CN114481626A - Conductive elastic non-woven material and preparation method thereof - Google Patents
Conductive elastic non-woven material and preparation method thereof Download PDFInfo
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- CN114481626A CN114481626A CN202210072628.7A CN202210072628A CN114481626A CN 114481626 A CN114481626 A CN 114481626A CN 202210072628 A CN202210072628 A CN 202210072628A CN 114481626 A CN114481626 A CN 114481626A
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- 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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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- 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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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
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Abstract
The invention provides a conductive elastic non-woven material and a preparation method thereof, which are used for solving the technical problems of poor heating performance, complex preparation process, low softness and poor wearing comfort of a heating fabric. The conductive elastic non-woven material prepared by the invention has excellent thinness, flexibility, softness, elasticity and controllable conductivity; the intelligent heating device is not only practical and intelligent and wearable, but also applicable to intelligent heating in various fields such as medical treatment, health and industry; meanwhile, the preparation method has the characteristics of short process flow, high production speed and low cost, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the field of fiber materials, relates to an ultrafine fiber elastic conductive material, and particularly relates to a conductive elastic non-woven material and a preparation method thereof.
Background
The heating fabric is used as one of intelligent wearable clothes, can generate heat through an external power supply to resist cold, has the advantages of good heating performance and wearing performance, is soft and comfortable to wear, and has the characteristics of light weight, thinness, softness and the like. Existing heating fabrics are mainly classified into two categories:
(1) passive heat generating thermal fabrics, also known as passive heat generation, provide increased thermal performance by providing thermal insulation properties to the fabric itself or by providing increased static air content or a thermal insulation layer to block heat transfer. Most of the traditional warm-keeping clothes are passive fabrics such as cotton clothes, down coats and the like. Passive heat-generating thermal fabrics simply maintain the constant temperature of the body by blocking the heat loss of the human body, for example, patent CN204080289U proposes to weave fabrics with hollow profiled fibers, and improve the thermal performance of the fabrics by static air in the hollow fibers. The passive thermal fabric needs to contain a large amount of still air for improving the thermal performance, so that the thickness of the fabric is difficult to reduce while the thermal performance is considered.
(2) The active heat-generating fabric converts other forms of energy (moisture absorption heating, electric heating, chemical energy heating, phase change heating, solar heating and the like) into heat energy when needed through special materials. The fabric can additionally provide heat to keep the temperature of the object to be covered under the extremely cold condition and the condition that the object to be covered generates heat and is not enough to survive. For example, patent CN213383346U proposes a moisture-absorbing and heat-generating fabric; patent CN213370134U proposes a heating scarf with an electric heating mechanism. The active heat generation can well adapt to the heat preservation of severe cold areas at high altitude and extremely cold areas in polar regions, and can also be applied to thin cold-proof fabrics (such as cold-proof sportswear, ski wear and the like).
The heating fabric prepared by adopting an electric heating mode has the advantages of high heating efficiency, controllable heating process and the like, and becomes the main research direction of the current wearable intelligent heat-insulating material. Adopt low resistance material to improve the performance that generates heat at present, the material that generates heat in the fabric that generates heat is mostly noble metal materials such as gold, silver and copper, but prepares this kind of conductive fabric and has the shortcoming that the price is high, the technology is complicated and the comfort of wearing is poor, and the benefit and the price/performance ratio of large-scale production exist inadequately. On the other hand, research and development personnel also pay more attention to the comfort and the air permeability of the fabric when improving the fabric heating efficiency, so that the current intelligent fabric with high heating efficiency and comfortable and breathable wearing is still a research and development difficulty.
The melt-blown non-woven material is a fiber aggregate consisting of superfine fibers, has the characteristics of softness, softness and porosity, has the characteristics of certain elasticity and toughness when the polyolefin elastomer is used as a raw material, and is a natural heating fabric base material. Therefore, the melt-blown elastic material can be developed to be used for thin, flexible and soft heating fabrics, and meanwhile, the melt-blown elastic material also has wide application prospects in multiple fields of intelligent wearability, medical health, industry and the like.
Disclosure of Invention
The invention provides a conductive elastic non-woven material and a preparation method thereof, aiming at the technical problems of thicker thickness, complex structure, low softness and poor wearing comfort of a heating fabric.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the structure of the conductive elastic non-woven material is characterized in that the non-woven material is an integrated structure formed by embedding a porous membrane and an ultrafine fiber aggregate.
