CN117947654B - Polyethylene non-woven fabric, preparation method and application - Google Patents

Polyethylene non-woven fabric, preparation method and application Download PDF

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CN117947654B
CN117947654B CN202410345605.8A CN202410345605A CN117947654B CN 117947654 B CN117947654 B CN 117947654B CN 202410345605 A CN202410345605 A CN 202410345605A CN 117947654 B CN117947654 B CN 117947654B
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polyethylene
fiber
slurry
pulping
fibers
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CN117947654A (en
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孙静
张峻华
刘萍
李明涛
王裕成
李东
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Yantai Metastar Special Paper Co ltd
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Yantai Metastar Special Paper Co ltd
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Abstract

The invention provides a polyethylene non-woven fabric, a preparation method and application thereof, belonging to the technical field of non-woven fabrics, wherein the polyethylene non-woven fabric comprises the following components: polyethylene pulp fiber: 20-70wt%; polyethylene fibrids: 10-60wt%; polyethylene chopped fiber: 20-75wt%; the polyethylene non-woven fabric is prepared by cutting, pulping and beating fibers prepared by flash spinning, wherein the beating degree of the fibers is 10-80 DEG SR, the beating degree of the polyethylene fibrid is 10-70 DEG SR, the length of the polyethylene chopped fibers is 3-10 mm, the fiber denier is 1-3D, and the fibers are mixed and manufactured by wet papermaking, squeezing, drying and hot pressing. The polyethylene non-woven fabric with high peel strength and puncture strength is prepared by organically combining the polyethylene pulp fiber, the polyethylene fibrid and the polyethylene chopped fiber prepared by flash spinning.

Description

Polyethylene non-woven fabric, preparation method and application
Technical Field
The invention belongs to the technical field of non-woven fabrics, and particularly relates to a polyethylene non-woven fabric, a preparation method and application thereof.
Background
Polyethylene has the characteristics of good low-temperature flexibility, solvent resistance, insulation, self-lubrication and the like, and the flash evaporation method polyethylene non-woven fabric attracts a great deal of research of institutions and enterprises at home and abroad because of the excellent mechanical property, waterproof air permeability and the like. The flash evaporation non-woven fabric is characterized in that polyethylene and solvent form a homogeneous spinning solution under a high-temperature and high-pressure state, the spinning solution adopts a flash evaporation spinning nozzle to prepare continuous long fibers, the long fibers are made into the non-woven fabric through swinging, net forming and hot pressing, the continuous long fibers are formed into a net through multidirectional, crossed and stacked, one fiber forms a thin fiber net, and the thin fiber nets are stacked on a net belt to form the non-woven fabric, so that the inside of the flash evaporation non-woven fabric does not directly penetrate through the fibers in the whole thickness direction from the front surface to the back surface, the stacked long fibers have low interlayer bonding strength, and the risk of delamination exists during long-term use.
In order to solve the problem of low interlayer bonding strength of flash evaporation non-woven fabrics, the U.S. patent with publication number of US3478141A adopts a patterned roller as a hot roller, and raised patterns on the patterned roller are utilized to increase the delamination resistance of the non-woven fabrics, but the non-woven fabrics prepared by the method have large surface roughness and obvious difference between two surfaces, and are not suitable for being applied to double-sided printing, lithium battery diaphragms and other applications.
The flash spinning fiber prepared by the prior art has large length and is easy to flocculate, paper sheets with low beating degree can not be molded, and polyethylene paper or non-woven fabric sheets can not be prepared by adopting a wet papermaking technology; the short cutting of flash spun fiber directly cannot prepare polyethylene non-woven fabric by wet papermaking technology due to low beating degree, and even if the wet papermaking technology is adopted for pulping, the physical properties of the polyethylene non-woven fabric are poor, such as low peeling strength and puncture strength.
Disclosure of Invention
In order to solve the problems, the invention provides a polyethylene non-woven fabric, a preparation method and application. The polyethylene non-woven fabric with high peel strength and puncture strength is prepared by organically combining the polyethylene pulp fiber, the polyethylene fibrid and the polyethylene chopped fiber prepared by flash spinning.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The invention provides a polyethylene non-woven fabric, which comprises the following components: polyethylene pulp fiber: 20-70wt%; polyethylene fibrids: 10-60wt%; polyethylene chopped fiber: 20-75wt%; the polyethylene non-woven fabric is prepared by cutting, pulping and beating fibers prepared by flash spinning, wherein the beating degree of the fibers is 10-80 DEG SR, the beating degree of the polyethylene fibrid is 10-70 DEG SR, the length of the polyethylene chopped fibers is 3-10 mm, the fiber denier is 1-3D, and the fibers are mixed and manufactured by wet papermaking, squeezing, drying and hot pressing.
Further, the diameter range of the polyethylene pulp fiber is 0.1-18 mu m, the length after cutting is 0.1-20.0 mm, and the grain size ratio of the polyethylene pulp fiber is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1.
Further, the crystallinity of the polyethylene pulp fiber is 60-70%, and the profile degree is 20-80%.
Further, the polyethylene fibrids have a crystallinity of not more than 20%.
Further, the mass ratio of the polyethylene pulp fiber to the polyethylene fibrid to the polyethylene chopped fiber is as follows: (1.2-2): 1: (1.5-2.1).
Further, the polyethylene chopped fiber has a degree of profile of 30-80%.
Further, the polyethylene chopped fibers are high density polyethylene filament chopped fibers or ultra-high molecular weight polyethylene filament chopped fibers.
The invention provides a preparation method of the polyethylene non-woven fabric, which comprises the following steps: preparing polyethylene pulp fiber slurry; preparing polyethylene fibrid slurry; preparing a polyethylene chopped fiber slurry; and respectively pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
Further, preparing a polyethylene pulp fiber slurry includes: adding polyethylene and a solvent R1 into a reaction kettle, controlling the reaction kettle to reach 140-250 ℃ at a heating rate of 0.1-10 ℃/min, keeping the pressure of 3-20 mpa, and preparing flash spinning fibers in a flash evaporation mode; cutting the flash spinning fiber to 0.1-20 mm, and carrying out pulping and beating treatment to ensure that the beating degree of the polyethylene pulp fiber is 10-80 DEG SR; and after drying, carrying out hydrophilic treatment on the polyethylene pulp fiber to obtain the polyethylene pulp fiber.
Further, the pulping treatment process comprises the following steps: performing pulping treatment according to the concentration of 0.1-5wt% until the beating degree is 5-20 DEG SR; the pulping treatment process comprises the following steps: after pulping, adding deionized water until the concentration is 0.01-0.1wt% for fluffing for 5-50 min, wherein the pulping pressure of the first stage is 8-22 kg, and the pulping time is 1-10 min; the second stage pulping pressure is 2-7 kg, and the pulping time is 30-200 min.
Further, the solvent R1 is one or more of water, alcohol, acid, amine, ester, ether, ketone, nitrile, amide, halogenated hydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, aromatic hydrocarbon and unsaturated hydrocarbon; the temperature and pressure in the reaction kettle are controlled through auxiliary gas and heating, wherein the auxiliary gas is one or more of nitrogen, argon, helium, carbon dioxide and neon.
Further, the flash evaporation mode is that polymer spinning solution is sprayed into nitrogen with the temperature of 50-500 ℃ through a decompression nozzle of flash evaporation spinning equipment; or the flash evaporation mode is to spray the polymer spinning solution into a mixture of a good solvent and a poor solvent of the polyethylene through a decompression nozzle of flash evaporation spinning equipment, wherein the good solvent accounts for 30-70%.
Further, cutting the flash spun fiber to 0.1-20 mm comprises: and cutting off the flash spun fibers to obtain five lengths of fibers with the lengths ranging from 0.1 to 0.5mm, 1.5 to 5.5mm, 9 to 11mm, 14 to 16mm and 19 to 20mm respectively, and mixing the five lengths of flash spun chopped fibers with the same mass.
Further, the preparation of polyethylene fibrids comprises: adding polyethylene and a solvent R2 into a reaction kettle, heating and stirring the reaction kettle to 160-200 ℃ to obtain a polyethylene solution; and mixing the polyethylene solution with a precipitating agent, shearing at least 10 minutes at the rotating speed of 2000-3000 r/min to form fibrids, cooling, molding and cleaning to obtain the polyethylene fibrids.
