CN114934355A - Preparation method of high-flux PP melt-blown nano-microporous folded liquid filter material - Google Patents
Preparation method of high-flux PP melt-blown nano-microporous folded liquid filter material Download PDFInfo
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- CN114934355A CN114934355A CN202210498270.4A CN202210498270A CN114934355A CN 114934355 A CN114934355 A CN 114934355A CN 202210498270 A CN202210498270 A CN 202210498270A CN 114934355 A CN114934355 A CN 114934355A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
- D04H1/544—Olefin series
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/08—Filter cloth, i.e. woven, knitted or interlaced material
- B01D39/083—Filter cloth, i.e. woven, knitted or interlaced material of organic material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/56—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C15/00—Calendering, pressing, ironing, glossing or glazing textile fabrics
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/02—Types of fibres, filaments or particles, self-supporting or supported materials
- B01D2239/0208—Single-component fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0622—Melt-blown
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Filtering Materials (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a preparation method of a high-flux PP melt-blown nano-micropore folding liquid filter material, which belongs to the technical field of liquid filter materials and comprises the steps of preparing a mixture, spinning, hot air blowing, forming a net, performing surface treatment and calendaring; the preparation method comprises the steps of preparing a mixture, namely uniformly mixing polypropylene resin, high-surface-energy particles and induced nanoparticles to obtain a mixture; wherein, the mass ratio of the polypropylene resin, the high surface energy particles and the induced nanoparticles is 100-110:5-8: 3-5; the invention can improve the folding forming stability, the dirt holding capacity and the service life of the liquid filtering material, and simultaneously improve the filtering efficiency of 1-2 mu m particles.
Description
Technical Field
The invention relates to the technical field of liquid filter materials, in particular to a preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material.
Background
The liquid filtering material makes a great contribution to solving the global health, environment, food, drinking water, national safety and other problems, and particularly, the non-woven liquid filtering material based on the melt-blown superfine fiber as the main body structure has obvious structural advantages and excellent application prospects compared with other filtering materials due to the small pore size and the uniform and isotropic porous structure. However, as China is relatively beautiful in scientific research and industrial layout, and is started late in developed countries such as the day, the produced liquid filter material has great difference from foreign imported products in the aspects of technical indexes such as filtration efficiency, performance stability, service life and the like, particularly in the field of preparation of high-precision microporous folding nonwoven filter materials and submicron pore folding filter membranes, the filter material processing technology is monopolized by international companies, the filter material is expensive, is easy to be restricted by people in a key period, and brings great hidden danger to the strategic safety of China.
In the field of large-flux microporous non-woven liquid filter materials, the main performance of domestic products is close to that of imported products. For example, the new filter material developed by the U.S. Finetex technology company using nanofibers is a composite structure product using electrospun nanofiber web and traditional nonwoven fabrics, the Coats TM series of Finetex technology company is used for liquid filtration, and can effectively remove 1-2 μm particles, and the nanoporous nonwoven membrane material produced by the company and the Roki company in cooperation has also been applied to the field of liquid material separation. The Tianjin tada in China is earlier researched in the field, products of 5-10 mu m are industrialized at present, and the materials of 1-2 mu m have the problems of poor folding forming stability, low filtration efficiency and pollutant carrying capacity and short service life. More importantly, in the field of preparation of high-precision microporous folded nonwoven filter materials and submicron-pore folded filter membranes, filter material processing techniques have been monopolized by international and international companies, such as 3M company, coddebo, ostone and the like, which are expensive and easily controlled by people in a critical period. Particularly, with the increasing friction of trade in China and America in recent years, foreign high-technology high-value products stop exporting or tighten exporting in China, and great hidden danger is brought to strategic safety in China.
