CN111593493A - Composite nanofiber membrane and preparation method and application thereof - Google Patents
Composite nanofiber membrane and preparation method and application thereof Download PDFInfo
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- CN111593493A CN111593493A CN202010464129.3A CN202010464129A CN111593493A CN 111593493 A CN111593493 A CN 111593493A CN 202010464129 A CN202010464129 A CN 202010464129A CN 111593493 A CN111593493 A CN 111593493A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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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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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/43—Acrylonitrile series
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Abstract
The invention discloses a preparation method of a composite nanofiber membrane, which comprises the following steps: 1) preparing a graphene oxide dispersion liquid; 2) adding nano silicon dioxide powder and polyacrylonitrile into graphene oxide dispersion liquid, and then adding metal ions to obtain an electrostatic spinning solution; 3) and (3) carrying out electrostatic spinning on the electrostatic spinning solution to obtain the composite nanofiber membrane. The roughness and the adsorption performance are improved by adding the graphene oxide nanoparticles, the filtering effect of the composite nanofiber membrane is further improved, the filtering resistance is reduced to 40.67Pa under the condition that the filtering efficiency is not influenced, and the reduction amplitude is large; by adding metal ions, the composite nanofiber membrane has excellent antibacterial property while filtering. The composite nanofiber membrane prepared by the method can be prepared into an efficient and low-resistance antibacterial air filtering material, is suitable for indoor air filtration and PM2.5 individual protection, and has good practical value.
Description
Technical Field
The invention belongs to the technical field of nanofiber membranes, and particularly relates to a composite nanofiber membrane and a preparation method and application thereof.
Background
In recent years, with the rapid development of industrial production and automobile industry, environmental pollution is increased, and especially inhalable particulate matters such as PM2.5 (commonly called haze and also called fine particulate matters) become one of the most concerned indexes at the present stage. PM2.5 can be suspended in the air for a long time, the higher the content concentration of the PM in the air, the more serious the air pollution is, the health of people is seriously threatened, and the requirements on the improvement of the living quality and the environmental purification are very urgent. Therefore, the development of a high-performance filter material is one of effective measures.
The air filter material mainly comprises a fiber filter material, a membrane filter material, a porous carbon material (such as activated carbon and the like), a porous ceramic material (such as zeolite and the like), a porous metal material and the like. The fiber air filtering material is developed rapidly by the advantages of simple process, low cost, easy structure control, excellent filtering effect and the like. The nanofiber air filter material rapidly draws attention of people due to the characteristics of small fiber diameter, large specific surface area, high porosity and the like. Recently, electrospun nanofibers have been favored by filter material researchers because of their advantages such as extremely large specific surface area, porosity, and extremely high filtration accuracy. The nano-scale fiber with the diameter of dozens or hundreds of nanometers can be obtained by utilizing the electrostatic spinning method, and is very suitable for being used as a filter material. The application of the electrostatic spinning nanofiber product to the air filtering technology provides a new way for manufacturing high-precision air filtering materials.
The filtering material prepared by the electrostatic spinning method at present has large filtering resistance and can not meet the market demand.
Disclosure of Invention
One of the purposes of the invention is to provide a preparation method of a composite nanofiber membrane, which increases graphene oxide for modification and reduces filtration resistance.
The second object of the present invention is to provide a composite nanofiber membrane having a lower filtration resistance and antibacterial properties.
The invention also aims to provide application of the composite nanofiber membrane.
The invention is realized by the following technical scheme:
a preparation method of a composite nanofiber membrane comprises the following steps:
1) preparing a graphene oxide dispersion liquid;
2) preparing an electrostatic spinning solution:
adding nano silicon dioxide powder and polyacrylonitrile into the graphene oxide dispersion liquid obtained in the step 1), heating and stirring, then adding metal ions, and uniformly mixing to obtain an electrostatic spinning solution;
wherein, calculated by mass percent, polyacrylonitrile: metal ions: electrostatic spinning solution (10-15): (0.5-4.5): 100, respectively;
and (3) graphene oxide: nano silicon dioxide powder: polyacrylonitrile (0.3-2): (2-6): 100, respectively;
3) and (3) performing electrostatic spinning on the electrostatic spinning solution obtained in the step 2) to obtain the composite nanofiber membrane.
