CN114232349A - Preparation method and equipment of high-conductivity superfine fiber synthetic leather - Google Patents

Preparation method and equipment of high-conductivity superfine fiber synthetic leather Download PDF

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Publication number
CN114232349A
CN114232349A CN202111491376.3A CN202111491376A CN114232349A CN 114232349 A CN114232349 A CN 114232349A CN 202111491376 A CN202111491376 A CN 202111491376A CN 114232349 A CN114232349 A CN 114232349A
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superfine fiber
synthetic leather
resin
film forming
conductivity
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张鹏
王剑
罗晓民
王怡然
冯见艳
刘丽成
曹植
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0004—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using ultra-fine two-component fibres, e.g. island/sea, or ultra-fine one component fibres (< 1 denier)
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C11/00—Component parts, details or accessories not specifically provided for in groups B05C1/00 - B05C9/00
    • B05C11/10—Storage, supply or control of liquid or other fluent material; Recovery of excess liquid or other fluent material
    • B05C11/1039—Recovery of excess liquid or other fluent material; Controlling means therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
    • B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
    • B05C3/09—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
    • D06N3/0075—Napping, teasing, raising or abrading of the resin coating
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
    • D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N2209/00—Properties of the materials
    • D06N2209/04—Properties of the materials having electrical or magnetic properties
    • D06N2209/041—Conductive
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    • D06N2211/00—Specially adapted uses
    • D06N2211/12—Decorative or sun protection articles
    • D06N2211/28—Artificial leather

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)

Abstract

A preparation method of high-conductivity superfine fiber synthetic leather comprises the following steps: 1) pretreating superfine fiber non-woven fabric; 2) roller coating of composite resin; 3) polishing the surface; 4) front pressure driving film forming; 5) hot-pressing and shaping; the front-pressure driven film forming equipment is in a high-pressure closed environment, the conductive nano film forming solution is stored in the tank body, the bottom of the tank body is provided with a porous supporting filter plate, and the top of the tank body is provided with a high-pressure air inlet adjusting valve; the high-conductivity superfine fiber synthetic leather prepared by the invention has a gradient conductive multilayer structure, the surface of the high-conductivity superfine fiber synthetic leather is a compact and orderly stacked nano conductive layer, the middle layer is a composite resin layer with a porous structure, and the bottom of the high-conductivity superfine fiber synthetic leather is an insulated superfine fiber substrate. The preparation method is simple in process and low in cost, is expected to realize industrial production, and has potential application value in the fields of smart home, electromagnetic shielding, wearable equipment and military protection.

Description

Preparation method and equipment of high-conductivity superfine fiber synthetic leather
Technical Field
The invention belongs to the technical field of functional synthetic leather, and particularly relates to a preparation method and equipment of high-conductivity superfine fiber synthetic leather.
Background
Along with the continuous development of internet of things science and technology, the demand of fields such as intelligent home, flexible wearable equipment and protective equipment on flexible conducting materials is also more and more. The superfine fiber synthetic leather has extremely excellent wear resistance, excellent cold resistance, air permeability and aging resistance by virtue of the three-dimensional network structure of the imitated natural leather, and has gradually become one of the mainstream directions for the development of high-performance synthetic leather. Among them, the conductive superfine fiber synthetic leather has a very important position in the fields of public transportation, military protection and intelligence. However, the current technology for preparing conductive synthetic leather is that nano-fillers (such as graphene, carbon nanotubes, carbon black, nano-metal particles, etc.) with conductive properties are added into a resin matrix and then compounded into a base fabric through processes of dipping, coating, spraying, etc. Even if the nano conductive materials are subjected to surface modification, the nano conductive materials are difficult to uniformly disperse in a resin matrix to form a stable conductive path, so that the conductivity of the composite resin is relatively low. In addition, the nano metal filler is liable to cause precipitation, agglomeration and the like in the resin matrix due to its high specific gravity. And the interaction force between part of the nano conductive filler and the resin is weaker, so that the physical property of the resin is easily reduced. This is not conducive to the practical production and application of the conductive synthetic leather. Therefore, it is important to develop a technology for preparing high-conductivity type microfiber synthetic leather.
