CN117531296A - Filter element made of efficient stain-resistant material and preparation method thereof - Google Patents

Filter element made of efficient stain-resistant material and preparation method thereof Download PDF

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CN117531296A
CN117531296A CN202311570736.8A CN202311570736A CN117531296A CN 117531296 A CN117531296 A CN 117531296A CN 202311570736 A CN202311570736 A CN 202311570736A CN 117531296 A CN117531296 A CN 117531296A
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fiber layer
fiber
filter
filter element
solution
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CN117531296B (en
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李大伟
聂涛
赵文浩
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Jiangsu Sheke Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/02Loose filtering material, e.g. loose fibres
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/10Chemical after-treatment of artificial filaments or the like during manufacture of carbon
    • D01F11/12Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
    • D01F11/125Carbon
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/02Types of fibres, filaments or particles, self-supporting or supported materials
    • B01D2239/0216Bicomponent or multicomponent fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2239/00Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10Filtering material manufacturing

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Filtering Materials (AREA)

Abstract

The invention relates to the technical field of filter element materials, in particular to a filter element made of high-efficiency stain-resistant materials and a preparation method thereof. The filter element is composed of a plurality of layers of fibers, the filter aperture is gradually increased from inside to outside, the filter area and the sewage containing amount are increased, the filter precision is high, the filter effect is good, the service life is greatly prolonged, the innermost inner fine filter fiber layer is composed of a composite fiber material and polytetrafluoroethylene fibers in an interweaving mode, wherein the polytetrafluoroethylene fibers have high strength and high extensibility and good stability, and are matched with the composite fiber material for use, so that the filter element has excellent mechanical property and sewage containing property, and the high-efficiency filter effect and long-time service life can be realized.

Description

Filter element made of efficient stain-resistant material and preparation method thereof
Technical Field
The invention relates to the technical field of filter element materials, in particular to a filter element made of efficient pollution-resistant materials and a preparation method thereof.
Background
With the rapid development of industry, water, air and soil pollution are increasingly serious, water quality of water sources in China is continuously deteriorated, a plurality of urban groundwater and superficial water are seriously polluted, the rapid development of a purified water market is aggravated by the water quality deterioration of the water sources, the water treated by the water purifier basically meets the safety of drinking water, most of mineral substances and organic substances such as ions in the water can be removed by adopting the reverse osmosis purified water purifier in the related technology, the water quality is acidic, the taste is green and astringent, the sanitary safety requirement is met, the water quality and the taste are greatly discounted, the original fresh and sweet characteristics of the water are completely lost, and with the improvement of people on the safety and the taste of the drinking water, the water with good taste is increasingly favored by consumers.
For example, the invention patent with publication number CN107285396a discloses a degradable PLA water purification filter element, the main material of the filter element is PLA fiber, the PLA fiber is extruded from a spinning die head at 160-200 ℃ after being blended by PLLA, PDLA, PGLA and a water purifying agent, and a fiber net is formed and shaped by a rolling collector; the water purifying agent is one or more of nano zinc oxide, nano silver and active carbon; the filter element can realize physical filtration and simultaneously has relatively effective bacteriostasis and sterilization effects, and meanwhile, after the filter element made of PLA material is replaced, the filter element can be completely degraded in a composting environment; however, in the use process of the filter element, the water purifying agent loaded in the PLA fiber is easy to separate under the action of water flow, so that the water purifying agent loaded in the PLA fiber is gradually reduced, and the purification effect is affected.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a filter element made of high-efficiency and dirt-resistant materials and a preparation method thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the filter element is cylindrical and sequentially comprises an inner fine filter fiber layer, an adsorptive fiber layer, a middle fine filter fiber layer, a framework fiber layer and an outer coarse filter fiber layer from inside to outside in the radial direction, wherein the filter pore diameter of each of the inner fine filter fiber layer, the middle fine filter fiber layer and the outer coarse filter fiber layer is gradually increased from inside to outside in the radial direction;
the inner fine filtration fiber layer is formed by interweaving a composite fiber material and polytetrafluoroethylene fibers;
the composite fiber material is prepared by taking porous carbon fiber as a matrix, loading nano rods after hydrothermal reaction to obtain composite porous carbon fiber, activating nano activated carbon and then penetrating the activated nano activated carbon into gaps of the composite porous carbon fiber in a vacuum impregnation mode.