Further, based on the recognition that the core of the conductive network is to reduce the resistance of the interface to be connected in series to form the conductive network, the porous membrane is preferably composed of aqueous polyurethane and graphene.
Furthermore, based on the comprehensive properties of softness, softness and elasticity of the hand feeling of the elastic heating fabric, the invention preferably selects the superfine fiber aggregate to be composed of the micro-nano conductive whiskers and the fibers composed of the polyolefin elastomer.
Further, in order to achieve the mutual embedment of the porous membrane and the ultrafine fiber aggregate, it is preferable that the ultrafine fiber aggregate of the present invention is characterized in that the porosity of the ultrafine fiber aggregate is 85 to 96%, and the areal density is 20 to 300g/m2Diameter of fiber<The number ratio of 2 μm is 20-30%, the fiber diameter is 2-10 μm and is 40-60%, and the fiber diameter is>The content of 10 μm is 10-40%.
Further, in the present invention, it is preferable that the mass ratio of the porous membrane to the ultrafine fiber aggregate is (1-10): (90-99).
A method of making a conductive elastic nonwoven material comprising the steps of:
(1) preparing an ultrafine fiber aggregate: the micro-nano conductive whiskers and the polyolefin elastomer are used as raw materials and are subjected to heterogeneous blending and melt-blowing to obtain the superfine fiber aggregate.
Further, the resistance of the melt-blown fiber product is mainly influenced by the resistance and the content of the conductive substance in the fiber; meanwhile, the carbon nano tube is a plurality of layers of coaxial circular tubes mainly composed of carbon atoms arranged in a hexagon shape, and has excellent electrical properties; therefore, in order to obtain controllable conductivity (resistance), the micro-nano conductive whiskers are preferably carbon nano tubes.
Further, in the present invention, it is preferable that the content of the carbon nanotubes in the ultrafine fiber aggregate is 0.5 to 3%.
Further, based on the knowledge of the melt-blowing forming process, equipment and material characteristics of the ultrafine fiber aggregate, the fiber diameter of the ultrafine fiber aggregate obtained by the melt-blowing method is mostly below 5 μm, and the diameter of the melt-blown spinneret orifice is mostly distributed between 0.2 mm and 0.4 mm; therefore, to avoid clogging of the spinneret orifices and to ensure production continuity, the present invention prefers carbon nanotubes to have a diameter of <300 nm.
Further, based on the knowledge of the melt-blowing process, equipment and material characteristics of the ultrafine fiber aggregate, the diameter of the fiber is mainly affected by the die temperature of melt-blowing and the viscosity of the raw material; the preferred polyolefin elastomer of the present invention is an ethylene-octene copolymer having a melt index of 35-1000g/10 min.
Further, based on the recognition that the polyolefin elastomer is an ethylene-octene copolymer, the preferred die temperature for the present invention is 180 ℃ and 280 ℃.
Further, based on the knowledge of the melt-blown forming process, equipment and material characteristics of the ultrafine fiber aggregate, the fiber crimp morphology and porosity are mainly affected by the acceptance distance and the hot air temperature; the temperature of the hot air is preferably 10-15 ℃ lower than the temperature of the die head, and the receiving distance is 15-50 cm.
(2) Preparing the conductive coating: and uniformly stirring the graphene dispersion liquid, the waterborne polyurethane, the wetting agent and the water to form the conductive coating.
Further, the resistance to the film material is mainly influenced by the resistance and the content of the conductive substance in the film; meanwhile, the graphene is a conductive material with a single-layer two-dimensional honeycomb lattice structure formed by tightly stacking carbon atoms; based on this, the present invention prefers graphene as the conductive substance within the membrane material.
Furthermore, the preferred graphene of the invention is characterized by the thickness of 1-3nm, the lamella diameter of 0.5-10 μm, the specific surface area of 500-2000m2/g。
Furthermore, the waterborne polyurethane is a polyurethane emulsion taking water as a solvent, a film is easy to form after drying, the viscosity can be easily adjusted by adding the proportion of water, no pollution is caused in the using process, and stimulation to the skin of a human body is not easy to generate; therefore, the invention prefers the waterborne polyurethane as the main film forming material of the film material.
