CN113174699B - Preparation method of graphene doped polypropylene melt-blown nonwoven fabric, melt-blown fabric and application of melt-blown fabric - Google Patents
Preparation method of graphene doped polypropylene melt-blown nonwoven fabric, melt-blown fabric and application of melt-blown fabric Download PDFInfo
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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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
- D01D5/0985—Melt spinning methods with simultaneous stretching by means of a flowing gas (e.g. melt-blowing)
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- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- 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
- D01F1/103—Agents inhibiting growth of microorganisms
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- 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
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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
- D04H1/56—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
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- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
Abstract
The application discloses a preparation method of graphene doped polypropylene non-woven fabric, which comprises the steps of uniformly dispersing functionalized graphene, preparing spinning raw materials, mixing by a high-speed mixer, feeding into a double-screw extruder, carrying out melt extrusion, carrying out cold cutting granulation to obtain a special melt-blown material, feeding the special melt-blown material into a single-screw extruder, carrying out heating and melting, extruding by a die head, forming nascent fibers by high-speed hot air drafting, cooling the nascent fibers into a net by cold air, and carrying out rolling to obtain the graphene doped polypropylene non-woven fabric. The prepared graphene doped polypropylene non-woven fabric plays multiple-effect protection functions of graphene, such as antibiosis, antivirus, antistatic, sealing and blocking, and has the advantages of good fiber web uniformity, fluffy and soft structure and good mechanical property.
Description
Technical Field
The application belongs to the technical field of non-woven fabrics, and particularly relates to a preparation method of graphene doped polypropylene melt-blown non-woven fabric, the melt-blown fabric and application thereof.
Background
The melt-blown nonwoven fabric is a nonwoven fabric which is produced by melting a polymer chip by a screw extruder, drawing a polymer melt stream extruded from a die orifice by a high-speed hot air stream, thereby forming a ultrafine fiber, collecting the ultrafine fiber on a screen or a drum, and bonding the ultrafine fiber to the screen or the drum by itself. The melt-blown nonwoven fabric has superfine fiber, good fiber web uniformity, fluffy and soft structure, and the superfine fiber in the fiber web is randomly arranged, has better filtering characteristics and a large number of tiny pores, and is widely applied to the aspects of filtering materials, sanitary materials, medical masks, battery diaphragms, oil absorbing materials and the like.
As nanomaterials have specific functions, particularly as nanomaterial fabrication techniques develop, their functionality becomes more and more apparent, researchers have added different functional nanomaterial particles to melt blown nonwovens according to different needs to improve their characteristics or impart new functions thereto. Currently, the addition of functional nanomaterial particles to meltblown fibers is mainly three ways: firstly, functional nano material particles and resin are extruded after being melted and blended in a screw, and the functional nano material melt-blown non-woven fabric is formed by high-speed hot air flow injection, and the method is reported in patents ZL200310107113.3 and US 6858551B 1. The method can uniformly disperse the nano material in the melt-blown fiber body to prevent dust falling, but easily causes stress concentration of the fiber to influence the mechanical property of the non-woven fabric to a certain extent. Secondly, the method is a post-finishing coating technology, functional nano material particles are adhered to the surface of melt fibers by means of an adhesive, but the functional nano material is difficult to exert all effects due to the coating effect of the adhesive, and the method has the defect of poor sanitation. Thirdly, when the molten resin is sprayed and molded under the action of high-speed hot air flow, functional nano particles are added near a die head, and most of melt-blown fibers still have viscosity at the moment, and particles adhere to the surfaces of the fibers or in gaps of a fiber net, so that the method is easy to play the effects of nano material particles, but the bonding fastness of the particles and the melt-blown fibers is weaker, and dust falling phenomenon is easy to generate. The melt-blown nonwoven fabric prepared by the method has the problems of low interception efficiency, incapability of directly killing harmful bacteria and the like, and limits the application range of the nonwoven fabric.
The graphene and the derivative are used as emerging two-dimensional multifunctional nano materials, have the advantages of excellent broad-spectrum antibacterial and antiviral capability, no generation of drug resistance of bacteria, simple preparation process, good biocompatibility and the like, and have good application potential in the fields of biomedicine, home textile, building engineering and the like compared with the traditional antibacterial and antiviral components. The antibacterial and antiviral capabilities of graphene materials are mainly based on the mixed synergistic effect of the following mechanisms: physical cutting, membrane surface component extraction, physical capture, oxidative stress, etc.
At present, the preparation methods of graphene modified nonwoven fabrics (such as ZL201710969519.4, CN108499220A and the like) mainly comprise a post-finishing coating method and a modified graphene oxide grafted resin masterbatch method, and the preparation methods are difficult to exert all effects of graphene and influence the mechanical properties of the nonwoven fabrics. At present, a method for preparing the graphene doped polypropylene melt-blown nonwoven fabric by adopting a double-screw blending granulation and single-screw melt-blown spinning process is not reported.
Disclosure of Invention
The graphene doped polypropylene non-woven fabric plays multiple-effect protection functions of graphene, such as antibiosis, antivirus, antistatic, sealing and blocking, has the advantages of good fiber web uniformity, fluffy and soft structure and good mechanical property, solves the difficult problems of graphene dispersion and composite forming, realizes the functionalization of the multifunctional protection non-woven material, is environment-friendly, and is convenient for industrial implementation.