Further, the step 1) is specifically as follows: placing graphene oxide in a solvent, and performing ultrasonic treatment to obtain a graphene oxide dispersion liquid;
further, in the step 1), the solvent is N, N-dimethylacetamide or dimethyl sulfoxide.
Further, in the step 1), the ultrasonic treatment time is 30-120 min.
Further, the metal ion is specifically any one or two of Ag, Cu, Fe and W elements.
Further, the electrospinning conditions were: the distance between the needle and the receiver is 15 cm-25 cm, and the spinning voltage is 12 KV-18 KV.
The invention also discloses a composite nanofiber membrane prepared by the preparation method of the composite nanofiber membrane.
Furthermore, the average diameter of the composite nanofiber membrane is 340-410 nm.
Furthermore, the filtration resistance of the composite nanofiber membrane is 36-48.5 Pa.
The invention also discloses application of the composite nanofiber membrane in preparation of an air filter material.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the preparation method of the composite nanofiber membrane, the graphene oxide and the silicon dioxide are loaded on the polyacrylonitrile by means of an electrostatic spinning technology, and the roughness and the adsorption performance of the fiber membrane are improved by adding the graphene oxide nanoparticles and the silicon dioxide; and after GO is added, the fiber diameter tends to decrease. In the diameter distribution table, the fiber diameter mode decreases from 490nm to 340 nm. Obviously, during the spinning process of GO, the lamellar orientation effect of GO can effectively promote the reduction of the fiber diameter so as to reduce the pore diameter of the nanofiber membrane and further improve the adsorption performance. In conclusion, the roughness and the adsorption performance of the fiber membrane are further improved by adding the graphene oxide nanoparticles, the filtering effect of the composite nanofiber membrane is further improved, the filtering resistance can be reduced to 40.67Pa under the condition of not influencing the filtering efficiency, and the reduction amplitude is large; the physical size of the electrospun fiber has high controllability, high specific surface area and developed porosity, which is beneficial to filtering particulate matters; by adding the metal ions, the composite nanofiber membrane has excellent antibacterial property while having filtering performance due to the antibacterial property of the metal ions.
Furthermore, graphene oxide sheet layers with different sizes are obtained under the ultrasonic stripping condition, so that the graphene oxide is better loaded on polyacrylonitrile.
The composite nanofiber membrane disclosed by the invention has lower filtration resistance, antibacterial property and excellent performance.
The composite nanofiber membrane disclosed by the invention can be prepared into an efficient and low-resistance antibacterial air filtering material, is suitable for indoor air filtration and PM2.5 individual protection, and has a very good practical value.
Drawings
FIG. 1 is a topographical view of graphene oxide lamellae obtained after ultrasonic exfoliation in accordance with the present invention;
FIG. 2 is a scanning electron microscope image of the composite nanofiber prepared by the present invention;
FIG. 3 is a graph showing the effect of the addition of graphene oxide on the filtration efficiency and filtration resistance of 500 nm NaCl particles according to the present invention;
FIG. 4 shows the effect of the addition amount of graphene oxide on the quality factor.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
1) Mixing 11 parts of Polyacrylonitrile (PAN) and 0.44 part of nano silicon dioxide (SiO)2) Directly dissolving the raw materials in N, N-dimethylacetamide (DMAc), adding 4.0 parts of W ions and Ag ions, and uniformly mixing to obtain an electrostatic spinning solution;
2) putting the spinning solution obtained in the step 1) into an electrostatic spinning machine, adjusting the distance between a needle head and a receiver to be 21cm and the spinning voltage to be 14KV, and collecting the spinning solution on a receiving roller wrapping non-woven fabric to obtain the composite nanofiber membrane, wherein the average diameter of the nanofiber membrane is 490nm as shown in table 1.