Therefore, the development of a preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material is a technical problem which needs to be solved urgently at present, and the preparation method can improve the folding forming stability, the dirt holding capacity and the service life of the liquid filter material and improve the filtering efficiency of 1-2 mu m particles.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the high-flux PP melt-blown nano-microporous folded liquid filter material, which can improve the folding forming stability, the dirt holding capacity and the service life of the liquid filter material and improve the filtering efficiency of 1-2 mu m particles.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material comprises the steps of preparing a mixture, carrying out spinning, carrying out hot air blowing, forming a net, carrying out surface treatment and calendaring.
The preparation method comprises the steps of preparing a mixture, namely uniformly mixing polypropylene resin, high-surface-energy particles and induced nanoparticles to obtain a mixture;
wherein, the mass ratio of the polypropylene resin, the high surface energy particles and the induced nanoparticles is 100-110:5-8: 3-5;
the melt index of the polypropylene resin is 100-120g/10 min;
the preparation method of the high surface energy particle comprises the following steps: setting the temperature of a reaction kettle to be 2-5 ℃, adding acrylic acid, maleic anhydride, nano aluminum oxide, titanate coupling agent TMC-TTS, Tween 80 and deionized water into the reaction kettle, starting stirring, controlling the stirring speed to be 250-plus-one (300 rpm), then heating at the heating speed of 1.2-1.5 ℃/min, heating to 65-70 ℃, stirring at 65-70 ℃ for 30-40min, adding sodium persulfate and isopropanol, stirring at 65-70 ℃ for 20-30min, raising the temperature of the reaction kettle to 75-80 ℃, adding sodium hydroxide and sodium dodecyl sulfate, stirring at 75-80 ℃ for 35-40min, stopping stirring, naturally returning to room temperature, filtering to obtain primary particles, placing the primary particles at 40-45 ℃ for 2.5-3h, then placing the primary particles in liquid carbon dioxide at-70 ℃ to-65 ℃ to treat 15-plus-one Taking out after 20min to obtain high surface energy particles;
wherein the weight ratio of acrylic acid, maleic anhydride, nano-alumina, titanate coupling agent TMC-TTS, Tween 80, deionized water, sodium persulfate, isopropanol, sodium hydroxide and sodium dodecyl sulfate is 100: 110:10-12:13-15:1-2:2-3: 280: 300:0.1-0.3:2-3:1-2: 1-1.5;
the weight ratio of the primary particles to the liquid carbon dioxide is 1: 1.3-1.5;
the preparation method of the induced nanoparticles comprises the following steps: soaking nano silicon dioxide into a surface active agent at 45-50 ℃, standing for 20-30min at 45-50 ℃ to obtain nano particle liquid after surface activation, placing the nano particle liquid after surface activation into a closed container for pressurization treatment, controlling the pressure of the closed container to be 1-1.2MPa, controlling the temperature to be 150-160 ℃, performing pressurization treatment in the closed container for 30-40min, filtering, and placing filter residues into 50-60 ℃ for drying for 3-3.5h to obtain induced nano particles;
the particle size of the nano silicon dioxide is 300-350 nm;
the surface active agent comprises the following components in parts by weight: 100 portions of deionized water, 110 portions of stearic acid, 5 to 7 portions of xanthan gum, 1 to 3 portions of sodium thiosulfate and 0.3 to 0.5 portion of betaine;
the weight ratio of the nano silicon dioxide to the surface active agent is 1: 1.3-1.5.
The spinning comprises the steps of adding the mixture into a double-screw extruder through a metering pump, controlling the temperature of the double-screw extruder to be 230-240 ℃, sending the molten mixture into a spinneret plate after the molten mixture is extruded through the metering pump and a filter, controlling the temperature of a die head of the spinneret plate to be 260-270 ℃, and extruding primary polymer filaments;
the rotating speed of the metering pump is 14-15 rpm.
The hot air blowing is carried out, the primary polymer filaments are subjected to hot air blowing, and the polymer filaments are thinned and elongated under the impact of high-speed hot air flows at two sides to obtain the hot air-blown polymer filaments;
the flow rate of the high-speed hot air flow is 680-730m 3 The hot air temperature is 270-280 ℃.
