CN115582028A - Preparation method of ultrahigh-efficiency air filtering material - Google Patents
Preparation method of ultrahigh-efficiency air filtering material Download PDFInfo
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Classifications
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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
-
- 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
-
- 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
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nonwoven Fabrics (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses a preparation method of an ultrahigh-efficiency air filtering material, which comprises the following steps: preparing a polymer solution, which comprises a functional polymer stock solution and a reinforced structure high molecular material stock solution; the prepared solution is placed in a set number of electrostatic spinning units according to a set sequence, and is sprayed on the surface of a receiving substrate through an electrostatic spinning process to form micro-nano fibers, so that a micro-nano fiber air filtering membrane with a composite structure is obtained; and (3) preparing the micro-nano fiber air filtering membrane with the composite structure into the filtering membrane coiled material through a subsequent process. According to the invention, by compounding the stock solution and alternately spraying, the material is endowed with higher mechanical strength on the premise of realizing ultrahigh efficiency, prolonging the service life and increasing the dust holding capacity. The filtering efficiency of the filtering material can reach 99.9999 percent, the wind resistance is below 300Pa, the dust capacity is higher than that of a competitive product filtering material with the same size, and the service life is prolonged by 30 to 50 percent.
Description
Technical Field
The invention relates to a preparation method of an air filtering material with ultrahigh efficiency, high dust holding capacity, long service life and high strength, in particular to a method for industrially preparing a nanofiber membrane by using functional polymer materials with different structures as raw materials and adopting a multi-module combined electrostatic spinning method.
Background
The fields of semiconductors, electronic devices, medicines, foods, cosmetics and the like have high requirements on production and processing environments, and the environmental cleanliness directly influences the yield and quality of terminal products, so that the filtration performance of a high-efficiency filtration material (HEPA) and an ultra-high efficiency filtration material (ULPA) and related components of a matched ultra-clean production workshop directly determines the cleanliness grade of an ultra-clean room. Especially, the production environment with the cleanliness grade exceeding one hundred grades puts higher requirements on the filter material.
Currently, most of the filter materials used for HEPA or ULPA are glass fibers or Polytetrafluoroethylene (PTFE) and other chemical fiber materials. The glass fiber has excellent performances of high filtering efficiency, stable chemical resistance, high temperature resistance and the like, but is easy to brittle fracture, so that the glass fiber is dispersed in a clean space, and on one hand, the reject ratio of a terminal product is increased; on the other hand, the fine glass fiber is absorbed into human body, is difficult to metabolize and brings health hidden trouble to production workers. In addition, the filter made of glass fiber has the big defect of high material resistance, so that the structural resistance of the filter is high and the energy consumption is high. Although the PTFE material overcomes the defects that glass fiber is easy to break and absorb and causes defective rate, the PTFE material is unstable in uniformity and high in filtration resistance due to the self-processing process. Under the current global environment of promoting energy consumption reduction, the filter material with ultrahigh efficiency and relatively low resistance is developed, so that the energy consumption is greatly reduced, and the service life is prolonged, which is very important for the production field of the matched ultra-clean workshop.
Compared with the ultra-high efficiency filter material, the composite nanofiber material with high strength, high filtration efficiency and low resistance has obvious competitive advantage. A method for preparing a high-efficiency low-resistance filtering membrane by preparing a composite nanofiber membrane [ Ding Bin and the like. ZL201410108986.4, 2014-03-24] can be used for preparing a filter membrane with the filtering effect of 95% -99.97% and the resistance of less than 300Pa. However, the filtering material prepared by the method has low efficiency, and the defects of low material strength, easy fragmentation, relatively high resistance and low productivity cannot be overcome, so that the method becomes a main bottleneck for application in various fields.
Based on the advantages and defects of the air filtering material prepared by the electrostatic spinning method, a method for preparing the composite nanofiber material capable of being industrially produced, and endowing the nanomaterial with higher filtering efficiency, lower filtering resistance, longer service life and good air permeability is required to be developed.
Disclosure of Invention
The invention aims to provide a composite micro-nanofiber material with high dust holding capacity, long service life, ultrahigh filtering efficiency and relatively low resistance and a preparation method thereof.
