CN111249927A - Meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane and preparation method thereof - Google Patents

Meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane and preparation method thereof Download PDF

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CN111249927A
CN111249927A CN202010111735.7A CN202010111735A CN111249927A CN 111249927 A CN111249927 A CN 111249927A CN 202010111735 A CN202010111735 A CN 202010111735A CN 111249927 A CN111249927 A CN 111249927A
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meta
aramid
polysulfonamide
solution
silicon dioxide
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辛斌杰
田旭
周曦
高伟洪
刘岩
郑元生
许晋豪
于佳
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Shanghai University of Engineering Science
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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
    • B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
    • 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
    • B01D46/0001—Making filtering elements
    • 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
    • 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
    • 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
    • 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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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention provides a meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane and a preparation method thereof, wherein the preparation method comprises the following steps: diluting the meta-aramid solution by using an N, N-dimethylacetamide/lithium chloride mixed solvent system to obtain a diluted meta-aramid solution, and performing ultrasonic defoaming treatment; mixing the meta-aramid solution and the polysulfonamide solution to obtain a meta-aramid/polysulfonamide mixed solution, and performing ultrasonic defoaming treatment; adding silicon dioxide particles into the meta-aramid/polysulfonamide mixed solution to obtain a mixed solution, and using an electrostatic spinning technology process to obtain the meta-aramid/polysulfonamide/silicon dioxide composite air filtering membrane; the preparation method disclosed by the invention is simple in steps, strong in operability, relatively low in production cost and relatively high in safety; the filter membrane has good hydrolytic resistance and ultraviolet resistance, and has comprehensive filtering effect of high filtering precision and low filtering resistance.

Description

Meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane and preparation method thereof
Technical Field
The invention belongs to the technical field of high-temperature industrial waste gas filtering membranes, and particularly relates to a meta-aramid/polysulfonamide/silicon dioxide composite air filtering membrane and a preparation method thereof.
Background
With the increasing pace of industrial development, the large amount of industrial exhaust gas emissions in the fields of steel, cement, metallurgy, waste incineration, automobiles, and the like are considered to be a major cause of global air pollution. Among Particulate Matter (PM) of different particle sizes, particles having a particle size of 2.5 μm or less, called PM2.5, are commonly present in the above-mentioned industrial exhaust gas and seriously impair the healthy survival of animals and plants. The traditional high-temperature filter bag is mainly made of non-woven fabric, the fiber size of the traditional high-temperature filter bag is in a micron-sized range, the traditional high-temperature filter bag has a good filtering effect on micron-sized particles with large sizes, and the interception efficiency on PM2.5 micro particles is not high. Electrostatic spinning is a high-efficiency and universal nano and sub-micron fiber preparation technology, and is widely concerned by scholars at home and abroad. The electrostatic spinning nano-fiber has the characteristics of high specific surface area, small pore diameter, high porosity, uniform pore diameter distribution and the like, is favorable for improving the surface interception efficiency and the filtration precision of micro-nano particles, and has obvious advantages in the aspect of air filtration application.
Aramid 1313(MPIA) is an organic synthetic high polymer with high strength, high modulus, high temperature resistance and chemical corrosion resistance, polysulfone amide (PSA) is an aromatic polyamide organic high temperature resistant synthetic material independently developed in China,has good thermal stability and flame retardant property, so the two can be used for preparing materials for high-temperature industrial waste gas filtering membranes. However, because the industrial high-temperature gas has high moisture content, and the high-temperature flue gas is condensed and condensed to cause failure of the filter bag, water vapor is adsorbed on the surface of the filter material and is adhered with dust to paste the bag, so that the filter bag is hydrolyzed, damaged or blocked to cause failure. Especially for synthetic fibers produced by polycondensation, such as MPIA and PSA, the hydrolysis resistance is poor, molecular chain breakage is easy to occur under high temperature and high humidity, and both MPIA and PSA contain polar group amide groups, and when water molecules enter the fibers, the hydrogen bond structure can be damaged. In order to improve the characteristic of poor hydrolysis resistance of the filter membrane, the filter membrane needs to be subjected to water repellent treatment. Second, MPIA and PSA are sensitive to uv light, which can cause a loss of strength if exposed to outdoor sunlight for a long period of time. Nano silicon dioxide (SiO)2) The material is a non-toxic, tasteless and pollution-free environment-friendly material, has excellent high temperature resistance and ultraviolet resistance, and can improve the strength and the ageing resistance of other materials. After the nano silicon dioxide is subjected to hydrophobic modification, the acting force with water can be obviously improved, and the hydrophobic performance of the nano silicon dioxide composite material can be improved.