The addition amount of PAN is 11% of the electrostatic spinning solution, and the nano SiO2The addition amount of PAN is 4%, and the sum of the addition amounts of W ions and Ag ions is 4.0% of the electrostatic spinning solution.
The composite nanofiber membrane obtained in this example was measured for filtration efficiency and filtration resistance, and the filtration efficiency was 95.41% as shown in fig. 3, and the filtration resistance was 50Pa as shown in fig. 3.
Example 2
1) Placing 0.045 part of Graphene Oxide (GO) in N, N-dimethylacetamide (DMAc), and carrying out ultrasonic stripping treatment for 30min to obtain a GO dispersion liquid; the topography of the graphene oxide lamellae is shown in fig. 1.
2) Mixing 15 parts of Polyacrylonitrile (PAN) and 0.45 part of nano silicon dioxide (SiO)2) And (2) directly dissolving the components in the Graphene Oxide (GO) dispersion liquid obtained in the step 1), and then adding 0.4 part of Ag ions, and uniformly mixing to obtain an electrostatic spinning solution.
3) Placing the electrostatic spinning solution obtained in the step 2) in an electrostatic spinning machine, adjusting the distance between a needle head and a receiver to be 18cm and the spinning voltage to be 12KV, and collecting the solution on a receiving roller wrapping non-woven fabric to obtain the composite nanofiber membrane. As shown in table 1, the nanofiber membrane had an average diameter of 460 nm.
In this example, the addition amount of graphene oxide is 0.3% of Polyacrylonitrile (PAN), the addition amount of PAN is 15% of the electrospinning solution, and nano SiO is added2The addition amount of the Ag ion is 3% of PAN, and the addition amount of the Ag ion is 0.4% of the spinning solution.
The morphology, filtration efficiency and filtration resistance of the composite nanofiber membrane obtained in the example were measured, and a scanning electron microscope image thereof is shown in fig. 2, the filtration efficiency is 96.36% as shown in fig. 3, and the filtration resistance is 48.5Pa as shown in fig. 3.
Example 3
1) Placing 0.055 part of Graphene Oxide (GO) in N, N-dimethylacetamide (DMAc), and carrying out ultrasonic stripping treatment for 55min to obtain a GO dispersion liquid;
2) mixing 11 parts of Polyacrylonitrile (PAN) and 0.44 part of nano silicon dioxide (SiO)2) Directly dissolving the materials in the Graphene Oxide (GO) dispersion liquid obtained in the step 1), adding 3.7 parts of W ions and Ag ions, and uniformly mixing to obtain an electrostatic spinning solution;
3) putting the spinning solution obtained in the step 2) into an electrostatic spinning machine, adjusting the distance between a needle head and a receiver to be 20cm and the spinning voltage to be 16KV, and collecting the spinning solution on a receiving roller wrapping non-woven fabric to obtain a composite nanofiber membrane, wherein the average diameter of the nanofiber membrane is 410nm as shown in table 1.
The addition amount of the graphene oxide is 0.5 percent of Polyacrylonitrile (PAN); the addition amount of PAN is 11% of the electrostatic spinning solution, and the nano SiO2AddingThe amount of PAN was 4%, and the sum of the amounts of W ion and Ag ion added was 3.7% of the electrospinning solution.
The morphology, filtration efficiency and filtration resistance of the composite nanofiber membrane obtained in the example were measured, and a scanning electron microscope image thereof is shown in fig. 2, the filtration efficiency is 97.73% as shown in fig. 3, and the filtration resistance is 46.33Pa as shown in fig. 3.