Further, the preferred waterborne polyurethanes of the present invention are characterized by a solids content of 30% to 80%.
Further, in the present invention, in order to improve the interfacial compatibility between the film and the ultrafine fiber aggregate and to form a structure in which the film and the ultrafine fiber aggregate are embedded with each other, a wetting agent is preferably used as a film-forming aid.
Furthermore, the active substance of the wetting agent is octyl phenol polyoxyethylene ether, the content is more than 70 percent, and the PH value is 6.0-7.5.
Furthermore, the preferred mass ratio of the graphene dispersion liquid to the aqueous polyurethane to the wetting agent to water in the invention is (10-18): (2-10): 4: 1.
(3) compounding a base material and a conductive coating: and (3) compounding the superfine fiber aggregate prepared in the step (1) and the conductive coating prepared in the step (2) through a multi-time padding process to form a composite material.
Further, based on the knowledge of the non-woven composite process, the present invention preferably compounds the ultrafine fiber aggregate prepared in the step (1) with the conductive coating prepared in the step (2) by a padding process.
Furthermore, the invention preferably repeats the padding process and the drying for 1-5 times to improve the wetting property and the uniformity.
Further, the liquid carrying rate of the padding process is 100-150%.
(4) Formation of the ultrafine fibrous conductive nonwoven material: and (4) drying the composite material prepared in the step (3) to form the conductive elastic non-woven material.
Further, based on the knowledge of the characteristics of the graphene dispersion, the aqueous polyurethane, the wetting agent, the polyolefin elastomer and the carbon nanotube, the preferred drying temperature of the present invention is 80 to 95 ℃.
The invention has the following beneficial effects:
(1) the conductive elastic non-woven material obtained by the invention fully utilizes the characteristics of flexibility, softness and conductivity of the graphene-polyurethane porous membrane and the carbon nano tube-polyolefin elastic superfine fiber aggregate, and forms an integrated structure by embedding the graphene-polyurethane porous membrane and the carbon nano tube-polyolefin elastic superfine fiber aggregate, so that the conductive elastic non-woven material not only has the characteristics of excellent thinness, softness and elasticity, but also has controllable conductivity, and can meet the technical requirements of the conductive elastic non-woven material in the fields of clothing, industry, medical use and the like;
(2) the method for preparing the superfine fiber aggregate by using the carbon nano tube and the polyolefin elastomer as raw materials and adopting the melt-blowing process has the advantages of simple production process, controllable performance, convenient operation, environmental protection and low cost; the obtained superfine fiber aggregate has good superfine fiber structure and bonding form among fibers; as can be known by a Phabrometer test method (AATCC TM 202), the material has excellent flexibility when the flexibility score is 5-90 and the smoothness score is 2-80 (AATCC TM 202-2014);
(3) the conductive coating is prepared by taking the graphene dispersion liquid, the waterborne polyurethane, the wetting agent and the water as raw materials, and is compounded with the superfine fiber aggregate by a padding process, so that the conductive coating has the characteristics of easiness in film formation, no pollution, no stimulation and controllable liquid carrying rate; the prepared conductive elastic non-woven material has the longitudinal elongation at break of 370-650 percent, the transverse elongation at break of 190-310 percent (GB/T24218.3-2010), the transverse elastic recovery of 65-80 percent and the longitudinal elastic recovery of 70-90 percent (FZT 01034-;
(4) the conductive elastic non-woven material obtained by the invention has the advantages of good conductivity, small resistance and the like, so that the conductive elastic non-woven material has good effect in the active heating process; the conductive elastic nonwoven material has an areal density of 80g/m2When the resistance is high (GB/T24218.1-2009), the resistance of the material is 20-3000 omega;
(5) in conclusion, the conductive elastic non-woven material prepared by the invention is suitable for multiple fields of intelligent wearability, medical treatment, health, industry and the like, and is also suitable for intelligent heating; meanwhile, the preparation method has the characteristics of short process flow, high production speed and low cost, and is suitable for large-scale industrial production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic representation of the preparation of an assembly of ultrafine fibers according to example 1;