Further, the solvent R2 is one or more of decalin, white oil, 1,2, 4-trichlorobenzene, mineral oil, paraffin oil or kerosene.
Further, the concentration of the polyethylene solution is 5-15wt%; the precipitating agent is benzene solution or glycerin solution with concentration of 40-70wt% of solvent R2, the temperature of the precipitating agent is 80-120 ℃, and the mass ratio of the polyethylene solution to the precipitating agent is 1: 5-50.
Further, preparing the polyethylene chopped fiber includes: and carrying out hydrophilic treatment on the polyethylene chopped fibers with the length of 3-10 mm, the fiber denier of 1-3D and the degree of dysmorphism of 30-80%.
Further, the hydrophilic treatment is to increase the surface energy of the fibers to at least 38 mN/m.
Further, the hydrophilic treatment is corona treatment, and the corona treatment process is as follows: the voltage of corona treatment is 4000-16000V, the frequency is 12-26 KHz, the distance between an electrode rod and the absolute dry polymer fiber is 1-10 mm, and the air flow is 300-600 m 3/h; or the hydrophilic treatment is plasma treatment, and the plasma treatment process is as follows: the ionization power is 200-500W, the treatment time is 1-6 min, and the volume flow of the high-purity oxygen is 0.008-0.02L/min.
Further, respectively adding deionized water into the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry to carry out fluffing pulping to obtain a slurry aqueous solution with the concentration of 0.01-0.1wt%; the grain size ratio of the polyethylene pulp fiber slurry is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1, a step of; according to the polyethylene pulp fiber slurry: 20-70wt% of polyethylene fibrid slurry: 10-60 wt% of polyethylene chopped fiber slurry: and mixing 20-75wt% of the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the aqueous solution of the polyethylene chopped fiber slurry.
Further, the mass concentration of sizing is 0.001-0.05% in wet papermaking; the hot pressing adopts a mode of combining preheating and hot rolling, the preheating temperature is 80-115 ℃, the vehicle speed is 1-100 m/min, the line pressure is 0-50N/mm, and the preheating times are 1-5 times; the hot rolling temperature is 115-145 ℃, the speed is 1-100 m/min, the line pressure is 10-100N/mm, and the hot rolling times are 1-5.
The invention provides application of the polyethylene non-woven fabric, which is applied to the fields of insulation packaging, honeycomb core material, printing packaging, building waterproof, ground covering, medical sterilization packaging, composite material reinforcement and lithium battery diaphragm.
The technical scheme provided by the embodiment of the invention has the beneficial effects that:
(1) The fiber prepared by flash spinning has high crystallinity, the fiber is highly split and fibrillated after being cut and pulped, the high crystallinity can improve the strength and the thermal stability of the polyethylene non-woven fabric, the fiber is highly split and thinned after being cut and pulped, so that the fiber can form an effective three-dimensional interpenetrating network structure in the non-woven fabric, the interlayer bonding strength of the polyethylene non-woven fabric is improved, and particularly, the fiber diameter range prepared by flash spinning is 0.1-18 mu m, wherein 80% of the fiber diameter range is 1-10 mu m, after the fiber in the range is subjected to subsequent pulping treatment, the prepared fiber is more split, single fiber is split at least more than 5 and is in a bulk shape, and the fiber has higher toughness, so that the fiber presents a three-dimensional interpenetrating network structure in the polyethylene non-woven fabric and is fully bonded with polyethylene chopped fibers and polyethylene fibrids, and the bonding strength between the three is improved; and secondly, the polyethylene fibrids prepared by the application are in a film-like floating sheet structure, have low crystallinity and large specific surface area, wrap the polyethylene pulp fibers and the polyethylene chopped fibers, and improve the mechanical properties of the polyethylene non-woven fabric.
(2) The invention limits the grain size proportion of polyethylene pulp fiber, the proportion of the grain size is not more than one third of the proportion of the grain size which is larger than 10 meshes, the proportion of the grain size which is smaller than or equal to 100 meshes is larger than 10%, the branching of the small grain size fiber after pulping is less, but the degree of freedom is higher, the fiber is easy to bend, the degree of freedom of the fiber with larger grain size is lower, but the branching of the fiber after pulping is more, and only the small grain size, the medium grain size and the large grain size are matched with each other, so that the three-dimensional network structure is uniformly distributed on the space structure of the product, agglomeration or segregation is not easy to be caused, and the mechanical property is uniform.
(3) The fiber is prepared from 100% pure polyethylene, and molecular chains are effectively bonded at the temperature of the fiber interface near the melting point during hot press molding. The excellent characteristics of the polyethylene are maintained, and the polyethylene is insulating, self-lubricating, wear-resistant, solvent-resistant and chemical-resistant.
(4) The polyethylene non-woven fabric is prepared by adopting a papermaking process, the rod-shaped polyethylene chopped fibers can penetrate through the thickness of the whole paper sheet, the polyethylene pulp fibers can be effectively overlapped with each other, the polyethylene fibrid wraps the chopped fibers and the pulp fibers, and the long fibers penetrate through the thickness direction of the whole non-woven fabric, so that the problem of low layering bonding strength of the non-woven fabric is solved. In the pulping process, the structural uniformity of the polyethylene non-woven fabric is effectively improved through means of pulping, surface treatment, dispersing agents and the like. In the papermaking process, the fine gaps are reserved in the paper sheet after the fibers are uniformly filtered, so that the air permeability and the moisture vapor transmission rate of the polyethylene non-woven fabric are improved; and secondly, the deionized water takes away impurities on the fiber surface in the wet papermaking process, so that the content of harmful substances such as halogen, heavy metal and the like is obviously reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a polarized light micrograph of a polyethylene pulp fiber prepared according to example 1 of the present invention;
FIG. 2 is a polarized light micrograph of polyethylene fibrids prepared in example 1 of the present invention;
fig. 3 is an SEM image of the polyethylene nonwoven fabric prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the drawings and the embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent.
The embodiment of the invention discloses a polyethylene non-woven fabric, which comprises the following components: polyethylene pulp fiber: 20-70wt%; polyethylene fibrids: 10-60wt%; polyethylene chopped fiber: 20-75wt%; the polyethylene non-woven fabric is prepared by cutting, pulping and beating fibers prepared by flash spinning, wherein the beating degree of the fibers is 10-80 DEG SR, the beating degree of the polyethylene fibrid is 10-70 DEG SR, the length of the polyethylene chopped fibers is 3-10 mm, the fiber denier is 1-3D, and the fibers are mixed and manufactured by wet papermaking, squeezing, drying and hot pressing.
The fiber prepared by flash spinning has high crystallinity, the fiber is highly split and fibrillated after being cut and pulped, the high crystallinity can improve the strength of the polyethylene non-woven fabric, the fiber is highly split and thinned after being cut and pulped, so that the fiber can form an effective three-dimensional interpenetrating network structure in the non-woven fabric, the interlayer bonding strength of the polyethylene non-woven fabric is improved, and particularly, the fiber diameter range prepared by flash spinning is 0.1-18 mu m, wherein 80% of the fiber diameter range is 1-10 mu m, after the fiber in the range is subjected to subsequent pulping treatment, the prepared fiber is more branched, single fiber is at least more than 5 and is in a bulk shape, and the fiber has higher toughness due to the high crystallinity, so that the fiber exhibits a three-dimensional interpenetrating network structure in the polyethylene non-woven fabric and is fully bonded with polyethylene chopped fibers and polyethylene fibrids, and the bonding strength between the three is improved; and secondly, the polyethylene fibrids prepared by the application are in a film-like floating sheet structure, have low crystallinity and large specific surface area, wrap the polyethylene pulp fibers and the polyethylene chopped fibers, and improve the mechanical properties of the polyethylene non-woven fabric.
It is noted that the use of polyethylene in the present invention includes not only polyethylene homopolymers but also copolymers wherein at least 85% of the repeat units in the copolymer are ethylene units, preferably linear polyethylene homopolymers.