Example 4
1) Placing 0.12 part of Graphene Oxide (GO) in dimethyl sulfoxide (DMSO), and carrying out ultrasonic stripping treatment for 70min to obtain a GO dispersion liquid;
2) mixing 12 parts of Polyacrylonitrile (PAN) and 0.24 part of nano silicon dioxide (SiO)2) Directly dissolving the components in Graphene Oxide (GO) dispersion liquid obtained in the step 1), adding 1.6 parts of Cu ions, and uniformly mixing to obtain an electrostatic spinning solution;
3) putting the spinning solution obtained in the step 2) into an electrostatic spinning machine, adjusting the distance between a needle head and a receiver to be 15cm and the spinning voltage to be 14KV, and collecting the spinning solution on a receiving roller wrapping non-woven fabric to obtain a composite nanofiber membrane, wherein the average diameter of the nanofiber membrane is 340nm as shown in table 1.
In this embodiment, the addition amount of graphene oxide is 1.0% of Polyacrylonitrile (PAN); PAN relative spinning solution is 12 wt.%, nano SiO2Relative PAN of 2 wt.%, Cu ions of 1.6 wt.% relative to the dope.
The morphology, filtration efficiency and filtration resistance of the composite nanofiber membrane obtained in the example were measured, and a scanning electron microscope image thereof is shown in fig. 2, the filtration efficiency is 98.15% as shown in fig. 3, and the filtration resistance is 40.67Pa as shown in fig. 3.
Example 5
1) Placing 0.15 part of Graphene Oxide (GO) in N, N-dimethylacetamide (DMAc), and carrying out ultrasonic stripping treatment for 100min to obtain a GO dispersion liquid;
2) mixing 10 parts of Polyacrylonitrile (PAN) and 0.5 part of nano silicon dioxide (SiO)2) Directly dissolving the materials in the Graphene Oxide (GO) dispersion liquid obtained in the step 1), adding 4.5 parts of Fe ions and Ag ions, and uniformly mixing to obtain an electrostatic spinning solution;
3) putting the spinning solution obtained in the step 2) into an electrostatic spinning machine, adjusting the distance between a needle head and a receiver to be 23cm and the spinning voltage to be 18KV, and collecting the spinning solution on a receiving roller wrapping non-woven fabric to obtain a composite nanofiber membrane, wherein the average diameter of the nanofiber membrane is 370nm as shown in table 1.
The concentration of graphene oxide dispersion was 1.5 wt.% relative to Polyacrylonitrile (PAN); PAN at 10 wt.% relative to the spinning solution, nano SiO2Relative PAN 5 wt.%, sum of Fe ions and Ag ions 4.5 wt.% relative to the dope.
The morphology, filtration efficiency and filtration resistance of the composite nanofiber membrane obtained in the example were measured, and a scanning electron microscope image thereof is shown in fig. 2, the filtration efficiency is 97.67% shown in fig. 3, and the filtration resistance is 41.5Pa shown in fig. 3.
Example 6
1) Placing 0.26 part of Graphene Oxide (GO) in dimethyl sulfoxide (DMSO), and carrying out ultrasonic stripping treatment for 120min to obtain a GO dispersion liquid;
2) 13 parts of Polyacrylonitrile (PAN) and 0.78 part of nano silicon dioxide (SiO)2) Directly dissolving the materials in the Graphene Oxide (GO) dispersion liquid obtained in the step 1), adding 2.8 parts of Fe ions, and uniformly mixing to obtain an electrostatic spinning solution;
3) putting the spinning solution obtained in the step 2) into an electrostatic spinning machine, adjusting the distance between a needle head and a receiver to be 25cm and the spinning voltage to be 17KV, and collecting the spinning solution on a receiving roller wrapping non-woven fabric to obtain a composite nanofiber membrane, wherein the average diameter of the nanofiber membrane is 390nm as shown in table 1.
The addition amount of the graphene oxide is 2.0% of Polyacrylonitrile (PAN); the adding amount of PAN is 13 percent of the mass of the spinning solution, and the nano SiO2The addition amount of the Fe ions is 6 percent of the PAN, and the addition amount of the Fe ions is 2.8 percent of the mass of the spinning solution.
The morphology, filtration efficiency and filtration resistance of the composite nanofiber membrane obtained in the example were measured, and a scanning electron microscope image thereof is shown in fig. 2, the filtration efficiency is 95.05% shown in fig. 3, and the filtration resistance is 36Pa shown in fig. 3.
