CN119340004A - Ultra-fine copper foil composite conductor with a diameter of 0.02mm to 0.05mm - Google Patents
Ultra-fine copper foil composite conductor with a diameter of 0.02mm to 0.05mm Download PDFInfo
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Abstract
本发明公开了一种直径0.02mm至0.05mm的超微细铜箔丝复合导线，属于复合导线加工技术领域，用于解决现有技术中超细微铜箔丝复合导线的耐腐蚀性能、机械强度、电磁屏蔽性能和绝缘强度有待进一步提高的技术问题；本发明包括铜箔丝线芯、含氟防腐层和外防护层，绝缘层包括含氟防腐层和外防护层，含氟防腐层由氟增强改性树脂熔融包覆在铜箔丝线芯外部固化后得到，本发明是通过优化含氟防腐层与外防护层的材料组成，通过氟防腐层与外防护层相互配合，在提高复合导线机械强度和耐腐蚀性能的同时，还提高复合导线的电磁屏蔽效能与绝缘强度。
The invention discloses an ultrafine copper foil composite conductor with a diameter of 0.02 mm to 0.05 mm, belongs to the technical field of composite conductor processing, and is used to solve the technical problem in the prior art that the corrosion resistance, mechanical strength, electromagnetic shielding performance and insulation strength of the ultrafine copper foil composite conductor need to be further improved; the invention comprises a copper foil core, a fluorine-containing anti-corrosion layer and an outer protective layer, the insulating layer comprises a fluorine-containing anti-corrosion layer and an outer protective layer, the fluorine-containing anti-corrosion layer is obtained by melt-coating a fluorine-reinforced modified resin on the outside of the copper foil core and then curing, the invention optimizes the material composition of the fluorine-containing anti-corrosion layer and the outer protective layer, and cooperates with the fluorine anti-corrosion layer and the outer protective layer, thereby improving the mechanical strength and corrosion resistance of the composite conductor while also improving the electromagnetic shielding effectiveness and insulation strength of the composite conductor.
Description
Technical Field
The invention relates to the technical field of composite wire processing, in particular to an ultra-fine copper foil wire composite wire with the diameter of 0.02mm to 0.05mm.
Background
The ultra-fine copper foil wire is a wire material which adopts an ultra-fine copper foil wire as a conductive core and combines the copper foil wire with an insulating layer, a protective sleeve and the like through a specific compounding process, so that the ultra-fine copper foil wire not only maintains the advantages of the traditional copper foil wire, but also further improves the miniaturization and integration level of the wire.
In the prior art, a Chinese patent with the publication number of CN107170535A discloses a superfine sheath-core wire lead and manufacturing equipment thereof, the lead comprises a sheath layer and a core layer, the section of the lead is round, the section of the core layer is round, the section of the sheath layer is circular, the sheath layer wraps the outside of the core layer, the core layer is made of a conductive material consisting of a mixture of carbon black particles and polyaniline, the sheath layer is made of a high polymer insulating material, the outside of the sheath layer is also provided with a wear-resisting groove, and the wear-resisting groove winds the outside of the sheath layer from top to bottom;
In the prior art, flexible electronic products such as flexible display screens, flexible sensors and the like require that wires have extremely high flexibility and microminiaturization level, and ultra-fine copper foil wire wires become ideal connecting wire materials for the products due to good flexibility and microminiaturization characteristics of the wires, but traditional ultra-fine copper foil wire composite wires are made of copper as a main material, are easy to be corroded by the outside, have low mechanical strength, are easy to break due to the external acting force in the use process, and are easy to be subjected to electromagnetic interference in the environment in a highly integrated circuit environment, and the traditional composite wires generally improve the electromagnetic shielding performance of the materials in a mode of adding conductive particles into the materials by sacrificing the insulation resistance of an external insulation layer, so that the insulation performance of the composite wires needs to be further improved.
In view of the technical drawbacks of this aspect, a solution is now proposed.
Disclosure of Invention
The invention aims to provide an ultra-fine copper foil wire composite wire with the diameter of 0.02-0.05 mm, which is used for solving the technical problems that the ultra-fine copper foil wire composite wire in the prior art is poor in corrosion resistance and mechanical strength, and the electromagnetic shielding performance and the insulation strength of the composite wire are required to be further improved.