The micro-nanofiber air filtering membrane with the composite structure can be applied to the fields of semiconductors, electronic devices, medicines and the like which have high requirements on processing environments, and can be used as a filter material of a clean room. The micro-nanofiber air filtering membrane with the composite structure is formed by alternately spraying the functional additive material and the micro-nanofiber material on the surfaces of the polyester framework material and the composite melt-blown material by means of a method combining electrostatic spinning and electrostatic spraying, so that the bonding strength between the composite materials is enhanced, and the materials are endowed with the performance characteristics of ultrahigh filtering efficiency, relatively low filtering resistance, high dust holding capacity, long service life and the like. Compared with the glass fiber and PTFE fiber materials commonly used in the field, the composite micro-nano fiber material has the filtering efficiency as high as 99.9999 percent, and the corresponding resistance can be controlled below 300Pa which is far lower than the air filtering resistance of the glass fiber and PTFE fiber materials of the same grade.
In order to solve the technical problem, the invention aims to realize that:
the invention relates to a preparation method of an ultrahigh-efficiency air filtering material, which comprises the following specific steps:
(1) Preparing a polymer solution, wherein the polymer solution comprises a functional polymer stock solution for realizing ultrahigh filtration efficiency performance and a reinforced structure high polymer material stock solution for realizing material strength improvement;
(2) Placing the prepared functional polymer stock solution and the prepared reinforced structure high polymer material stock solution into a set number of electrostatic spinning units according to a set sequence, taking non-woven fabrics as receiving base materials, and spraying the non-woven fabrics on the surface of the receiving base materials through an electrostatic spinning process to form micro-nano fibers so as to obtain a micro-nano fiber air filtering membrane with a composite structure;
(3) And (3) drying, rolling and cutting the obtained micro-nanofiber air filtering membrane with the composite structure by using an oven to obtain a filtering membrane coil required by the ultra-efficient air filter.
Preferably, the filtering efficiency of the prepared micro-nanofiber air filtering membrane is 99.999-99.9999% under the test conditions of NaCl aerosol and flow rate of 5.33cm/S, and the filtering resistance is not higher than 300Pa.
Preferably, in the step (1), the functional polymer used in the preparation of the stock solution of the functional polymer comprises one or more of the following high molecular polymers: polyacrylonitrile, polyurethane, polyamide, polystyrene, polyether, polyvinylidene fluoride, nylon 6, polyvinyl alcohol and polylactic acid.
Preferably, in the step (1), the solvent used in the preparation process of the stock solution of the functional polymer is one or more of the following solvents: formic acid, ethanol, methanol, acetic acid, N-dimethylformamide, N-dimethylacetamide, trifluoroacetic acid, tetrahydrofuran, acetone, dichloromethane, trichloromethane and hexafluoroisopropanol.
Preferably, in the step (1), in the preparation process of the stock solution of the functional polymer, the mass ratio of the functional polymer to the solvent is 1:5-1:3, and the final polymer solution concentration is 5-25%.
Preferably, in the step (1), the reinforced structure polymer material used in the preparation process of the reinforced structure polymer material stock solution includes one or more of the following polymer materials: phenolic resin, epoxy resin, polyurethane, urea resin, polymethacrylate, polyacrylate, polyimide and alkyd resin.
Preferably, in the step (1), a curing agent is further added in the preparation process of the reinforced structure polymer material stock solution, and the mass ratio of the reinforced structure polymer material stock solution to the curing agent is 6:1-3:1.
preferably, in the step (2), in the processing process of the micro-nanofiber air filtering membrane, the specific process parameters are as follows: spinning voltage is 40-70kV, receiving distance is 15-25cm, and speed is 0.5-10 m/min.
Preferably, in step (2), there are 10 electrospinning units, the ratio of the reinforced structural polymer material stock solution to the functional polymer stock solution can be dynamically designed according to the required material strength, and the spinning ratio of the reinforced structural polymer material stock solution to the functional polymer stock solution is 1:20-1:1.
preferably, in the step (2), the receiving substrate is one or more of a melt-blown non-woven fabric, a hot air non-woven fabric, a spun-bonded non-woven fabric and a polyester filament non-woven fabric.
According to the invention, by combining the spinning process, the ultrahigh-efficiency micro-nanofiber air filtering membrane is obtained, and meanwhile, the strength of the material is ensured, so that the defect of low material strength inherent in the electrostatic spinning process is fundamentally solved. According to different requirements on the speed of the spinning, the proportion of the concentration of the reinforced polymer solution participating in spinning is adjusted, so that on one hand, the super-high-efficiency micro-nano fiber air filtering membrane can be obtained, and the filtering efficiency can reach 99.999% -99.9999%; on the other hand, the bonding strength between the fiber membrane and the base material is also ensured. In addition, the multi-module combined spinning mode ensures that the productivity is basically ensured, and the single-day productivity can realize more than 1 ten thousand square meters.