As a further preferred aspect of the present invention, the absorbent fiber layer is composed of carbon fibers or plant fibers;
the middle fine filter fiber layer and the outer coarse filter fiber layer are formed by polyester fibers or nylon fibers;
the skeleton fiber layer is composed of glass fibers or polyethylene fibers.
As a further preferable scheme of the invention, the framework fiber layer and the outer rough filtration fiber layer are embedded with an active agent, and the active agent is ion exchange resin particles and zeolite particles according to the weight ratio of 1: the ion exchange resin particles are prepared by mixing the dosage proportion of (1-2), wherein the weight ratio of the anion exchange resin particles to the cation exchange resin particles is 1: and (2-4) in proportion.
As a further preferable scheme of the invention, the preparation method of the composite porous carbon fiber comprises the following steps:
1) Sequentially adding polyacrylonitrile powder and dimethyl sulfoxide into a container, uniformly stirring at 60-65 ℃ to prepare a solution, then adding potassium carbonate into the solution, continuously stirring for 5-10h, uniformly mixing to obtain a spinning solution, extruding the spinning solution into a potassium carbonate aqueous solution at 55-58 ℃ under the pressure of 0.3-0.8MPa for solidification, and drying the solidified fiber in a vacuum drying oven at 60-70 ℃ for 45-50h to obtain polypropylene fiber;
2) Placing polypropylene fibers in an oven, respectively treating at 180-190 ℃ and 230-240 ℃ for 10-20min and 30-50min, then transferring into a crucible, treating at 800-850 ℃ for 1-3h under nitrogen atmosphere, naturally cooling to room temperature after the treatment is finished, repeatedly cleaning with hydrochloric acid solution, and drying to obtain porous carbon fibers;
3) Dissolving polyvinylpyrrolidone in 1-amyl alcohol, adding sodium citrate solution, fully stirring and dissolving, sequentially adding deionized water, concentrated hydrochloric acid and tetrabutyl titanate, fully stirring and dissolving to obtain titanium dioxide source solution, immersing porous carbon fiber in the titanium dioxide source solution, transferring the porous carbon fiber into a reaction kettle, sealing, carrying out hydrothermal reaction at 90-120 ℃ for 15-25h, repeatedly washing the product with deionized water and absolute ethyl alcohol after the reaction is finished, and drying with nitrogen to obtain the composite porous carbon fiber.
As a further preferred embodiment of the invention, in step 1), the solution has a solids content of 20-25wt%;
the addition amount of the potassium carbonate is 1-5% of the mass of the polyacrylonitrile;
the concentration of the potassium carbonate aqueous solution is 1-5wt%.
As a further preferable mode of the present invention, in the step 2), the flow rate of the nitrogen gas is 1.0 to 1.6L/min.
As a further preferable scheme of the invention, in the step 3), the dosage proportion of polyvinylpyrrolidone, 1-amyl alcohol, sodium citrate solution, deionized water, concentrated hydrochloric acid and tetrabutyl titanate is (0.5-1.0) g: (5-10) mL: (100-200) μl: (5-13) mL: (5-10) mL: (200-300) μL;
the concentration of the sodium citrate solution is 0.3-0.5mol/L;
the concentration of the concentrated hydrochloric acid is 12-14mol/L;
the addition amount of the porous carbon fiber is 3-8% of the total mass of the titanium dioxide source solution.
As a further preferable embodiment of the present invention, the preparation method of the composite fiber material is as follows:
1) Drying high-carbon ash at 105-115 ℃ for 2-5 hours, grinding into fine powder by superfine grinding, uniformly mixing with potassium hydroxide with equal mass, transferring into a reactor, heating to 1200-1300 ℃ under nitrogen atmosphere, preserving heat for 1-3 hours, cooling to room temperature after treatment is finished, pickling with hydrochloric acid solution with the concentration of 10-13wt%, repeatedly washing to neutrality by deionized water, drying, crushing and grinding to obtain activated nano active carbon;
2) Dispersing activated nano activated carbon in deionized water to obtain dispersion liquid, then placing the composite porous carbon fiber in a vacuum impregnator, vacuumizing to 50-100Pa, maintaining for 5-10min, then injecting sufficient dispersion liquid, vacuumizing to 10-30Pa, continuously maintaining for 20-40min, slowly releasing pressure to normal pressure, repeating the operation for 2-5 times, centrifuging and drying to obtain the composite fiber material.