The ultra-fine copper foil wire composite lead with the diameter of 0.02mm to 0.05mm comprises a copper foil wire core, a fluorine-containing anti-corrosion layer and an outer protective layer, wherein the insulating layer comprises the fluorine-containing anti-corrosion layer and the outer protective layer, the fluorine-containing anti-corrosion layer is obtained by melting and coating fluorine-reinforced modified resin on the outer part of the copper foil wire core for solidification, a plurality of grooves which are parallel to the copper foil wire core are arranged on the outer surface of the fluorine-containing anti-corrosion layer, and the outer protective layer is obtained by melting and coating composite polyethylene on the outer part of the fluorine-containing anti-corrosion layer for solidification;
the composite polyethylene consists of 100 parts by weight of a polyethylene mixture and 10-15 parts by weight of epoxy resin, wherein the polyethylene mixture consists of 100 parts by weight of low-density polyethylene, 30-40 parts by weight of modified polyethylene and 12-16 parts by weight of modified graphite.
Further, the fluorine reinforced modified resin is processed by the following steps:
A1, adding butyl acrylate, perfluorooctyl acrylate, vinyl-terminated silicone oil, oleylamine and toluene into a reaction kettle protected by nitrogen, stirring, increasing the temperature of the reaction kettle to 75-85 ℃, adding an initiator into the reaction kettle, carrying out heat preservation reaction for 6-8h, and carrying out post-treatment to obtain fluorine-containing resin;
The synthetic reaction formula of the fluorine-containing resin is:
Wherein:
The synthetic reaction principle of the fluorine-containing resin is as follows:
Under the action of an initiator, an olefin double bond on butyl acrylate, perfluorooctyl acrylate, vinyl-terminated silicone oil and oleylamine molecules is used as an active reaction site to initiate a free radical polymerization reaction to form a polyolefin chain segment crosslinked by a polysiloxane chain segment, and fluorine-containing branched chains, alkane branched chains and Xin An branched chains are modified on the polyolefin chain segment to prepare the fluorine-containing resin.
And A2, adding the fluorine-containing resin and the epoxy resin into a reaction kettle, stirring, and raising the temperature of the reaction kettle to 190-200 ℃, and carrying out melt mixing for 30-50min to obtain the fluorine-reinforced modified resin.
Further, in the step A1, the dosage ratio of the butyl acrylate to the perfluorooctyl acrylate to the vinyl-terminated silicone oil to the oleylamine to the toluene to the initiator is 60-70g to 15-18g to 10-12g to 17-19g to 500mL to 0.8-1.2g, the initiator is azodiisobutyronitrile, the post-treatment comprises the steps of after the reaction is finished, the temperature of a reaction kettle is increased to 80-90 ℃, the solvent is distilled off under reduced pressure, and the fluorine-containing resin is obtained, in the step A2, the weight ratio of the fluorine-containing resin to the epoxy resin is 7:2-3, and the epoxy resin is bisphenol A type epoxy resin E-51.
Further, the modified polyethylene is processed by the following steps:
B1, uniformly mixing low-density polyethylene powder, tea polyphenol, glycidyl methacrylate and an initiator, adding the mixture into an internal mixer at 185-195 ℃, setting the rotating speed of the internal mixer to be 50-60r/min, and carrying out internal mixing for 10-15min to obtain a mixture;
and B2, transferring the mixture into a flat vulcanizing machine, raising the temperature of the flat vulcanizing machine to 190-200 ℃, raising the pressure to 9-10MPa, carrying out heat preservation and pressure maintaining treatment for 5-10min, and carrying out post treatment to obtain the modified polyethylene.
The synthetic reaction mechanism of the modified polyethylene is as follows:
Tea polyphenol is used as an antioxidant, low-density polyethylene powder, glycidyl methacrylate and an initiator are uniformly mixed, olefin double bonds on the glycidyl methacrylate are used as active reaction sites, and the crosslinking bonding between the glycidyl methacrylate and a low-density polyethylene molecular chain is promoted through vulcanization treatment, so that a large number of epoxy groups are modified on the polyethylene molecular chain, and the modified polyethylene is prepared.
In the step B1, the weight ratio of the low-density polyethylene powder to the tea polyphenol to the glycidyl methacrylate to the initiator is 100:1:5-7:0.5, the initiator is benzoyl peroxide, in the step B2, the post-treatment comprises the steps of cooling, discharging, crushing, adding the powder and the dimethylbenzene into a reaction kettle according to the concentration of 1g to 200mL, stirring, heating the reaction kettle to reflux, keeping the temperature, stirring until the system is dissolved, reducing the temperature of the reaction kettle to room temperature, adding petroleum ether into the reaction kettle, precipitating a large amount of solids, carrying out suction filtration, transferring a filter cake into a drying oven with the temperature of 60-70 ℃, and drying to constant weight to obtain the modified polyethylene.