Specifically, the diameter range of the polyethylene pulp fiber is 0.1-18 mu m, the length after cutting is 0.1-20.0 mm, and the grain diameter ratio of the polyethylene pulp fiber is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1. the diameter range of the polyethylene pulp fiber prepared by flash spinning is 0.1-18 mu m, in order to achieve better pulping and form an effective three-dimensional interpenetrating network structure in a non-woven fabric, the chopped length and the grain size ratio of the polyethylene pulp fiber are limited, in particular, the length after cutting is 0.1-20mm, the proper size length can ensure that the refined fiber after pulping can form an effective network structure in a product, the comprehensive mechanical property of the product is improved, such as the peeling strength and the puncture resistance are improved, the longer length has negative influence on the uniformity of the pulp, the shorter length improves the uniformity of the pulp, but the comprehensive mechanical property of the product is reduced; finally, the grain size ratio of the polyethylene pulp fiber is limited, the grain size ratio is not more than one third of the grain size ratio which is larger than 10 meshes, the grain size ratio is smaller than or equal to 100 meshes and is larger than 10%, the branching of the small grain size fiber after pulping is less, the degree of freedom is higher, the fiber is easy to bend, the degree of freedom of the fiber with larger grain size is lower, the branching of the fiber after pulping is more, the three-dimensional network structure can be uniformly distributed on the space structure of the product only by the mutual matching of the small grain size, the medium grain size and the large grain size, agglomeration or segregation is not easy to cause, and the mechanical property is uniform.
Specifically, the crystallinity of the polyethylene pulp fiber is 60-70%, and the profile degree is 20-80%. The crystallinity of the polyethylene pulp fiber prepared by flash spinning is high, but the crystallinity is not too high, so that the strength of the fiber is large, the mechanical properties of the prepared product are easy to be uneven in all directions, and the amorphous polyethylene pulp fiber is easier to produce wrapping property with other fibers, so that the range of the crystallinity needs to be controlled, and the polyethylene pulp fiber can ensure the uniformity of the mechanical properties and the bonding strength of three fibers. The calculation formula of the dysmorphism adopts the existing calculation mode, namely: in general, the higher the degree of the profile, the better the mechanical properties such as tensile strength of the polyethylene non-woven fabric, but the too high degree of the profile, the condition that part of fibers fall off and fiber flocks are clustered in the subsequent beating process, and the better net structure cannot be realized, so the degree of the profile is limited.
Specifically, the polyethylene fibrids have a crystallinity of not more than 20%. The polyethylene fibrids are in a film-shaped floating sheet structure, the crystallinity is low, the specific surface area is large, the polyethylene fibrids have good wrapping effect in wet papermaking, the polyethylene pulp fibers and the polyethylene chopped fibers are wrapped, the mechanical property of the polyethylene non-woven fabric is improved, the wrapping property of the polyethylene fibrids can be reduced due to high crystallinity, and therefore the crystallinity is not suitable to be large.
Specifically, the mass ratio of the polyethylene pulp fiber to the polyethylene fibrid to the polyethylene chopped fiber is as follows: (1.2-2): 1: (1.5-2.1). The polyethylene chopped fibers can penetrate through the thickness of the whole paper sheet, the polyethylene pulp fibers can be effectively overlapped with each other, the polyethylene fibrids wrap the chopped fibers and the pulp fibers, and the long fibers penetrate through the thickness direction of the whole non-woven fabric, so that the optimal performance can be realized when the content of the chopped fibers, the pulp fibers and the long fibers is in the range.
Specifically, the polyethylene chopped fiber has a degree of profile of 30-80%. The polyethylene chopped fiber mainly provides a skeleton effect, so that the mechanical property of the product is improved, and the higher the degree of special-shaped polyethylene chopped fiber is, the higher the bonding strength between the polyethylene chopped fiber and other fibers is.
Specifically, the polyethylene chopped fiber is a high-density polyethylene filament chopped fiber or an ultra-high molecular weight polyethylene filament chopped fiber. Linear polyethylenes having molecular weights up to 3,000,000 to 6,000,000 are known as Ultra High Molecular Weight Polyethylenes (UHMWPE). The ultra-high molecular weight polyethylene has very high strength and can be used for making bulletproof clothes; the high-density polyethylene is linear polyethylene, the crystallinity is more than 45%, the density is 0.95-0.96 g/cm 3, the melting temperature is 124-138 ℃, and the glass transition temperature is-75-120 ℃.
The invention also provides a preparation method of the polyethylene non-woven fabric, which comprises the following steps:
s1, preparing polyethylene pulp fiber slurry.
The preparation of the polyethylene pulp fiber slurry comprises: and adding polyethylene and a solvent R1 into a reaction kettle, controlling the reaction kettle to reach 140-250 ℃ at a heating rate of 0.1-10 ℃/min, maintaining the pressure of 3-20 mpa, and preparing the flash spinning fiber in a flash evaporation mode.
In the embodiment of the invention, polyethylene and a solvent R1 are added into a reaction kettle to obtain polyethylene spinning solution with the concentration of 1-30wt%.
The solvent R1 is one or more of water, alcohol, acid, amine, ester, ether, ketone, nitrile, amide, halohydrocarbon, aliphatic hydrocarbon, alicyclic hydrocarbon, aromatic hydrocarbon and unsaturated hydrocarbon.
The temperature and pressure in the reaction kettle are controlled through auxiliary gas and heating, wherein the auxiliary gas is one or more of nitrogen, argon, helium, carbon dioxide and neon.
The flash evaporation mode is that polymer spinning solution is sprayed out into nitrogen with the temperature of 50-500 ℃ through a decompression spray head of flash evaporation spinning equipment; or the flash evaporation mode is to spray the polymer spinning solution into a mixture of a good solvent and a poor solvent of the polyethylene through a decompression nozzle of flash evaporation spinning equipment, wherein the good solvent accounts for 30-70%.
It should be noted that the judgment criteria for the good solvent and the poor solvent are common knowledge in the art, and will not be described in detail herein.
Cutting the flash spinning fiber to 0.1-20 mm, and carrying out pulping and beating treatment to obtain the polyethylene pulp fiber with the beating degree of 10-80 DEG SR.
Cutting the flash spun fiber to 0.1-20 mm comprises: and cutting off the flash spun fibers to obtain five lengths of fibers with the lengths ranging from 0.1 to 0.5mm, 1.5 to 5.5mm, 9 to 11mm, 14 to 16mm and 19 to 20mm respectively, and mixing the five lengths of flash spun chopped fibers with the same mass. For example, the fiber can be five lengths of 0.1mm, 1.5mm, 9mm, 14mm and 19mm, and the fiber can be five lengths of 0.2mm, 1.6mm, 10mm, 15mm and 20mm, so long as the five lengths are respectively in the five ranges, and the physical lap joint between the fibers with different lengths is improved by limiting the lengths of the fibers, so that the prepared polyethylene non-woven fabric has good strength.
The pulping treatment process comprises the following steps: performing pulping treatment according to the concentration of 0.1-5wt% until the beating degree is 5-20 DEG SR; the pulping treatment process comprises the following steps: after pulping, adding deionized water until the concentration is 0.01-0.1wt% for fluffing for 5-50 min, wherein the pulping pressure of the first stage is 8-22 kg, and the pulping time is 1-10 min; the second stage pulping pressure is 2-7 kg, and the pulping time is 30-200 min. After beating, the beating degree of the polyethylene pulp fiber is 10-80 DEG SR, the beating pressure in the first section is long, so that the fiber is expanded, the cohesion is reduced, the tissue in the fiber is relaxed, the contact area is effectively increased, the strength of the subsequent polyethylene non-woven fabric is improved, but the beating time in the first section is not more than 10min, and the air permeability of the non-woven fabric is reduced after the larger beating pressure is used for a long time; the second stage of beating pressure is small, beating time is long, the fiber is split longitudinally, two ends are broomed, the fiber surface is split and fluffed, the specific surface area of the fiber is greatly increased, and the combination of hydrogen chains is promoted.
And after drying, carrying out hydrophilic treatment on the polyethylene pulp fiber to obtain the polyethylene pulp fiber.
S2, preparing polyethylene fibrid slurry.