After high-pressure blowing, spraying the polymer filaments subjected to hot air blowing to a web forming curtain to form a web, and performing air suction, cooling and solidification to obtain a liquid filtering base material;
the air suction flow is 2400-2500m 3 The net forming speed is 9-10 m/min.
And the surface treatment comprises the step of irradiating the liquid filtering base material with ultraviolet rays, wherein the wavelength of the ultraviolet rays is controlled to be 260-300nm, the time of the ultraviolet rays is 35-40min, the temperature during the ultraviolet rays is 45-50 ℃, and the base cloth is obtained after the ultraviolet rays are irradiated.
And in the step of calendering, calendering is carried out after 2-3 layers of base fabrics are overlapped, the calendering speed is controlled to be 5.5-6.5m/min, the calendering temperature is 90-95 ℃, the calendering pressure is 2.0-2.5MPa, and the microporous liquid filtering material is obtained after calendering is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the high-flux PP melt-blown nano-microporous folding liquid filter material can improve the hydrostatic pressure, longitudinal stiffness, transverse stiffness, air permeability and dirt holding capacity of the liquid filter material, and the gram weight of the liquid filter material prepared by the invention is 80-90g/m 2 The average pore diameter is 1.0-2.0 μm, the thickness is 0.19-0.20mm, the hydrostatic pressure is 159-164cmH 2 O, the longitudinal stiffness is 94-98N, the transverse stiffness is 52-58N, the fiber fineness is 1.8-2.2 mu m,the air permeability is 1.5-2.5mm/s, and the dirt holding capacity is 79-85g/m 2 ；
(2) The preparation method of the high-flux PP melt-blown nano-microporous folded liquid filter material can improve the pure water flux of the liquid filter material and the filtering efficiency of the liquid filter material on particles with the particle size of 1-2 mu m, and the pure water flux of the liquid filter material prepared by the invention is 5450-5550 L.m -2 •h -1 The filtration efficiency of particles with a particle size of 1-2 μm is 95.5-96.2%, and the pure water flux after 24h treatment at 70 ℃ is 5350-5500 L.m -2 •h -1 The filtration efficiency of particles with the particle size of 1-2 mu m after being treated for 24 hours at 70 ℃ is 94.2-95.1 percent;
(3) the preparation method of the high-flux PP melt-blown nano-microporous folding liquid filter material can improve the folding forming stability of the liquid filter material, and the pure water flux of the folding filter element prepared from the liquid filter material is 5400-5550 L.m -2 •h -1 The filtration efficiency of particles with the particle size of 1-2 μm is 95.1-95.7%, and the pure water flux after 24h treatment at 70 ℃ is 5300-5400 L.m -2 •h -1 The filtration efficiency of particles with a particle size of 1-2 μm after treatment at 70 ℃ for 24h is 94.0-94.9%, and the pure water flux after normal use for 6 months is 5200-5300 L.m -2 •h -1 The filtration efficiency of the particles with the particle size of 1-2 mu m after being normally used for 6 months is 92.9-93.8 percent;
(4) the high-flux PP melt-blown nano-microporous folded liquid filter material prepared by the invention has the advantages that the surface layer fibers are arranged and oriented tidily, the fiber uniformity is good, and the relationship among the filtering precision, the flux and the dirt holding capacity is balanced through the accurate regulation and control of the pressure and the temperature during the rolling.