The preparation method of the graphene doped polypropylene melt-blown nonwoven fabric comprises the following steps:
preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under a protective atmosphere, uniformly stirring, and adding hydrazine hydrate to obtain a functionalized graphene dispersion;
preparing a functionalized graphene doped polypropylene spinning raw material: the preparation method comprises the steps of mixing polypropylene resin, a dispersing agent, a coupling agent, a high-temperature stabilizer, an antioxidant and a plasticizer by a high-speed mixer, adding a functionalized graphene dispersion liquid (the functionalized graphene dispersion liquid can be added into a kneading-mixing machine for mixing uniformly to obtain a spinning raw material at normal temperature), and obtaining the spinning raw material with the graphene dispersed uniformly by the high-temperature kneading-mixing machine, wherein the dosage of the functionalized graphene in the spinning raw material is 3-15 wt%, the dosage of the dispersing agent is 1-8 wt%, the dosage of the coupling agent is 2-5 wt%, the dosage of the high-temperature stabilizer is 1-4 wt%, the dosage of the antioxidant is 0.1-2 wt%, and the dosage of the plasticizer is 1-4 wt%. The dosage of the polypropylene resin is the balance;
extruding, granulating and melt-blowing the spinning raw material to form the non-woven fabric. Preparing a special functionalized graphene doped polypropylene melt-blown material (i.e. granulating): and (3) feeding the spinning raw materials into a double-screw extruder, carrying out melt extrusion, and carrying out cold cutting granulation to obtain the special melt-blown material. Preparing graphene doped polypropylene nonwoven fabric (namely melt-blown nonwoven fabric): and (3) feeding the prepared special melt-blown material into a single-screw extruder, heating and melting, extruding through a die head, and forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and winding to obtain the graphene doped polypropylene non-woven fabric.
Preferably, the temperature of the twin-screw extruder is set to 80-110℃in the first zone, 110-140℃in the second zone, 140-160℃in the third zone, 160-180℃in the fourth zone, and 170-190℃in the fifth zone.
Preferably, the temperature of the single screw extruder is set to 120-140 ℃ in the first zone, 140-170 ℃ in the second zone, 170-190 ℃ in the third zone, 190-220 ℃ in the fourth zone, 190-220 ℃ in the fifth zone, and 200-220 ℃ in the die head.
Preferably, the spinneret has a pore size of 0.15 to 0.35 μm and an aspect ratio of (10 to 20): 1.
Preferably, the temperature of the hot air flow is 200-300 ℃ and the pressure is 0.2-0.5MPa.
Preferably, the cold air temperature is 10-20 ℃.
The application relates to an improvement of a preparation method of graphene doped polypropylene melt-blown nonwoven fabric, which comprises the steps of 0.5-5wt.% of graphene oxide, 50-75wt.% of phenylenediamine and 1-2wt.% of hydrazine hydrate when preparing functionalized graphene dispersion liquid.
According to the improvement of the preparation method of the graphene doped polypropylene melt-blown nonwoven fabric, when the functionalized graphene dispersion liquid is prepared, the atmosphere of a protector is nitrogen atmosphere or helium atmosphere.
According to the improvement of the preparation method of the graphene-doped polypropylene melt-blown nonwoven fabric, when the functionalized graphene-doped polypropylene spinning raw material is prepared, the dispersing agent is one or more of low-molecular-weight polyethylene wax, low-molecular-weight polypropylene wax and glyceryl tristearate.
According to the improvement of the preparation method of the graphene-doped polypropylene melt-blown nonwoven fabric, when the functionalized graphene-doped polypropylene spinning raw material is prepared, the coupling agent is one of silane coupling agents.
According to the improvement of the preparation method of the graphene-doped polypropylene melt-blown nonwoven fabric, when the functionalized graphene-doped polypropylene spinning raw material is prepared, the high-temperature stabilizer is one or more of zinc stearate, calcium stearate and dibutyl tin dimaleate.
According to the improvement of the preparation method of the graphene-doped polypropylene melt-blown nonwoven fabric, when the functionalized graphene-doped polypropylene spinning raw material is prepared, the antioxidant is one or more of hindered phenol antioxidants.
According to the improvement of the preparation method of the graphene-doped polypropylene melt-blown nonwoven fabric, when the functionalized graphene-doped polypropylene spinning raw material is prepared, the plasticizer is one or more of dioctyl adipate, dibutyl phthalate or dioctyl phthalate.
The application discloses a melt-blown cloth prepared by a preparation method of graphene doped polypropylene melt-blown non-woven cloth.
The melt-blown cloth of the application is applied to filter materials, sanitary materials, medical masks, battery diaphragms and oil absorbing materials.
The fiber diameter range of the graphene doped polypropylene non-woven fabric prepared by the preparation method is 0.2-2 mu m, and the weight is 20-100g/m 2 The total bacterial colony count is less than 200CFU/g, the total fungal colony count is less than 100CFU/g, the antibacterial rate to staphylococcus aureus and escherichia coli is more than 97%, the particulate matter filtering efficiency is more than 90%, and the bacterial filtering efficiency is more than 95%, and can be used as a protective material for preventing/killing/inhibiting viruses.
The method comprises the steps of uniformly dispersing functionalized graphene dispersion liquid, preparing spinning raw materials, carrying out melt extrusion in a double-screw extruder, carrying out cold cutting granulation to obtain a special melt-blown material, feeding the special melt-blown material into a single-screw extruder, carrying out heating and melting, extruding through a die head, forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and carrying out winding to obtain the graphene doped polypropylene non-woven fabric.