Disclosure of Invention
In order to overcome the above defects of the prior art, the primary object of the present invention is to provide a meta-aramid (MPIA)/Polysulfonamide (PSA)/Silica (SiO) based electrospinning technology2) And (3) compounding an air filtering membrane. MPIA has many advantages such as high strength and modulus, alkali resistance, high temperature resistance, light weight, etc. The PSA has excellent high temperature resistance, thermal stability and flame retardant properties. However, the two materials are easy to break molecular chains under high temperature and high humidity, and have poor hydrolysis resistance and ultraviolet resistance, so that the defects of the above performances are overcome by adding hydrophobic nano silica particles into MPIA/PSA.
The second purpose of the invention is to provide a meta-aramid/polysulfonamide/silicon dioxide composite air filtration membrane.
In order to achieve the above purpose, the solution of the invention is as follows:
a preparation method of a meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane comprises the following steps:
(1) diluting a meta-aramid fiber (MPIA) solution by using an N, N-dimethylacetamide/lithium chloride (DMAc/LiCl) mixed solvent system, stirring to obtain the diluted meta-aramid fiber (MPIA) solution, and performing ultrasonic defoaming treatment;
(2) stirring and mixing the defoamed meta-aramid fiber (MPIA) solution and polysulfone amide (PSA) solution to obtain a meta-aramid fiber/polysulfone amide (MPIA/PSA) mixed solution, and performing ultrasonic defoaming treatment;
(3) adding silicon dioxide (SiO) into the defoamed meta-aramid/polysulfonamide (MPIA/PSA) mixed solution2) Granulating, and stirring to obtain meta-aramid/polysulfonamide/silicon dioxide (MPIA/PSA/SiO)2) Mixing the solution, and performing ultrasonic defoaming treatment;
(4) and defoaming the m-aramid fiber/polysulfonamide/silicon dioxide (MPIA/PSA/SiO)2) The mixed solution is subjected to an electrostatic spinning process to obtain meta-aramid/polysulfonamide/silicon dioxide (MPIA/PSA/SiO)2) And (3) compounding an air filtering membrane.
Preferably, in the step (1), the mass ratio of the N, N-dimethylacetamide to the lithium chloride in the N, N-dimethylacetamide/lithium chloride mixed solvent system is 0.03:1-0.08:1, and the stirring time of the N, N-dimethylacetamide/lithium chloride mixed solvent system is 1-2 h.
Preferably, in the step (1), the concentration of the meta-aramid solution is 20-25 wt%; stirring for 2-3 h; the time for ultrasonic defoaming is 3-4 h.
Preferably, in the step (1), the concentration of the diluted meta-aramid solution is 6-16 wt%.
Preferably, in the step (2), the concentration of the polysulfonamide solution is 6-16 wt%, wherein the concentration of the diluted meta-aramid solution is the same as that of the polysulfonamide solution (i.e. the solid content of the MPIA solution is the same as that of the PSA solution when the MPIA solution and the PSA solution are mixed).
Preferably, in the step (2), the mass ratio of the meta-aramid to the polysulfonamide in the meta-aramid/polysulfonamide mixed solution is 0.4:1-3.0: 1.
Preferably, in the step (2), the stirring time is 3-4 h; the time for ultrasonic defoaming is 3-4 h.
Preferably, in step (3), the amount of silica added is 0.5 to 1.5 wt%. The particle size of the silicon dioxide is 5-40 nm.
Preferably, in the step (3), the stirring time is 3-4 h; the time for ultrasonic defoaming is 3-4 h.
Preferably, in the step (4), the voltage of electrostatic spinning in the electrostatic spinning process is 25-30kV, the solution advancing speed is 0.003-0.008mm/s, the spinning distance is 15 +/-1 cm, and the rotating speed of a receiver is 35-40 r/min.
Preferably, in the step (4), the ambient temperature of the electrostatic spinning is 25-30 ℃ and the ambient humidity is 35-40%.
The meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane is prepared by the preparation method.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the preparation method of the composite air filtering membrane has the advantages of simple steps, strong operability, relatively low production cost and high safety.
Secondly, after the meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane is boiled in a water bath kettle at 90 ℃ for 144 hours, the loss of mechanical strength is smaller than that of the meta-aramid/polysulfonamide composite filter membrane, and the hydrolysis resistance is good (silicon dioxide is adopted); an anti-ultraviolet transmission analyzer is used for carrying out solid ultraviolet reflection on the filter membrane, and the anti-ultraviolet performance of the filter membrane is better than that of a meta-aramid fiber/polysulfonamide composite filter membrane; the filtering material testing platform is used for testing the filtering performance of the composite filtering membrane, the filtering membrane has higher filtering efficiency on Polystyrene (PSL) aerosol particles with the particle size of 0.1 mu m, 0.2 mu m and 0.3 mu m generated in the filtering material testing platform, and compared with a meta-aramid/polysulfonamide composite filtering membrane, the ternary composite membrane has lower filtering resistance, and achieves the comprehensive filtering effect of high filtering efficiency and low filtering resistance in the true sense.
Drawings
FIG. 1 shows MPIA/PSA/SiO of the present invention2Schematic view of the micro-morphology of the composite air filtering membrane.
FIG. 2 shows MPIA/PSA/SiO in accordance with the present invention2Dynamic water of composite air filtering membraneContact angle is shown schematically.
FIG. 3 shows MPIA/PSA/SiO in accordance with the present invention2The ultraviolet resistance spectrum of the composite air filtering membrane is shown schematically (the abscissa wavelet is the Wavelength, and the ordinate Transmittance is the Transmittance).
FIG. 4 shows MPIA/PSA/SiO in accordance with the present invention2Filtration Efficiency of the composite air Filtration membrane (a) is shown schematically (Particle Size on abscissa and Filtration Efficiency on ordinate).
FIG. 5 shows MPIA/PSA/SiO in accordance with the present invention2The Filtration Resistance of the composite air Filtration membrane (b) is shown schematically (Filtration Resistance is shown by ordinate).
Detailed Description
The present invention will be further described with reference to comparative examples and examples.
Comparative example 1:
(1) preparation of MPIA solution:
firstly weighing a certain mass of MPIA solution with the concentration of 20 wt% for later use, calculating the mass of a DMAc dilution solvent according to a solution dilution law, then weighing the mass of LiCl particles according to the mass ratio of DMAc/LiCl of 0.05, and then mixing the LiCl particles and the DMAc/LiCl mixed solvent system to obtain the DMAc/LiCl mixed solvent system. And mechanically stirring the mixed solvent system, adding the mixed solvent system into a weighed 20 wt% MPIA solution after stirring for 1h, stirring for 3h, and ultrasonically defoaming for 4h to finally obtain a 12 wt% MPIA solution.
(2) Preparing a PSA solution:
directly weighing a certain amount of PSA spinning solution with the mass concentration of 12 wt% for mechanical stirring, wherein the stirring time is 3h, and ultrasonically defoaming for 4h for later use.
(3) Preparation of MPIA/PSA (mass ratio 3/7) solution:
mixing the MPIA solution in the step (1) and the PSA solution in the step (2) according to the mass ratio of 3/7 ≈ 0.43, mechanically stirring for 3h, and ultrasonically defoaming for 4h for later use.
(4) Preparing electrostatic spinning:
the MPIA/PSA mixed solution was injected into a 5mL syringe. The electrostatic spinning process parameters are set as follows: the receiving distance is set to be 15cm, the solution advancing speed is 0.005mm/s, the electrostatic field voltage value is 25kV, the rotating speed of a receiver roller is 40r/min, the ambient temperature is 25 ℃, the ambient humidity is 35%, and the spinning time is 3 h. Finally, the MPIA/PSA nano composite air filter membrane (PPAS-0 for short) with the mass ratio of 3/7 is prepared.