Chinese patent (CN 108130720A) discloses a preparation method and equipment of conductive microfiber leather, the method comprises the steps of sequentially carrying out activation, graphene impregnation, hydrogen sulfide modification, strong alkaline strong reducing agent impregnation, desulfurization, reduction and other processes on short fibers to prepare a conductive non-woven fabric, and the graphene and the microfiber short fibers are combined by chemical bond acting force, so that the firm strength between the graphene and the microfiber short fibers is effectively improved. However, the preparation method uses hydrogen sulfide gas with high toxicity in the processing process, and has certain environmental risks. In addition, the prepared non-woven fabric needs wet processing in the later period, PU resin impregnation, alkali reduction, and a buffing dyeing and finishing process. Among them, the influence of the polyurethane and the dye on the surface conductivity after the coating and treatment of the conductive nonwoven fabric is unknown.
Chinese patent (CN 111005218A) applies for a preparation method of conductive superfine fiber suede leather, the technology enables a carbon fiber conductive network to be arranged in a suede leather fiber matrix through carbon fiber modification PA6, a large amount of conductive transition metal fine particles are adsorbed in superfine fiber leather micropores through citrate sol finishing liquid impregnated with transition metal, the contact property of the carbon fiber conductive network partially coated by insulating polyurethane and the surface conductive fine particles is improved, and the conductive performance of a product can be obviously improved through the combined action of the carbon fiber conductive network and the surface conductive fine particles. However, the bonding force between the adsorbed transition metal particles and the carbon fibers is weak, and the strength and the use stability of the material are to be further improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method and equipment of high-conductivity type superfine fiber synthetic leather, wherein the high-conductivity type superfine fiber synthetic leather mainly comprises a superfine fiber non-woven fabric substrate, a composite resin layer and a densely stacked nano conductive layer; firstly, pretreating superfine fiber non-woven fabric; then roll-coating with composite resin; grinding and polishing the compact resin surface layer after wet solidification; depositing a conductive layer on the surface of the base cloth by utilizing a front-pressure driving film former; finally, hot-pressing and shaping to obtain the high-conductivity superfine fiber synthetic leather. The front-pressure driven film forming equipment is in a high-pressure closed environment, the conductive nano film forming solution is stored in the tank body, the bottom of the tank body is provided with a porous supporting filter plate, and the top of the tank body is provided with a high-pressure air inlet adjusting valve. The prepared high-conductivity superfine fiber synthetic leather has a gradient conductive multilayer stacked structure, the surface of the high-conductivity superfine fiber synthetic leather is a compact and orderly stacked nano conductive layer, the middle layer is a composite resin layer with a porous structure, and the bottom of the high-conductivity superfine fiber synthetic leather is an insulated superfine fiber substrate. The preparation method is simple in process and low in cost, is expected to realize industrial production, and has potential application value in the fields of smart home, electromagnetic shielding, wearable equipment, military protection and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of high-conductivity superfine fiber synthetic leather mainly comprises a superfine fiber non-woven fabric substrate, a composite resin layer and a densely stacked nano conductive layer; the equipment is used for assembling the nano conductive material on the surface of the superfine fiber synthetic leather in a highly ordered way, is a key for preparing the densely stacked nano conductive layer, and is characterized by comprising the following steps:
step 1, soaking and ultrasonically cleaning superfine fiber base cloth by using ethanol and deionized water in sequence, and ironing by using a hot press for standby;