The composite air filtering material prepared by the invention can realize batch production, has good uniformity and repeatability and simple process, and has the advantages of reduced resistance by 30-50%, higher safety and the like compared with the existing competitive glass fiber; compared with the existing competitive product PTFE filter material, the PTFE filter material has the advantages of 10-20% reduction of resistance, lower cost and higher uniformity, and has optimistic prospect in the application field of ultra-efficient filter materials.
Compared with the prior art, the invention has the advantages that:
(1) Compared with the product prepared by the existing electrostatic spinning process technology, the bonding strength of the ultra-efficient composite micro-nano fiber film obtained by the invention and the base material is obviously enhanced, so that the final material is endowed with higher strength and wear resistance, and the service life of the product is prolonged.
(2) The invention selects the non-woven material with thinner fiber diameter as the receiving material, can realize the air filtration efficiency up to 99.9999 percent, and simultaneously control the resistance below 300Pa, generally about 200-250Pa, which is a performance index difficult to realize by related competitive products at present.
(3) The combined multi-module electrostatic spinning process adopted by the invention enables the introduction of functional materials to be very simple and convenient, and the functional polymer materials can be processed into the nanofibers and simultaneously exert the advantage of strong bonding property, thereby improving the overall strength of the materials, which is not reported in related documents at home and abroad.
(4) The processing method adopted by the invention is simple and easy to implement, ensures high productivity while ensuring excellent performance, and provides a precondition for realizing batch production.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
Dissolving 10Kg of Polyacrylonitrile (PAN) in 90Kg of N, N-dimethylformamide, and stirring for 20 hours until the Polyacrylonitrile (PAN) is completely dissolved to obtain polyacrylonitrile/N, N-dimethylformamide spinning solution; and then mixing the epoxy resin and the curing agent in a proportion of 3:1, and uniformly mixing. Spinning by adopting multi-module electrostatic spinning equipment, wherein a first module, namely a first electrostatic spinning unit, is loaded with mixed solution of epoxy resin and a curing agent, the rest nine modules are loaded with polyacrylonitrile/N, N-dimethylformamide spinning solution, a receiving base material is melt-blown non-woven fabric, and spinning parameters are as follows: the voltage is 45KV, the receiving distance is 18cm, and the vehicle speed is 2m/min; and cutting and winding the polyacrylonitrile nano-fiber air filter material by a drying box body of spinning equipment to finally obtain the polyacrylonitrile nano-fiber air filter material with higher bonding strength and different widths.
Example 2
Dissolving 15Kg of polyacrylonitrile in 85Kg of N, N-dimethylformamide, and stirring for 20 hours until the polyacrylonitrile is completely dissolved to obtain a polyacrylonitrile/N, N-dimethylformamide spinning solution; and then mixing the epoxy resin and the curing agent in a ratio of 3:1, and uniformly mixing. Spinning by adopting multi-module electrostatic spinning equipment, wherein the first module and the second module are loaded with mixed solution of epoxy resin and a curing agent, the other eight modules are loaded with polyacrylonitrile/N, N-dimethylformamide spinning solution, and the receiving base material is polyester filament non-woven fabric; the spinning parameters are as follows: the voltage is 45KV, the receiving distance is 18cm, and the vehicle speed is 1.5m/min; the polyacrylonitrile nano-fiber air filter material with higher bonding strength and different widths is finally obtained after slitting and rolling through a drying box body of spinning equipment.
Example 3
Dissolving 10Kg of polyurethane (TPU) in 90Kg of N, N-dimethylacetamide, and stirring for 15 hours until the TPU is completely dissolved to obtain polyurethane/N, N-dimethylacetamide spinning solution; and then the polyurethane and the curing agent are mixed according to the proportion of 4:1, and uniformly mixing. Spinning by adopting multi-module electrostatic spinning equipment, wherein the first module is loaded with an epoxy resin solution, the rest nine modules are loaded with a polyurethane and curing agent mixed solution, and a receiving base material is a hot air non-woven fabric; the spinning parameters are as follows: the voltage is 45KV, the receiving distance is 18cm, and the vehicle speed is 1m/min; the polyurethane nanofiber air filter material with high bonding strength and different widths is finally obtained after being cut and rolled by a drying box body of spinning equipment.