Drawings
FIG. 1 shows a gram weight of 40g/m prepared in example 1 2 Scanning electron microscope pictures of the base fabric;
FIG. 2 shows a gram weight of 45g/m prepared in example 2 2 Scanning electron microscope images of the base fabric.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material comprises the following specific steps:
1. preparing a mixture: uniformly mixing polypropylene resin, high-surface-energy particles and induced nanoparticles to obtain a mixture;
wherein the mass ratio of the polypropylene resin, the high surface energy particles and the induced nanoparticles is 100:5: 3;
the melt index of the polypropylene resin is 100g/10 min;
the preparation method of the high surface energy particle comprises the following steps: setting the temperature of a reaction kettle to be 2 ℃, adding acrylic acid, maleic anhydride, nano-alumina, titanate coupling agent TMC-TTS, Tween 80 and deionized water into the reaction kettle, starting stirring, controlling the stirring speed to be 250rpm, heating at the heating speed of 1.2 ℃/min, stirring at 65 ℃ for 30min, adding sodium persulfate and isopropanol, stirring at 65 ℃ for 20min, raising the temperature of the reaction kettle to 75 ℃, adding sodium hydroxide and sodium dodecyl sulfate, stirring at 75 ℃ for 35min, stopping stirring, naturally returning to room temperature, filtering to obtain primary particles, drying the primary particles at 40 ℃ for 2.5h, placing the primary particles in liquid carbon dioxide at-70 ℃ for processing for 15min, and taking out to obtain high-surface-energy particles;
wherein the weight ratio of acrylic acid, maleic anhydride, nano alumina, titanate coupling agent TMC-TTS, tween 80, deionized water, sodium persulfate, isopropanol, sodium hydroxide and sodium dodecyl sulfate is 100:10:13:1:2:280:0.1:2:1: 1;
the weight ratio of the primary particles to the liquid carbon dioxide is 1: 1.3;
the preparation method of the induced nanoparticles comprises the following steps: soaking nano silicon dioxide into a surfactant at 45 ℃, standing for 20min at 45 ℃ to obtain nano particle liquid after surface activation, placing the nano particle liquid after surface activation into a closed container for pressurization treatment, controlling the pressure of the closed container to be 1MPa and the temperature to be 150 ℃, pressurizing in the closed container for 30min, filtering, and placing filter residues at 50 ℃ for drying for 3h to obtain induced nano particles;
the particle size of the nano silicon dioxide is 300 nm;
the surface active agent comprises the following components in parts by weight: 100 parts of deionized water, 5 parts of stearic acid, 2 parts of xanthan gum, 1 part of sodium thiosulfate and 0.3 part of betaine;
the weight ratio of the nano silicon dioxide to the surface active agent is 1: 1.3.
2. Spinning: adding the mixture into a double-screw extruder through a metering pump, controlling the temperature of the double-screw extruder to be 230 ℃, after extrusion, feeding the molten mixture into a spinneret plate through the metering pump and a filter, controlling the temperature of a die head of the spinneret plate to be 260 ℃, and extruding primary polymer filaments;
the metering pump speed was 14 rpm.
3. Hot air blowing: carrying out hot air blowing on the primary polymer filaments, and thinning and extending the polymer filaments under the impact of high-speed hot air flows at two sides to obtain hot air blown polymer filaments;
the flow rate of the high-speed hot air flow is 680m 3 The hot air temperature is 270 ℃.
4. Forming a net: after high-pressure blowing, spraying the polymer filaments subjected to hot air blowing to a web forming curtain for web forming, and performing air suction, cooling and curing to obtain a liquid filtering base material;
the air suction flow is 2400m 3 The web forming speed is 9 m/min.
5. Surface treatment: irradiating the liquid filtering base material with ultraviolet ray with wavelength of 260nm for 35min at 45 deg.C to obtain base cloth with gram weight of 40g/m 2 And performing electron microscope scanning analysis on the base fabric, wherein the analysis result is shown in figure 1, and as can be seen from figure 1, the prepared base fabric has the advantages that the surface fibers are arranged and oriented neatly and the uniformity of the fibers is good.
6. And (3) calendering: and (3) superposing the 2 layers of base cloth prepared in the step 5, then calendering, controlling the calendering speed to be 5.5m/min, the calendering temperature to be 90 ℃, and the calendering pressure to be 2.5MPa, and obtaining the microporous liquid filtering material after calendering.