The preparation of polyethylene fibrids comprises: adding polyethylene and a solvent R2 into a reaction kettle, heating and stirring the reaction kettle to 160-200 ℃ to obtain a polyethylene solution; and mixing the polyethylene solution with a precipitating agent, shearing at least 10 minutes at the rotating speed of 2000-3000 r/min to form fibrids, cooling, molding and cleaning to obtain the polyethylene fibrid slurry.
The solvent R2 is one or more of decalin, white oil, 1,2, 4-trichlorobenzene, mineral oil, paraffin oil or kerosene.
The concentration of the polyethylene solution is 5-15wt%; the precipitating agent is benzene solution or glycerin solution with concentration of 40-70wt% of solvent R2, the temperature of the precipitating agent is 80-120 ℃, and the mass ratio of the polyethylene solution to the precipitating agent is 1: 5-50.
S3, preparing polyethylene chopped fiber slurry.
And carrying out hydrophilic treatment on the polyethylene chopped fiber with the length of 3-10 mm, the fiber denier of 1-3D and the profile degree of 80%.
The polyethylene chopped fiber used in the invention is cleaned by adopting a surfactant and deionized water before use to remove surface stains, wherein the surfactant can adopt ionic surfactants (including cationic surfactants, anionic surfactants and amphoteric surfactants), nonionic surfactants, compound surfactants, other surfactants and the like in the prior art. The surfactant adopted by the invention is sodium dodecyl benzene sulfonate.
And S4, pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
And respectively adding deionized water into the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry to carry out fluffing pulping to obtain a slurry aqueous solution with the concentration of 0.01-0.1wt%. The grain size ratio of the polyethylene pulp fiber slurry is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1.
According to the polyethylene pulp fiber slurry: 20-70wt% of polyethylene fibrid slurry: 10-60 wt% of polyethylene chopped fiber slurry: and mixing 20-75wt% of the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the aqueous solution of the polyethylene chopped fiber slurry. The mass concentration of sizing is 0.001-0.05% during wet papermaking; the hot pressing adopts a mode of combining preheating and hot rolling, the preheating temperature is 80-115 ℃, the vehicle speed is 1-100 m/min, the line pressure is 0-50N/mm, and the preheating times are 1-5 times; the hot rolling temperature is 115-145 ℃, the speed is 1-100 m/min, the line pressure is 10-100N/mm, and the hot rolling times are 1-5. A step of
The hot rolling process is realized by a hot roller, wherein the hot roller is a metal roller, a patterned roller or an elastic roller with patterns on the surface, and specific size parameters can be determined based on actual production conditions.
The hydrophilic treatment of the present application is to increase the surface energy of the fiber to at least 38 mN/m. The surface of the fibers may be treated to increase the surface energy using prior art techniques. Corona treatment and plasma treatment are preferably used in the present application.
When the hydrophilic treatment is corona treatment, the corona treatment process comprises the following steps: the corona treatment voltage is 4000-16000V, the frequency is 12-26 KHz, the distance between the electrode rod and the absolute dry polymer fiber is 1-10 mm, and the air flow is 300-600 m 3/h.
When the hydrophilic treatment is plasma treatment, the plasma treatment process is as follows: the ionization power is 200-500W, the treatment time is 1-6 min, and the volume flow of the high-purity oxygen is 0.008-0.02L/min.
The polyethylene non-woven fabric is applied to the fields of insulating packaging, honeycomb core material, printing packaging, building waterproofing, ground covering, medical sterilization packaging, composite material reinforcement, lithium battery diaphragm and the like.
In order to better illustrate the embodiments of the present invention, the present invention will be described in further detail by way of specific examples.
Example 1
The embodiment of the invention provides a preparation method of polyethylene non-woven fabric, which comprises the following steps of;
s1, preparing polyethylene pulp fiber slurry.
Adding polyethylene (Dushan petrochemical 5502 XA) and methylene dichloride into a reaction kettle, heating to 200 ℃ under the stirring state of 150r/min, controlling the pressure in the kettle to 15MPa through nitrogen, obtaining spinning solution with the mass concentration of 8wt% of polymer, and spraying the spinning solution into hot nitrogen with the temperature of 60 ℃ through a decompression nozzle to obtain netlike flash spinning fiber with the diameter range of 0.5-20 mu m; the fiber strength was 3.9g/d, the crystallinity of the fiber was 63%, and the degree of irregularity was 20%.
Cutting off the flash spun fiber by a cutter to obtain polyethylene short fibers with lengths of 0.1mm, 3mm, 10mm, 15mm and 20mm respectively, and simultaneously pulping the polyethylene short fibers with five lengths of the same weight, wherein the pulping concentration of the pulping treatment is 5wt%, the clearance between grinding sheets is 3.0mm, and the pulping degree is 20 DEG SR after pulping. The pulping treatment is that deionized water is added to be fluffed for 10min, the pulp concentration during pulping is 0.01wt%, the pulping pressure in the first stage is 8kg, the pulping time is 3min, the pulping pressure in the second stage is 2kg, and the pulping time is 100min. Filtering water, drying, carrying out corona treatment on the absolute dry polyethylene short fibers, wherein the voltage of the corona treatment is 4000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fibers is 8mm, and the air flow is 1000m 3/h; the resulting polyethylene pulp fiber slurry had a pulp freeness of 45 ° SR, and the prepared polyethylene pulp fiber slurry was shown in fig. 1.
The performance index of the solitary petrochemical 5502XA is as follows: 2.16kg of raw material, the melt flow rate of which is measured to be 0.2g/10min by adopting ISO 1133; the density is 954kg/m 3 measured by ISO 1872/1; the tensile strength is 26MPa and the elongation at break is more than 300 percent by adopting ISO R527/2D.
S2, preparing polyethylene fibrid slurry.
Polyethylene (Dushan petrochemical 5502 XA) and 51# white oil are added into a reaction kettle, the temperature is raised to 150 ℃ under the stirring state of 100r/min, and the heating rate is 10 ℃/min, so that a polyethylene solution with the mass concentration of 5wt% of the polymer is obtained. The precipitation agent is prepared by stirring and heating 51# white oil and benzene to 90 ℃ in a closed device, wherein the 51# white oil accounts for 60wt% of the solution. Simultaneously and continuously and stably introducing the polyethylene solution and the precipitating agent into the precipitating equipment through a pipeline, wherein the flow rate of the polyethylene solution is 5kg/h, and the flow rate of the precipitating agent is 250kg/h. High-speed shearing to form fibrid by a fibrid precipitation device, discharging into a water washing tank for further cooling and molding, removing solvent by a sodium dodecyl sulfate aqueous solution and multi-stage water washing to obtain polyethylene fibrid slurry, measuring the beating degree of the polyethylene fibrid slurry to be 70 DEG SR and the crystallinity to be 18%, and preparing the polyethylene fibrid slurry as shown in figure 2.
S3, preparing polyethylene chopped fiber slurry.
Cutting the ultra-high molecular weight polyethylene fiber with the cross section of broad bean shape, the degree of special shape of 30 percent and the fineness of 2D into 6mm, adopting sodium dodecyl benzene sulfonate solution and deionized water to wash away surface oiling agent, filtering and drying, carrying out oxygen plasma treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the ionization power is set to be 300W, the treatment time is 1min, and the volume flow of high-purity oxygen is 0.02L/min.
And S4, pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 2:7:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
The polyethylene fibrid slurry is fluffed in deionized water to obtain the aqueous solution of the polyethylene fibrid slurry with the mass concentration of 0.01 weight percent.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.01 weight percent.
Mixing the aqueous solution of the sizing agent with the absolute dry weight of polyethylene pulp fiber of 20 wt percent, the absolute dry weight of polyethylene fibrid of 20 wt percent and the absolute dry weight of ultra-high molecular weight polyethylene chopped fiber of 60 wt percent, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine during papermaking is 0.001 wt percent; obtained by squeezing and drying, the preheating temperature is 80 ℃, the vehicle speed is 1m/min, the line pressure is 50N/mm, and the preheating times are 2 times; the hot rolling temperature is 125 ℃, the speed is 1m/min, the line pressure is 100N/mm, and the hot rolling times are 2 times; the polyethylene nonwoven fabric was obtained, the basis weight of the polyethylene nonwoven fabric was 40g/m 2, the thickness was 115. Mu.m, and the prepared polyethylene nonwoven fabric was shown in FIG. 3.