step 2, mixing the carbon nano tube with N, N-dimethylformamide, and reacting for 0.5h at 70 ℃ for later use; uniformly mixing the composite resin in N, N-dimethylformamide, placing in an anhydrous three-neck flask, heating and stirring, controlling the heating temperature at 70 ℃, reacting for 3.5 hours, adding the prepared carbon nano tube and the N, N-dimethylformamide compound, uniformly mixing, continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished. Uniformly coating composite resin on the surface of the microfiber base cloth treated in the step 1, and then placing the microfiber base cloth in a coagulating bath H2In O-DMF, after the resin is completely solidified, forming a resin coating with a microporous structure on the surface of the superfine fiber base cloth;
step 3, performing surface polishing treatment on the superfine fiber base cloth obtained in the step 2 by using a grinding machine;
step 4, fixing the superfine fiber base cloth subjected to surface polishing treatment in the step 3 on a porous supporting filter plate of a synthetic leather forward-pressing driving film forming device, preparing a nano conductive film forming solution containing graphene, injecting the nano conductive film forming solution into a tank body, wherein the concentration of the graphene is 0.05-2.0 mg/mL, the volume of the nano conductive film forming solution is 100-1000 mL, performing forward-pressing driving assembly film forming under the operating pressure of 0.1-1.0 bar, and allowing the nano conductive film forming solution to completely flow out;
and 5, placing the product obtained in the step 4 on a flat hot press for hot press molding, and finally obtaining the high-conductivity superfine fiber synthetic leather.
In the step 1, the gram weight value of the superfine fiber base cloth ranges from 0.8 to 2.0g/cm3。
In the step 2, the composite resin is one or more of polyacrylonitrile, polyurethane, polyethylene glycol, polyvinyl alcohol, a carbon nano tube, graphene oxide and UiO-66, and the film forming thickness is 0.5-100 μm.
The mass fraction of polyacrylonitrile is 12wt%, the mass fraction of polyurethane is 5wt%, the mass fraction of polyethylene glycol is 2wt%, and the mass fraction of carbon nano tube is 0.05 wt%.
In the step 3, the surface polishing treatment time can be adjusted according to actual needs, and the abrasion depth of the surface polishing treatment is 0.2-50 μm.
In the step 4, the nano conductive film-forming solution contains one or more of graphene, graphene oxide, aluminum tannin, aluminum ions, carbon nano tubes, polyaniline, MXene, nano silver wires, polydopamine, dopamine and waterborne polyurethane, and the total mass concentration range is 0.5-20 mg/L.
In step 5, the surface conductivity of the high-conductivity superfine fiber synthetic leather is 1.0 multiplied by 104~1.0×106Sm-1。
A preparation device of high-conductivity superfine fiber synthetic leather comprises a gas pressure regulating buffer tank, a liquid storage tank, a silica gel sealing strip, a superfine fiber base cloth fixing groove, a porous seepage filter plate and a liquid collecting port; wherein, the rear end of the air pressure regulating buffer tank is communicated with the front end of the liquid storage tank; the silica gel sealing strip is positioned between the liquid storage tank and the superfine fiber base cloth fixing groove; the liquid collecting port is arranged right below the porous percolation plate; the rear end of the liquid storage tank is communicated with the superfine fiber base cloth fixing groove.
The pressurizing range of the gas pressure regulating buffer tank is 0.1-1.0 Mpa, and the capacity of the liquid storage tank is 0.5-10L.
The invention has the beneficial effects that:
the invention firstly effectively solves the problem of preparing the high-conductivity superfine fiber synthetic leather. Meanwhile, by means of the advantages of good flexibility, air permeability, mechanical properties and the like of the superfine fibers, the high-conductivity superfine fiber synthetic leather material with gradient conductivity is prepared by utilizing the processes of resin roll coating, wet solidification, surface smoothing, forward pressure driving assembly, hot press forming and the like. Finally, after hot pressing treatment, firmness among multiple layers of the high-conductivity superfine fiber synthetic leather material is more stable, and conductivity is more excellent.