Compared with the prior art, the application has the beneficial effects that:
(1) The method plays the multi-effect protection functions of graphene, such as antibiosis, antivirus, antistatic, sealing and blocking, and the like, mainly solves the problems of graphene dispersion and composite forming, and realizes the functionalization of the multifunctional protection nonwoven material.
(2) The graphene doped polypropylene non-woven fabric prepared by the method has the advantages of good fiber web uniformity, fluffy and soft structure and good mechanical property, solves the key technical bottleneck problems of poor compatibility between nano material particles and melt-blown polymer resin, easiness in dust falling phenomenon and other application processes, and provides scientific basis for applying a new generation of non-woven material in the field of filtration protection.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a physical diagram of a graphene doped polypropylene nonwoven fabric of the present application;
FIG. 2 is a surface morphology electron microscope image of the graphene doped polypropylene nonwoven fabric prepared in example 11 of the present application;
fig. 3 is a cross-sectional morphology electron microscopy image of the graphene doped polypropylene nonwoven fabric of fig. 2.
Detailed Description
The present application will be described in detail with reference to the following embodiments. The embodiments are not intended to limit the application, but structural, methodological, or functional modifications of the application from those skilled in the art are included within the scope of the application.
Example 01
The preparation method of the nonwoven fabric in this embodiment includes preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under nitrogen atmosphere, stirring uniformly, and adding hydrazine hydrate to obtain a functionalized graphene dispersion liquid, wherein the dispersion liquid comprises 5wt.% of graphene oxide (the content of related components is the concentration in a solvent, the same applies below), 55wt.% of phenylenediamine and 1wt.% of hydrazine hydrate;
preparing a functionalized graphene doped polypropylene spinning raw material: mixing polypropylene resin, a dispersing agent low molecular weight polyethylene wax, a coupling agent silane coupling agent A172, a high-temperature stabilizer zinc stearate, an antioxidant hindered phenol antioxidant, and a plasticizer in a mass ratio of 2:3:4 by a high-speed mixer, adding a functionalized graphene dispersion liquid (the mixture can be added into a kneading-mixing machine for mixing uniformly to obtain a spinning raw material at once), and obtaining a spinning raw material with uniformly dispersed graphene by the high-temperature kneading-mixing machine at normal temperature, wherein the dosage of the polypropylene resin and the rest of the spinning raw material are 12wt.%, the dosage of the functionalized graphene is 1wt.%, the dosage of the dispersing agent is 2.5wt.%, the dosage of the coupling agent is 1.4wt.%, the dosage of the high-temperature stabilizer is 1.4wt.%, and the dosage of the plasticizer is 2wt.%;
granulating the spinning raw material by a screw extruder, wherein a double screw extruder can be adopted, and the temperature is controlled to be 80-110 ℃ in the first region, 110-140 ℃ in the second region, 140-160 ℃ in the third region, 160-180 ℃ in the fourth region and 170-190 ℃ in the fifth region; and extruding the melt-blown non-woven fabric by a single screw extruder, wherein the single screw extruder can be adopted, the control temperature is 120-140 ℃ in the first region, 140-170 ℃ in the second region, 170-190 ℃ in the third region, 190-220 ℃ in the fourth region, 190-220 ℃ in the fifth region, 200-220 ℃ in the die head, 0.30 mu m in the hole diameter of the spinneret plate, 10:1 in the length-diameter ratio, 220 ℃ in the hot air flow temperature, 0.2MPa in the pressure and 16 ℃ in the cold air temperature.
Example 02
The preparation method of the nonwoven fabric in this embodiment includes preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under helium atmosphere, stirring uniformly, and adding hydrazine hydrate to obtain a functionalized graphene dispersion liquid, wherein the dispersion liquid comprises 0.5wt.% of graphene oxide, 70wt.% of phenylenediamine and 2wt.% of hydrazine hydrate;
preparing a functionalized graphene doped polypropylene spinning raw material: mixing polypropylene resin, a dispersing agent glyceryl tristearate, a coupling agent silane coupling agent KH560, a high-temperature stabilizer dibutyl tin dimaleate, an antioxidant hindered phenol antioxidant, dioctyl adipate and dibutyl phthalate with a mass ratio of a plasticizer of 1:4 by a high-speed mixer, adding a functionalized graphene dispersion liquid (the mixture can be added into a kneading-mixing machine for mixing uniformly to obtain a spinning raw material at once), and obtaining a spinning raw material with uniformly dispersed graphene by the high-temperature kneading-mixing machine at normal temperature, wherein the dosage of the polypropylene resin is the balance, the functionalized graphene is 8 wt%, the dispersing agent is 8 wt%, the coupling agent is 5 wt%, the high-temperature stabilizer is 4 wt%, the antioxidant is 0.8 wt%, and the plasticizer is 3 wt%;
granulating the spinning raw material by a screw extruder, wherein a double screw extruder can be adopted, and the temperature is controlled to be 80-110 ℃ in the first region, 110-140 ℃ in the second region, 140-160 ℃ in the third region, 160-180 ℃ in the fourth region and 170-190 ℃ in the fifth region; and extruding the melt-blown non-woven fabric by a single screw extruder, wherein the single screw extruder can be adopted, the control temperature is 120-140 ℃ in the first region, 140-170 ℃ in the second region, 170-190 ℃ in the third region, 190-220 ℃ in the fourth region, 190-220 ℃ in the fifth region, 200-220 ℃ in the die head, 0.20 mu m in the spinneret aperture, 15:1 in the length-diameter ratio, 280 ℃ in the hot air flow temperature, 0.5MPa in the pressure and 18 ℃ in the cold air temperature.