FIG. 2 is a schematic surface electron microscope showing the production of an ultrafine fibrous aggregate according to example 1;
FIG. 3 is a schematic cross-sectional electron microscope illustrating the preparation of an ultrafine fiber aggregate according to example 1;
FIG. 4 is a schematic view of a process for preparing an assembly of ultrafine fibers. Wherein 4-1 is a feeding funnel, 4-2 is a screw extruder, 4-3 is a polymer melt, 4-4 is a spinning manifold, 4-5 is superfine fiber, 4-6 is a vacuum suction system, and 4-7 is a net collecting curtain;
FIG. 5 is a schematic view of a composite process flow of the ultrafine fiber aggregate and the conductive coating, wherein 5-1 is the ultrafine fiber aggregate, 5-2 is a container, 5-3 is the graphene dispersion, 5-4 is the waterborne polyurethane, 5-5 is water, 5-6 is the wetting agent, 5-7 is the melt-blown elastic nonwoven material, 5-8 is a press roll, and 5-9 is an oven;
FIG. 6 is a surface electron micrograph of a conductive elastic nonwoven;
FIG. 7 is a high power electron micrograph of the surface of a conductive elastic nonwoven;
FIG. 8 is a cross-sectional electron micrograph of a conductive elastic nonwoven;
FIG. 9 is a representation of an electrically conductive elastic nonwoven material;
FIG. 10 is a graph of the heating curve of a conductive elastic nonwoven material;
fig. 11 is an infrared thermography of the conductive elastic nonwoven material when it heats up.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
The preparation process of the superfine fiber aggregate is shown in figure 4, the polyolefin elastomer slice and the carbon nano tube are mixed and then added into a feeding funnel 4-1, the polyolefin elastomer slice is preheated and melted by a screw extruder 4-2 to form a polymer solution 4-3 which enters a spinning manifold 4-4, the polymer solution is drafted by a spinneret to form superfine fibers 4-5, and the superfine fibers 4-5 are deposited on a collecting net curtain 4-7 by utilizing a vacuum suction system 4-6 to obtain the superfine fiber aggregate;
the compounding process of the superfine fiber aggregate and the conductive coating is shown in figure 5, the superfine fiber aggregate 5-1 is placed in a container 5-2 filled with a conductive solution, when a mixed solution consisting of 5-3 parts of graphene dispersion, 5-4 parts of waterborne polyurethane, 5-5 parts of water and 5-6 parts of a wetting agent is completely immersed in pores of the superfine fiber aggregate 5-1, a compression roller 5-8 is utilized to pressurize, redundant solution on the surface of the material is removed, and the material is placed in an oven 5-9 to be dried, so that the melt-blown elastic non-woven material 5-7 is obtained.
Example 1
The preparation method of the conductive elastic non-woven material comprises the following steps:
preparing an ultrafine fiber aggregate: slicing the polyolefin elastomer and the carbon nanotubes in a weight ratio of 7: 3 after being uniformly mixed, the mixture is formed by a melt spinning process, the diameter of which is 10-14um, the porosity of which is 70-80 percent and the surface density of which is 75-85g/m2The ultrafine fiber aggregate of (2). The type of the polyolefin elastomer is 7050FL, the ethylene component is about 13%, the melt index (190 ℃/2.16 kg) is 10-30g/10min, and the melt flow rate (230 ℃/2.16 kg) is 30-50g/10 min; the resistivity of the multi-wall carbon nano tube is 0.2-0.3 omega cm. The specific melt-blown process parameters are set as follows: metering pump temperature 200 ℃, melt-blown die temperature 250 ℃, screw extruder temperature (first zone-fourth zone): 200 ℃, 230 ℃, 250 ℃ and 250 ℃; the speed of the metering pump is 5Hz, and the receiving distance is 15 cm;
preparing the conductive coating: mixing graphene dispersion liquid, waterborne polyurethane, wetting agent X405 and water according to mass ratio64: 16: 16: 4, mixing and uniformly stirring to obtain the conductive coating. The graphene purity in the graphene dispersion liquid is 99%, the graphene thickness is 3.4-8nm, and the specific surface area is 100-2(ii)/g, conductivity 105S/m; the solid content of the waterborne polyurethane is 60 percent, and the specific gravity is 1.5g/cm3(ii) a The content of active substance octyl phenol polyoxyethylene ether in the wetting agent is 70 percent, the PH value is 6.0-7.5, and the HLB is 17.9;
preparing a conductive elastic non-woven material: and (3) soaking the prepared superfine fiber aggregate in a conductive coating, pressing the soaked material by a compression roller, removing redundant conductive solution on the surface of the material, and then putting the material into an oven for drying to prepare the conductive elastic non-woven material.