Example 2
A preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material comprises the following specific steps:
1. preparing a mixture: uniformly mixing polypropylene resin, high-surface-energy particles and induced nanoparticles to obtain a mixture;
wherein the mass ratio of the polypropylene resin, the high surface energy particles and the induced nanoparticles is 105:7: 4;
the melt index of the polypropylene resin is 110g/10 min;
the preparation method of the high surface energy particle comprises the following steps: setting the temperature of a reaction kettle to be 3 ℃, adding acrylic acid, maleic anhydride, nano-alumina, titanate coupling agent TMC-TTS, Tween 80 and deionized water into the reaction kettle, starting stirring, controlling the stirring speed to be 270rpm, heating at the heating speed of 1.3 ℃/min, stirring at 67 ℃ for 35min, adding sodium persulfate and isopropanol, stirring at 67 ℃ for 25min, raising the temperature of the reaction kettle to 77 ℃, adding sodium hydroxide and sodium dodecyl sulfate, stirring at 77 ℃ for 37min, stopping stirring, naturally returning to room temperature, filtering to obtain primary particles, drying the primary particles at 42 ℃ for 2.7h, placing the primary particles in liquid carbon dioxide at-67 ℃ for treatment for 17min, and taking out to obtain high-surface-energy particles;
wherein, the weight ratio of acrylic acid, maleic anhydride, nano alumina, titanate coupling agent TMC-TTS, Tween 80, deionized water, sodium persulfate, isopropanol, sodium hydroxide and sodium dodecyl sulfate is 105:11:14:1.5:2.5:290:0.2:2.5:1.5: 1.2;
the weight ratio of the primary particles to the liquid carbon dioxide is 1: 1.4;
the preparation method of the induced nanoparticles comprises the following steps: soaking nano silicon dioxide into a surfactant at 47 ℃, standing for 25min at 47 ℃ to obtain nano particle liquid after surface activation, putting the nano particle liquid after surface activation into a closed container for pressurization treatment, controlling the pressure of the closed container to be 1.1MPa, controlling the temperature to be 155 ℃, carrying out pressurization treatment in the closed container for 35min, filtering, and drying filter residues at 55 ℃ for 3.2h to obtain induced nano particles;
the particle size of the nano silicon dioxide is 320 nm;
the surface active agent comprises the following components in parts by weight: 105 parts of deionized water, 6 parts of stearic acid, 2.5 parts of xanthan gum, 2 parts of sodium thiosulfate and 0.4 part of betaine;
the weight ratio of the nano silicon dioxide to the surface active agent is 1: 1.4.
2. Spinning: adding the mixture into a double-screw extruder through a metering pump, controlling the temperature of the double-screw extruder to be 235 ℃, after extrusion, feeding the molten mixture into a spinneret plate through the metering pump and a filter, controlling the temperature of a die head of the spinneret plate to be 265 ℃, and extruding primary polymer filaments;
the rotational speed of the metering pump is 14.5 rpm.
3. Hot air blowing: carrying out hot air blowing on the primary polymer filaments, and thinning and extending the polymer filaments under the impact of high-speed hot air flows at two sides to obtain hot air blown polymer filaments;
the flow rate of the high-speed hot air flow is 700m 3 The hot air temperature is 275 ℃.
4. Forming a net: after high-pressure blowing, spraying the polymer filaments blown by hot air to a web forming curtain for web forming, sucking, cooling and curing to obtain a liquid filtering base material;
the induced draft flow is 2450m 3 The web forming speed is 9.5 m/min.
5. Surface treatment: irradiating the liquid filter substrate with ultraviolet rays at wavelength of 280nm for 37min at 47 deg.C to obtain base cloth with gram weight of 45g/m 2 And performing electron microscope scanning analysis on the base fabric, wherein the analysis result is shown in fig. 2, and as can be seen from fig. 2, the prepared base fabric has the advantages of regular surface fiber arrangement and orientation and good fiber uniformity.