As a further preferable scheme of the invention, the temperature rising rate is 10-20 ℃/min under the nitrogen atmosphere;
the concentration of the dispersion is 3-8wt%.
A preparation method of a filter element made of high-efficiency stain-resistant materials specifically comprises the following steps:
winding the composite fiber material and polytetrafluoroethylene fiber into a cylindrical inner fine filtration fiber layer by alternating hot melt spinning, winding an adsorptive fiber layer on the inner fine filtration fiber layer, winding a middle fine filtration fiber layer on the adsorptive fiber layer, winding a skeleton fiber layer on the middle fine filtration fiber layer, and winding an outer coarse filtration fiber layer on the skeleton fiber layer.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the polypropylene fiber is obtained by wet spinning with the potassium carbonate as an additive, then the porous carbon fiber with a porous structure is obtained by synchronous carbonization and activation, then the porous carbon fiber is used as a carrier, and a large amount of titanium dioxide nanorods are deposited in the porous carbon fiber by a microemulsion hydrothermal method, so that the composite porous carbon fiber is obtained, the abundant pore structure provides sufficient places for the deposition of the titanium dioxide nanorods, the deposited titanium dioxide nanorods are mutually stacked to form a crossed skeleton structure, on one hand, the void of the composite porous carbon fiber can be supported, and the void collapse phenomenon in the subsequent vacuum impregnation process is avoided, so that the nano activated carbon can smoothly infiltrate into the void in the subsequent vacuum impregnation process, and on the other hand, the skeleton structure formed in the void increases the meandering degree of the void, so that the moving path and the friction resistance of the nano activated carbon which infiltrates subsequently are prolonged, the effect of preventing the nano activated carbon from losing can be effectively achieved, and the stability of the nano activated carbon load is realized.
According to the invention, high-carbon ash is used as a raw material, potassium hydroxide is adopted for high-temperature alkali activation treatment, so that the original pore structure in fine ash collapses, the carbon skeleton structure is broken to generate more micropore structures, and the blocked pores in the reaction process can be dredged through subsequent acid washing, so that nano activated carbon with high porosity can be obtained, then the nano activated carbon is infiltrated into the composite porous carbon fiber in a vacuum impregnation mode, so that a composite fiber material is obtained, the composite fiber material is internally provided with abundant micropore structures, tiny particles and bacteria in a filter medium can be filtered under the capillary action, so that the cleanness of the filter medium is ensured, the filtering effect is improved, and the titanium dioxide nanorods loaded in the composite fiber material have good sterilization and decontamination effects under illumination, so that the filtered bacteria and dirt can be cleaned with high efficiency, the cleaning of the composite fiber material is improved, the composite fiber material can be repeatedly used for multiple times, and the pollution resistance of the composite fiber material is improved.
The filter element is composed of a plurality of layers of fibers, the filter aperture is gradually increased from inside to outside, the filter area and the sewage containing amount are increased, the filter precision is high, the filter effect is good, the service life is greatly prolonged, the innermost inner fine filter fiber layer is composed of a composite fiber material and polytetrafluoroethylene fibers in an interweaving mode, wherein the polytetrafluoroethylene fibers have high strength and high extensibility and good stability, and are matched with the composite fiber material for use, so that the filter element has excellent mechanical property and sewage containing property, and the high-efficiency filter effect and long-time service life can be realized.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the embodiment of the invention, the absorptive fiber layer is composed of carbon fibers; the middle fine filter fiber layer and the outer coarse filter fiber layer are formed by polyester fibers; the skeleton fiber layer is made of glass fibers.
The framework fiber layer and the outer rough filtration fiber layer are embedded with an active agent, wherein the active agent is ion exchange resin particles and zeolite particles according to the weight ratio of 1:2, and the ion exchange resin particles are prepared by mixing anion exchange resin particles and cation exchange resin particles according to the weight ratio of 1:3, wherein the anion exchange resin is HasterJET 4200Cl anion exchange resin of Tao Shiluo phylum HasterJET, U.S. and the cation exchange resin is Blastet C100E cation exchange resin of England.