Example 2
The embodiment of the invention provides a preparation method of polyethylene non-woven fabric, which comprises the following steps of;
s1, preparing polyethylene pulp fiber slurry.
Adding polyethylene (5301 AA of Shanghai Seisaceae) and methylene dichloride into a reaction kettle, heating to 140 ℃ under the stirring state of 150r/min, controlling the pressure in the kettle to 20MPa through nitrogen, obtaining spinning solution with the mass concentration of 5wt% of the polymer, and spraying the spinning solution into hot nitrogen with the temperature of 80 ℃ through a decompression nozzle to obtain net-shaped flash-evaporation spinning fibers, wherein the diameter range of the fibers is 0.1-10 mu m; the fiber strength was 4.0g/d, the crystallinity of the fiber was 65%, and the degree of irregularity was 30%.
Performance indexes of Shanghai raceae 5301AA are as follows: 2.16kg of raw material, the melt index of which is measured to be 0.08g/10min by adopting ISO 1133; the density is 950kg/m 3 measured by ISO 1872/1; the tensile yield strength of MD is 32MPa, tensile yield strength of TD is 26MPa, elongation at break of MD is 460%, elongation at break of TD is 950%, tensile breaking strength of MD is 77MPa and tensile breaking strength of TD is 57MPa measured by ISO 1184.
Cutting off the flash spun fiber by a cutter to obtain polyethylene short fibers with lengths of 0.1mm, 3mm, 10mm, 15mm and 20mm respectively, and simultaneously pulping the polyethylene short fibers with five lengths of the same weight, wherein the pulping concentration of the pulping treatment is 1wt%, the clearance between grinding sheets is 2.0mm, and the pulping degree after pulping is 15 DEG SR. The pulping treatment is that deionized water is added to be fluffed for 40min, the pulp concentration during pulping is 0.02%, the pulping pressure in the first stage is 8kg, the pulping time is 5min, the pulping pressure in the second stage is 5kg, and the pulping time is 50min. Filtering water, drying, carrying out corona treatment on the absolute dry polyethylene short fibers, wherein the voltage of the corona treatment is 5000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fibers is 5mm, and the air flow is 1000m 3/h; the polyethylene pulp fiber slurry is obtained, and the pulp beating degree is 45 DEG SR.
S2, preparing polyethylene fibrid slurry.
Polyethylene (Serani 4118) and 1,2, 4-trichlorobenzene are added into a reaction kettle, the temperature is raised to 160 ℃ under the stirring state of 150r/min, and the heating rate is 5 ℃/min, so that a polyethylene solution with the mass concentration of 5wt% of the polymer is obtained. The precipitant is prepared by stirring and heating 1,2, 4-trichlorobenzene and glycerin to 100 ℃ in a closed container, wherein the mass fraction of the 1,2, 4-trichlorobenzene in the solution is 70wt%. Simultaneously and continuously and stably introducing the polyethylene solution and the precipitating agent into the precipitating equipment through a pipeline, wherein the flow rate of the polyethylene solution is 100kg/h, and the flow rate of the precipitating agent is 500kg/h. High-speed shearing to form fibrid by a fibrid device, discharging into a water washing tank for further cooling and molding, and removing solvent by ultrasonic cleaning, detergent aqueous solution and multi-stage water washing to obtain polyethylene fibrid slurry. The polyethylene fibrid slurry was measured to have a freeness of 55 ° SR and a crystallinity of 15%.
S3, preparing polyethylene chopped fiber slurry.
Cutting the 3D ultra-high molecular weight polyethylene fiber with the cross section in the shape of broad beans, the degree of special shape of 40 percent and the fineness of 10mm, adopting sodium dodecyl benzene sulfonate solution and deionized water to wash away surface oil, filtering and drying, carrying out corona treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the voltage of the corona treatment is 14000V, the frequency is 20KHz, the distance between an electrode rod and the absolute dry polymer fiber is 10mm, and the air flow rate is 600m 3/h.
And S4, pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:8:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
The polyethylene fibrid slurry is fluffed in deionized water to obtain the aqueous solution of the polyethylene fibrid slurry with the mass concentration of 0.1 weight percent.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.1%.
Mixing the aqueous solution of the sizing agent with 30 wt percent of absolute dry weight of polyethylene pulp fiber, 20 wt percent of absolute dry weight of polyethylene fibrid and 50 wt percent of absolute dry weight of ultra-high molecular weight polyethylene chopped fiber, and adopting an inclined wire paper machine, wherein the sizing mass concentration of the paper machine is 0.001 wt percent during papermaking; obtained by squeezing and drying, the preheating temperature is 95 ℃, the vehicle speed is 10m/min, the line pressure is 50N/mm, and the preheating times are 1 time; the hot rolling temperature is 127 ℃, the speed is 10m/min, the line pressure is 30N/mm, and the hot rolling times are 3 times; the polyethylene nonwoven fabric was obtained, and the basis weight of the polyethylene nonwoven fabric was 15g/m 2, and the thickness was 43. Mu.m.
Example 3
The embodiment of the invention provides a preparation method of polyethylene non-woven fabric, which comprises the following steps of;
s1, preparing polyethylene pulp fiber slurry.
Adding polyethylene (Yangzi petrochemical 7000F) and hexafluoroisopropanol into a reaction kettle, heating to 180 ℃ under the stirring state of 200r/min, controlling the pressure in the kettle to 10MPa through nitrogen, obtaining spinning solution with the mass concentration of 3wt% of polymer, spraying the spinning solution into a coagulating bath through a decompression nozzle, wherein the coagulating bath consists of hexafluoroisopropanol and 51# white oil, and the liquid flow speed of the coagulating bath is 200m/min along the outlet direction of the nozzle of the decompression nozzle, wherein the hexafluoroisopropanol accounts for 50wt% of the solution, so as to obtain crushed slag-like polyethylene fibers, the diameter range of the fibers is 0.1-20 mu m, the crystallinity of the fibers is 60%, and the special-shaped degree is 50%.
Cutting polyethylene scraps by a cutter to obtain polyethylene short fibers with lengths of 0.1mm, 5mm, 10mm, 15mm and 20mm respectively, and simultaneously pulping the polyethylene short fibers with five lengths of the same weight, wherein the pulping concentration of the pulping treatment is 0.1wt%, the clearance between grinding sheets is 1.0mm, and the pulping degree after pulping is 20 DEG SR. The pulping treatment is that deionized water is added to be fluffed for 40min, the pulp concentration during pulping is 0.05%, the pulping pressure in the first stage is 10kg, the pulping time is 4min, the pulping pressure in the second stage is 7kg, and the pulping time is 100min. Filtering water, drying, carrying out corona treatment on the absolute dry polyethylene short fibers, wherein the voltage of the corona treatment is 15000V, the frequency is 26KHz, the distance between an electrode rod and the absolute dry polymer fibers is 1mm, and the air flow is 2000m 3/h; the polyethylene pulp fiber slurry is obtained, and the pulp beating degree is 65 DEG SR.
S2, preparing polyethylene fibrid slurry.
Polyethylene (Yangzi petrochemical 7000F) and decalin are added into a reaction kettle, the temperature is raised to 160 ℃ under the stirring state of 200r/min, and the heating rate is 3 ℃/min, so that the polyethylene solution with the mass concentration of the polymer of 15wt% is obtained. Stirring and heating decalin and glycerin to 120 ℃ in a closed device to obtain the precipitant, wherein decalin accounts for 50 weight percent of the solution. Simultaneously and continuously and stably introducing the polyethylene solution and the precipitating agent into the precipitating equipment through a pipeline, wherein the flow rate of the polyethylene solution is 200kg/h, and the flow rate of the precipitating agent is 1500kg/h. High-speed shearing to form fibrid by a fibrid device, discharging into a water washing tank for further cooling and molding, and removing solvent by ultrasonic cleaning, detergent aqueous solution and multi-stage water washing to obtain polyethylene fibrid slurry. The polyethylene fibrid slurry was measured to have a freeness of 20 ° SR and a crystallinity of 10%.
S3, preparing polyethylene chopped fiber slurry.