Example 03
The preparation method of the nonwoven fabric in this embodiment includes preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under helium atmosphere, stirring uniformly, and adding hydrazine hydrate to obtain a functionalized graphene dispersion liquid, wherein the dispersion liquid comprises 1wt.% of graphene oxide, 65wt.% of phenylenediamine and 1.2wt.% of hydrazine hydrate;
preparing a functionalized graphene doped polypropylene spinning raw material: mixing polypropylene resin, dispersant low molecular polypropylene wax, coupling agent silane coupling agent KH550, high-temperature stabilizer calcium stearate, antioxidant hindered phenol antioxidant and plasticizer dibutyl phthalate by a high-speed mixer, adding functional graphene dispersion liquid (the functional graphene dispersion liquid can be added into a kneading-mixing machine for mixing uniformly to obtain spinning raw materials at once), and obtaining spinning raw materials with uniformly dispersed graphene by the high-temperature kneading-mixing machine at normal temperature, wherein the dosage of the polypropylene resin is the rest of the spinning raw materials, the dosage of the functional graphene is 10 wt%, the dosage of the dispersant is 6 wt%, the dosage of the coupling agent is 4 wt%, the dosage of the high-temperature stabilizer is 1 wt%, the dosage of the antioxidant is 2 wt%, and the dosage of the plasticizer is 1 wt%;
granulating the spinning raw material by a screw extruder, wherein a double screw extruder can be adopted, and the temperature is controlled to be 80-110 ℃ in the first region, 110-140 ℃ in the second region, 140-160 ℃ in the third region, 160-180 ℃ in the fourth region and 170-190 ℃ in the fifth region; and extruding the melt-blown non-woven fabric by a single screw extruder, wherein the single screw extruder can be adopted, the control temperature is 120-140 ℃ in the first region, 140-170 ℃ in the second region, 170-190 ℃ in the third region, 190-220 ℃ in the fourth region, 190-220 ℃ in the fifth region, 200-220 ℃ in the die head, 0.25 mu m in the hole diameter of the spinneret plate, 12:1 in the length-diameter ratio, 250 ℃ in the hot air flow temperature, 0.3MPa in the pressure and 15 ℃ in the cold air temperature.
Example 04
The preparation method of the nonwoven fabric in this embodiment includes preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under helium atmosphere, stirring uniformly, and adding hydrazine hydrate to obtain a functionalized graphene dispersion liquid, wherein the dispersion liquid comprises 2wt.% of graphene oxide, 50wt.% of phenylenediamine and 1.6wt.% of hydrazine hydrate;
preparing a functionalized graphene doped polypropylene spinning raw material: mixing polypropylene resin, low molecular weight polyethylene wax and low molecular weight polypropylene wax with the mass ratio of a dispersing agent of 1:5, a coupling agent silane coupling agent A-151, calcium stearate and dibutyl tin dimaleate with the mass ratio of a high-temperature stabilizer of 2:3, an antioxidant hindered phenol antioxidant and a plasticizer dioctyl adipate by a high-speed mixer, adding a functionalized graphene dispersion liquid (the functionalized graphene dispersion liquid can be optionally added into a kneading-mixing mill for mixing uniformly to obtain a spinning raw material at once), and obtaining a spinning raw material with uniformly dispersed graphene by the high-temperature kneading-mixing mill at normal temperature, wherein the dosage of the polypropylene resin and the functionalized graphene in the spinning raw material is 15 wt%, the dosage of the dispersing agent is 4 wt%, the dosage of the coupling agent is 3 wt%, the dosage of the high-temperature stabilizer is 3 wt%, the dosage of the antioxidant is 0.1 wt%, and the dosage of the plasticizer is 4 wt%;
granulating the spinning raw material by a screw extruder, wherein a double screw extruder can be adopted, and the temperature is controlled to be 80-110 ℃ in the first region, 110-140 ℃ in the second region, 140-160 ℃ in the third region, 160-180 ℃ in the fourth region and 170-190 ℃ in the fifth region; and extruding the melt-blown non-woven fabric by a single screw extruder, wherein the single screw extruder can be adopted, the control temperature is 120-140 ℃ in the first region, 140-170 ℃ in the second region, 170-190 ℃ in the third region, 190-220 ℃ in the fourth region, 190-220 ℃ in the fifth region, 200-220 ℃ in the die head, 0.35 mu m in the hole diameter of the spinneret plate, 18:1 in the length-diameter ratio, 300 ℃ in the hot air flow temperature, 0.4MPa in the pressure and 20 ℃ in the cold air temperature.