6. And (3) calendering: and (3) laminating the 2 layers of base cloth prepared in the step 5, then calendering, controlling the calendering speed to be 6m/min, the calendering temperature to be 92 ℃, and the calendering pressure to be 2.3MPa, and obtaining the microporous liquid filtering material after calendering.
Example 3
A preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material comprises the following specific steps:
1. preparing a mixture: uniformly mixing polypropylene resin, high-surface-energy particles and induced nanoparticles to obtain a mixture;
wherein the mass ratio of the polypropylene resin, the high surface energy particles and the induced nanoparticles is 110:8: 5;
the melt index of the polypropylene resin is 120g/10 min;
the preparation method of the high surface energy particle comprises the following steps: setting the temperature of a reaction kettle to be 5 ℃, adding acrylic acid, maleic anhydride, nano-alumina, titanate coupling agent TMC-TTS, Tween 80 and deionized water into the reaction kettle, starting stirring, controlling the stirring speed to be 300rpm, heating at the heating speed of 1.5 ℃/min, stirring at 70 ℃ for 40min, adding sodium persulfate and isopropanol, stirring at 70 ℃ for 30min, raising the temperature of the reaction kettle to 80 ℃, adding sodium hydroxide and sodium dodecyl sulfate, stirring at 80 ℃ for 40min, stopping stirring, naturally returning to room temperature, filtering to obtain primary particles, drying the primary particles at 45 ℃ for 3h, treating the primary particles in liquid carbon dioxide at-65 ℃ for 20min, and taking out to obtain high-surface-energy particles;
wherein the weight ratio of acrylic acid, maleic anhydride, nano alumina, titanate coupling agent TMC-TTS, tween 80, deionized water, sodium persulfate, isopropanol, sodium hydroxide and sodium dodecyl sulfate is 110:12:15:2:3:300:0.3:3:2: 1.5;
the weight ratio of the primary particles to the liquid carbon dioxide is 1: 1.5;
the preparation method of the induced nanoparticles comprises the following steps: soaking nano silicon dioxide into a surfactant at 50 ℃, standing for 30min at 50 ℃ to obtain nano particle liquid after surface activation, putting the nano particle liquid after surface activation into a closed container for pressurization treatment, controlling the pressure of the closed container to be 1.2MPa, controlling the temperature to be 160 ℃, carrying out pressurization treatment in the closed container for 40min, filtering, and putting filter residues into a temperature of 60 ℃ for drying for 3.5h to obtain induced nano particles;
the particle size of the nano silicon dioxide is 350 nm;
the surface active agent comprises the following components in parts by weight: 110 parts of deionized water, 7 parts of stearic acid, 3 parts of xanthan gum, 3 parts of sodium thiosulfate and 0.5 part of betaine;
the weight ratio of the nano silicon dioxide to the surface active agent is 1: 1.5.
2. Spinning: adding the mixture into a double-screw extruder through a metering pump, controlling the temperature of the double-screw extruder to be 240 ℃, after extrusion, feeding the molten mixture into a spinneret plate through the metering pump and a filter, controlling the temperature of a die head of the spinneret plate to be 270 ℃, and extruding primary polymer filaments;
the rotating speed of the metering pump is 15 rpm.
3. Hot air blowing: carrying out hot air blowing on the primary polymer filaments, and thinning and extending the polymer filaments under the impact of high-speed hot air flows at two sides to obtain hot air blown polymer filaments;
the flow rate of the high-speed hot air flow is 730m 3 The hot air temperature is 280 ℃.
4. Forming a net: after high-pressure blowing, spraying the polymer filaments subjected to hot air blowing to a web forming curtain for web forming, and performing air suction, cooling and curing to obtain a liquid filtering base material;
the air suction flow is 2500m 3 The web forming speed is 10 m/min.