The equipment can be fast, stable assemble electrically conductive nano-material in substrate material surface, compare in technologies such as simple spraying, blade coating, nano-material can be more orderly, high-efficient, level and even attached to base surface, has the expansibility.
Drawings
FIG. 1 is a diagram of the preparation process of the high-conductivity superfine fiber synthetic leather in the examples of the present application.
Fig. 2(a) is a photograph of an ultrafine fiber base fabric in an embodiment of the present application.
FIG. 2(b) is a photograph showing an example of the embodiment of the present application.
FIG. 2(c) is a photograph showing a photograph of a high-conductivity type microfine fiber synthetic leather.
FIG. 2(d) is a cross-sectional micro-topography of the microfiber substrate cloth of FIG. 2 (a).
FIG. 2(e) is a cross-sectional micro-topography of the composite resin/microfiber substrate cloth, wherein a composite resin layer is formed on the microfiber substrate cloth, and the gaps of the substrate cloth are filled with resin.
Fig. 2(f) is a cross-sectional microscopic morphology diagram of the high-conductivity type superfine fiber synthetic leather, which has an obvious three-layer stacked structure, wherein the upper layer is a compact nano conductive layer, the middle layer is a resin layer, and the lower layer is a superfine fiber base cloth layer.
FIG. 3(a) is a schematic structural diagram of an apparatus for front-press driving assembly film formation in the embodiment of the present application.
FIG. 3(b) is a photograph of an apparatus for front-press driving assembly film formation in the example of the present application.
FIG. 4 is a photograph showing the conductivity test of the high conductivity type microfine synthetic leather according to the example of the present application.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
The superfine fiber base cloth is fiber base cloth with monofilament fineness of 0.3-1.0 dtex.
The invention relates to a preparation method of high-conductivity superfine fiber synthetic leather, which is realized by the following steps:
step 1, pretreating superfine fiber base cloth, taking superfine fiber non-woven cloth with proper size, respectively ultrasonically washing the superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min, drying the superfine fiber non-woven cloth in a blast drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use.
Step 2, preparing composite resin, namely mixing polyacrylonitrile with the mass fraction of 12%, polyethylene glycol with the mass fraction of 2% and polyurethane with the mass fraction of 5% in an organic solvent, heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of carbon nano tubes with the mass fraction of 0.05% and N, N-Dimethylformamide (DMF) for reaction for 0.5 hour at 70 ℃ into the reaction system, continuously heating and quickly stirring for 1 hour, and obtaining the composite resin after the reaction is finished;
it is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, wherein the coating thickness is 0.5-100 mu m, then integrally placing the superfine fiber base cloth into a coagulating bath, soaking for 18h, the coagulating temperature is 25-40 ℃, after shaping and drying, treating the surface layer of the resin by using a grinding machine, the grinding time is 5-30 min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
the coagulating bath contains one or more of DMF, water, and sodium chloride;
step 4, preparing a nano conductive film forming solution, namely respectively taking 0.1-1.0 mg of graphene oxide, 0.5-5 mg of graphene, 0.1-1.0 mg of carbon nano tube, 0.5-5 mg of aluminum ion and 1.0-10.0 mg of polydopamine to ultrasonically disperse in an aqueous solution, ultrasonically treating for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.1-1.0 MPa, and after the nano conductive film forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 1
A preparation method of high-conductivity superfine fiber synthetic leather comprises the following steps:
step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to the thickness of 100 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 40 ℃, shaping and dryingThen, a grinding machine is used for processing the resin surface layer, the grinding time is 5min, and the resin/superfine fiber composite substrate is obtained after surface treatment;
step 4, preparing a nano conductive film forming solution, ultrasonically dispersing 1.0mg of graphene oxide, 0.5mg of graphene and 5mg of aluminum chloride in a deionized water solution for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.5Mpa, and allowing the nano conductive film forming solution to completely flow out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 2
Step 1, pretreating superfine fiber base cloth, sequentially and respectively ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min, drying the superfine fiber non-woven cloth in a blast drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the laboratory instruments and chemical reagents in the experiment need to be dehydrated and dried before use.
