CN106540490B - Composite nano filter material, preparation method and application thereof - Google Patents
Composite nano filter material, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a nano filter material, in particular to a composite nano filter material, a preparation method and application thereof, wherein the nano filter material comprises a substrate supporting layer (1), a nanofiber layer (2) and a protective layer (3); wherein the base support layer (1), the nanofiber layer (2) and the protective layer (3) are bonded by a high temperature resistant adhesive. The nano filter material has high filtering efficiency, the filtering efficiency on PM2.5 and other micro particles is more than 99.5 percent, and the filtering residual resistance can be controlled within 200 Pa; the nano filter material can be used for a long time at the temperature of 180 ℃ plus 240 ℃, can resist the temperature of 260 ℃ instantly, has stronger acid-base resistance and thermal oxidation resistance and long service life.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a nano filter material, and particularly relates to a composite nano filter material, and a preparation method and application thereof.
Background
At present, air pollution is very serious in China, large-area haze events frequently occur, normal life of people is seriously influenced, and the frequently-occurring haze weather also draws wide attention at home and abroad. The main component in the haze is PM2.5, and the fine particles have great harm to human bodies, can directly enter bronchus through the breath of people, and are absorbed by the human bodies to cause a plurality of diseases such as asthma, bronchitis, pneumoconiosis, cardiovascular diseases and the like. Meanwhile, PM2.5 contains a plurality of soluble particles, such as sulfate, nitrate, ammonium salt, organic acid salt and the like, which have strong water absorption, and the soluble particles can easily absorb moisture to form a dust-haze weather. Such weather severely reduces the visibility of the air, which can lead to traffic accidents, resulting in casualties and property damage.
According to the statistical data of the national ministry of environmental protection, 85.6% of the smoke (powder) emission of China is from the emission of industrial dust, and the emission of the industrial dust is mainly from the combustion of fossil energy, particularly the mass use of coal resources. According to statistics, the consumption of coal energy accounts for 70% of national energy consumption, and coal combustion generates a large amount of smoke, which is the main source of PM 2.5.
The bag type dust collector is a method for effectively removing dust particles in smoke (powder) gas, waste gas passes through a filtering device, gas-solid two phases in the waste gas are separated, and a key factor determining the dust removal efficiency of the bag type dust collector is a filtering material. The bag type dust collector is widely applied to the fields of electric power, steel, cement, non-ferrous metal smelting industry, waste incineration and the like, and different use environments and smoke components provide new requirements for filter materials of the dust collector.
The discharge temperature of the dust-containing flue gas in the coal-fired industry is about 200 ℃, but the fluctuation range of the discharge temperature of the dust-containing gas is large, so that the used filter material is required to be used for a long time in the environment of 180 ℃ and 240 ℃. Currently, the major high temperature resistant filter materials on the market are polyphenylene sulfide, polytetrafluoroethylene, aramid, polyimide, polysulfonamide, etc., wherein polytetrafluoroethylene is generally used as a film coating material. Compared with the developed countries in China, the mulching technology in China is still immature, and the problems of membrane cracking, falling and the like often occur, so that the popularization and the use of the material are seriously influenced. The filter material of the bag-type dust collector widely used in the market is mainly needle felt non-woven fabric, the fiber diameter of the filter material is more than 5 micrometers, the pore diameter is more than 20 micrometers commonly, the filter efficiency of small particle dust is low, and the current filter material cannot meet the filter requirement according to the latest published environmental quality standard GB3095-2012 of the state and the atmospheric pollutant emission standard GB13223-2011 of a thermal power plant.
CN 103505942A adopts the melt-blown process to prepare nanofiber filter material, has explained the advantage of nanofiber in the aspect of granule dust filtration in detail, but the material of preparing can't use for a long time under high temperature, and the material intensity is low, can't bear many times high pressure pulse and wash. CN 101795747A describes an air filter material containing nanofibers, which explains the feasibility of preparing high-efficiency and low-resistance filter materials in detail, but the filter material has poor protective effect of a nanofiber layer, cannot automatically clean ash, and has poor repeated and continuous usability. CN 102527158A describes a high temperature resistant filter material, which uses polyphenylene sulfide or polytetrafluoroethylene nanofiber, but the prepared material has larger pores and lower filtering efficiency on small particle dust.
According to the filtration theory, the filtration efficiency of the filtration material is improved along with the reduction of the fiber diameter, when the fiber diameter is reduced to the micro-nanometer level, the fiber non-woven material presents a high specific surface area and a micro-aperture structure which is tightly connected, the reduction of the fiber diameter enables the movement of dust on the fiber surface to be changed, and the filtration pressure drop is controlled within a small range while the filtration material provides high filtration efficiency. The appearance of the high-temperature-resistant micro-nanofiber filtering material provides a new thought and method for filtering and purifying high-temperature dust-containing smoke, so that high-efficiency and low-resistance filtering is realized.
Disclosure of Invention
Aiming at the defects and actual requirements of the prior art, the invention provides the composite air filtration nano filter material and the preparation method thereof, the preparation method has simple process, and the prepared product has high stability and high temperature resistance and can be used for smoke dust treatment in the industrial fields of coal-fired power plants, cement, waste incineration and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a composite nano filter material, which comprises a substrate supporting layer, a nanofiber layer and a protective layer;
wherein the base support layer, nanofiber layer and protective layer are bonded by a high temperature resistant adhesive. According to the invention, the substrate supporting layer and the nanofiber layer are bonded by adopting the high-temperature-resistant adhesive, the bonding effect is good, the substrate supporting layer and the protective layer are respectively arranged above and below the nanofiber layer, so that the nanofiber layer is not easy to damage, and the problems of poor mechanical property, easiness in falling and easiness in crushing of nanofibers are solved. The nanofiber layer can effectively improve the filtering efficiency of the filtering material on fine dust particles, the filtering efficiency of the most easily penetrated particles with the particle size of 0.3 mu m reaches more than 90%, and meanwhile, the filtering pressure drop is controlled in a small range, so that the preparation of the high-efficiency low-resistance filtering material is realized.