Further, the modified graphite is obtained by processing the following steps:
c1, adding flake graphite powder and a modifier into a reaction kettle, stirring for 30-40min at room temperature, and performing post-treatment to obtain activated graphite powder;
C2, placing the activated graphite powder into a tube furnace in a nitrogen atmosphere, increasing the temperature of the tube furnace to 300-350 ℃, carrying out heat preservation treatment for 10-20min, and cooling and discharging to obtain expanded graphite;
Adding the expanded graphite, the iron pentacarbonyl and the kerosene into a high-pressure reaction kettle protected by nitrogen, sealing and stirring, raising the temperature of the high-pressure reaction kettle to 260-280 ℃, carrying out heat preservation treatment for 90-120min, and carrying out post-treatment to obtain the load type expanded graphite;
The synthesis reaction mechanism of the supported expanded graphite is as follows:
Mixing flake graphite powder with a modifier, stirring at room temperature, wherein an oxidizing substance in the modifier attacks carbon atoms of graphite to form carbon-oxygen bonds, so that the active site on the surface of the graphite is increased, the surface property of the graphite is changed, conditions are provided for subsequent high-temperature expansion, the carbon atoms on the surface of the graphite are further oxidized by hydrogen peroxide to form more carbon-oxygen bonds and carboxyl functional groups, activated graphite powder is obtained, at high temperature, oxidation products such as water vapor and carbon dioxide among graphite layers rapidly escape to generate huge internal pressure, and meanwhile, the carbon atoms among the graphite layers are rearranged at high temperature to form a more loose structure, so that the graphite rapidly expands at high temperature to form expanded graphite, and at high temperature, pentacarbonyl iron is decomposed to generate iron atoms or iron nanoparticles and carbon monoxide, and the generated iron atoms or iron nanoparticles are adsorbed on the expanded graphite to form load-type expanded graphite.
And C4, adding the supported expanded graphite, the modified nano silicon dioxide, the tetraethoxysilane and the absolute ethyl alcohol into a reaction kettle, performing ultrasonic dispersion for 30-50min, stirring, heating the reaction kettle to 50-60 ℃, adding a catalyst into the reaction kettle, performing heat preservation reaction for 60-90min, and performing post-treatment to obtain the modified graphite.
The synthetic reaction mechanism of the modified graphite is as follows:
under alkaline condition, the siloxane bond in the modified nano silicon dioxide and tetraethoxysilane molecule is hydrolyzed to generate silicon hydroxyl, the silicon hydroxyl is used as a reaction active site to perform condensation reaction with active oxygen-containing groups on the surface of the load type expanded graphite, and the surface of the load type expanded graphite is coated with a layer of nano silicon dioxide and polysiloxane coating layer to prepare the modified graphite.
Further, in the step C1, the dosage ratio of the crystalline flake graphite powder to the modifier is 1g:8-12mL, the modifier is obtained by uniformly mixing potassium permanganate and 80-90wt% sulfuric acid according to the dosage ratio of 1g:7mL, the post-treatment comprises the steps of after the reaction is finished, carrying out suction filtration until no liquid drops, adding a filter cake and 20-30wt% hydrogen peroxide according to the dosage ratio of 1g:8-10mL into a reaction kettle, stirring, increasing the temperature of the reaction kettle to 75-85 ℃, stirring for 60-80min, reducing the temperature of the reaction kettle to room temperature, carrying out suction filtration, washing a filter cake with purified water to be neutral, carrying out suction filtration, transferring the filter cake into a drying box with the temperature of 70-80 ℃ to obtain activated graphite powder, carrying out vacuum drying, wherein the dosage ratio of the expanded graphite, pentacarbonyl iron and kerosene is 7g:1g:500mL, the post-treatment comprises the steps of after the reaction is finished, reducing the pressure of the high-pressure reaction kettle to room temperature, centrifuging, washing the solid with acetone for 5 times, carrying out suction filtration, transferring the filter cake to 60-70 ℃ to the temperature of the constant temperature, carrying out suction filtration until the temperature of the filter cake is 5:70 ℃ and the catalyst is equal to 3:10 mol/3, carrying out vacuum drying to the catalyst, carrying out vacuum drying, and carrying out the filter cake is carried out vacuum drying, and carrying out the vacuum drying to obtain the catalyst, and drying to be dried to obtain the activated graphite powder, and the catalyst.
Further, the modified nano silicon dioxide is obtained by processing the following steps:
D1, adding nano silicon dioxide, absolute ethyl alcohol and 3-aminopropyl triethoxysilane into a reaction kettle, stirring, increasing the temperature of the reaction kettle to 50-60 ℃, adding a catalyst into the reaction kettle, carrying out heat preservation reaction for 50-60min, and carrying out aftertreatment to obtain activated silicon dioxide powder;
And D2, adding activated silicon dioxide powder and toluene into a reaction kettle protected by nitrogen, stirring, adding isocyanic acid propyl triethoxysilane into the reaction kettle at room temperature, stirring for 40-50min, and performing post-treatment to obtain the modified nano silicon dioxide.