Example 1
The filter element is cylindrical and sequentially comprises an inner fine filter fiber layer, an adsorptive fiber layer, a middle fine filter fiber layer, a framework fiber layer and an outer coarse filter fiber layer from inside to outside in the radial direction, wherein the filter pore diameter of each of the inner fine filter fiber layer, the middle fine filter fiber layer and the outer coarse filter fiber layer gradually increases from inside to outside in the radial direction;
wherein the inner fine filter fiber layer is formed by interweaving a composite fiber material and polytetrafluoroethylene fibers;
the composite fiber material is prepared by taking porous carbon fiber as a matrix, loading nano rods after hydrothermal reaction to obtain composite porous carbon fiber, activating nano activated carbon and then penetrating the activated nano activated carbon into gaps of the composite porous carbon fiber in a vacuum impregnation mode;
the preparation method of the filter element specifically comprises the following steps:
winding the composite fiber material and polytetrafluoroethylene fiber into a cylindrical inner fine filtration fiber layer by alternating hot melt spinning, winding an adsorptive fiber layer on the inner fine filtration fiber layer, winding a middle fine filtration fiber layer on the adsorptive fiber layer, winding a skeleton fiber layer on the middle fine filtration fiber layer, and winding an outer coarse filtration fiber layer on the skeleton fiber layer.
The preparation method of the composite fiber material comprises the following steps:
1) Sequentially adding polyacrylonitrile powder and dimethyl sulfoxide into a container, uniformly stirring at 60 ℃ to prepare a solution with the solid content of 20wt%, then adding potassium carbonate into the solution and continuously stirring for 5 hours, wherein the adding amount of the potassium carbonate is 1% of the mass of the polyacrylonitrile, uniformly mixing to obtain a spinning solution, extruding the spinning solution into a potassium carbonate aqueous solution with the concentration of 1wt% at 55 ℃ under the pressure of 0.3MPa for solidification, and placing the solidified fiber into a 60 ℃ vacuum drying oven for drying for 45 hours to obtain polypropylene fiber;
2) Placing polypropylene fibers in an oven, respectively treating for 10min and 30min at 180 ℃ and 230 ℃, then moving the polypropylene fibers into a crucible, treating for 1h at 800 ℃ under the nitrogen atmosphere, naturally cooling to room temperature after the treatment is finished, repeatedly cleaning with hydrochloric acid solution, and drying to obtain porous carbon fibers;
3) Dissolving 0.5g of polyvinylpyrrolidone in 5mL of 1-amyl alcohol, adding 100 mu L of sodium citrate solution with the concentration of 0.3mol/L, fully stirring and dissolving, sequentially adding 5mL of deionized water, 5mL of concentrated hydrochloric acid with the concentration of 12mol/L and 200 mu L of tetrabutyl titanate, fully stirring and dissolving to obtain a titanium dioxide source solution, immersing porous carbon fibers in the titanium dioxide source solution, controlling the adding amount of the porous carbon fibers to be 3% of the total mass of the titanium dioxide source solution, transferring the porous carbon fibers into a reaction kettle, performing hydrothermal reaction for 15h at 90 ℃ after sealing, repeatedly washing a product by using deionized water and absolute ethyl alcohol after the reaction is finished, and drying by using nitrogen to obtain the composite porous carbon fibers;
4) Drying high-carbon ash at 105 ℃ for 2 hours, superfine grinding into fine powder, uniformly mixing with potassium hydroxide with equal mass, transferring into a reactor, heating to 1200 ℃ at a speed of 10 ℃/min under nitrogen atmosphere, preserving heat for 1 hour, cooling to room temperature after treatment is finished, pickling with hydrochloric acid solution with the concentration of 10wt%, repeatedly washing to be neutral by deionized water, drying, crushing and grinding to obtain activated nano activated carbon;
5) Dispersing activated nano activated carbon in deionized water to obtain a dispersion liquid with the concentration of 3wt%, then placing the composite porous carbon fiber in a vacuum impregnator, vacuumizing to 50Pa, maintaining for 5min, then injecting a sufficient amount of dispersion liquid, vacuumizing to 10Pa, continuously maintaining for 20min, slowly releasing pressure to normal pressure, repeating the operation for 2 times, and drying after centrifugal separation to obtain the composite fiber material.