According to the invention, a high-temperature-resistant adhesive is adopted for bonding, and the adhesive penetrates through the nanofiber layer through hot-pressing solidification, so that the three layers of materials are effectively bonded together, the composite type nano filter material forms a sandwich structure with a stable structure, and the high-temperature-resistant nano filter material with stable mechanical property and excellent physical and chemical properties is obtained, so that the filter material can be guaranteed to be capable of withstanding long-time and high-frequency back flushing oscillation, the service life of the material is prolonged, and the nanofiber layer is well protected. The influence of the adhesive on the performance of the filter material after curing is extremely small, and the performances of the aperture, the porosity and the like of the substrate material are basically not influenced.
Preferably, the high temperature resistant adhesive is an adhesive resistant to a temperature of 180 ℃ or higher, and the temperature may be 180 ℃, 181 ℃, 182 ℃, 185 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 280 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃ or 700 ℃, for example.
Preferably, the high temperature resistant adhesive is selected from any one or a combination of at least two of epoxy resin type adhesive, silica gel adhesive, polyimide adhesive or maleimide adhesive, the selected adhesive is soft solid after curing, has excellent flexibility, can be repeatedly folded, and ensures industrial application of filter materials, and the epoxy resin type adhesive is more favorable for bonding between fibers, has high bonding strength, and has high flexibility after curing, and is preferably the epoxy resin type adhesive.
Preferably, the base support layer is a non-woven material resistant to 180 ℃ or higher, such as 180 ℃, 181 ℃, 182 ℃, 185 ℃, 190 ℃, 200 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 280 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃ or 700 ℃, preferably 180 ℃ or 240 ℃.
Preferably, the base support layer is selected from any one or a mixture of at least two of polyimide, polyphenylene sulfide, aramid, polysulfonamide, glass fiber, polytetrafluoroethylene or polyether ether ketone, preferably from any one or a mixture of at least two of aramid, polyimide or polyphenylene sulfide non-woven fabrics.
Preferably, the fiber diameter of the nonwoven material of the base support layer is 1-200 μm, for example 1, 2, 3, 4, 5, 8, 10, 20, 30, 50, 60, 80, 100, 120, 130, 150, 160, 180 or 200 μm, preferably 3-100 μm, more preferably 15-80 μm.
Preferably, the non-woven material of the base support layer has a fiber pore size of 10-100 μm, which may be, for example, 10 μm, 11 μm, 12 μm, 13 μm, 15 μm, 16 μm, 18 μm, 20 μm, 22 μm, 23 μm, 25 μm, 26 μm, 28 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm, preferably 20-80 μm, and more preferably 30-60 μm.
Preferably, the nonwoven material of the base support layer has a porosity of greater than 75%, for example, may be 75%, 76%, 77%, 78%, 79%, 80%, 82%, 85%, 88%, 90%, 92%, 95%, 96%, 98% or 99%.
Preferably, the nonwoven material of the base support layer has a grammage of 100-2For example, it may be 100g/m2、101g/m2、102g/m2、103g/m2、105g/m2、108g/m2、110g/m2、130g/m2、150g/m2、160g/m2、180g/m2、200g/m2、230g/m2、250g/m2、280g/m2、300g/m2、310g/m2、330g/m2、350g/m2、380g/m2、400g/m2、420g/m2、440g/m2、460g/m2、480g/m2、500g/m2、600g/m2、700g/m2Or 800g/m2Preferably 200-500g/m2。
Preferably, the nanofiber layer is a polymer nanofiber resistant to 180 ℃ or higher, and may be, for example, a polymer nanofiber resistant to 180 ℃, 181 ℃, 182 ℃, 185 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 280 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃ or 700 ℃, preferably to 180 ℃ or 240 ℃.
Preferably, the nanofiber layer is selected from any one or a mixture of at least two of polyimide, aramid, polysulfonamide, polyether ether ketone, polytetrafluoroethylene, polybenzimidazole or polyphenylene sulfide, the polyimide is an aromatic heterocyclic polymer compound containing imide group chain links in a molecular structure, the polyimide is one of the known organic polymer materials with the best comprehensive performance, the selected P84 type polyimide has good solubility, can be well dissolved in non-protonic solvents such as NMP, DMAc and DMF, like other polyimides, the P84 can be used for a long time at the temperature of-200-300 ℃, and is good in spinnability, strong in insulating property and high in mechanical strength, and the polyimide is preferably selected.
Preferably, the nanofiber layer has a nanofiber diameter of 1 to 2000nm, and may be, for example, 1nm, 2nm, 3nm, 5nm, 6nm, 8nm, 10nm, 12nm, 15nm, 16nm, 18nm, 20nm, 22nm, 25nm, 26nm, 28nm, 30nm, 32nm, 35nm, 36nm, 38nm, 40nm, 50nm, 100nm, 200nm, 300nm, 500nm, 600nm, 800nm, 1000nm, 1200nm, 1500nm, 1800nm or 2000nm, preferably 2 to 1000nm, and more preferably 5 to 800 nm.