As shown in FIGS. 1-3, the morphology structure of the ultrafine fiber aggregate shows that the fiber aggregate has uniform morphology and certain adhesion between fibers, which is beneficial to improving the mechanical properties of the fiber aggregate. The surface structure of the conductive elastic non-woven material is shown in figure 9, the surface structure is shown in figures 6-7, the cross-sectional structure is shown in figure 8, the conductive coating is uniformly loaded and successfully permeates into the empty pores of the fiber aggregate, so that the conductivity of the elastic non-woven material and the uniformity of film forming are improved.
Example 2
The method for preparing the conductive elastic nonwoven material is different from the method of example 1 in that the weight ratio of the polyolefin elastomer chip to the carbon nanotube in the preparation of the ultrafine fiber aggregate is 5: 5, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 3
The method for preparing the conductive elastic nonwoven material is different from the method of example 1 in that the weight ratio of the polyolefin elastomer chip to the carbon nanotube in the preparation of the ultrafine fiber aggregate is 6: 4, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 4
The method for preparing the conductive elastic nonwoven material is different from the method of example 1 in that the weight ratio of the polyolefin elastomer chip to the carbon nanotube in the preparation of the ultrafine fiber aggregate is 8: 2, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 5
The difference between the preparation method of the conductive elastic nonwoven material and the embodiment 1 is that the mass mixing ratio of the graphene dispersion liquid, the aqueous polyurethane, the wetting agent X405 and the water is 40: 40: 16: 4, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 6
The difference between the preparation method of the conductive elastic nonwoven material and the embodiment 1 is that the mass mixing ratio of the graphene dispersion liquid, the aqueous polyurethane, the wetting agent X405 and the water is 48: 32: 16: 4, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 7
The difference between the preparation method of the conductive elastic nonwoven material and the embodiment 1 is that the mass mixing ratio of the graphene dispersion liquid, the aqueous polyurethane, the wetting agent X405 and the water is 56: 24: 16: 4, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 8
The difference between the preparation method of the conductive elastic nonwoven material and the embodiment 1 is that the mixing ratio of the graphene dispersion liquid, the aqueous polyurethane, the wetting agent X405 and the water is 72: 8: 16: 4, the prepared conductive elastic non-woven material has the surface density of 80g/m2。
Example 9
The preparation method of the conductive elastic non-woven material comprises the following steps: the difference between this example and example 1 is that the impregnation, roll passing and drying process was repeated 2 times to improve the wettability and uniformity, and the resulting conductive elastic nonwoven material had an areal density of 80g/m2。
Example 10
The preparation method of the conductive elastic non-woven material comprises the following steps: this example is different from example 1 in that the impregnation-roll and drying process was repeated 3 times to obtain a conductive elastic nonwoven material having an areal density of 80g/m2。
Examples of the effects of the invention
The ultrafine fibrous conductive nonwoven materials prepared in examples 1 to 10 were subjected to tests for areal density, thickness, transverse and longitudinal rupture strength, transverse and longitudinal rupture elongation, transverse and longitudinal elastic recovery, burst strength, air permeability, flexibility score, electrical resistance and heat generation, and the related test methods were as follows:
test for areal Density
The test method comprises the following steps: the test is carried out by adopting a sample of 100cm2Sampling by a disc sampler, taking five samples, taking the samples to test on a balance, and then averaging.
And (4) testing standard: GB/T24218.1-2009 textile nonwoven test methods part 1: determination of Mass per area
Testing an instrument: high precision electronic balance (BK-303G model, Dongguan Yi Xue electronics Co., Ltd., China)
Thickness measurement
The test method comprises the following steps: sampling was performed with a 100cm2 disk sampler, five samples were taken, and 5 data were sequentially tested and averaged.
And (4) testing standard: GB/T24218.2-2009 textile nonwoven test methods part 2: thickness measurement.
Testing an instrument: digital fabric thickness gauge (model YG141D, Darong textile instruments Inc., Wenzhou, China).