(5) The MPIA/PSA nano composite air filter membrane (PPAS-0 for short) has the following properties:
after the dynamic water contact angle of the filter membrane is over 11s, the contact angle disappears, and the hydrophilic performance is presented (figure 2); the filter membrane has the highest ultraviolet transmittance in the UVB wave band range (275-320nm) and the UVA wave band range (320-420nm), and the anti-ultraviolet performance is poor (figure 3). The filtration efficiency of the filter membrane on 0.1 μm, 0.2 μm and 0.3 μm PSL aerosol particles is 96.7%, 98.3% and 99.6% respectively (FIG. 4), the filtration resistance is high, and the value is 79Pa (FIG. 5); the retention rate of the breaking strength of the filter membrane after being baked and boiled in a water bath kettle at 90 ℃ for 144 hours is the lowest, and is only 56.278% (Table 1).
Comparative example 2:
the meta-aramid nonwoven filter cloth commonly used in the market is used for comparison test of filtering performance, the filtering efficiency of the filter cloth to PSL aerosol particles of 0.1 mu m, 0.2 mu m and 0.3 mu m is respectively 22.19 percent, 35.50 percent and 42.44 percent (figure 4), and the filter cloth can not meet the filtering requirement on PM 2.5.
Example 1:
(1)MPIA/PSA/SiO2(SiO2concentration of 0.5 wt.%) solution preparation:
MPIA/PSA (mass ratio 3/7) blend dope was prepared according to comparative example 1. Then hydrophobic nano SiO with the concentration of 0.5 wt% is added into the mixed spinning solution2And (3) granulating, mechanically stirring for 3 hours, and ultrasonically defoaming for 4 hours for later use.
(2) Preparing electrostatic spinning:
mixing the above MPIA/PSA/SiO2The mixed solution was injected into a 5mL syringe. The electrostatic spinning process parameters are set as follows: the receiving distance is set to be 15cm, the solution advancing speed is 0.005mm/s, the electrostatic field voltage value is 25kV, the rotating speed of a receiver roller is 40r/min, the ambient temperature is 25 ℃, the ambient humidity is 35%, and the spinning time is 3 h. Finally preparing to obtainTo MPIA/PSA/SiO2And a ternary composite air filtering membrane (PPAS-0.5 for short).
(3) The MPIA/PSA/SiO2The performance of the ternary composite air filter membrane is as follows:
the initial water contact angle of the filter membrane is 122.5 degrees, after 180s, the contact angle is reduced to 118 degrees, and the filter membrane can show good hydrophobic performance for a long time (figure 2); the ultraviolet transmittance of the filter membrane is better than that of PPAS-0 in the comparative example 1 in the UVB wave band range (275-320nm) and the UVA wave band range (320-420nm), and the anti-ultraviolet performance is improved (figure 3). The filtration efficiency of the filter membrane for 0.1 μm, 0.2 μm and 0.3 μm PSL aerosol particles was 96.64%, 97.62% and 99.60%, respectively (FIG. 4), and the filtration resistance was better than that of PPAS-0 in comparative example 1, and its value was 68.5Pa (FIG. 5); after the filter membrane is baked and boiled in a water bath kettle at 90 ℃ for 144 hours, the breaking strength retention rate of the filter membrane is improved, and the value is 82.591% (table 1).
Example 2:
(1)MPIA/PSA/SiO2(SiO2concentration 1.0 wt.%) solution preparation:
MPIA/PSA (mass ratio 3/7) blend dope was prepared according to comparative example 1. Then hydrophobic nano SiO with the concentration of 1.0 wt% is added into the mixed spinning solution2And (3) granulating, mechanically stirring for 3 hours, and ultrasonically defoaming for 4 hours for later use.
(2) Preparing electrostatic spinning:
mixing the above MPIA/PSA/SiO2The mixed solution was injected into a 5mL syringe. The electrostatic spinning process parameters are set as follows: the receiving distance is set to be 15cm, the solution advancing speed is 0.005mm/s, the electrostatic field voltage value is 25kV, the rotating speed of a receiver roller is 40r/min, the ambient temperature is 25 ℃, the ambient humidity is 35%, and the spinning time is 3 h. Finally MPIA/PSA/SiO is prepared2Ternary composite air filtering membrane (PPAS-1.0 for short).