Example 2
The filter element is cylindrical and sequentially comprises an inner fine filter fiber layer, an adsorptive fiber layer, a middle fine filter fiber layer, a framework fiber layer and an outer coarse filter fiber layer from inside to outside in the radial direction, wherein the filter pore diameter of each of the inner fine filter fiber layer, the middle fine filter fiber layer and the outer coarse filter fiber layer gradually increases from inside to outside in the radial direction;
wherein the inner fine filter fiber layer is formed by interweaving a composite fiber material and polytetrafluoroethylene fibers;
the composite fiber material is prepared by taking porous carbon fiber as a matrix, loading nano rods after hydrothermal reaction to obtain composite porous carbon fiber, activating nano activated carbon and then penetrating the activated nano activated carbon into gaps of the composite porous carbon fiber in a vacuum impregnation mode;
the preparation method of the filter element specifically comprises the following steps:
winding the composite fiber material and polytetrafluoroethylene fiber into a cylindrical inner fine filtration fiber layer by alternating hot melt spinning, winding an adsorptive fiber layer on the inner fine filtration fiber layer, winding a middle fine filtration fiber layer on the adsorptive fiber layer, winding a skeleton fiber layer on the middle fine filtration fiber layer, and winding an outer coarse filtration fiber layer on the skeleton fiber layer.
The preparation method of the composite fiber material comprises the following steps:
1) Sequentially adding polyacrylonitrile powder and dimethyl sulfoxide into a container, uniformly stirring at 63 ℃ to prepare a solution with the solid content of 23wt%, then adding potassium carbonate into the solution and continuously stirring for 7 hours, wherein the adding amount of the potassium carbonate is 3% of the mass of the polyacrylonitrile, uniformly mixing to obtain a spinning solution, extruding the spinning solution into a potassium carbonate aqueous solution with the concentration of 3wt% at 56 ℃ under the pressure of 0.5MPa for solidification, and placing the solidified fiber into a 65 ℃ vacuum drying oven for drying for 48 hours to obtain polypropylene fiber;
2) Placing polypropylene fibers in an oven, respectively treating for 15min and 40min at 185 ℃ and 235 ℃, then moving the polypropylene fibers into a crucible, treating for 2h at 830 ℃ under the nitrogen atmosphere, naturally cooling to room temperature after the treatment is finished, repeatedly cleaning with hydrochloric acid solution, and drying to obtain porous carbon fibers;
3) Dissolving 0.7g of polyvinylpyrrolidone in 7mL of 1-amyl alcohol, adding 150 mu L of sodium citrate solution with the concentration of 0.4mol/L, fully stirring and dissolving, sequentially adding 10mL of deionized water, 8mL of concentrated hydrochloric acid with the concentration of 13mol/L and 260 mu L of tetrabutyl titanate, fully stirring and dissolving to obtain a titanium dioxide source solution, immersing porous carbon fibers in the titanium dioxide source solution, controlling the adding amount of the porous carbon fibers to be 5% of the total mass of the titanium dioxide source solution, transferring the porous carbon fibers into a reaction kettle, performing hydrothermal reaction for 20h at 110 ℃ after sealing, repeatedly washing a product by using deionized water and absolute ethyl alcohol after the reaction is finished, and drying by using nitrogen to obtain the composite porous carbon fibers;
4) Drying high-carbon ash at 110 ℃ for 3 hours, superfine grinding into fine powder, uniformly mixing with potassium hydroxide with equal mass, transferring into a reactor, heating to 1250 ℃ at a speed of 15 ℃/min under nitrogen atmosphere, preserving heat for 2 hours, cooling to room temperature after treatment is finished, pickling with hydrochloric acid solution with the concentration of 12wt%, repeatedly washing to be neutral by deionized water, drying, crushing and grinding to obtain activated nano activated carbon;
5) Dispersing activated nano activated carbon in deionized water to obtain a dispersion liquid with the concentration of 5wt%, then placing the composite porous carbon fiber in a vacuum impregnator, vacuumizing to 70Pa, maintaining for 7min, then injecting a sufficient amount of dispersion liquid, vacuumizing to 20Pa, continuously maintaining for 30min, slowly releasing pressure to normal pressure, repeating the operation for 3 times, and drying after centrifugal separation to obtain the composite fiber material.