Example 05
The preparation method of the nonwoven fabric in this embodiment includes preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under nitrogen atmosphere, stirring uniformly, and adding hydrazine hydrate to obtain a functionalized graphene dispersion liquid, wherein the dispersion liquid comprises 4wt.% of graphene oxide, 75wt.% of phenylenediamine and 1.8wt.% of hydrazine hydrate;
preparing a functionalized graphene doped polypropylene spinning raw material: polypropylene resin, low molecular weight polyethylene wax, low molecular weight polypropylene wax, glyceryl tristearate, coupling agent silane coupling agent vinyl trimethoxysilane, zinc stearate, calcium stearate, dibutyl tin dimaleate, antioxidant hindered phenol antioxidant and plasticizer dioctyl phthalate with the mass ratio of 1:1:1:1 are mixed by a high-speed mixer, then added into functional graphene dispersion liquid (the functional graphene dispersion liquid can be added into a kneading-mixing machine for mixing uniformly to obtain spinning raw materials at one time), and the spinning raw materials with uniform graphene dispersion are obtained by the high-temperature kneading-mixing machine at normal temperature, wherein the dosage of the polypropylene resin in the spinning raw materials is the balance, the dosage of the functional graphene is 3 wt%, the dosage of the dispersing agent is 7 wt%, the dosage of the coupling agent is 2 wt%, the dosage of the high-temperature stabilizer is 2 wt%, the dosage of the antioxidant is 1.2 wt%, and the dosage of the plasticizer is 2.5 wt%.
Granulating the spinning raw material by a screw extruder, wherein a double screw extruder can be adopted, and the temperature is controlled to be 80-110 ℃ in the first region, 110-140 ℃ in the second region, 140-160 ℃ in the third region, 160-180 ℃ in the fourth region and 170-190 ℃ in the fifth region; and extruding the melt-blown non-woven fabric by a single screw extruder, wherein the single screw extruder can be adopted, the control temperature is 120-140 ℃ in the first region, 140-170 ℃ in the second region, 170-190 ℃ in the third region, 190-220 ℃ in the fourth region, 190-220 ℃ in the fifth region, 200-220 ℃ in the die head, 0.15 mu m in the hole diameter of the spinneret plate, 20:1 in the length-diameter ratio, 200 ℃ in the hot air flow temperature, 0.25MPa in the pressure and 10 ℃ in the cold air temperature.
Specifically, embodiments including but not limited to the following may be further employed:
example 11
The preparation method of the graphene doped polypropylene nonwoven fabric of the embodiment comprises the following steps:
A. adding Graphene Oxide (GO) into deionized water to form GO dispersion liquid, adding phenylenediamine and ammonia water into the GO dispersion liquid under the protection of N2, magnetically stirring to form uniform mixed liquid, and adding a reducing agent hydrazine hydrate into the mixed liquid to obtain functionalized (aminated modified) graphene, wherein the mass fraction of GO in the GO dispersion liquid is 0.5 wt%, the mass fraction of phenylenediamine is 55 wt%, and the mass fraction of hydrazine hydrate is 1 wt%.
B. Preparation of spinning raw materials: mixing polypropylene resin, low molecular weight polyethylene wax, vinyl trimethoxy silane, zinc stearate, 2, 6-di-tert-butylphenol and dibutyl phthalate by a high-speed mixer, adding a functionalized graphene dispersion liquid, and obtaining a spinning raw material with uniformly dispersed graphene by a high-temperature kneading-mixing machine; wherein the polypropylene resin is used in an amount of 70wt.%, the functionalized graphene is 20wt.%, the low molecular weight polyethylene wax is 4.5wt.%, the vinyltrimethoxysilane is 2.5wt.%, the zinc stearate is 1.5wt.%, the 2, 6-di-tert-butylphenol is 0.5wt.%, and the dibutyl phthalate is 1wt.%.
C. Preparation of special melt-blown materials: and (3) feeding the spinning raw materials into a double-screw extruder, carrying out melt extrusion, cold cutting and granulating to obtain the special melt-blown material, wherein the temperature of the double-screw extruder is set to be 90 ℃ in a first region, 110 ℃ in a second region, 140 ℃ in a third region, 160 ℃ in a fourth region and 180 ℃ in a fifth region.
D. Preparing graphene doped polypropylene non-woven fabric: and (3) feeding the prepared special melt-blown material into a single-screw extruder, heating and melting, extruding through a die head, and forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and winding to obtain the graphene doped polypropylene non-woven fabric. Wherein the temperature of the single screw extruder is set to be 130 ℃ in the first area, 150 ℃ in the second area, 170 ℃ in the third area, 190 ℃ in the fourth area, 200 ℃ in the fifth area and 210 ℃ in the die head. The aperture of the spinneret plate is 0.2 mu m, and the length-diameter ratio is 12:1. The temperature of the hot air flow is 220 ℃, and the pressure is 0.25MPa. The cool air temperature was 15 ℃.
The fiber diameter range of the prepared graphene doped polypropylene non-woven fabric is 0.5-0.85 mu m, the weight is 25g/m < 2 >, and the filtration efficiency of the graphene doped polypropylene non-woven fabric on particles with the particle diameter below 0.26 is 90.8% by adopting a TSI8130 filtration efficiency tester. The antibacterial/bacteriostatic test method is adopted to test that the antibacterial rate of staphylococcus aureus and escherichia coli reaches 99.2 percent, and the bacterial filtration efficiency reaches 99.1 percent.