Step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, wherein the coating thickness is 0.5 mu m, and then putting the whole into (DMF-H)2O) in a coagulating bath, soaking for 18h, wherein the coagulating temperature is 25 ℃; after shaping and drying, treating the resin surface layer by using a grinding machine, wherein the grinding time is 25min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
step 4, preparing a nano conductive film forming solution, ultrasonically dispersing 0.5mg of graphene oxide, 2mg of graphene and 2mg of aluminum chloride in a deionized water solution for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 1Mpa, and allowing the nano conductive film forming solution to completely flow out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 3
Step 1, pretreating superfine fiber base cloth, sequentially and respectively ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min, drying the superfine fiber non-woven cloth in a blast drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the laboratory instruments and chemical reagents in the experiment need to be dehydrated and dried before use.
Step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to a thickness of 50 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h, wherein the coagulating temperature is 33 ℃; after shaping and drying, treating the resin surface layer by using a grinding machine, wherein the grinding time is 25min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
step 4, preparing a nano conductive film forming solution, ultrasonically dispersing 0.1mg of graphene oxide, 5mg of graphene and 0.5mg of aluminum chloride in a deionized water solution for 30min, introducing the prepared conductive nano particle dispersion solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.1MPa, and allowing the nano conductive film forming solution to completely flow out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 4
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, wherein the coating thickness is 0.5 mu m, and then putting the whole into (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 25 ℃, shaping and drying, then treating the resin surface layer by using a grinding machine for 5min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
and 4, preparing a nano conductive film forming solution, and ultrasonically dispersing 1.0mg of graphene oxide, 0.5mg of graphene and 1mg of carbon nano tube in a deionized water solution for 30 min. Guiding the prepared nano conductive film-forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a forward pressure driving assembly film-forming device, adjusting the pressure range of a gas buffer tank to be 0.1Mpa, and allowing the nano conductive film-forming solution to completely flow out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 5
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to the thickness of 40 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 28 ℃, shaping and drying, then treating the resin surface layer by using a grinding machine for 17min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
step 4, preparing a nano conductive film forming solution, ultrasonically dispersing 0.5mg of graphene oxide, 2mg of graphene and 0.5mg of carbon nano tube in a deionized water solution for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.4 MPa, and allowing the nano conductive film forming solution to completely flow out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 6
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to the thickness of 100 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h, wherein the coagulating temperature is 40 ℃. After shaping and drying, treating the resin surface layer by using a grinding machine for 30min, and obtaining a resin/superfine fiber composite substrate after surface treatment;
step 4, preparing a nano conductive film forming solution, ultrasonically dispersing 0.1mg of graphene oxide, 5mg of graphene and 0.1mg of carbon nano tube in a deionized water solution for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure-driven assembly film forming device, adjusting the pressure range of a gas buffer tank to be 1MPa, and after the nano conductive film forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 7
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to the thickness of 100 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 40 ℃, shaping and drying, then treating the resin surface layer by using a grinding machine for 30min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
and 4, preparing a nano conductive film forming solution, and ultrasonically dispersing 1mg of graphene oxide, 0.5mg of graphene and 10mg of polydopamine in a deionized water solution for 30 min. Introducing the prepared nano conductive film-forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a forward pressure driving assembly film-forming device, adjusting the pressure range of a gas buffer tank to be 1Mpa, and after the nano conductive film-forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 8
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to a thickness of 70 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 32 ℃, shaping and drying, then treating the resin surface layer by using a grinding machine for 25min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