Preferably, the nanofiber layer has a nanofiber porosity of greater than 95%, for example, can be 95%, 96%, 97%, 98%, or 99%.
Preferably, the protective layer is a woven or non-woven fabric resistant to 180 ℃ or higher, such as 180 ℃, 181 ℃, 182 ℃, 185 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 280 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃ or 700 ℃, preferably 180 ℃ or 240 ℃.
Preferably, the protective layer is selected from any one of or a mixture of at least two of aramid woven fabric, aramid non-woven fabric, polysulfonamide non-woven fabric, polyimide non-woven fabric, polyphenylene sulfide non-woven fabric or polybenzimidazole non-woven fabric.
Preferably, the woven or nonwoven material of the protective layer has a fiber diameter of 1 to 800. mu.m, and may be, for example, 1. mu.m, 2. mu.m, 3. mu.m, 5. mu.m, 6. mu.m, 8. mu.m, 10. mu.m, 15. mu.m, 16. mu.m, 18. mu.m, 20. mu.m, 30. mu.m, 40. mu.m, 50. mu.m, 60. mu.m, 70. mu.m, 80. mu.m, 90. mu.m, 100. mu.m, 150. mu.m, 200. mu.m, 250. mu.m, 300. mu.m, 350. mu.m, 400. mu.m, 450. mu.m or 500. mu.m, preferably 3 to 500. mu..
Preferably, the pore size of the woven or nonwoven material of the protective layer is 10 to 500. mu.m, and may be, for example, 10. mu.m, 11. mu.m, 12. mu.m, 13. mu.m, 15. mu.m, 16. mu.m, 18. mu.m, 20. mu.m, 30. mu.m, 40. mu.m, 50. mu.m, 60. mu.m, 70. mu.m, 80. mu.m, 100. mu.m, 120. mu.m, 150. mu.m, 180. mu.m, 200. mu.m, 250. mu.m, 280. mu.m, 300. mu.m, 400. mu.m, or 500. mu.m, preferably 20 to 300. mu.m, and more.
Preferably, the grammage of the woven or non-woven material of the protective layer is 10-100g/m2For example, it may be 10g/m2、11g/m2、12g/m2、13g/m2、15g/m2、16g/m2、18g/m2、20g/m2、21g/m2、22g/m2、23g/m2、25g/m2、28g/m2、30g/m2、40g/m2、50g/m2、60g/m2、70g/m2、80g/m2、90g/m2Or 100g/m2Preferably 20 to 80g/m2。
According to the invention, the protective layer is used for protecting the nano-fibers from being damaged by dust abrasion and preventing the nano-fibers from falling off, and the selected woven fabric or non-woven fabric material has uniform pore size distribution, high comprehensive performances such as wear resistance, chemical resistance and the like, and good flame resistance and thermal resistance.
In a second aspect, the present invention provides a method for preparing a composite nano filter material according to the first aspect, including the following steps:
(A) spraying a high-temperature-resistant adhesive on the substrate supporting layer;
(B) spinning polymer nano-fibers on a substrate supporting layer containing a high-temperature adhesive by an electrostatic spinning method to obtain a nano-fiber layer;
(C) covering a thin protective layer on the nanofiber layer;
(D) and (C) carrying out hot-pressing curing on the composite material obtained in the step (C) to obtain the composite air filtration nano filter material with a sandwich structure.
In the invention, the liquid adhesive penetrates through the nanofiber layer in a hot pressing mode, is in contact with the protective layer and is solidified, so that the protective layer, the nanofiber layer and the substrate supporting layer are tightly bonded.
Optionally, the base support layer is further subjected to a hydrophilic treatment prior to step (a), and the base material is further subjected to a hydrophilization treatment to increase the surface energy of the material, thereby increasing the bonding force between the base material and the nanofibers.
Preferably, the hydrophilic treatment method includes a dry treatment and a wet treatment.
Preferably, the dry processing comprises low-temperature plasma, evaporation and ionization activation; the wet process includes chemical reagent treatment and electrode precipitation.
Preferably, the base support layer is hydrophilically treated by a low temperature plasma technique.
In the invention, the binding force between the substrate supporting layer and the nanofiber layer is related to the surface energy of the material, if the selected substrate material has low surface energy, the binding force between the substrate supporting layer and the nanofiber layer is relatively poor, and the surface of the high-temperature resistant material with low surface energy, such as polyphenylene sulfide, is optimally subjected to activation treatment, so that the binding force between the substrate supporting layer and the nanofiber layer is increased; the low-temperature plasma technology is more environment-friendly, the treatment time is short, and the physical property and the mechanical property of the material can be ensured not to be changed.
In the invention, the hydrophilic treatment process is to use a Europlasma CD400 low-temperature plasma device to carry out hydrophilic treatment for 15-40min in an oxygen atmosphere at the temperature of 30-40 ℃, the power of 200W, the oxygen flow rate of 40m L/min and the air pressure of 13-15 Pa.
Preferably, the step (a) of spraying the high temperature resistant adhesive is to uniformly spray the high temperature resistant adhesive on the substrate support layer by means of electrostatic spraying.
Preferably, the electrostatic spraying is carried out in the specific steps of adjusting the rotating speed of a rotating roller to be 10-500r/min, the liquid supply speed of a single needle head to be 6.35-63.5 mu L/min and the translation speed of the needle head to be 0.5-5m/min within the range of 10-30cm from the substrate supporting layer under the conditions of positive voltage of 10-50kv and negative voltage of 0-10kv, wherein the electrostatic spraying time is 20-120 min.