Cutting ultra-high molecular weight polyethylene fiber with the cross section of broad bean shape, the degree of special shape of 60 percent and the fineness of 2.5D into 8mm, adopting sodium dodecyl benzene sulfonate solution and deionized water to wash away surface oil, filtering and drying, carrying out oxygen plasma treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the ionization power is set to be 300W, the treatment time is 4min, and the volume flow of high-purity oxygen is 0.008L/min.
And S4, pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 5:4:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.05 wt%.
The polyethylene fibrid slurry is fluffed in deionized water to obtain the aqueous solution of the polyethylene fibrid slurry with the mass concentration of 0.05 weight percent.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.1%.
Mixing the aqueous solution of the sizing agent, wherein the absolute dry weight of the polyethylene pulp fiber is 30 wt%, the absolute dry weight of the polyethylene fibrid is 30 wt%, the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber is 40 wt%, and the sizing mass concentration of a paper machine is 0.001wt% when a slant wire paper machine is used for making paper; obtained by squeezing and drying, the preheating temperature is 115 ℃, the vehicle speed is 100m/min, the line pressure is 50N/mm, and the preheating times are 2 times; the hot rolling temperature is 145 ℃, the speed is 100m/min, the line pressure is 10N/mm, and the hot rolling times are 2 times; the polyethylene nonwoven fabric was obtained, and the basis weight of the polyethylene nonwoven fabric was 60g/m 2, and the thickness was 170. Mu.m.
Example 4
The embodiment of the invention provides a preparation method of polyethylene non-woven fabric, which comprises the following steps of;
s1, preparing polyethylene pulp fiber slurry.
Adding polyethylene, n-pentane and cyclopentane into a reaction kettle (the mass ratio of the n-pentane to the cyclopentane is 1:1), heating to 210 ℃ under the stirring state of 200r/min, controlling the pressure in the kettle to 18MPa through argon so as to obtain a spinning solution with the mass concentration of 20wt% of polymer, and spraying the spinning solution into nitrogen at 80 ℃ through a decompression nozzle so as to obtain long fibrous polyethylene fibers, wherein the diameter range of the fibers is 0.1-20 mu m; the crystallinity of the fiber was 70% and the profile was 70%.
The polyethylene fibers are cut off by a cutter to obtain polyethylene short fibers with lengths of 0.1mm, 5mm, 10mm, 15mm and 20mm respectively, and the polyethylene short fibers with five lengths with the same weight are subjected to pulping treatment simultaneously, wherein the pulping concentration of the pulping treatment is 5%, the clearance of a grinding disc is 1.0mm, and the beating degree after pulping is 5 DEG SR. The pulping treatment comprises the steps of adding deionized water to fluffe for 50min, wherein the pulp concentration during pulping is 0.08%, the pulping pressure in the first stage is 22kg, the pulping time is 10min, the pulping pressure in the second stage is 7kg, the pulping time is 200min, and the pulping is stopped when the fibers are completely dispersed without pulp points. Filtering water, drying, and carrying out corona treatment on the absolute dry polyethylene short fibers, wherein the voltage of the corona treatment is 16000V, the frequency is 18KHz, the distance between an electrode rod and the absolute dry polymer fibers is 3mm, and the air flow is 3000m 3/h; the polyethylene pulp fiber slurry is obtained, and the pulp beating degree is 70 DEG SR.
S2, preparing polyethylene fibrid slurry.
Adding polyethylene and 51# white oil into a reaction kettle, heating to 160 ℃ under the stirring state of 200r/min, and heating at the rate of 3 ℃/min to obtain polyethylene solution with the mass concentration of polymer of 15 wt%. The precipitation agent is prepared by stirring and heating 51# white oil and glycerin to 120 ℃, wherein the 51# white oil accounts for 50wt% of the solution. Simultaneously and continuously and stably introducing the polyethylene solution and the precipitating agent into a precipitating device, wherein the flow rate of the polyethylene solution is 300kg/h, and the flow rate of the precipitating agent is 15000kg/h. High-speed shearing to form fibrid by a fibrid device, discharging into a water washing tank for further cooling and molding, and removing solvent by ultrasonic cleaning, detergent aqueous solution and multi-stage water washing to obtain polyethylene fibrid slurry. The polyethylene fibrid slurry was measured to have a freeness of 60 ° SR and a crystallinity of 8%.
S3, preparing polyethylene chopped fiber slurry.
Cutting 3D high-density polyethylene fiber with cross section of broad bean shape, degree of special-shaped 80% and fineness into 5mm, washing away surface oil agent with sodium dodecyl benzene sulfonate solution and deionized water, filtering, drying, corona treating the ultra-high molecular weight polyethylene chopped fiber with voltage of 10000V, frequency of 12KHz, distance between electrode rod and the ultra-dry polymer fiber of 1mm, and air flow rate of 5000m 3/h.
And S4, pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 8:1:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.1 wt%.
The polyethylene fibrid slurry is fluffed in deionized water to obtain the aqueous solution of the polyethylene fibrid slurry with the mass concentration of 0.05 weight percent.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.01%.
Mixing the aqueous solution of the sizing agent, wherein the absolute dry weight of the polyethylene pulp fiber is 30wt%, the absolute dry weight of the polyethylene fibrid is 20wt%, the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber is 50wt%, and the sizing mass concentration of a paper machine is 0.001wt% when the paper machine is used for papermaking; obtained by squeezing and drying, the preheating temperature is 115 ℃, the vehicle speed is 80m/min, the line pressure is 50N/mm, and the preheating times are 3 times; the hot rolling temperature is 138 ℃, the speed is 80m/min, the line pressure is 10N/mm, and the hot rolling times are 4 times; the polyethylene nonwoven fabric was obtained, and the basis weight of the polyethylene nonwoven fabric was 70g/m 2, and the thickness was 200. Mu.m.
Example 5
The embodiment of the invention provides a preparation method of polyethylene non-woven fabric, which comprises the following steps of;
s1, preparing polyethylene pulp fiber slurry.
Adding polyethylene, hexafluoroisopropanol and dichloroacetic acid into a reaction kettle (the mass ratio of hexafluoroisopropanol to dichloroacetic acid is 95:5), heating to 180 ℃ under the stirring state of 250r/min, heating at the speed of 4 ℃/min, controlling the pressure in the kettle to 20MPa by neon to obtain spinning solution with the mass concentration of 25wt% of polymer, and spraying the spinning solution into nitrogen at the temperature of 100 ℃ through a decompression nozzle to obtain long fibrous polyethylene fibers, wherein the diameter of the fibers is 0.1-10 mu m; the crystallinity of the fiber was 63% and the profile was 80%.
The polyethylene fibers are cut off by a cutter to obtain polyethylene short fibers with lengths of 0.1mm, 5mm, 10mm, 15mm and 20mm respectively, and the polyethylene short fibers with five lengths with the same weight are subjected to pulping treatment simultaneously, wherein the pulping concentration of the pulping treatment is 3%, the grinding disc clearance is 3.0mm, and the beating degree after pulping is 8 DEG SR. The pulping treatment comprises adding deionized water to fluffe for 5min, wherein the pulp concentration during pulping is 0.1%, the pulping pressure in the first stage is 8kg, the pulping time is 2min, the pulping pressure in the second stage is 7kg, the pulping time is 30min, and the pulping is stopped when the fiber is completely dispersed without pulp points. Filtering water, drying, and carrying out corona treatment on the absolute dry polyethylene short fibers, wherein the voltage of the corona treatment is 6000V, the frequency is 12KHz, the distance between an electrode rod and the absolute dry polymer fibers is 5mm, and the air flow is 6000m 3/h; the polyethylene pulp fiber slurry is obtained, and the pulp beating degree is 30 DEG SR.
S2, preparing polyethylene fibrid slurry.