and 4, preparing a nano conductive film forming solution, and ultrasonically dispersing 0.5mg of graphene oxide, 2.5 mg of graphene and 4mg of polydopamine in a deionized water solution for 30 min. Guiding the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a forward pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.7Mpa, and after the film forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 9
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, wherein the coating thickness is 0.5 mu m, and then putting the whole into (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 25 ℃. After shaping and drying, treating the resin surface layer by using a grinding machine for 5min, and obtaining a resin/superfine fiber composite substrate after surface treatment;
step 4, preparing a nano conductive film forming solution, ultrasonically dispersing 0.1mg of graphene oxide, 5mg of graphene and 1mg of polydopamine in a deionized water solution for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.1MPa, and after the nano conductive film forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 10
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to the thickness of 100 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 40 ℃, shaping and drying, then treating the resin surface layer by using a grinding machine for 30min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
and 4, preparing a nano conductive film forming solution, namely ultrasonically dispersing 1.0mg of graphene oxide, 0.5mg of graphene, 1.0mg of carbon nano tube, 5.0mg of aluminum ions and 10.0mg of polydopamine in a deionized water solution for 30 min. Introducing the prepared nano conductive film-forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a forward pressure driving assembly film-forming device, adjusting the pressure range of a gas buffer tank to be 1.0Mpa, and after the nano conductive film-forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 11
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, coating the composite resin to a thickness of 80 mu m, and then putting the composite resin into the superfine fiber base cloth (DMF-H)2O) in a coagulating bath, soaking for 18h, wherein the coagulating temperature is 34 ℃. After shaping and drying, treating the resin surface layer by using a grinding machine, wherein the grinding time is 26min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
and 4, preparing a nano conductive film forming solution, and ultrasonically dispersing 0.6mg of graphene oxide, 4.0mg of graphene, 0.5mg of carbon nano tube, 1.0mg of aluminum ions and 2.0mg of polydopamine in a deionized water solution for 30 min. Introducing the prepared nano conductive film-forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a forward pressure driving assembly film-forming device, adjusting the pressure range of a gas buffer tank to be 0.8 Mpa, and after the nano conductive film-forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
Example 12
Step 1, pretreating superfine fiber base cloth, namely sequentially ultrasonically washing the cut superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min respectively, drying the superfine fiber non-woven cloth in a forced air drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing 12% by mass of polyacrylonitrile, 2% by mass of polyethylene glycol and 5% by mass of polyurethane in N, N-Dimethylformamide (DMF), heating and stirring at 70 ℃ for reaction for 3.5 hours, adding a mixed solution of 0.05% by mass of carbon nanotubes and N, N-Dimethylformamide (DMF) which react at 70 ℃ for 0.5 hour into the reaction system, and continuously heating and rapidly stirring for 1 hour; and obtaining the composite resin after the reaction is finished.
It is noted that the experimental instruments and chemical reagents in the experiment need to be dehydrated and dried before use;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, wherein the coating thickness is 0.5 mu m, and then putting the whole into (DMF-H)2O) in a coagulating bath, soaking for 18h at a coagulating temperature of 25 ℃. After shaping and drying, treating the resin surface layer by using a grinding machine for 5min, and obtaining a resin/superfine fiber composite substrate after surface treatment;
and 4, preparing a nano conductive film forming solution, and ultrasonically dispersing 0.1mg of graphene oxide, 5mg of graphene, 0.1mg of carbon nano tube, 0.5mg of aluminum ions and 1mg of polydopamine in a deionized water solution for 30 min. Introducing the prepared nano conductive film-forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a forward pressure driving assembly film-forming device, adjusting the pressure range of a gas buffer tank to be 0.1Mpa, and after the nano conductive film-forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
See fig. 2(d) for disordered fiber structure and the presence of large voids; FIG. 2(e) is a cross-sectional micro-topography of the composite resin/microfiber substrate cloth, wherein a composite resin layer is arranged on the upper layer of the microfiber substrate cloth, and gaps of the substrate cloth are filled with resin; fig. 2(f) is a cross-sectional microscopic morphology diagram of the high-conductivity type superfine fiber synthetic leather, which has an obvious three-layer stacked structure, wherein the upper layer is a compact nano conductive layer, the middle layer is a resin layer, and the lower layer is a superfine fiber base cloth layer.