Longitudinal and transverse rupture strength and rupture elongation test
The test method comprises the following steps: the specification of a sample specified by the national standard is longer than 200mm, the width is 50mm, the clamping distance is 200mm, but the specification is limited by a test prototype, the breadth of the prepared melt-blown elastic cloth is about 200mm, and the elastic cloth has good elasticity and cannot meet the standard requirement. Therefore, the experimental samples are reduced in equal proportion, 5 samples are adopted in the experiment in the longitudinal and transverse directions, the sample specification is 170mm in length and 50mm in width, the clamping distance is 50mm, the stretching speed is 100mm/min, and the average value is calculated.
And (4) testing standard: GB/T24218.3-2010 textile nonwoven test method part 3: determination of breaking Strength and elongation at Break ".
Testing the instrument: comprehensive experiment machine for mechanical properties of fabric (model YG026MD, Wenzhou Square and round instruments, Inc., China).
Longitudinal and transverse elastic recovery test
The test method comprises the following steps: the test sample is reduced in equal proportion by the same test of the stretching performance of the elastic polyolefin melt-blown non-woven fabric under the influence of the specification of the non-woven sample fabric, and the test sample adopts 5 pieces of each sample in the longitudinal and transverse directions, wherein the sample specification is 170mm in length and 50mm in width, the clamping distance is 50mm, the stretching speed is 50mm/min, the return speed is 25mm/min, the elongation is 15%, the holding time is 10 s, the rest time is 20 s, and the cycle is carried out for 2 times.
And (4) testing standard: since no nonwoven elasticity standard was found, the test was performed according to the textile fabric standard: method for testing tensile elastic recovery rate of fabric knitted by FZT 70006-.
Testing an instrument: mechanical property analyzer (HD 026S-100, Nantong grand laboratory instruments Co., Ltd, China)
Burst strength test
And (3) testing conditions are as follows: sampling by using a 100cm2 disc sampler, taking five samples, wherein the head end of the ejector rod is a polishing steel ball, the diameter of the ball is 25mm, and the bursting speed is 300 mm/min. Each sample was tested for 5 groups and averaged.
And (4) testing standard: GB/T19976 Specification of the bursting Strength of textile materials 2005.
Testing an instrument: comprehensive experiment machine for mechanical properties of fabric (model YG026MD, Wenzhou Square and round instruments, Inc., China).
Air permeability test
And (3) testing conditions are as follows: by 100cm2Sampling with a disc sampler, taking five samples, adjusting the equipment to an automatic mode, testing the pressure difference to be 100Pa, and testing the area to be 20cm2The air permeability of each sample was recorded and averaged.
And (4) testing standard: GB/T24218.15-2018 test method for textile nonwovens section 15 determination of air permeability.
Testing the instrument: full-automatic air permeameter (YG 461E-III, Ningbo textile machinery Mill, China).
Flexibility test
And (3) testing conditions are as follows: a disc sampler having an area of 100cm2 was used to cut out 3 pieces of the sample, and the sample was conditioned in a constant temperature and humidity cabinet for 24 hours. During the test, all weights are removed, the softness of the sample is tested under the condition of no pressure, and the result is averaged.
And (4) testing standard: AATCC TM202 textile garment assessment relative to hand value: instrumental methods.
Testing an instrument: PhabrOmeter fabric stylizer (F1S 3-10, literary science and technology limited, usa).
Resistance testing
And (3) testing conditions are as follows: the sample is cut into a rectangular sample with the length of 50mm and the width of 30mm, the positive pole and the negative pole are placed at the two ends of the sample to measure the resistance, ten data are tested on each sample, and the average value is calculated.
Testing an instrument: resistance meter (TH 2516B, Council electronics, Inc., China).
Heating test
And (3) testing conditions are as follows: the positive and negative electrodes of a direct current power supply are placed on two sides of a sample, a certain voltage is introduced, a temperature controller is started, and the heating temperature of the melt-blown base elastic heating body is detected through a temperature sensor. FIG. 10 shows the heat generation test curve, and FIG. 11 shows the heat generation effect of the sample.
Testing an instrument: a single-channel direct-current power supply (UDP 5306, uli de tech ltd., china), and a temperature controller (SIN-7000C, co-testing automation technology ltd., china).