In the invention, in order to solve the problems of large glue application amount, uneven glue application and the like of the traditional glue application process, the electrostatic spraying process is adopted, so that the substrate supporting layer and the nanofiber layer can be effectively bonded, sprayed adhesive particles are small and well dispersed on the surface of the substrate fiber, the influence on the aperture, porosity and air permeability of the substrate material is small, the glue application measurement can be accurately controlled by controlling the glue spraying time, the glue application uniformity can be well ensured, and the whole composite type nano filter material still maintains the original filtering efficiency.
Preferably, the solvent for electrostatic spinning in step (B) is an aprotic solvent, preferably one or a mixture of at least two of DMF, DMAc or NMP, the volatilization speed of DMF and DMAc is greatly influenced by the ambient humidity, after the ambient humidity exceeds 35%, DMF and DMAc are easily combined with water in the air, so that the spinning needle is blocked, and the P84/NMP spinning solution can be normally spun under the humidity condition of 10-70%, and further preferably NMP.
Preferably, the solvent for electrospinning has a mass concentration of 5 to 30%, and for example, may be 5%, 6%, 7%, 8%, 9%, 10%, 12%, 13%, 15%, 16%, 18%, 20%, 21%, 23%, 25%, 26%, 28%, or 30%, preferably 8 to 25%.
Preferably, the electrostatic spinning in the step (B) is carried out by adjusting the rotating speed of a rotating roller to be 10-500r/min, the liquid supply speed of a single needle to be 0.38-31.75 mu L/min and the translation speed of the needle to be 0.5-5m/min within the range of 7-30cm away from a substrate supporting layer sprayed with the high-temperature resistant adhesive under the conditions of positive voltage of 10-50kv and negative voltage of 0-10 kv.
Preferably, the pressure of the thermocompression curing in step (D) is 100-.
Preferably, the curing temperature of the hot press curing in step (D) is 50 to 300 ℃, for example, 50 ℃, 51 ℃, 52 ℃, 55 ℃, 58 ℃, 60 ℃, 62 ℃, 65 ℃, 68 ℃, 70 ℃, 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, 90 ℃, 100 ℃, 110 ℃, 130 ℃, 150 ℃, 180 ℃, 200 ℃, 250 ℃ or 300 ℃, preferably 80 to 200 ℃, and more preferably 100 to 180 ℃.
Preferably, the curing time of the hot press curing in the step (D) is 1 to 8 hours, for example, 1 hour, 2 hours, 3 hours, 4 hours, 5 hours, 6 hours, 7 hours or 8 hours, preferably 1 to 6 hours, and more preferably 1 to 4 hours.
Optionally, the composite nano filter material prepared in the step (D) is subjected to protective layer hydrophobic treatment, preferably low-temperature plasma technology.
The specific process of the hydrophobic treatment comprises the steps of adopting Europlasma CD400 type low-temperature plasma equipment, activating for 6min by using argon, controlling the power to be 100W, controlling the flow to be 10m L/min, the air pressure to be 40mTorr, the temperature to be 30-45 ℃ and the treatment time to be 15-40min in fluoride-containing atmosphere.
In the invention, considering that the dust-containing flue gas discharged by industries such as coal-fired power plants contains a large amount of water vapor, small particle dust is easy to adhere to the surface of the fiber due to the influence of the water vapor, the fiber pores are blocked, the fiber filtration resistance is increased to a certain extent, and the difficulty in removing filter cakes is increased. Therefore, the protective layer is subjected to hydrophobic treatment, the water contact angle is larger than 120 degrees, the surface energy of the material is further reduced, and dust is not easy to adhere to the surface of the fiber, so that ash is removed more conveniently, and the service life of the material is prolonged.
In a third aspect, the invention provides an application of the composite nano filter material in the first aspect in filtering high-temperature dust-containing flue gas.
Preferably, the filter material is used for preparing a filter bag, and the filter bag can be used in a bag-type dust removal filter.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the protective layer, the nanofiber layer and the substrate supporting layer are bonded by the high-temperature resistant adhesive, and the substrate supporting layer, the nanofiber layer and the protective layer are tightly bonded to form a sandwich structure by a hot-pressing curing technology, so that the high-temperature resistant nano filter material with stable mechanical property and excellent physical and chemical properties is obtained, and the problems of poor mechanical property, easy falling, easy crushing and the like of the nanofiber are solved;
(2) the nano filter material has high filtering efficiency, the filtering efficiency on PM2.5 and other micro particles is more than 99.5 percent, and the filtering residual resistance can be controlled within 200 Pa;
(3) the nano filter material can be used for a long time at the temperature of 180 ℃ plus 240 ℃, can resist the temperature of 260 ℃ instantly, has stronger acid-base resistance and thermal oxidation resistance and long service life.
Drawings
FIG. 1 is a schematic diagram of a three-layer structure of the composite nano-filter material of the present invention; wherein, 1-a substrate support layer; 2-a nanofiber layer; and 3, a protective layer.
Detailed Description
To further illustrate the technical means and effects of the present invention, the following further describes the technical solutions of the present invention by way of specific embodiments with reference to the drawings, but the present invention is not limited to the scope of the embodiments.