Example 3
The filter element is cylindrical and sequentially comprises an inner fine filter fiber layer, an adsorptive fiber layer, a middle fine filter fiber layer, a framework fiber layer and an outer coarse filter fiber layer from inside to outside in the radial direction, wherein the filter pore diameter of each of the inner fine filter fiber layer, the middle fine filter fiber layer and the outer coarse filter fiber layer gradually increases from inside to outside in the radial direction;
wherein the inner fine filter fiber layer is formed by interweaving a composite fiber material and polytetrafluoroethylene fibers;
the composite fiber material is prepared by taking porous carbon fiber as a matrix, loading nano rods after hydrothermal reaction to obtain composite porous carbon fiber, activating nano activated carbon and then penetrating the activated nano activated carbon into gaps of the composite porous carbon fiber in a vacuum impregnation mode;
the preparation method of the filter element specifically comprises the following steps:
winding the composite fiber material and polytetrafluoroethylene fiber into a cylindrical inner fine filtration fiber layer by alternating hot melt spinning, winding an adsorptive fiber layer on the inner fine filtration fiber layer, winding a middle fine filtration fiber layer on the adsorptive fiber layer, winding a skeleton fiber layer on the middle fine filtration fiber layer, and winding an outer coarse filtration fiber layer on the skeleton fiber layer.
The preparation method of the composite fiber material comprises the following steps:
1) Sequentially adding polyacrylonitrile powder and dimethyl sulfoxide into a container, uniformly stirring at 65 ℃ to prepare a solution with the solid content of 25wt%, then adding potassium carbonate into the solution and continuously stirring for 10 hours, wherein the adding amount of the potassium carbonate is 5% of the mass of the polyacrylonitrile, uniformly mixing to obtain a spinning solution, extruding the spinning solution into a potassium carbonate aqueous solution with the concentration of 5wt% at 58 ℃ under the pressure of 0.8MPa for solidification, and placing the solidified fiber into a vacuum drying oven at 70 ℃ for drying for 50 hours to obtain polypropylene fiber;
2) Placing polypropylene fibers in an oven, respectively treating at 190 ℃ and 240 ℃ for 20min and 50min, then moving the polypropylene fibers into a crucible, treating at 850 ℃ for 3h under nitrogen atmosphere, naturally cooling to room temperature after the treatment is finished, repeatedly cleaning with hydrochloric acid solution, and drying to obtain porous carbon fibers;
3) Dissolving 1.0g of polyvinylpyrrolidone in 10mL of 1-amyl alcohol, adding 200 mu L of sodium citrate solution with the concentration of 0.5mol/L, fully stirring and dissolving, sequentially adding 13mL of deionized water, 10mL of concentrated hydrochloric acid with the concentration of 14mol/L and 300 mu L of tetrabutyl titanate, fully stirring and dissolving to obtain a titanium dioxide source solution, immersing porous carbon fibers in the titanium dioxide source solution, controlling the adding amount of the porous carbon fibers to be 8% of the total mass of the titanium dioxide source solution, transferring the porous carbon fibers into a reaction kettle, performing hydrothermal reaction at 120 ℃ for 25 hours after sealing, repeatedly washing a product by using deionized water and absolute ethyl alcohol after the reaction is finished, and drying by using nitrogen to obtain the composite porous carbon fibers;
4) Drying high-carbon ash at 115 ℃ for 5 hours, superfine grinding into fine powder, uniformly mixing with potassium hydroxide with equal mass, transferring into a reactor, heating to 1300 ℃ at a speed of 20 ℃/min under nitrogen atmosphere, preserving heat for 3 hours, cooling to room temperature after treatment is finished, pickling with hydrochloric acid solution with the concentration of 13wt%, repeatedly washing to be neutral by deionized water, drying, crushing and grinding to obtain activated nano activated carbon;
5) Dispersing activated nano activated carbon in deionized water to obtain a dispersion liquid with the concentration of 8wt%, then placing the composite porous carbon fiber in a vacuum impregnator, vacuumizing to 100Pa, maintaining for 10min, then injecting a sufficient amount of dispersion liquid, vacuumizing to 30Pa, continuously maintaining for 40min, slowly releasing pressure to normal pressure, repeating the operation for 5 times, and drying after centrifugal separation to obtain the composite fiber material.