Adding polyethylene and 51# white oil into a reaction kettle, heating to 160 ℃ under the stirring state of 200r/min, and heating at the rate of 3 ℃/min to obtain polyethylene solution with the mass concentration of polymer of 15 wt%. The precipitation agent is prepared by stirring and heating 51# white oil and glycerin to 120 ℃, wherein the 51# white oil accounts for 50wt% of the solution. Simultaneously and continuously and stably introducing the polyethylene solution and the precipitating agent into a precipitating device, wherein the flow rate of the polyethylene solution is 300kg/h, and the flow rate of the precipitating agent is 15000kg/h. High-speed shearing to form fibrid, discharging into a water washing tank, further cooling and forming, and removing solvent by ultrasonic cleaning, cleaning powder water solution and multi-stage water washing to obtain polyethylene fibrid. The polyethylene fibrids were measured to have a freeness of 60 ° SR and a crystallinity of 9%.
S3, preparing polyethylene chopped fiber slurry.
Cutting 3D high-density polyethylene fiber with a broad bean-shaped cross section, a special-shaped degree of 60% and fineness into 5mm, washing away a surface oil agent by adopting sodium dodecyl benzene sulfonate solution and deionized water, filtering and drying, and performing oxygen plasma treatment and corona treatment on the ultra-high molecular weight polyethylene chopped fiber which is absolute dry, wherein the ionization power is set to be 400W, the treatment time is 2min, and the volume flow of high-purity oxygen is 0.015L/min.
And S4, pulping and mixing the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry according to a proportion, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric.
The polyethylene pulp fiber slurry is prepared according to the particle size ratio of less than or equal to 100 meshes: 10-100 mesh: gtoreq 10 mesh = 1:8:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.1 wt%.
The polyethylene fibrid slurry is fluffed in deionized water to obtain the aqueous solution of the polyethylene fibrid slurry with the mass concentration of 0.05 weight percent.
Mechanically defibering the ultra-high molecular weight polyethylene chopped fiber slurry, and concentrating to obtain an aqueous solution of the ultra-high molecular weight polyethylene chopped fiber slurry with the mass concentration of 0.01%.
Mixing the aqueous solution of the sizing agent, wherein the absolute dry weight of the polyethylene pulp fiber is 40 percent wt percent, the absolute dry weight of the polyethylene fibrid is 40 percent, the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber is 20 percent, and the sizing mass concentration of a paper machine is 0.001 percent when a paper machine is used for making paper; obtained by squeezing and drying, the preheating temperature is 115 ℃, the vehicle speed is 50m/min, the line pressure is 30N/mm, and the preheating times are 2 times; the hot rolling temperature is 125 ℃, the speed is 50m/min, the line pressure is 100N/mm, and the hot rolling times are 5 times; the polyethylene nonwoven fabric was obtained, and the basis weight of the polyethylene nonwoven fabric was 150g/m 2, and the thickness was 430. Mu.m.
Example 6
Unlike example 1, in S4 of this example, the above aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 40wt%, the absolute dry weight of the polyethylene fibrid was 20% by weight, and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 40% by weight.
Example 7
Unlike example 1, in S4 of this example, the above aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 40wt%, the absolute dry weight of the polyethylene fibrid was 25% by weight, and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 35% by weight.
Comparative example 1
Unlike example 1, in S4 of this comparative example, the above aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 18 wt%, the absolute dry weight of the polyethylene fibrid was 25% by weight, and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 57% by weight.
Comparative example 2
Unlike example 1, in S4 of this comparative example, the above aqueous slurry was mixed so that the absolute dry weight of the polyethylene pulp fiber was 22 wt%, the absolute dry weight of the polyethylene fibrid was 8wt%, and the absolute dry weight of the ultra-high molecular weight polyethylene chopped fiber was 70 wt%.
Comparative example 3
Unlike example 1, in S4 of this comparative example, the polyethylene pulp fiber slurry was prepared in a particle size ratio of 100 mesh or less: 10-100 mesh: gtoreq 10 mesh = 9:8:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Comparative example 4
Unlike example 1, in S4 of this comparative example, the polyethylene pulp fiber slurry was prepared in a particle size ratio of 100 mesh or less: 10-100 mesh: gtoreq 10 mesh = 1:1:1.1, mixing, mechanically dispersing the mixed polyethylene pulp fiber pulp and deionized water, and concentrating to obtain the polyethylene pulp fiber pulp aqueous solution with the mass concentration of 0.01 wt%.
Comparative example 5
Unlike example 1, in S4 of this comparative example, the polyethylene pulp fiber slurry was prepared in a particle size ratio of 100 mesh or less: 10-100 mesh: gtoreq 10 mesh = 8:9:1, mechanically dispersing the mixed polyethylene pulp fiber slurry and deionized water, and concentrating to obtain the polyethylene pulp fiber slurry aqueous solution with the mass concentration of 0.01 wt%.
Comparative example 6
Unlike example 1, in step S1 of this comparative example, a polyethylene fiber was cut with a cutter to obtain a polyethylene staple fiber having a length of 10 mm.
Comparative example 7
Unlike example 1, in step S1 of this comparative example, the polyethylene fibers were cut with a cutter to obtain polyethylene staple fibers having lengths of 0.1mm, 3mm, 10mm and 15 mm.
The properties of the polyethylene nonwoven fabrics prepared in examples 1 to 7 and comparative examples 1 to 7 were examined, and the examination criteria were: after the non-woven fabric is subjected to constant temperature and humidity treatment, the quantitative measurement standard is GB/T451.2-2002; the thickness measurement standard is GB/T451.3-2002; the tensile strength and elongation measurement standard is GB/T12914-2008; the tear strength measurement standard is GB/T455-2002; the burst measurement standard is ISO 2758 (01); gurley air permeability measurement standard TAPPI T460; hydrostatic pressure measurement standard DIN EN 20811 (1992); peel strength test standard FZ/T80007.1-2006; puncture resistance strength test standard ASTM D3420. The results obtained by the detection are shown in table 1,
TABLE 1 physical Property measurement results
As is apparent from comparison of example 1 with comparative examples 1 and 2, when the ratio of polyethylene pulp fiber, polyethylene fibrids and ultra-high molecular weight chopped fibers does not fall within the scope of the present application, the mechanical and physical properties thereof are poor, mainly because the three fibers have different physical properties, and by reasonable collocation of the three different fibers, a polyethylene nonwoven fabric having excellent mechanical and physical properties is finally achieved, and more or less of any one material may cause deterioration of properties.
As is clear from examples 1, comparative examples 3, 4 and 5, the particle size of the polyethylene pulp fiber has a large influence on the mechanical and physical properties of the polyethylene nonwoven fabric, and the small-particle-size fiber has less branching after beating, but has a high degree of freedom, is easy to bend, and has a large particle size, and the large-particle-size fiber has a low degree of freedom, but has more branching after beating, and only the small-particle-size fiber, the medium-particle-size fiber and the large-particle-size fiber are matched with each other, so that the three-dimensional network structure is uniformly distributed on the spatial structure of the product, agglomeration or segregation is not easy to cause, and the mechanical properties are uniform.
As is apparent from examples 1, comparative examples 6 and 7, by limiting the length of the polyethylene staple fibers, physical overlap between the different length fibers is improved, so that the prepared polyethylene nonwoven fabrics have good mechanical properties.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (15)

1. A polyethylene nonwoven fabric, characterized in that the polyethylene nonwoven fabric comprises the following components:
Polyethylene pulp fiber: 20-70wt%;
polyethylene fibrids: 10-60wt%;
Polyethylene chopped fiber: 20-75wt%;
The polyethylene pulp fiber is prepared by flash spinning, after cutting, pulping and beating, the beating degree is 10-80 DEG SR, the beating degree of the polyethylene fibrid is 10-70 DEG SR, the length of the polyethylene chopped fiber is 3-10 mm, the fiber denier is 1-3D, and the polyethylene non-woven fabric is prepared by wet papermaking, squeezing, drying and hot pressing treatment after mixing;
the diameter range of the polyethylene pulp fiber is 0.1-18 mu m, the length after cutting is 0.1-20.0 mm, and the grain diameter ratio of the polyethylene pulp fiber is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1, a step of;
The crystallinity of the polyethylene pulp fiber is 60-70%, and the profile degree is 20-80%;
the polyethylene fibrids have a crystallinity of not more than 20%;
the polyethylene chopped fiber has a degree of profile of 30-80%.
2. The polyethylene nonwoven fabric according to claim 1, wherein the mass ratio of the polyethylene pulp fibers, the polyethylene fibrids and the polyethylene chopped fibers is: (1.2-2): 1: (1.5-2.1).