TABLE 1 Effect of GO addition on average nanofiber membrane diameter
The experimental result shows that the roughness and the adsorption performance are improved by adding the graphene oxide nanoparticles, and the filtering effect of the composite nanofiber membrane is further improved, as shown in fig. 3, the filtering resistance is reduced from 50Pa, in which the graphene oxide is not added, to 36Pa, and the reduction amplitude is 38.89%.
The Quality Factor (QF) is an index reflecting the comprehensive filtering performance of the filtering material, and the larger the quality factor is, the better the comprehensive filtering performance of the filtering material is. The method is calculated according to a formula QF- (ln (1- η)/delta P) according to the test results of the filtering efficiency (η) and the filtering resistance (P).
Under the condition that the filtering efficiency is not influenced, the quality factor is comprehensively considered, after calculation, as shown in fig. 4, the change trend that the quality factor is increased firstly and then reduced is consistent with the filtering efficiency, and when the addition amount of the graphene oxide is 1%, the graphene oxide reaches 0.1, and is the maximum value in all test samples; at this time, the filtration efficiency was 98.15% as shown in FIG. 3, and the filtration resistance was 40.67Pa as shown in FIG. 3. By adding the metal ions, the composite nanofiber membrane has excellent antibacterial property while filtering due to the antibacterial property of the metal ions. The developed high-efficiency low-resistance antibacterial composite nanofiber air filtering material is suitable for indoor air filtration and PM2.5 individual protection, and has good practical value.
Claims (10)
1. A preparation method of a composite nanofiber membrane is characterized by comprising the following steps:
1) preparing a graphene oxide dispersion liquid;
2) preparing an electrostatic spinning solution:
adding nano silicon dioxide powder and polyacrylonitrile into the graphene oxide dispersion liquid obtained in the step 1), heating and stirring, then adding metal ions, and uniformly mixing to obtain an electrostatic spinning solution;
wherein, calculated by mass percent, polyacrylonitrile: metal ions: electrostatic spinning solution (10-15): (0.5-4.5): 100, respectively;
and (3) graphene oxide: nano silicon dioxide powder: polyacrylonitrile (0.3-2): (2-6): 100, respectively;
3) and (3) performing electrostatic spinning on the electrostatic spinning solution obtained in the step 2) to obtain the composite nanofiber membrane.
2. The method for preparing a composite nanofiber membrane as claimed in claim 1, wherein the step 1) is specifically: and placing the graphene oxide in a solvent, and performing ultrasonic treatment to obtain a graphene oxide dispersion liquid.
3. The method for preparing a composite nanofiber membrane as claimed in claim 2, wherein the solvent is N, N dimethylacetamide or dimethylsulfoxide.
4. The preparation method of the composite nanofiber membrane as claimed in claim 2, wherein in the step 1), the ultrasonic treatment time is 30-120 min.
5. The method of claim 1, wherein the metal ions are selected from the group consisting of Ag, Cu, Fe and W.
6. The method for preparing a composite nanofiber membrane as claimed in claim 1, wherein the electrospinning conditions are: the distance between the needle and the receiver is 15 cm-25 cm, and the spinning voltage is 12 KV-18 KV.
7. The composite nanofiber membrane prepared by the method for preparing a composite nanofiber membrane as claimed in any one of claims 1 to 6.
8. The composite nanofiber membrane according to claim 7, wherein the composite nanofiber membrane has an average diameter of 340 to 410 nm.
9. The composite nanofiber membrane as claimed in claim 7, wherein the filtration resistance of the composite nanofiber membrane is 36-48.5 Pa.
10. Use of the composite nanofiber membrane of claim 7 in the preparation of an air filter material.
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| CN114232122A (en) * | 2021-04-13 | 2022-03-25 | 海宁恒爱新材料有限公司 | Preparation method of polyacrylonitrile composite fiber membrane with antibacterial property |
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Application publication date: 20200828 |