Example 12
The preparation method of the graphene doped polypropylene nonwoven fabric of the embodiment comprises the following steps:
A. adding Graphene Oxide (GO) into deionized water to form GO dispersion liquid, adding phenylenediamine and ammonia water into the GO dispersion liquid under the protection of N2, magnetically stirring to form uniform mixed liquid, and adding a reducing agent hydrazine hydrate into the mixed liquid to obtain functionalized (aminated modified) graphene, wherein the mass fraction of GO in the GO dispersion liquid is 1.5wt.%, the mass fraction of phenylenediamine is 65wt.%, and the mass fraction of hydrazine hydrate is 1.5wt.%.
A. Preparation of spinning raw materials: mixing polypropylene resin, glyceryl tristearate, vinyl triethoxysilane, calcium stearate, 2, 8-di-tert-butyl-4-methylphenol and dioctyl adipate by a high-speed mixer, adding a functionalized graphene dispersion liquid, and obtaining a spinning raw material with uniformly dispersed graphene by a high-temperature kneading-mixing machine; wherein the polypropylene resin is used in an amount of 75wt.%, the functionalized graphene is 16wt.%, the glyceryl tristearate is 3.5wt.%, the vinyltriethoxysilane is 2.5wt.%, the calcium stearate is 1wt.%, the 2, 8-di-tert-butyl-4-methylphenol is 1wt.%, and the dioctyl adipate is 1wt.%.
B. Preparation of special melt-blown materials: and (3) feeding the spinning raw materials into a double-screw extruder, carrying out melt extrusion, cold cutting and granulating to obtain the special melt-blown material, wherein the temperature of the double-screw extruder is set to be 92 ℃ in a first region, 117 ℃ in a second region, 145 ℃ in a third region, 170 ℃ in a fourth region and 182 ℃ in a fifth region.
C. Preparing graphene doped polypropylene non-woven fabric: and (3) feeding the prepared special melt-blown material into a single-screw extruder, heating and melting, extruding through a die head, and forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and winding to obtain the graphene doped polypropylene non-woven fabric. Wherein the temperature of the single screw extruder is set to be 132 ℃ in the first zone, 156 ℃ in the second zone, 177 ℃ in the third zone, 192 ℃ in the fourth zone, 207 ℃ in the fifth zone and 211 ℃ in the die head. The spinneret aperture is 0.25 μm, and the length-diameter ratio is 13:1. The temperature of the hot air flow is 240 ℃ and the pressure is 0.3MPa. The cool air temperature was 15 ℃.
The fiber diameter range of the prepared graphene doped polypropylene non-woven fabric is 0.4-0.75 mu m, the weight is 30g/m < 2 >, and the filtration efficiency of the graphene doped polypropylene non-woven fabric on particles with the particle diameter below 0.26 is 93.6% by adopting a TSI8130 filtration efficiency tester. The antibacterial/bacteriostatic test method is adopted to test that the antibacterial rate of staphylococcus aureus and escherichia coli reaches 99.3 percent, and the bacterial filtration efficiency reaches 99.2 percent.
Example 13
The preparation method of the graphene doped polypropylene nonwoven fabric of the embodiment comprises the following steps:
A. adding Graphene Oxide (GO) into deionized water to form GO dispersion liquid, adding phenylenediamine and ammonia water into the GO dispersion liquid under the protection of N2, magnetically stirring to form uniform mixed liquid, and adding a reducing agent hydrazine hydrate into the mixed liquid to obtain functionalized (aminated modified) graphene, wherein the mass fraction of GO in the GO dispersion liquid is 2.5wt.%, the mass fraction of phenylenediamine is 70wt.%, and the mass fraction of hydrazine hydrate is 1.7wt.%.
B. Preparation of spinning raw materials: mixing polypropylene resin, low-molecular polypropylene wax, vinyl triethoxysilane, dibutyl tin dimaleate, 2, 6-di-tert-butylphenol and diethyl phthalate by a high-speed mixer, adding functional graphene dispersion liquid, and obtaining spinning raw materials with uniformly dispersed graphene by a high-temperature kneading-mixing machine; wherein the polypropylene resin is used in an amount of 79wt.%, the functionalized graphene is 12wt.%, the low molecular polypropylene wax is 2.5wt.%, the vinyltriethoxysilane is 3wt.%, the dibutyltin dimaleate is 1.2wt.%, the 2, 6-di-tert-butylphenol is 0.8wt.%, and the diethyl phthalate is 1.5wt.%.
C. Preparation of special melt-blown materials: and (3) feeding the spinning raw materials into a double-screw extruder, carrying out melt extrusion, cold cutting and granulating to obtain the special melt-blown material, wherein the temperature of the double-screw extruder is set to be 95 ℃ in a first region, 120 ℃ in a second region, 150 ℃ in a third region, 171 ℃ in a fourth region and 183 ℃ in a fifth region.
D. Preparing graphene doped polypropylene non-woven fabric: and (3) feeding the prepared special melt-blown material into a single-screw extruder, heating and melting, extruding through a die head, and forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and winding to obtain the graphene doped polypropylene non-woven fabric. Wherein the temperature of the single screw extruder is set to 127 ℃ in the first zone, 151 ℃ in the second zone, 177 ℃ in the third zone, 196 ℃ in the fourth zone, 210 ℃ in the fifth zone and 213 ℃ in the die head. The aperture of the spinneret plate is 0.2 mu m, and the length-diameter ratio is 15:1. The temperature of the hot air flow is 250 ℃, and the pressure is 0.3MPa. The cool air temperature was 10 ℃.