The test results were as follows:
as can be seen, the conductive elastic nonwoven material prepared in the present application sufficiently balances flexibility and electrical resistance. Meanwhile, the superfine fiber aggregate prepared from the polyolefin elastomer is used as a base material, and the elastic material endows the superfine fiber aggregate with excellent elasticity; the superfine fiber main body structure and the physical entanglement form endow the fabric with excellent flexibility. In addition, the table shows that the conductive elastic non-woven material prepared by the invention also has better mechanical property, is different from the traditional woven structure, is used for clothing materials, and has good heating effect and mechanical property.
In conclusion, the conductive elastic non-woven material prepared by the method is an integrated structure with flexibility, elasticity and various pore characteristics, can meet the technical requirements of application in the fields of clothing, industry, medical use and the like, achieves the purpose of active heating, has a wider application range and has better usability.
Claims (10)
1. An electrically conductive elastic nonwoven material characterized by: the conductive coating is prepared by mixing graphene dispersion liquid, waterborne polyurethane, wetting agent solution and water.
2. The conductive elastic nonwoven material of claim 1, wherein: the mass ratio of the porous membrane to the superfine fiber aggregate is (1-10): (90-99).
3. The conductive elastic nonwoven material of claim 2, wherein: the superfine fiber aggregate has porosity of 85-96% and area density of 20-300g/m2Diameter of fiber<The number ratio of 2 μm is 20-30%, the fiber diameter is 2-10 μm and is 40-60%, and the fiber diameter is>The content of 10 μm is 10-40%.
4. The conductive elastic nonwoven material of claim 3, wherein: the polyolefin elastomer is an ethylene-octene copolymer, and the melt index of the ethylene-octene copolymer is 35-1000g/10 min; the micro-nano conductive whiskers are carbon nano tubes, and the diameters of the carbon nano tubes are less than 300 nm; the content of the carbon nano-tube in the superfine fiber aggregate is 0.5-3%.
5. The electrical conduction of claim 2An elastic nonwoven material characterized by: the thickness of the graphene in the graphene dispersion liquid is 1-3nm, the sheet diameter of the graphene is 0.5-10 mu m, and the specific surface area is 500-2000m2(iv) g; the solid content of the waterborne polyurethane is 30-80%; the active component in the wetting agent is octyl phenol polyoxyethylene ether.
6. The conductive elastic nonwoven material of claim 5, wherein: the mass ratio of graphene dispersion liquid, waterborne polyurethane, wetting agent and water in the conductive coating is (10-18): (2-10): 4: 1.
7. the conductive elastic nonwoven material of any of claims 1-6, wherein: the conductive elastic non-woven material has the surface density of 30-330g/m2The elongation at break in the longitudinal direction is 370% -650%, the elongation at break in the transverse direction is 190% -310%, the transverse elastic recovery rate is 65-80%, and the longitudinal elastic recovery rate is 70% -90%; the resistance of the conductive elastic non-woven material is 20-3000 omega, the flexibility score is 5-90, and the smoothness score is 2-80.
8. The method of preparing an electrically conductive elastic nonwoven material of claim 7 comprising the steps of:
preparing an ultrafine fiber aggregate: mixing the micro-nano conductive whiskers and the polyolefin elastomer, and carrying out heterogeneous blending and melt-blowing to prepare a superfine fiber aggregate;
preparing the conductive coating: uniformly stirring the graphene dispersion liquid, the aqueous polyurethane solution, the wetting agent and water to prepare the conductive coating;
preparing a conductive elastic non-woven material: and compounding the superfine fiber aggregate in the conductive coating through a padding process to form a composite material, and drying to obtain the conductive elastic non-woven material.
9. The method of preparing a conductive elastic nonwoven material of claim 8, wherein: the die head temperature of the heterogeneous blending melt-blowing process in the preparation process of the superfine fiber aggregate is 180-280 ℃, the hot air temperature is 10-15 ℃ lower than the die head temperature, and the receiving distance is 15-50 cm.
10. The method of preparing a conductive elastic nonwoven material of claim 8, wherein: the padding and drying processes are repeated for 1-5 times in the preparation of the conductive elastic non-woven material, and the temperature of the padding liquid is 8-45 ℃; the composite material is characterized by the liquid carrying rate of 100-150%; the drying temperature is 80-95 ℃.
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