the composite filtering membrane;
2. oxidizing the SiC precursor fiber at 190 ℃ for 6h for non-melting treatment;
3. mixing Al2O3Precursor fiber 2, SiC precursor fiber 3, Al2O3Standing the precursor fiber 4 at room temperature for 24 hours, performing hot pressing treatment at 100-150 ℃, performing heat treatment at 1000-1500 ℃ for 1-6 hours, and performing polymer decomposition, high-temperature oxidation and other processes to obtain the composite high-temperature-resistant Al2O3a/SiC fiber layer, as shown in FIG. 2;
4. preparing a PVDF high molecular polymer nanofiber membrane 5 as a base material of the composite filtering membrane;
5. and (3) standing the 3 layers of nanofiber membranes obtained in the previous step at room temperature for 24 hours, and then carrying out hot pressing treatment at 100-150 ℃ to improve the composite strength, so as to obtain the composite nanofiber membrane, as shown in figure 1.
Example 3
1. Preparing a PVDF high molecular polymer nanofiber membrane 6 as a base material of the composite filtering membrane;
2. oxidizing the SiC precursor fiber at 190 ℃ for 6h for non-melting treatment, then performing heat treatment at 1000-1500 ℃ for 1-6 h, decomposing PCS to obtain SiC nanofiber and obtain a super high temperature resistant SiC nanofiber layer 7;
3. mixing Al2O3The precursor fiber is subjected to heat treatment for 1-6 h at 1000-1500 ℃, the polymer is decomposed, and Al is formed by high-temperature oxidation2O3 A fiber layer 8;
4. oxidizing the SiC precursor fiber at 190 ℃ for 6h for non-melting treatment, then performing heat treatment at 1000-1500 ℃ for 1-6 h, decomposing PCS to obtain SiC nanofiber and obtaining the ultra-high temperature resistant SiC nanofiber layer 9;
5. preparing a PVDF high molecular polymer nanofiber membrane 10 as a base material of the composite filtering membrane;
6. and (3) standing the 5 layers of nanofiber membranes obtained in the previous step at room temperature for 24 hours, and then carrying out hot pressing treatment at 100-150 ℃ to improve the composite strength to obtain the composite nanofiber membrane, wherein the composite nanofiber membrane is shown in figure 3.
Example 4
1. Preparing a PVDF high molecular polymer nanofiber membrane 6 as a base material of the composite filtering membrane;
2. oxidizing the SiC precursor fiber at 190 ℃ for 6h for non-melting treatment;
3.SiC precursor fiber 7, Al2O3Standing the precursor fiber 8 and the SiC precursor fiber 9 at room temperature for 24 hours, performing hot pressing treatment at 100-150 ℃, performing heat treatment at 1000-1500 ℃ for 1-6 hours, and performing polymer decomposition, high-temperature oxidation and other processes to obtain the composite high-temperature resistant SiC/Al2O3Fibrous layers, as shown in fig. 4;
4. preparing a PVDF high molecular polymer nanofiber membrane 10 as a base material of the composite filtering membrane;
5. and (3) standing the 3 layers of nanofiber membranes obtained in the previous step at room temperature for 24 hours, and then carrying out hot pressing treatment at 100-150 ℃ to improve the composite strength, so as to obtain the composite nanofiber membrane, as shown in fig. 3.