Example 4
8Kg of polyamide 6 (PA 6) is dissolved in 92Kg of mixed solvent of formic acid and acetic acid, and is stirred for 15 hours until the polyamide 6 (PA 6) is completely dissolved, thus obtaining polyamide/formic acid spinning solution; and then the polyurethane and the curing agent are mixed according to the proportion of 4:1, and uniformly mixing. Spinning by adopting multi-module electrostatic spinning equipment, wherein the first module is loaded with an epoxy resin solution, the rest nine modules are loaded with a polyamide solution, and a receiving substrate is melt-blown non-woven fabric; the spinning parameters are as follows: the voltage is 45KV, the receiving distance is 18cm, and the vehicle speed is 2m/min; after being cut and rolled by a drying box body of spinning equipment, the polyamide nanofiber air filter material with high bonding strength and different widths is finally obtained.
Example 5
Dissolving 5Kg of polylactic acid (PLA) in 95Kg of mixed solvent of chloroform and N, N-dimethylformamide, and stirring for 20 hours until the PLA/chloroform and N, N-dimethylformamide are completely dissolved to obtain a polylactic acid/chloroform and N, N-dimethylformamide spinning solution; and then mixing the epoxy resin and the curing agent in a ratio of 3:1, and uniformly mixing. Spinning by adopting multi-module electrostatic spinning equipment, wherein the first module is loaded with a mixed solution of epoxy resin and a curing agent, the other nine modules are loaded with a polyacrylonitrile spinning solution, and a receiving base material is polylactic acid hot air non-woven fabric; the spinning parameters are as follows: the voltage is 45KV, the receiving distance is 18cm, and the vehicle speed is 2m/min; the polylactic acid nano fiber air filtering material with higher bonding strength and different widths is finally obtained after being cut and rolled by a drying box body of spinning equipment.
The air filter materials prepared in examples 1 to 5 were compared with the filter materials of the comparative examples in terms of filter performance. The grammage of the nonwoven fabric used as the substrate in examples 1 to 5 was the same.
TABLE 1 Filter Performance index for ultra high efficiency filter materials
| Sample numbering | Filter material | Filtration efficiency @5.33cm/S | Resistance (Pa) | Dust holding capacity (g) |
| Comparative example | Glass fiber | 99.99％ | 350 | 379.6 |
| Example 1 | PAN nanofiberFilm | 99.999％ | 229 | 785.3 |
| Example 2 | PAN nanofiber membrane | 99.9999％ | 267 | 815.6 |
| Example 3 | TPU nanofiber membrane | 99.995％ | 182 | 601.8 |
| Example 4 | PA6 nanofiber membrane | 99.995％ | 164 | 790.2 |
| Example 5 | PLA nanofiber membranes | 99.99％ | 191 | 721.8 |
The air filter materials prepared in examples 1 to 5 were compared in physical properties with those of the filter materials of comparative examples 1 and 2. The widths were the same when tested for transverse strength and longitudinal strength.
TABLE 2 composite nanofiber membrane bond strength
| Sample numbering | Processing technology | Transverse strength/N | Longitudinal strength/N |
| Comparative example 1 | Common electrospun membrane | 19.2 | 48 |
| Comparative example 2 | Glass fiber filter material | 59.3 | 118.5 |
| Example 1 | Combined Process as described in example 1 | 87.3 | 243.2 |
| Example 2 | Combined Process as described in example 2 | 88.3 | 234.9 |
| Example 3 | Combined Process as described in example 3 | 73.4 | 286.6 |
| Example 4 | Combined Process as described in example 4 | 65 | 252.1 |
| Example 5 | Combined Process as described in example 5 | 62 | 240 |
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. A preparation method of an ultra-high efficiency air filtering material comprises the following specific steps:
(1) Preparing a polymer solution, wherein the polymer solution comprises a functional polymer stock solution for realizing ultrahigh filtration efficiency performance and a reinforced structure high polymer material stock solution for realizing material strength improvement;
(2) Placing the prepared functional polymer stock solution and the prepared reinforced structure high polymer material stock solution into a set number of electrostatic spinning units according to a set sequence, taking non-woven fabrics as receiving base materials, and spraying the non-woven fabrics on the surface of the receiving base materials through an electrostatic spinning process to form micro-nano fibers so as to obtain a micro-nano fiber air filtering membrane with a composite structure;
(3) And (3) drying, rolling and cutting the obtained micro-nanofiber air filtering membrane with the composite structure by using an oven to obtain a filtering membrane coil required by the ultra-efficient air filter.