The fiber diameter range of the prepared graphene doped polypropylene non-woven fabric is 0.3-0.65 mu m, the weight is 35g/m < 2 >, and the filtration efficiency of the graphene doped polypropylene non-woven fabric on particles with the particle diameter below 0.26 is 95.5% by adopting a TSI8130 filtration efficiency tester. The antibacterial/bacteriostatic test method is adopted to test that the antibacterial rate of staphylococcus aureus and escherichia coli reaches 99.3 percent, and the bacterial filtration efficiency reaches 99.5 percent.
Example 14
The preparation method of the graphene doped polypropylene nonwoven fabric of the embodiment comprises the following steps:
A. adding Graphene Oxide (GO) into deionized water to form GO dispersion liquid, adding phenylenediamine and ammonia water into the GO dispersion liquid under the protection of N2, magnetically stirring to form uniform mixed liquid, and adding a reducing agent hydrazine hydrate into the mixed liquid to obtain functionalized (aminated modified) graphene, wherein the mass fraction of GO in the GO dispersion liquid is 3.5wt.%, the mass fraction of phenylenediamine is 75wt.%, and the mass fraction of hydrazine hydrate is 1.9wt.%.
B. Preparation of spinning raw materials: polypropylene resin, low molecular polypropylene wax, vinyl tri (beta-methoxyethoxy) silane, dibutyl tin dimaleate, 2, 8-di-tert-butyl-4-methylphenol and dioctyl adipate are mixed by a high-speed mixer, then functionalized graphene dispersion liquid is added, and a spinning raw material with uniformly dispersed graphene is obtained by a high-temperature kneading-mixing machine; wherein the polypropylene resin is used in an amount of 83wt.%, the functionalized graphene is 9wt.%, the low molecular polypropylene wax is 2wt.%, the vinyltris (β -methoxyethoxy) silane is 2wt.%, the dibutyltin dimaleate is 2wt.%, the 2, 8-di-tert-butyl-4-methylphenol is 0.7wt.%, and the dioctyl adipate is 1.3wt.%.
C. Preparation of special melt-blown materials: and (3) feeding the spinning raw materials into a double-screw extruder, carrying out melt extrusion, cold cutting and granulating to obtain the special melt-blown material, wherein the temperature of the double-screw extruder is set to be 100 ℃ in a first region, 130 ℃ in a second region, 156 ℃ in a third region, 172 ℃ in a fourth region and 185 ℃ in a fifth region.
D. Preparing graphene doped polypropylene non-woven fabric: and (3) feeding the prepared special melt-blown material into a single-screw extruder, heating and melting, extruding through a die head, and forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and winding to obtain the graphene doped polypropylene non-woven fabric. Wherein the temperature of the single screw extruder is set to be 130 ℃ in the first region, 155 ℃ in the second region, 180 ℃ in the third region, 200 ℃ in the fourth region, 211 ℃ in the fifth region and 215 ℃ in the die head. The spinneret aperture is 0.25 μm, and the length-diameter ratio is 15:1. The temperature of the hot air flow is 260 ℃ and the pressure is 0.35MPa. The cool air temperature was 12 ℃.
The fiber diameter range of the prepared graphene doped polypropylene non-woven fabric is 0.55-0.75 mu m, the weight is 40g/m < 2 >, and the filtration efficiency of the graphene doped polypropylene non-woven fabric on particles with the particle diameter below 0.26 is 96.2% by adopting a TSI8130 filtration efficiency tester. The antibacterial/bacteriostatic test method is adopted to test that the antibacterial rate of staphylococcus aureus and escherichia coli reaches 99.3 percent, and the bacterial filtration efficiency reaches 99.6 percent.
Example 15
The preparation method of the graphene doped polypropylene nonwoven fabric of the embodiment comprises the following steps:
A. adding Graphene Oxide (GO) into deionized water to form GO dispersion liquid, adding phenylenediamine and ammonia water into the GO dispersion liquid under the protection of N2, magnetically stirring to form uniform mixed liquid, and adding a reducing agent hydrazine hydrate into the mixed liquid to obtain functionalized (aminated modified) graphene, wherein the mass fraction of GO in the GO dispersion liquid is 4.5wt.%, the mass fraction of phenylenediamine is 72wt.%, and the mass fraction of hydrazine hydrate is 1.2wt.%.
B. Preparation of spinning raw materials: polypropylene resin, low molecular weight polyethylene wax, vinyl tri (beta-methoxyethoxy) silane, calcium stearate, 2, 8-di-tert-butyl-4-methylphenol and diethyl phthalate are mixed by a high-speed mixer, and then functionalized graphene dispersion liquid is added, and a spinning raw material with uniformly dispersed graphene is obtained by a high-temperature kneading-mixing machine; wherein the polypropylene resin is used in an amount of 84wt.%, the functionalized graphene is 7wt.%, the low molecular weight polyethylene wax is 3wt.%, the vinyltris (β -methoxyethoxy) silane is 2.2wt.%, the calcium stearate is 1.3wt.%, the 2, 8-di-tert-butyl-4-methylphenol is 0.4wt.%, and the diethyl phthalate is 1.6wt.%.
C. Preparation of special melt-blown materials: and (3) feeding the spinning raw materials into a double-screw extruder, carrying out melt extrusion, cold cutting and granulating to obtain the special melt-blown material, wherein the temperature of the double-screw extruder is set to be 102 ℃ in a first region, 131 ℃ in a second region, 153 ℃ in a third region, 170 ℃ in a fourth region and 181 ℃ in a fifth region.