Claims (10)

1. A preparation method of high-conductivity superfine fiber synthetic leather is characterized by comprising the following steps:
step 1, soaking and ultrasonically cleaning superfine fiber base cloth by using ethanol and deionized water in sequence, and ironing the superfine fiber base cloth by using a hot press for standby after drying;
step 2, mixing the carbon nano tube with N, N-dimethylformamide, and reacting for 0.5h at 70 ℃ for later use; uniformly mixing the composite resin in N, N-dimethylformamide, placing in an anhydrous three-neck flask, heating and stirring, controlling the heating temperature at 70 ℃, reacting for 3.5H, adding the prepared mixed solution of the carbon nano tube and the N, N-dimethylformamide, uniformly coating the composite resin on the surface of the super-fiber base cloth treated in the step (1), and then placing in a coagulating bath H2In O-DMF, after the resin is completely solidified, forming a resin coating with a microporous structure on the surface of the superfine fiber base cloth;
step 3, performing surface polishing treatment on the superfine fiber base cloth obtained in the step 2 by using a grinding machine;
step 4, fixing the superfine fiber base cloth subjected to surface polishing treatment in the step 3 on a porous supporting filter plate of a synthetic leather forward-pressing driving film forming device, preparing a nano conductive film forming solution containing graphene, injecting the nano conductive film forming solution into a tank body, wherein the concentration of the graphene is 0.05-2.0 mg/mL, the volume of the nano conductive film forming solution is 100-1000 mL, performing forward-pressing driving assembly film forming under the operating pressure of 0.1-1.0 bar, and allowing the nano conductive film forming solution to completely flow out;
and 5, placing the product obtained in the step 4 on a flat hot press for hot press molding, and finally obtaining the high-conductivity superfine fiber synthetic leather.
2. The method for preparing high-conductivity superfine fiber synthetic leather according to claim 1, wherein in the step 1, the gram weight of the superfine fiber base cloth is in the range of 0.8-2.0 g/cm3。
3. The method for preparing high-conductivity superfine fiber synthetic leather according to claim 1, wherein in the step 2, the composite resin is one or more of polyacrylonitrile, polyurethane, polyethylene glycol, polyvinyl alcohol, carbon nanotubes, graphene oxide and UiO-66, and the film thickness is 0.5-100 μm.
4. The method for preparing high-conductivity superfine fiber synthetic leather according to claim 1, wherein the mass fraction of polyacrylonitrile is 12wt%, the mass fraction of polyurethane is 5wt%, the mass fraction of polyethylene glycol is 2wt%, and the mass fraction of carbon nanotube is 0.05 wt%.
5. The method for preparing high conductivity type microfiber synthetic leather according to claim 1, wherein in step 3, the surface polishing time is adjusted according to actual needs, and the abrasion depth of the surface polishing is 0.2-50 μm.
6. The method for preparing high-conductivity superfine fiber synthetic leather according to claim 1, wherein in the step 4, the nano conductive film forming solution contains one or more of graphene, graphene oxide, aluminum tannin, aluminum ions, carbon nanotubes, polyaniline, MXene, nano silver wires, polydopamine, dopamine and aqueous polyurethane, and the total mass concentration range is 0.5-20 mg/L.