Claims (2)
1. A preparation method of a high-temperature-resistant composite nanofiber filtering membrane is characterized by comprising the following steps:
1) the preparation method of the high molecular polymer solution comprises the following steps: dissolving high-temperature-resistant high-molecular polymer powder in an organic solvent, and stirring to obtain a high-molecular polymer solution; the high-molecular polymer powder comprises PVDF, PPS, PES and PTFE high-temperature resistant high-molecular polymers;
2) preparing a high molecular polymer fiber base material, wherein an electrostatic spinning device is adopted for preparing the high molecular polymer fiber base material, and the specific method comprises the following steps: a high-voltage electric field is formed between the spinning spray head and the collecting plate by using a high-voltage power supply, the anode of the high-voltage power supply is connected with the spinning spray head, and the cathode of the high-voltage power supply is connected with the collecting plate and is grounded; injecting a high molecular polymer solution into a spinning nozzle, after the liquid supply speed is stable, turning on a high-voltage power supply to generate a stretching effect on the polymer solution to form jet flow injection, volatilizing a solvent and solidifying the jet flow to obtain a high molecular polymer nanofiber membrane on a collecting plate, wherein the high molecular polymer nanofiber membrane is used as a base material of the composite filtering membrane; the spinning nozzle in the electrostatic spinning device adopts a single nozzle, multiple nozzles and a needle-free nozzle, and the needle-free nozzle adopts a line electrode, a roller electrode and a screw electrode; the high-voltage power supply is a direct-current power supply or an alternating-current power supply; the distance between the spinning nozzle and the collecting plate is 10-30 cm adjustable;
3) preparation of Al2O3The fiber precursor solution comprises the following specific steps: dissolving aluminum salt in acetone to obtain precursor solution of aluminum, adding ethanol solution containing PVP, and preparing Al from the mixed solution2O3Precursor solution of nano fiber; the aluminum salt comprises aluminum acetylacetonate, aluminum acetate and aluminum nitrate;
4) al preparation by electrostatic spinning device2O3The fiber layer comprises the following specific methods: preparing a nanofiber membrane by the electrostatic spinning method in the step 2), carrying out heat treatment for 1-6 h at 1000-1500 ℃, decomposing a polymer, and carrying out high-temperature oxidation to form Al2O3A fibrous layer;
5) the preparation method of the SiC fiber precursor solution comprises the following steps: dissolving polycarbosilane in toluene to form hydrophobic colloidal particles, dissolving PVP in water, mixing the two solutions to prepare high-temperature-resistant Al2O3Precursor solution of nano fiber;
6) preparing a SiC fiber layer by using an electrostatic spinning device, wherein the specific method for preparing the SiC fiber layer comprises the following steps: preparing a nanofiber membrane by the electrostatic spinning method in the step 2), oxidizing for 6 hours at 190 ℃ for non-melting treatment, then performing heat treatment for 1-6 hours at 1000-1500 ℃, decomposing polycarbosilane to obtain SiC nanofibers, and obtaining a super high temperature resistant SiC nanofiber layer;
7) repeating the step 3) and the step 4) to prepare upper Al layer2O3A high temperature resistant fiber layer;
8) repeating the step 1) and the step 2) to prepare an upper-layer high-molecular polymer substrate;
9) the preparation method of the high-temperature resistant composite nanofiber filtering membrane comprises the following steps: standing the nanofiber membrane obtained in the steps 2), 4), 6), 7) and 8) at room temperature for 24 hours, and then carrying out hot pressing treatment at 100-150 ℃ to improve the composite strength, so as to obtain a high-temperature-resistant composite nanofiber filtering membrane; the thickness of each layer of the composite nanofiber filtering membrane can be adjusted according to the actual high temperature resistance requirement.
2. The method for preparing a high temperature resistant composite nanofiber filter membrane according to claim 1, wherein in step 2), the method for preparing the high molecular polymer fiber substrate is a method for preparing a solution electrospinning or melt electrospinning fiber.
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| 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 |
| CN111905573B (en) * | 2020-07-16 | 2022-04-26 | 北京纳视达科技有限公司 | Carbon nano composite filter membrane and preparation method and protection device thereof |
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| CN114050053B (en) * | 2021-11-16 | 2023-05-23 | 莫纶(珠海)新材料科技有限公司 | Preparation method of flexible ceramic film capacitor |
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| WO2004112183A1 (en) * | 2003-06-17 | 2004-12-23 | Samshin Creation Co., Ltd. | A complex membrane for electrochemical device, manufacturing method and electrochemical device having the same |
| CN1739959A (en) * | 2005-07-20 | 2006-03-01 | 同济大学 | A kind of interlayer composite material and preparation method thereof |
| CN106541683A (en) * | 2016-11-01 | 2017-03-29 | 东莞巨微新材料科技有限公司 | A kind of preparation method of the multilayered structure nano-fiber composite film filtered for particulate in air |
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| WO2004112183A1 (en) * | 2003-06-17 | 2004-12-23 | Samshin Creation Co., Ltd. | A complex membrane for electrochemical device, manufacturing method and electrochemical device having the same |
| CN1739959A (en) * | 2005-07-20 | 2006-03-01 | 同济大学 | A kind of interlayer composite material and preparation method thereof |
| CN106541683A (en) * | 2016-11-01 | 2017-03-29 | 东莞巨微新材料科技有限公司 | A kind of preparation method of the multilayered structure nano-fiber composite film filtered for particulate in air |
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