5. Surface treatment: irradiating the liquid filter substrate with ultraviolet rays at wavelength of 300nm for 40min at temperature of 50 deg.C to obtain base cloth with gram weight of 45g/m 2 。
6. And (3) calendering: and (3) laminating the 2 layers of base cloth prepared in the step 5, then calendering, controlling the calendering speed to be 6.5m/min, the calendering temperature to be 95 ℃, and the calendering pressure to be 2MPa, and obtaining the microporous liquid filtering material after calendering.
Comparative example 1
The preparation method of the high-flux PP melt-blown nano-microporous folded liquid filter material in the embodiment 1 is adopted, and the difference is that: in the step 1 of preparing the mixture, the addition of high surface energy particles is omitted.
Comparative example 2
The preparation method of the high-flux PP melt-blown nano-microporous folded liquid filter material in the embodiment 1 is adopted, and the difference is that: in the step 1 of preparing the mixture, the addition of the induced nanoparticles is omitted.
Comparative example 3
The preparation method of the high-flux PP melt-blown nano-microporous folded liquid filter material in the embodiment 1 is adopted, and the difference is that: the 5 th surface treatment is omitted.
The liquid filter materials prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for grammage, pore size, thickness, hydrostatic pressure, longitudinal stiffness, transverse stiffness, air permeability, and stain holding capacity, and the test results were as follows:
the pure water flux of the liquid filter materials prepared in examples 1 to 3 and comparative examples 1 to 3, the filtration efficiency of particles having a particle size of 1 to 2 μm, the pure water flux after treatment at 70 ℃ for 24 hours, and the filtration efficiency of particles having a particle size of 1 to 2 μm after treatment at 70 ℃ for 24 hours were tested, and the test results were as follows:
after the liquid filter materials prepared in examples 1 to 3 and comparative examples 1 to 3 were manufactured into a pleated filter element, the pure water flux of the pleated filter element, the filtration efficiency of particles having a particle size of 1 to 2 μm, the pure water flux after treatment at 70 ℃ for 24 hours, the filtration efficiency of particles having a particle size of 1 to 2 μm after treatment at 70 ℃ for 24 hours, the pure water flux after normal use for 6 months, and the filtration efficiency of particles having a particle size of 1 to 2 μm after normal use for 6 months were tested, and the test results were as follows:
all percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-flux PP melt-blown nano-microporous folded liquid filter material is characterized by comprising the steps of preparing a mixture, carrying out spinning, carrying out hot air blowing, forming a net, carrying out surface treatment and calendaring;
the preparation method comprises the steps of uniformly mixing the polypropylene resin, the high-surface-energy particles and the induced nanoparticles to obtain a mixture;
wherein the mass ratio of the polypropylene resin, the high surface energy particles and the induced nanoparticles is 100-110:5-8: 3-5.
2. The method for preparing high-throughput PP melt-blown nano-microporous folded liquid filter material according to claim 1, wherein the method for preparing the high-surface-energy particles comprises the following steps: setting the temperature of a reaction kettle to be 2-5 ℃, adding acrylic acid, maleic anhydride, nano aluminum oxide, titanate coupling agent TMC-TTS, Tween 80 and deionized water into the reaction kettle, starting stirring, controlling the stirring speed to be 250-plus-one (300 rpm), then heating at the heating speed of 1.2-1.5 ℃/min, heating to 65-70 ℃, stirring at 65-70 ℃ for 30-40min, adding sodium persulfate and isopropanol, stirring at 65-70 ℃ for 20-30min, raising the temperature of the reaction kettle to 75-80 ℃, adding sodium hydroxide and sodium dodecyl sulfate, stirring at 75-80 ℃ for 35-40min, stopping stirring, naturally returning to room temperature, filtering to obtain primary particles, placing the primary particles at 40-45 ℃ for 2.5-3h, then placing the primary particles in liquid carbon dioxide at-70 ℃ to-65 ℃ to treat 15-plus-one Taking out after 20min to obtain high surface energy particles.