Comparative example 1: this comparative example is substantially the same as example 1 except that the inner fine filter fiber layer does not contain a composite fiber material.
Comparative example 2: this comparative example is essentially the same as example 1, except that in the preparation of the composite fiber material, the potassium carbonate in step 1) is omitted.
Comparative example 3: this comparative example is essentially the same as example 1, except that step 2) is omitted in the preparation of the composite fibrous material.
Comparative example 4: this comparative example is essentially the same as example 1, except that step 3) is omitted in the preparation of the composite fibrous material.
Comparative example 5: this comparative example is substantially the same as example 1, except that step 4) is omitted in the preparation of the composite fiber material, and the activated nano-activated carbon is replaced with nano-sized activated carbon.
Test experiment:
the composite fiber material samples provided in examples 1 to 3 and comparative examples 1 to 5 were respectively used, and were interwoven with polytetrafluoroethylene fibers to form an inner fine filter fiber layer, and then the initial stain resistance and the stain resistance after 50 times of washing were measured according to the standard AATCC130:2010 "method for testing soil release Property of textiles", and the test results are shown in Table 1.
TABLE 1
As is clear from Table 1, the inner fine filter fiber layer of the present invention has excellent stain resistance, and the filter element manufactured by the process has high-efficiency filtering effect and long service life.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.

Claims (10)

1. The filter element is characterized by comprising an inner fine filter fiber layer, an adsorptive fiber layer, a middle fine filter fiber layer, a framework fiber layer and an outer coarse filter fiber layer in sequence from inside to outside in the radial direction, wherein the filter pore diameter of each of the inner fine filter fiber layer, the middle fine filter fiber layer and the outer coarse filter fiber layer is gradually increased from inside to outside in the radial direction;
the inner fine filtration fiber layer is formed by interweaving a composite fiber material and polytetrafluoroethylene fibers;
the composite fiber material is prepared by taking porous carbon fiber as a matrix, loading nano rods after hydrothermal reaction to obtain composite porous carbon fiber, activating nano activated carbon and then penetrating the activated nano activated carbon into gaps of the composite porous carbon fiber in a vacuum impregnation mode.
2. The filter element of claim 1, wherein the adsorbent fiber layer is comprised of carbon fibers or plant fibers;
the middle fine filter fiber layer and the outer coarse filter fiber layer are formed by polyester fibers or nylon fibers;
the skeleton fiber layer is composed of glass fibers or polyethylene fibers.
3. The filter element made of high-efficiency and pollution-resistant materials as claimed in claim 1, wherein the framework fiber layer and the outer rough filtration fiber layer are embedded with an active agent, and the active agent is ion exchange resin particles and zeolite particles according to the weight ratio of 1: the ion exchange resin particles are prepared by mixing the dosage proportion of (1-2), wherein the weight ratio of the anion exchange resin particles to the cation exchange resin particles is 1: and (2-4) in proportion.
4. The efficient pollution-resistant filter element according to claim 1, wherein the preparation method of the composite porous carbon fiber is as follows:
1) Sequentially adding polyacrylonitrile powder and dimethyl sulfoxide into a container, uniformly stirring at 60-65 ℃ to prepare a solution, then adding potassium carbonate into the solution, continuously stirring for 5-10h, uniformly mixing to obtain a spinning solution, extruding the spinning solution into a potassium carbonate aqueous solution at 55-58 ℃ under the pressure of 0.3-0.8MPa for solidification, and drying the solidified fiber in a vacuum drying oven at 60-70 ℃ for 45-50h to obtain polypropylene fiber;
2) Placing polypropylene fibers in an oven, respectively treating at 180-190 ℃ and 230-240 ℃ for 10-20min and 30-50min, then transferring into a crucible, treating at 800-850 ℃ for 1-3h under nitrogen atmosphere, naturally cooling to room temperature after the treatment is finished, repeatedly cleaning with hydrochloric acid solution, and drying to obtain porous carbon fibers;
3) Dissolving polyvinylpyrrolidone in 1-amyl alcohol, adding sodium citrate solution, fully stirring and dissolving, sequentially adding deionized water, concentrated hydrochloric acid and tetrabutyl titanate, fully stirring and dissolving to obtain titanium dioxide source solution, immersing porous carbon fiber in the titanium dioxide source solution, transferring the porous carbon fiber into a reaction kettle, sealing, carrying out hydrothermal reaction at 90-120 ℃ for 15-25h, repeatedly washing the product with deionized water and absolute ethyl alcohol after the reaction is finished, and drying with nitrogen to obtain the composite porous carbon fiber.