7. The method of claim 1, wherein in step 5, the surface conductivity of the synthetic leather is 1.0 x 104~1.0×106Sm-1。
8. A preparation method of high-conductivity superfine fiber synthetic leather is characterized by comprising the following steps:
step 1, pretreating superfine fiber base cloth, taking superfine fiber non-woven cloth with proper size, respectively ultrasonically washing the superfine fiber non-woven cloth in absolute ethyl alcohol and deionized water for 30min in sequence, drying the superfine fiber non-woven cloth in a blast drying oven at 85 ℃, and ironing the superfine fiber non-woven cloth by using a hot press for later use;
step 2, preparing composite resin, namely mixing polyacrylonitrile with the mass fraction of 12%, polyethylene glycol with the mass fraction of 2% and polyurethane with the mass fraction of 5% in an organic solvent, heating and stirring at 70 ℃ for reaction for 3.5 hours, and mixing carbon nano tubes with the mass fraction of 0.05% and N, N-dimethylformamide; adding the mixed solution which reacts for 0.5h at 70 ℃ into the reaction system, continuously heating and rapidly stirring for 1h to obtain composite resin after the reaction is finished;
step 3, uniformly coating the composite resin synthesized in the step two on the superfine fiber base cloth obtained in the step one, wherein the coating thickness is 0.5-100 mu m, then integrally placing the superfine fiber base cloth into a coagulating bath, soaking for 18h, the coagulating temperature is 25-40 ℃, after shaping and drying, treating the surface layer of the resin by using a grinding machine, the grinding time is 5-30 min, and obtaining the resin/superfine fiber composite substrate after surface treatment;
step 4, preparing a nano conductive film forming solution, namely respectively taking 0.1-1.0 mg of graphene oxide, 0.5-5 mg of graphene, 0.1-1.0 mg of carbon nano tube, 0.5-5 mg of aluminum ion and 1.0-10.0 mg of polydopamine to ultrasonically disperse in an aqueous solution, ultrasonically treating for 30min, introducing the prepared nano conductive film forming solution into a storage tank for later use, placing the resin/superfine fiber composite substrate prepared in the step three into a front-pressure driving assembly film forming device, adjusting the pressure range of a gas buffer tank to be 0.1-1.0 MPa, and after the nano conductive film forming solution completely flows out;
and 5, transferring the composite synthetic leather into a hot press, carrying out hot pressing for 20min at the hot pressing temperature of 100 ℃, and finally obtaining the resin/superfine fiber composite synthetic leather coated with the nano conductive layer on the surface.
9. A preparation device of high-conductivity superfine fiber synthetic leather is characterized by comprising a gas pressure regulating buffer tank (1), a liquid storage tank (2), a silica gel sealing strip (3), superfine fiber base cloth fixing grooves (4), a porous seepage filter plate (5) and a liquid collecting port (6); wherein, the rear end of the air pressure regulating buffer tank (1) is communicated with the front end of the liquid storage tank (2); the silica gel sealing strip (3) is positioned between the liquid storage tank (2) and the superfine fiber base cloth fixing groove (4); the liquid collecting port (6) is arranged right below the porous seepage filter plate (5); the rear end of the liquid storage tank is communicated with the superfine fiber base cloth fixing groove (4).
10. The device for preparing high-conductivity superfine fiber synthetic leather according to claim 9, wherein the pressurizing range of the gas pressure regulating buffer tank (1) is 0.1-1.0 Mpa, and the capacity of the liquid storage tank (2) is 0.5L-10L.
CN202111491376.3A 2021-12-08 2021-12-08 Preparation method and equipment of high-conductivity superfine fiber synthetic leather Withdrawn CN114232349A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115094640A (en) * 2022-05-12 2022-09-23 陕西科技大学 Waterborne polyurethane superfine fiber conductive synthetic leather and preparation method thereof
CN115559109A (en) * 2022-11-18 2023-01-03 四川大学华西医院 Breathable antibacterial nano composite fiber material and preparation method and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115094640A (en) * 2022-05-12 2022-09-23 陕西科技大学 Waterborne polyurethane superfine fiber conductive synthetic leather and preparation method thereof
CN115094640B (en) * 2022-05-12 2024-01-12 陕西科技大学 Waterborne polyurethane superfine fiber conductive synthetic leather and preparation method thereof
CN115559109A (en) * 2022-11-18 2023-01-03 四川大学华西医院 Breathable antibacterial nano composite fiber material and preparation method and application thereof

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