3. The method for preparing the high-throughput PP melt-blown nano-microporous folded liquid filter material as claimed in claim 2, wherein the weight ratio of acrylic acid, maleic anhydride, nano-alumina, titanate coupling agent TMC-TTS, Tween 80, deionized water, sodium persulfate, isopropanol, sodium hydroxide and sodium dodecyl sulfate in the preparation of the high-surface-energy particles is 100-110:10-12:13-15:1-2:2-3:280-300:0.1-0.3:2-3:1-2: 1-1.5.
4. The method for preparing high-throughput PP melt-blown nano-microporous folded liquid filter material according to claim 2, wherein the weight ratio of the primary particles to liquid carbon dioxide in the preparation of the high-surface-energy particles is 1: 1.3-1.5.
5. The preparation method of the high-throughput PP melt-blown nano-microporous folded liquid filter material according to claim 1, wherein the preparation method of the induced nanoparticles comprises the following steps: soaking nano silicon dioxide into a surface active agent at 45-50 ℃, standing for 20-30min at 45-50 ℃ to obtain nano particle liquid after surface activation, placing the nano particle liquid after surface activation into a closed container for pressurization treatment, controlling the pressure of the closed container to be 1-1.2MPa, controlling the temperature to be 150-160 ℃, performing pressurization treatment in the closed container for 30-40min, filtering, and placing filter residues into 50-60 ℃ for drying for 3-3.5h to obtain induced nano particles.
6. The method for preparing high-throughput PP melt-blown nano-microporous folded liquid filter material according to claim 5, wherein the composition of the surfactant in the preparation of the induced nanoparticles comprises the following components in parts by weight: 100 portions of deionized water, 5 to 7 portions of stearic acid, 2 to 3 portions of xanthan gum, 1 to 3 portions of sodium thiosulfate and 0.3 to 0.5 portion of betaine.
7. The method for preparing high-throughput PP melt-blown nano-microporous folded liquid filter material according to claim 5, wherein the weight ratio of nano-silica to surfactant in the preparation of the induced nanoparticles is 1: 1.3-1.5.
8. The method for preparing high-throughput PP melt-blown nano-microporous pleated liquid filter material as claimed in claim 1, wherein the spinning comprises adding the mixture into a twin-screw extruder through a metering pump, controlling the temperature of the twin-screw extruder at 240 ℃, feeding the molten mixture into a spinneret plate after passing through the metering pump and a filter after the extrusion, controlling the die head temperature of the spinneret plate at 260-270 ℃, and extruding primary polymer filaments.
9. The preparation method of the high-throughput PP melt-blown nano-micro pore folded liquid filter material as claimed in claim 1, wherein the surface treatment comprises the steps of irradiating the liquid filter substrate with ultraviolet rays, controlling the wavelength of the ultraviolet rays to be 260-300nm, controlling the time of the ultraviolet rays to be 35-40min, controlling the temperature during the ultraviolet rays to be 45-50 ℃, and obtaining the base cloth after the ultraviolet rays are irradiated.
10. The preparation method of the high-throughput PP melt-blown nano-microporous folded liquid filter material as claimed in claim 1, wherein the calendering is performed after 2-3 layers of base fabrics are laminated, the calendering speed is controlled to be 5.5-6.5m/min, the calendering temperature is controlled to be 90-95 ℃, the calendering pressure is controlled to be 2-2.5MPa, and the microporous liquid filter material is obtained after the calendering is finished.
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| PCT/CN2023/088577 WO2023216809A1 (en) | 2022-05-09 | 2023-04-17 | Preparation method for high-flux pp melt blown nanoporous folded liquid filtering material |
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Denomination of invention: Preparation method of a high-throughput PP melt blown nanoporous folded liquid filtration material Granted publication date: 20230407 Pledgee: Bank of China Limited Dongying Branch Pledgor: DONGYING JUNFU PURIFICATION TECHNOLOGY CO.,LTD. Registration number: Y2024980008985 |
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