In a specific embodiment, the filter quality factor of the filter material can be comprehensively evaluated, and is defined as:
where P represents the particle penetration and Δ P represents the pressure drop. The filter figures of merit for the following examples are all calculated using the above formulaAnd (5) calculating to obtain.
Example 1
A preparation method of a composite nano filter material comprises the following steps:
(A) the epoxy resin type high-temperature resistant adhesive is uniformly coated on the surface of the substrate with the gram weight of 280g/m in an electrostatic spraying mode2The acceptance distance of the aramid fiber non-woven fabric is 11cm, the positive voltage is 12kv, the negative voltage is 2kv, the rotating speed of a rotating roller is 40r/min, the liquid supply speed is 6.35 mu L/min, the translation speed of a needle head is 0.5/min, and the sizing is 60 min;
(B) immediately spinning a polyimide nanofiber layer onto the sized aramid fiber non-woven fabric by an electrostatic spinning method after gluing, wherein the mass concentration of a solution is 10%, the receiving distance is 12cm, the positive voltage is 12kv, the negative voltage is 2kv, the rotating speed of a receiving roller is 15r/min, the liquid supply speed is 0.635 mu L/min, the translation speed of a needle is 0.5m/min, the spinning time is 90min, and the gram weight of the nanofiber layer is 6.5 g/square meter;
(C) after spinning, covering the nanofiber layer with a gram weight of 80g/m2The polyphenylene sulfide spunlace non-woven fabric protective layer;
(D) and (C) placing the composite material obtained in the step (C) into a flat plate rapid dryer, curing for 1h at 80 ℃, and then curing for 1h at 130 ℃ to obtain the composite nano filter material with a sandwich structure.
At the room temperature of 25 ℃, the flow rate of the dust-containing gas is controlled to be 20L/s, the filtration efficiency of the test material to 0.3 mu m particles is 99.44 percent, and the resistance of the clean filter material is 77.8Pa, QFWas 0.067.
Example 2
A preparation method of a composite nano filter material comprises the following steps:
(A) the epoxy resin type high-temperature resistant adhesive is uniformly coated on the surface of the substrate with the gram weight of 300g/m in an electrostatic spraying mode2The polyimide spunlace non-woven fabric is subjected to a positive voltage of 15kv and a negative voltage of 2kv at a receiving distance of 12cm, the rotating speed of a rotating roller is 40r/min, the liquid supply speed is 10 mu L/min, the translation speed of a needle head is 0.5m/min, and the glue is applied for 30 min;
(B) immediately spinning the polyimide nano-fiber layer on the glued polyimide spunlace non-woven fabric by an electrostatic spinning method after gluing,the mass concentration of the solution is 13 percent, the receiving distance is 12cm, the positive voltage is 14kv, the negative voltage is 2kv, the rotating speed of a receiving roller is 35r/min, the liquid supply speed is 0.635 mu L/min, the translation speed of a needle head is 0.5m/min, the spinning time is 75min, and the gram weight of a nanofiber layer is 6.8g/m2；
(C) After spinning, covering the nanofiber layer with a gram weight of 60g/m2The polytetrafluoroethylene non-woven fabric protective layer;
(D) and (C) placing the composite material obtained in the step (C) into a flat plate rapid dryer, curing for 1h at 80 ℃, and then curing for 1h at 130 ℃ to obtain the composite nano filter material with a sandwich structure.
At the room temperature of 25 ℃, the flow rate of the dust-containing gas is controlled to be 20L/s, the filtration efficiency of the test material to 0.3 mu m particles is 99.64 percent, and the resistance of the clean filter material is 86.5Pa, QFWas 0.065.
Example 3
A preparation method of a composite nano filter material comprises the following steps:
(A) passing through Europlasma CD400 type low temperature plasma equipment, under the conditions of oxygen atmosphere, 200W, 40m L/min oxygen flow rate, 14Pa pressure, 30 deg.C, the gram weight is 260g/m2Carrying out hydrophilic treatment on the polyphenylene sulfide needle-punched non-woven fabric for 15 min;
(B) uniformly coating the organic silicon type high-temperature-resistant adhesive on the polyphenylene sulfide non-woven fabric treated in the step (A) and the non-woven fabric which is not subjected to hydrophilic treatment in an electrostatic spraying mode, wherein the acceptance distance is 11cm, the positive voltage is 12kv, the negative voltage is 2kv, the rotating speed of a rotating roller is 30r/min, the liquid supply speed is 6.35 mu L/min, the translation speed of a needle head is 0.5m/min, and the glue is applied for 30 min;
(C) immediately spinning the polyimide nanofiber layer on the glued polyphenylene sulfide non-woven fabric by an electrostatic spinning method after gluing, wherein the mass concentration of the solution is 10 percent, the receiving distance is 12cm, the positive voltage is 10kv, the negative voltage is 2kv, the rotating speed of a receiving roller is 15r/min, the liquid supply speed is 0.635 mu L/min, the needle translation speed is 0.5m/min, the spinning time is 65min, and the gram weight of the nanofiber layer is respectively 5.5g/m of the treated polyphenylene sulfide non-woven fabric2And 4.8g/m of non-woven fabric without hydrophilic treatment2；
(D) After spinning is finishedCovering the nanofiber layer with a gram weight of 60g/m2The polytetrafluoroethylene non-woven fabric protective layer;
(E) and (D) placing the composite material obtained in the step (D) into a flat plate quick dryer, and curing for 3 hours at the temperature of 120 ℃ to obtain the composite nano filter material with a sandwich structure.