(3) The MPIA/PSA/SiO2The performance of the ternary composite air filtering membrane is as follows:
the initial water contact angle of the filter membrane is 129.1 degrees, the contact angle is reduced to 120.4 degrees after 180 seconds, and good hydrophobic performance can be shown for a long time (figure 2); the ultraviolet transmittance of the filter membrane in UVB wave band range (275-320nm) and UVA wave band range (320-420nm) is better than that of the PPAS-0 membrane in comparative example 1 and the PPAS-0.5 membrane in the example, and the anti-ultraviolet performance is improved (figure 3). The filtration membrane had filtration efficiencies of 79.41%, 82.33%, and 94.74% for aerosol particles of 0.1 μm, 0.2 μm, and 0.3 μm PSL, respectively (FIG. 4), which were lower than the PPAS-0 membrane of comparative example 1 and the PPAS-0.5 membrane of the example, and had a lower filtration resistance of 49.5Pa (FIG. 5); after the filtration membrane is baked and boiled in a water bath kettle at 90 ℃ for 144 hours, the breaking strength retention rate of the filtration membrane is improved, and the value is 87.031% (Table 1), which is higher than the PPAS-0 membrane in comparative example 1 and the PPAS-0.5 membrane in example 1.
TABLE 1 MPIA/PSA/SiO2The breaking strength of the ternary composite air filtering membrane is changed along with the hydrolysis time (90℃)
Figure BDA0002390271210000051
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.

Claims (10)

1. A preparation method of a meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane is characterized by comprising the following steps: which comprises the following steps:
(1) diluting the meta-aramid solution by using an N, N-dimethylacetamide/lithium chloride mixed solvent system, stirring to obtain the diluted meta-aramid solution, and performing ultrasonic defoaming treatment;
(2) stirring and mixing the defoamed meta-aramid fiber solution and the polysulfonamide solution to obtain a meta-aramid fiber/polysulfonamide mixed solution, and performing ultrasonic defoaming treatment;
(3) adding silicon dioxide particles into the defoamed meta-aramid/polysulfonamide mixed solution, stirring to obtain the meta-aramid/polysulfonamide/silicon dioxide mixed solution, and performing ultrasonic defoaming treatment;
(4) and performing an electrostatic spinning process on the defoamed meta-aramid/polysulfonamide/silicon dioxide mixed solution to obtain the meta-aramid/polysulfonamide/silicon dioxide composite air filtering membrane.
2. The method of claim 1, wherein: in the step (1), the mass ratio of the N, N-dimethylacetamide to the lithium chloride in the N, N-dimethylacetamide/lithium chloride mixed solvent system is 0.03:1-0.08:1, and the stirring time of the N, N-dimethylacetamide/lithium chloride mixed solvent system is 1-2 h.
3. The method of claim 1, wherein: in the step (1), the concentration of the meta-aramid solution is 20-25 wt%; the stirring time is 2-3 h; the time for ultrasonic defoaming is 3-4 h.
4. The method of claim 1, wherein: in the step (1), the concentration of the diluted meta-aramid solution is 6-16 wt%.
5. The method of claim 1, wherein: in the step (2), the concentration of the polysulfone amide solution is 6-16 wt%.
6. The method of claim 1, wherein: in the step (2), the mass ratio of the meta-aramid to the polysulfonamide in the meta-aramid/polysulfonamide mixed solution is 0.4:1-3.0: 1.
7. The method of claim 1, wherein: in the step (2), the stirring time is 3-4 h; the time for ultrasonic defoaming is 3-4 h.
8. The method of claim 1, wherein: in the step (3), the adding amount of the silicon dioxide is 0.5-1.5 wt%, and the particle size of the silicon dioxide is 5-40 nm; and/or the presence of a gas in the gas,
in the step (3), the stirring time is 3-4 h; the time for ultrasonic defoaming is 3-4 h.
9. The method of claim 1, wherein: in the step (4), the electrostatic spinning voltage in the electrostatic spinning process is 25-30kV, the solution advancing speed is 0.003-0.008mm/s, the spinning distance is 15 +/-1 cm, and the rotating speed of a receiver is 35-40 r/min; and/or the presence of a gas in the gas,
in the step (4), the ambient temperature of the electrostatic spinning is 25-30 ℃, and the ambient humidity is 35-40%.
10. The meta-aramid/polysulfonamide/silicon dioxide composite air filtering membrane is characterized in that: obtained by the process according to any one of claims 1 to 9.
CN202010111735.7A 2020-02-24 2020-02-24 Meta-aramid/polysulfonamide/silicon dioxide composite air filter membrane and preparation method thereof Pending CN111249927A (en)

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Application publication date: 20200609