2. The preparation method of the ultra-high efficiency air filtration material of claim 1, wherein the filtration efficiency of the prepared micro-nanofiber air filtration membrane is 99.999% -99.9999% and the filtration resistance is not higher than 300Pa under the test condition of NaCl aerosol and the flow rate of 5.33 cm/s.
3. The method for preparing an ultra-high efficiency air filtration material according to claim 1, wherein in the step (1), the functional polymer used in the preparation of the stock solution of the functional polymer comprises one or more of the following high molecular polymers: polyacrylonitrile, polyurethane, polyamide, polystyrene, polyether, polyvinylidene fluoride, nylon 6, polyvinyl alcohol and polylactic acid.
4. The method for preparing an ultra-high efficiency air filtration material according to claim 1, wherein in the step (1), the solvent selected in the preparation process of the stock solution of the functional polymer is one or more of the following solvents: formic acid, ethanol, methanol, acetic acid, N-dimethylformamide, N-dimethylacetamide, trifluoroacetic acid, tetrahydrofuran, acetone, dichloromethane, trichloromethane and hexafluoroisopropanol.
5. The method for preparing an ultra-high efficiency air filtration material according to claim 1, wherein in the step (1), in the functional polymer stock solution preparation process, the mass ratio of the functional polymer to the solvent is 1:5-1:3, and the final concentration of the polymer solution is 5-25%.
6. The method for preparing an ultra-high efficiency air filtration material according to claim 1, wherein in the step (1), the reinforced structure polymer material used in the preparation of the reinforced structure polymer material stock solution comprises one or more of the following polymer materials: phenolic resin, epoxy resin, polyurethane, urea resin, polymethacrylate, polyacrylate, polyimide and alkyd resin.
7. The method for preparing an ultra-high efficiency air filtration material according to claim 1, wherein in the step (1), a curing agent is further added in the preparation process of the reinforced structure polymer material stock solution, and the mass ratio of the reinforced structure polymer material stock solution to the curing agent is 6:1-3:1.
8. the preparation method of the ultra-high efficiency air filtering material according to claim 1, wherein in the step (2), the specific process parameters in the micro-nanofiber air filtering membrane processing process are as follows: spinning voltage is 40-70kV, receiving distance is 15-25cm, and speed is 0.5-10 m/min.
9. The method for preparing ultra-high efficiency air filtration material according to claim 1, wherein in step (2), there are 10 electrospinning units, the ratio of the stock solution of the structural enhancement polymer material to the stock solution of the functional polymer can be dynamically designed according to the required material strength, and the spinning ratio of the stock solution of the structural enhancement polymer material to the stock solution of the functional polymer is 1:20-1:1.
10. the method for preparing an ultra-high efficiency air filtration material according to claim 1, wherein in the step (2), the receiving substrate is one or more of melt-blown nonwoven fabric, hot air nonwoven fabric, spun-bonded nonwoven fabric and polyester filament nonwoven fabric.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103520999A (en) * | 2012-07-06 | 2014-01-22 | 北京服装学院 | Antibacterial composite nanometer fiber high-efficiency air filtering material and preparation method thereof |
| CN111359452A (en) * | 2020-03-18 | 2020-07-03 | 北京化工大学 | Structure-enhanced hydrotalcite-immobilized composite fiber membrane, and preparation method and application thereof |
| CN112755651A (en) * | 2020-12-31 | 2021-05-07 | 东华大学 | Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103520999A (en) * | 2012-07-06 | 2014-01-22 | 北京服装学院 | Antibacterial composite nanometer fiber high-efficiency air filtering material and preparation method thereof |
| CN111359452A (en) * | 2020-03-18 | 2020-07-03 | 北京化工大学 | Structure-enhanced hydrotalcite-immobilized composite fiber membrane, and preparation method and application thereof |
| CN112755651A (en) * | 2020-12-31 | 2021-05-07 | 东华大学 | Multi-combination functional electrostatic spinning submicron fiber air filter material and preparation thereof |
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