5. The filter element of claim 4, wherein in step 1), the solid content of the solution is 20-25wt%;
the addition amount of the potassium carbonate is 1-5% of the mass of the polyacrylonitrile;
the concentration of the potassium carbonate aqueous solution is 1-5wt%.
6. The filter element of claim 4, wherein in step 2), the flow rate of the nitrogen gas is 1.0-1.6L/min.
7. The filter element made of high-efficiency and pollution-resistant materials according to claim 4, wherein in the step 3), the dosage ratio of polyvinylpyrrolidone, 1-amyl alcohol, sodium citrate solution, deionized water, concentrated hydrochloric acid and tetrabutyl titanate is (0.5-1.0) g: (5-10) mL: (100-200) μl: (5-13) mL: (5-10) mL: (200-300) μL;
the concentration of the sodium citrate solution is 0.3-0.5mol/L;
the concentration of the concentrated hydrochloric acid is 12-14mol/L;
the addition amount of the porous carbon fiber is 3-8% of the total mass of the titanium dioxide source solution.
8. The efficient dirt-resistant filter element according to claim 1, wherein the preparation method of the composite fiber material is as follows:
1) Drying high-carbon ash at 105-115 ℃ for 2-5 hours, grinding into fine powder by superfine grinding, uniformly mixing with potassium hydroxide with equal mass, transferring into a reactor, heating to 1200-1300 ℃ under nitrogen atmosphere, preserving heat for 1-3 hours, cooling to room temperature after treatment is finished, pickling with hydrochloric acid solution with the concentration of 10-13wt%, repeatedly washing to neutrality by deionized water, drying, crushing and grinding to obtain activated nano active carbon;
2) Dispersing activated nano activated carbon in deionized water to obtain dispersion liquid, then placing the composite porous carbon fiber in a vacuum impregnator, vacuumizing to 50-100Pa, maintaining for 5-10min, then injecting sufficient dispersion liquid, vacuumizing to 10-30Pa, continuously maintaining for 20-40min, slowly releasing pressure to normal pressure, repeating the operation for 2-5 times, centrifuging and drying to obtain the composite fiber material.
9. The filter element made of high-efficiency pollution-resistant materials according to claim 8, wherein the temperature rising rate is 10-20 ℃/min under the nitrogen atmosphere;
the concentration of the dispersion is 3-8wt%.
10. The method for preparing the filter element made of the efficient stain-resistant material according to any one of claims 1 to 9, which is characterized by comprising the following steps:
winding the composite fiber material and polytetrafluoroethylene fiber into a cylindrical inner fine filtration fiber layer by alternating hot melt spinning, winding an adsorptive fiber layer on the inner fine filtration fiber layer, winding a middle fine filtration fiber layer on the adsorptive fiber layer, winding a skeleton fiber layer on the middle fine filtration fiber layer, and winding an outer coarse filtration fiber layer on the skeleton fiber layer.
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CN107999052A (en) * 2017-11-09 2018-05-08 马鞍山市心洲葡萄专业合作社 A kind of preparation method of photocatalytic degradation composite material
CN108607509A (en) * 2018-05-05 2018-10-02 安徽乐金环境科技有限公司 A kind of porous graphite alkenyl air purifying preparation
CN108691027A (en) * 2018-05-05 2018-10-23 安徽乐金环境科技有限公司 A kind of porous graphite alkenyl air purifying filter core and preparation method thereof
CN109244405A (en) * 2018-09-12 2019-01-18 肇庆市华师大光电产业研究院 A kind of lithium sulfur battery anode material and its lithium-sulfur cell

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CN107051419A (en) * 2017-05-10 2017-08-18 上海师范大学 A kind of super long titanium dioxide nano wire/three-dimensional porous composite of NACF and preparation method and application
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