The results are shown in table 1 below:
TABLE 1
As can be seen from Table 1, the performance of the nano filter material subjected to hydrophilic treatment is superior to that of the nano filter material not subjected to hydrophilic treatment in all aspects.
Example 4
A preparation method of a composite nano filter material comprises the following steps:
(A) passing through Europlasma CD400 type low temperature plasma equipment, under the conditions of oxygen atmosphere, 200W, 40m L/min oxygen flow rate, 14Pa pressure, 30 deg.C, the gram weight is 260g/m2Carrying out hydrophilic treatment on the polyphenylene sulfide needle-punched non-woven fabric for 15 min;
(B) uniformly coating the organic silicon type high-temperature-resistant adhesive on the polyphenylene sulfide non-woven fabric treated in the step (A) and the non-woven fabric which is not subjected to hydrophilic treatment in an electrostatic spraying mode, wherein the acceptance distance is 11cm, the positive voltage is 14kv, the negative voltage is 1.5kv, the rotating speed of a rotating roller is 30r/min, the liquid supply speed is 6.35 mu L/min, the translation speed of a needle head is 0.5m/min, and the glue application time is 35 min;
(C) immediately spinning the polyimide nanofiber layer on the glued polyphenylene sulfide non-woven fabric by an electrostatic spinning method after gluing, wherein the mass concentration of the solution is 12%, the receiving distance is 15cm, the positive voltage is 13kv, the negative voltage is 2kv, the rotating speed of a receiving roller is 35r/min, the liquid supply speed is 0.635 mu L/min, the needle translation speed is 0.5m/min, the spinning time is 75min, and the gram weight of the nanofiber layer is 6.3g/m of the treated polyphenylene sulfide non-woven fabric2And non-woven fabric 5.7g/m without hydrophilic treatment2；
(D) After spinning, covering the nanofiber layer with a gram weight of 50g/m2Polysulfonamide non-woven fabricA protective layer;
(E) placing the composite material obtained in the step (D) in a flat plate rapid dryer, curing for 1h at the temperature of 80 ℃, and then curing for 1h at the temperature of 130 ℃ to obtain a composite nano filter material with a sandwich structure;
(F) and finally, performing hydrophobic treatment on the treated polyphenylene sulfide non-woven fabric composite material by using Europlasma CD400 type low-temperature plasma equipment, performing activation treatment for 6min at the temperature of 35 ℃, controlling the power to be 100W, then performing treatment for 15min in fluoride-containing atmosphere, controlling the gas flow rate to be 10m L/min and the gas pressure to be 40mTorr, and thus obtaining the final high-temperature-resistant composite air filtration nano filter material.
The results are shown in table 2 below:
TABLE 2
As can be seen from Table 2, the nano filter material subjected to hydrophilic treatment and hydrophobic treatment has better performance in all aspects than other nano filter materials, and particularly, the filtering pressure is obviously reduced.
Example 5
A preparation method of a composite nano filter material comprises the following steps:
(A) the epoxy resin type high-temperature resistant adhesive is uniformly coated on the surface of the substrate with the gram weight of 300g/m in an electrostatic spraying mode2The acceptance distance of the aramid fiber non-woven fabric is 11cm, the positive voltage is 12kv, the negative voltage is 2kv, the rotating speed of a rotating roller is 30r/min, the liquid supply speed is 6.35 mu L/min, the translation speed of a needle head is 0.5m/min, and the sizing is 60 min;
(B) immediately spinning the polyimide nanofiber layer on the sized polyimide spunlace nonwoven fabric by an electrostatic spinning method after the sizing is finished, wherein the mass concentration of the solution is 10%, the receiving distance is 12cm, the positive voltage is 10kv, the negative voltage is 2kv, the rotating speed of a receiving roller is 15r/min, the liquid supply speed is 0.635 mu L/min, the translation speed of a needle is 0.5m/min, the spinning time is controlled to be 120min and 65min respectively, and the gram weight of the obtained two nanofiber layers is 8.3g/m respectively2And 4.6g/m2；
(C) After spinning, sodium hydroxide is addedThe gram weight covered above the rice fiber layer is 80g/m2The polyphenylene sulfide spunlace non-woven fabric protective layer;
(D) and (C) placing the composite material obtained in the step (C) into a flat plate rapid dryer, curing for 1h at 80 ℃, and then curing for 1h at 130 ℃ to obtain the composite nano filter material with a sandwich structure.
The results of particle filtration of two kinds of nano filter materials prepared under different spinning time conditions, at room temperature of 25 ℃, the flow rate of dust-containing gas of 20L/s, and the particle size of the filtration test of 0.3 μm are shown in the following table 3:
TABLE 3
As can be seen from Table 3, the gram weights of the nanofibers prepared at different spinning times are different, so that the filtration is obviously affected, and the filtration effect of the nanofibers with large gram weights is good.