3. The polyethylene nonwoven fabric of claim 1 wherein said polyethylene chopped fibers are high density polyethylene filament chopped fibers or ultra high molecular weight polyethylene filament chopped fibers.
4. The method for preparing a polyethylene nonwoven fabric according to any one of claims 1 to 3, comprising the steps of:
preparing polyethylene pulp fiber slurry;
Preparing polyethylene fibrid slurry;
preparing a polyethylene chopped fiber slurry;
Pulping and mixing polyethylene pulp fiber slurry, polyethylene fibrid slurry and polyethylene chopped fiber slurry according to a proportion respectively, and carrying out wet papermaking, squeezing, drying and hot pressing treatment to obtain the polyethylene non-woven fabric;
The preparation of the polyethylene pulp fiber slurry comprises:
Adding polyethylene and a solvent R1 into a reaction kettle, controlling the reaction kettle to reach 140-250 ℃ at a heating rate of 0.1-10 ℃/min, keeping the pressure of 3-20 mpa, and preparing flash spinning fibers in a flash evaporation mode;
cutting the flash spinning fiber to 0.1-20 mm, and carrying out pulping and beating treatment to ensure that the beating degree of the polyethylene pulp fiber is 10-80 DEG SR;
After drying, carrying out hydrophilic treatment on the polyethylene pulp fiber to obtain the polyethylene pulp fiber;
the preparation of polyethylene fibrids comprises:
adding polyethylene and a solvent R2 into a reaction kettle, heating and stirring the reaction kettle to 160-200 ℃ to obtain a polyethylene solution;
mixing the polyethylene solution with a precipitating agent, shearing at least 10 minutes at the rotating speed of 2000-3000 r/min to form fibrids, cooling, molding and cleaning to obtain polyethylene fibrids;
The preparation of the polyethylene chopped fiber comprises:
and carrying out hydrophilic treatment on the polyethylene chopped fibers with the length of 3-10 mm, the fiber denier of 1-3D and the degree of dysmorphism of 30-80%.
5. The method for preparing a polyethylene nonwoven fabric according to claim 4, wherein the pulping process comprises: performing pulping treatment according to the concentration of 0.1-5wt% until the beating degree is 5-20 DEG SR;
The pulping treatment process comprises the following steps: after pulping, adding deionized water until the concentration is 0.01-0.1wt% for fluffing for 5-50 min, wherein the pulping pressure of the first stage is 8-22 kg, and the pulping time is 1-10 min; the second stage pulping pressure is 2-7 kg, and the pulping time is 30-200 min.
6. The method for producing a polyethylene nonwoven fabric according to claim 4, wherein the solvent R1 is one or more of alcohol, acid, amine, ester, ether, ketone, nitrile, amide, halogenated hydrocarbon, aliphatic hydrocarbon, aromatic hydrocarbon;
the temperature and pressure in the reaction kettle are controlled through auxiliary gas and heating, wherein the auxiliary gas is one or more of nitrogen, argon, helium, carbon dioxide and neon.
7. The method for preparing polyethylene non-woven fabrics according to claim 4, wherein the flash evaporation mode is that polymer spinning solution is sprayed out into air at 50-500 ℃ through a decompression nozzle of flash evaporation spinning equipment;
or the flash evaporation mode is to spray the polymer spinning solution into a mixture of a good solvent and a poor solvent of the polyethylene through a decompression nozzle of flash evaporation spinning equipment, wherein the good solvent accounts for 30-70%.
8. The method of producing a polyethylene nonwoven fabric according to claim 4, wherein cutting the flash spun fibers to 0.1 to 20mm comprises: and cutting off the flash spun fibers to obtain five lengths of fibers with the lengths ranging from 0.1 to 0.5mm, 1.5 to 5.5mm, 9 to 11mm, 14 to 16mm and 19 to 20mm respectively, and mixing the five lengths of flash spun chopped fibers with the same mass.
9. The method for preparing a polyethylene nonwoven fabric according to claim 8, wherein the solvent R2 is one or more of decalin, white oil, 1,2, 4-trichlorobenzene, mineral oil, paraffin oil, and kerosene.
10. The method for preparing polyethylene non-woven fabric according to claim 9, wherein the concentration of the polyethylene solution is 5-15wt%;
The precipitating agent is benzene solution or glycerin solution with concentration of 40-70wt% of solvent R2, the temperature of the precipitating agent is 80-120 ℃, and the mass ratio of the polyethylene solution to the precipitating agent is 1: 5-50.
11. The method for producing a polyethylene nonwoven fabric according to claim 4, wherein the hydrophilic treatment is to raise the surface energy of the fibers to at least 38 mN/m.
12. The method for preparing a polyethylene nonwoven fabric according to claim 11, wherein the hydrophilic treatment is corona treatment, and the corona treatment process is as follows: the voltage of corona treatment is 4000-16000V, the frequency is 12-26 KHz, the distance between an electrode rod and the absolute dry polymer fiber is 1-10 mm, and the air flow is 300-600 m 3/h;
Or the hydrophilic treatment is plasma treatment, and the plasma treatment process is as follows: the ionization power is 200-500W, the treatment time is 1-6 min, and the volume flow of the high-purity oxygen is 0.008-0.02L/min.
13. The method for preparing a polyethylene non-woven fabric according to claim 4, wherein the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the polyethylene chopped fiber slurry are respectively added with deionized water for fluffing and pulping to obtain a slurry aqueous solution with the concentration of 0.01-0.1wt%;
The grain size ratio of the polyethylene pulp fiber slurry is as follows: less than or equal to 100 meshes: 10-100 mesh: not less than 10 mesh= (1-8): (1-8): 1, a step of;
According to the polyethylene pulp fiber slurry: 20-70wt% of polyethylene fibrid slurry: 10-60 wt% of polyethylene chopped fiber slurry: and mixing 20-75wt% of the polyethylene pulp fiber slurry, the polyethylene fibrid slurry and the aqueous solution of the polyethylene chopped fiber slurry.
14. The method for preparing the polyethylene non-woven fabric according to claim 13, wherein the mass concentration of sizing in wet papermaking is 0.001-0.05%; the hot pressing adopts a mode of combining preheating and hot rolling, the preheating temperature is 80-115 ℃, the vehicle speed is 1-100 m/min, the line pressure is 0-50N/mm, and the preheating times are 1-5 times; the hot rolling temperature is 115-145 ℃, the speed is 1-100 m/min, the line pressure is 10-100N/mm, and the hot rolling times are 1-5.
15. The use of the polyethylene nonwoven fabric according to any one of claims 1 to 3 or the polyethylene nonwoven fabric prepared by the preparation method according to any one of claims 4 to 14, characterized in that the polyethylene nonwoven fabric is applied to the fields of insulation packaging, honeycomb core material, printing packaging, building waterproofing, ground covering, medical sterilization packaging, composite reinforcement and lithium battery separator.
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CN1647904A (en) * 2004-12-21 2005-08-03 东华大学 Method for preparing polyacrylonitrile pomace
CN213203314U (en) * 2020-05-26 2021-05-14 上海兰邦工业纤维有限公司 Ultrahigh molecular weight polyethylene pulp-shaped fiber

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DE2346081C2 (en) * 1973-09-13 1982-06-03 Basf Ag, 6700 Ludwigshafen Process for the production of aqueous suspensions from short polyolefin fibers
DE2363671C3 (en) * 1973-12-21 1979-09-20 Basf Ag, 6700 Ludwigshafen Process for the production of short fibers from low-pressure polyethylene
US4608089A (en) * 1985-07-19 1986-08-26 E. I. Du Pont De Nemours And Company Cement matrix composites and method of making same
US5000824A (en) * 1987-05-19 1991-03-19 E. I. Du Pont De Nemours And Company Polyethylene pulp

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Publication number Priority date Publication date Assignee Title
CN1647904A (en) * 2004-12-21 2005-08-03 东华大学 Method for preparing polyacrylonitrile pomace
CN213203314U (en) * 2020-05-26 2021-05-14 上海兰邦工业纤维有限公司 Ultrahigh molecular weight polyethylene pulp-shaped fiber

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