D. Preparing graphene doped polypropylene non-woven fabric: and (3) feeding the prepared special melt-blown material into a single-screw extruder, heating and melting, extruding through a die head, and forming primary fibers through hot air high-speed drafting, cooling the primary fibers into a net through cold air, and winding to obtain the graphene doped polypropylene non-woven fabric. Wherein the temperature of the single screw extruder is set to 125 ℃ in a first area, 149 ℃ in a second area, 175 ℃ in a third area, 192 ℃ in a fourth area, 209 ℃ in a fifth area and 213 ℃ in a die head. The spinneret aperture is 0.3 mu m, and the length-diameter ratio is 16:1. The temperature of the hot air flow is 255 ℃, and the pressure is 0.25MPa. The cool air temperature was 11 ℃.
The fiber diameter range of the prepared graphene doped polypropylene non-woven fabric is 0.5-0.7 mu m, the weight is 50g/m < 2 >, and the filtration efficiency of the graphene doped polypropylene non-woven fabric on particles with the particle diameter below 0.26 is 98.3% by adopting a TSI8130 filtration efficiency tester. The antibacterial/bacteriostatic test method is adopted to test that the antibacterial rate of staphylococcus aureus and escherichia coli reaches 99.2 percent, and the bacterial filtration efficiency reaches 99.9 percent.
Including but not limited to the above embodiments, at least meets the following demonstrated good filtration and sterilization properties: the filtration efficiency of particles with the particle diameter of less than 0.26 is more than 90% by using a TSI8130 filtration efficiency tester. The sterilization/bacteriostasis test method is adopted to test the sterilization technical specification 2002, the bacteriostasis rate of staphylococcus aureus and escherichia coli is more than 99%, and the bacterial filtration efficiency is more than 99%.
It will be evident to those skilled in the art that the application is not limited to the details of the foregoing illustrative embodiments, and that the present application may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the application being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment contains only one independent technical solution, and that such description is provided for clarity only, and that the technical solutions of the embodiments may be appropriately combined to form other embodiments that will be understood by those skilled in the art.
Claims (9)
1. The preparation method of the graphene doped polypropylene melt-blown nonwoven fabric comprises the following steps:
preparing a functionalized graphene dispersion liquid: adding graphene oxide into deionized water, adding phenylenediamine and ammonia water under a protective atmosphere, uniformly stirring, and adding hydrazine hydrate to obtain a functionalized graphene dispersion liquid, wherein the graphene oxide is 0.5-5wt.%, the phenylenediamine is 50-75wt.%, and the hydrazine hydrate is 1-2wt.%;
preparing a functionalized graphene doped polypropylene spinning raw material: mixing polypropylene resin, a dispersing agent, a coupling agent, a high-temperature stabilizer, an antioxidant and a plasticizer by a high-speed mixer, adding a functionalized graphene dispersion liquid, and obtaining a spinning raw material with uniformly dispersed graphene by a high-temperature kneading-mixing mill, wherein the dosage of the polypropylene resin in the spinning raw material is 60-90 wt%, the dosage of the functionalized graphene is 5-25 wt%, the dosage of the dispersing agent is 1-10 wt%, the dosage of the coupling agent is 2-5 wt%, the dosage of the high-temperature stabilizer is 1-4 wt%, the dosage of the antioxidant is 0.1-2 wt%, and the dosage of the plasticizer is 1-4 wt%;
extruding, granulating and melt-blowing the spinning raw material to form the non-woven fabric.
2. The method for preparing the graphene-doped polypropylene melt-blown nonwoven fabric according to claim 1, wherein the protective gas atmosphere is a nitrogen atmosphere or a helium atmosphere when preparing the functionalized graphene dispersion liquid.
3. The method for preparing the graphene-doped polypropylene melt-blown nonwoven fabric according to claim 1, wherein the dispersing agent is one or more of low molecular weight polyethylene wax, low molecular weight polypropylene wax and glyceryl tristearate when preparing the functionalized graphene-doped polypropylene spinning raw material.
4. The method for preparing the graphene-doped polypropylene melt-blown nonwoven fabric according to claim 1, wherein the coupling agent is one of silane coupling agents when preparing the functionalized graphene-doped polypropylene spinning raw material.
5. The method for preparing the graphene-doped polypropylene melt-blown nonwoven fabric according to claim 1, wherein the high-temperature stabilizer is one or more of zinc stearate, calcium stearate and dibutyl tin dimaleate when preparing the functionalized graphene-doped polypropylene spinning raw material.
6. The method for preparing the graphene-doped polypropylene melt-blown nonwoven fabric according to claim 1, wherein the antioxidant is one or more of hindered phenol antioxidants when preparing the functionalized graphene-doped polypropylene spinning raw material.
7. The method for preparing the graphene-doped polypropylene melt-blown nonwoven fabric according to claim 1, wherein the plasticizer is one or more of dioctyl adipate, dibutyl phthalate or dioctyl phthalate when preparing the functionalized graphene-doped polypropylene spinning raw material.
8. The meltblown web produced by the process for producing a graphene-doped polypropylene meltblown nonwoven web according to any one of claims 1-7.
9. Use of the meltblown according to claim 8 in filtration materials, hygiene materials, medical masks, battery separators, oil absorbing materials.
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