In conclusion, the invention obviously improves the filtering effect of the nano filter material through hydrophilic treatment and hydrophobic treatment, and the nano filter material has high filtering efficiency, the filtering efficiency of the nano filter material on PM2.5 and other micro particles is more than 99.5 percent, and the filtering residual resistance can be controlled within 200 Pa.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (50)
1. The composite nano filter material is characterized by comprising a substrate support layer (1), a nanofiber layer (2) and a protective layer (3);
wherein the base support layer (1), the nanofiber layer (2) and the protective layer (3) are bonded by a high temperature resistant adhesive;
the high-temperature resistant adhesive is adhesive resistant to the temperature of more than 180 ℃;
the nanofiber layer (2) is selected from any one or a mixture of at least two of polyimide, aramid, polysulfonamide, polyether ether ketone, polytetrafluoroethylene, polybenzimidazole or polyphenylene sulfide;
the substrate supporting layer (1) is subjected to low-temperature plasma hydrophilic treatment in advance;
the hydrophilic treatment process comprises the following steps of carrying out hydrophilic treatment for 15-40min by using a Europlasma CD400 low-temperature plasma device in an oxygen atmosphere at the temperature of 30-40 ℃, the power of 200W, the oxygen flow rate of 40m L/min and the air pressure of 13-15 Pa;
the high-temperature resistant adhesive is uniformly sprayed on the substrate supporting layer (1) through electrostatic spraying;
the electrostatic spraying method comprises the specific steps of adjusting the rotating speed of a rotating roller to be 10-500r/min, the liquid supply speed of a single needle head to be 6.35-63.5 mu L/min and the translation speed of the needle head to be 0.5-5m/min within the range of 10-30cm from a substrate supporting layer (1) under the conditions of positive voltage of 10-50kv and negative voltage of 0-10kv, and performing electrostatic spraying for 20-120 min;
the nanofiber layer (2) is obtained by spinning polymer nanofibers on a substrate supporting layer (1) containing a high-temperature adhesive through electrostatic spinning;
the electrostatic spinning time is 75-120 min;
the protective layer (3) is subjected to hydrophobic treatment.
2. The nanofilter according to claim 1, wherein the high temperature resistant adhesive is selected from any one of or a combination of at least two of epoxy type adhesive, silicone adhesive, polyimide adhesive, or maleimide adhesive.
3. The nanofilter of claim 2, wherein the high temperature resistant adhesive is an epoxy type adhesive.
4. Nanofilter according to claim 1, characterized in that the base support layer (1) is a non-woven material resistant to temperatures above 180 ℃.
5. Nanofilter according to claim 4, characterized in that the base support layer (1) is a non-woven material resistant to 180-.
6. Nanofilter according to claim 5, characterized in that the base support layer (1) is selected from any one or a mixture of at least two of polyimide, polyphenylene sulfide, aramid, polysulfonamide, glass fiber, polytetrafluoroethylene or polyetheretherketone.
7. The nanofilter according to claim 6, wherein the substrate support layer (1) is one or a mixture of at least two of aramid, polyimide or polyphenylene sulfide non-woven fabrics.
8. Nanofilter according to claim 1, characterized in that the fiber diameter of the nonwoven material of the base support layer (1) is 1-200 μ ι η.
9. Nanofilter according to claim 8, characterized in that the fiber diameter of the nonwoven material of the base support layer (1) is 3-100 μm.
10. Nanofilter according to claim 9, characterized in that the fiber diameter of the non-woven material of the base support layer (1) is 15-80 μ ι η.
11. Nanofilter according to claim 1, characterized in that the non-woven material of the base support layer (1) has a fiber pore size of 10-100 μ ι η.
12. Nanofilter according to claim 11, characterized in that the non-woven material of the base support layer (1) has a fiber pore size of 20-80 μ ι η.
13. Nanofilter according to claim 12, characterized in that the non-woven material of the base support layer (1) has a fiber pore size of 30-60 μ ι η.
14. Nanofilter according to claim 1, characterized in that the porosity of the non-woven material of the base support layer (1) is greater than 75%.
15. The nanofilter according to claim 1, wherein the nonwoven material of the base support layer (1) has a grammage of 100-800g/m2。
16. The nanofilter according to claim 15, wherein the nonwoven material of the base support layer (1) has a grammage of 200-500g/m2。
17. Nanofilter according to claim 1, characterized in that the nanofibrous layer (2) is polyimide.
18. Nanofilter according to claim 1, characterized in that the nanofibrous diameter of the nanofibrous layer (2) is 1-2000 nm.
19. Nanofilter according to claim 18, characterized in that the nanofibrous diameter of the nanofibrous layer (2) is 2-1000 nm.
20. Nanofilter according to claim 19, characterized in that the nanofibrous diameter of the nanofibrous layer (2) is 5-800 nm.
21. Nanofilter according to claim 1, characterized in that the nanofibrous porosity of the nanofibrous layer (2) is higher than 95%.
22. The nanofilter according to claim 1, wherein the protective layer (3) is a woven or non-woven fabric resistant to temperatures above 180 ℃.
23. The nanofilter according to claim 22, wherein the protective layer (3) is a woven or non-woven fabric resistant to 180-.
24. The nanofilter according to claim 23, wherein the protective layer (3) is selected from any one of or a mixture of at least two of aramid woven fabric, aramid non-woven fabric, polysulfonamide non-woven fabric, polyimide non-woven fabric, polyphenylene sulfide non-woven fabric, or polybenzimidazole non-woven fabric.
25. Nanofilter according to claim 1, characterized in that the woven or non-woven material of the protective layer (3) has a fiber diameter of 1-800 μm.
26. Nanofilter according to claim 25, characterized in that the woven or non-woven material of the protective layer (3) has a fiber diameter of 3-500 μm.
27. Nanofilter according to claim 26, characterized in that the woven or non-woven material of the protective layer (3) has a fiber diameter of 5-400 μm.
28. Nanofilter according to claim 1, characterized in that the pore size of the woven or non-woven material of the protective layer (3) is 10-500 μm.
29. Nanofilter according to claim 28, characterized in that the pore size of the woven or non-woven material of the protective layer (3) is 20-300 μm.
30. Nanofilter according to claim 29, characterized in that the pore size of the woven or non-woven material of the protective layer (3) is 30-400 μ ι η.
31. Nanofilter according to claim 1, characterized in that the grammage of the woven or non-woven material of the protective layer (3) is 10-100g/m2。
32. -nanofilter according to claim 31, characterized in that the grammage of the woven or non-woven material of the protective layer (3) is between 20 and 80g/m2。
33. A method for preparing the composite nano filter material of any one of claims 1 to 32, which is characterized by comprising the following steps:
(A) spraying a high-temperature-resistant adhesive on the substrate supporting layer (1);
(B) spinning polymer nano-fibers on a substrate supporting layer (1) containing a high-temperature adhesive by an electrostatic spinning method to obtain a nano-fiber layer (2);
(C) covering a thin protective layer (3) on the nanofiber layer (2);
(D) hot-pressing and curing the composite material obtained in the step (C) to obtain a composite air filtration nano filter material with a sandwich structure;
carrying out hydrophilic treatment of a low-temperature plasma technology on the substrate supporting layer (1) in the step (A);
the spraying of the high-temperature-resistant adhesive in the step (A) is to uniformly spray the high-temperature-resistant adhesive on a substrate supporting layer (1) in an electrostatic spraying manner;
the electrostatic spraying method comprises the specific steps of adjusting the rotating speed of a rotating roller to be 10-500r/min, the liquid supply speed of a single needle head to be 6.35-63.5 mu L/min and the translation speed of the needle head to be 0.5-5m/min within the range of 10-30cm from a substrate supporting layer (1) under the conditions of positive voltage of 10-50kv and negative voltage of 0-10kv, and performing electrostatic spraying for 20-120 min;
and (D) carrying out hydrophobic treatment on the protective layer (3) on the composite nano filter material prepared in the step (D).
34. The method of claim 33, wherein the solvent for electrospinning in step (B) is an aprotic solvent.
35. The method according to claim 34, wherein the solvent for electrospinning in step (B) is any one or a mixture of at least two of N, N-Dimethylformamide (DMF), N-dimethylacetamide (DMAc), or N-methylpyrrolidone (NMP).
36. The method according to claim 35, wherein the solvent for electrospinning in step (B) is N-methylpyrrolidone (NMP).
37. The method of claim 33, wherein the solvent for electrospinning has a mass concentration of 5 to 30%.
38. The method of claim 37, wherein the solvent for electrospinning has a mass concentration of 8 to 25%.
39. The preparation method of claim 33, wherein the electrospinning in step (B) comprises the specific steps of regulating the rotating speed of the rotating roller to 10-500r/min, the single-needle liquid supply speed to 0.38-31.75 μ L/min and the needle translation speed to 0.5-5m/min within the range of 7-30cm from the substrate support layer (1) sprayed with the high-temperature resistant adhesive under the conditions of positive voltage of 10-50kv and negative voltage of 0-10 kv.
40. The method as claimed in claim 33, wherein the pressure of the thermocompression curing in step (D) is 100-500N.
41. The method as claimed in claim 40, wherein the pressure of the thermocompression curing in step (D) is 150-400N.
42. The method according to claim 33, wherein the curing temperature of the thermocompression curing in the step (D) is 50 to 300 ℃.
43. The method according to claim 42, wherein the curing temperature of the thermocompression curing in the step (D) is 80 to 200 ℃.
44. The method as claimed in claim 43, wherein the curing temperature of the thermocompression curing in the step (D) is 100-180 ℃.
45. The method of claim 33, wherein the curing time of the thermocompression curing in step (D) is 1 to 8 hours.
46. The method according to claim 45, wherein the curing time of the thermocompression curing in the step (D) is 1 to 6 hours.
47. The method according to claim 46, wherein the curing time of the thermocompression curing in the step (D) is 1 to 4 hours.
48. The preparation method according to claim 33, wherein the composite nano filter material prepared in the step (D) is subjected to hydrophobic treatment on the protective layer (3) by using a low-temperature plasma technology.
49. Use of a composite nanofilter according to any one of claims 1-32 in the filtration of high temperature dusty flue gas.
50. The use of claim 49, wherein the filter material is used to make a filter bag.
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| WO2019184099A1 (en) * | 2018-03-27 | 2019-10-03 | Focus Industries Limited | Nanomaterial including nanofibers and beads for hepa air filter media |
| CN110180260B (en) * | 2019-05-14 | 2021-12-10 | 中安瑞材(北京)科技有限公司 | Air purification filter element and preparation method thereof |
| CN110064248B (en) * | 2019-06-06 | 2021-08-03 | 北京科技大学 | Composite filter material, preparation method and performance test method thereof |
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| CN110898530A (en) * | 2019-12-09 | 2020-03-24 | 安徽省利特环保技术有限公司 | Folding type micro-fine particle lengthening filter cylinder |
| CN111467878B (en) * | 2020-03-17 | 2021-11-12 | 南京玻璃纤维研究设计院有限公司 | Nanofiber/glass fiber composite filter material, preparation method and application thereof |
| CN112370866A (en) * | 2020-10-28 | 2021-02-19 | 美埃(南京)纳米材料有限公司 | Degradable antibacterial nanofiber non-woven fabric composite filter material and preparation method thereof |
| CN113018982A (en) * | 2020-12-31 | 2021-06-25 | 东华大学 | Bonding method of high-temperature-resistant nanofiber/glass fiber woven fabric composite filter material |
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