The synthetic reaction mechanism of the modified silicon dioxide is as follows:
The preparation method comprises the steps of carrying out surface coating modification on nano silicon dioxide through 3-aminopropyl triethoxysilane to obtain activated silicon dioxide powder with a large amount of amino groups modified on the surface, and carrying out condensation reaction on isocyanate groups on the isocyanic propyl triethoxysilane and the amino groups on the surface of the activated silicon dioxide powder under the protection of nitrogen to obtain the modified nano silicon dioxide of the triethoxysilane modified activated silicon dioxide powder.
Further, in the step D1, the dosage ratio of the nano silicon dioxide to the absolute ethyl alcohol to the 3-aminopropyl triethoxysilane to the catalyst is 5g to 30mL to 1g to 5mL, the catalyst is 0.3-0.5mol/L sodium hydroxide solution, the post-treatment comprises the steps of after the reaction is completed, the temperature of a reaction kettle is reduced to room temperature, suction filtration, washing a filter cake with purified water to be neutral and then suction drying, placing the filter cake into a drying box with the temperature of 70-80 ℃ and vacuum drying to constant weight to obtain activated silicon dioxide powder, and in the step D2, the dosage ratio of the activated silicon dioxide powder to the toluene to the isocyanatopropyl triethoxysilane is 5g to 50mL to 2g, wherein the post-treatment comprises the steps of suction filtration, washing the filter cake with toluene for 3 times and suction drying, transferring the filter cake into the drying box with the temperature of 70-80 ℃ and vacuum drying to constant weight to obtain the modified nano silicon dioxide.
Further, the whole external diameter of the wire is 0.02 mm-0.05 mm, for example 0.02mm, 0.03mm, 0.04mm and 0.05mm, and the wire has good flexibility, good bending resistance, good tensile strength and good conductivity.
The invention has the following beneficial effects:
1. according to the ultra-fine copper foil wire composite wire, the fine copper foil wire is selected as the conductor core, the fluorine-containing anti-corrosion layer and the outer protective layer are sequentially formed outside the conductor core through thermal coating, the contact area between the fluorine-containing anti-corrosion layer and the outer protective layer is increased, meanwhile, the fluorine-containing anti-corrosion layer and the outer protective layer are tightly contacted, the mechanical strength and the corrosion resistance of the material are improved, and the electromagnetic shielding effectiveness of the composite wire material is improved and the insulation strength of the composite wire material is increased through the preparation method of materials with the optimized outer protective layer.
2. According to the ultra-fine copper foil wire composite wire, in the preparation process, the perfluorooctyl acrylate is introduced into the fluorine-containing resin to serve as a fluorine-containing monomer, so that the weather resistance, chemical corrosion resistance and thermal stability of the resin are improved, meanwhile, the flexibility and processability of the resin can be improved, the tensile strength of the composite wire is improved, the bisphenol A epoxy resin is introduced, the epoxy resin and active groups such as amino groups and hydroxyl groups are subjected to ring-opening condensation in a high-temperature environment to form crosslinking bonding, and the hydroxyl groups are formed, so that the crosslinking density and intermolecular acting force of the resin are enhanced, the tensile strength of the composite wire is further improved, the electronegativity of fluorine atoms is high, the polarization rate is low, the fluorine-containing resin has excellent insulating property, the volume resistivity of the composite wire is improved, and the bisphenol A epoxy resin has certain corrosion resistance and insulating property and is matched with the fluorine-containing resin, so that the corrosion resistance and the insulating strength of the composite wire are further improved.
3. The invention relates to an ultra-fine copper foil wire composite wire, which is characterized in that modified graphite and modified polyethylene are used as reinforcing modifiers to reinforce and modify low-density polyethylene, epoxy groups on modified polyethylene molecules and imino groups on modified graphite molecules are subjected to ring-opening condensation under the action of high temperature, a cross-linking reinforcing network is formed in a low-density polyethylene material to obtain a polyethylene mixture, graphite and polysiloxane all have good chemical stability, a multi-phase structure of the composite polyethylene is formed, and the interaction of all components is performed, a protective layer is formed outside a fluorine-containing anti-corrosion layer, the corrosion resistance of the composite wire is further improved, bisphenol A epoxy resin is used for reinforcing the polyethylene mixture to prepare the composite polyethylene, siloxane bonds in the composite polyethylene molecules are decomposed into silicon hydroxyl groups with high reactivity under the condition of high temperature and water vapor as catalysts, and react with hydroxyl groups, imino groups and the like in the surface of the fluorine-containing anti-corrosion layer or the composite polyethylene molecules to form cross-linking bonding, so that the cross-linking degree of the material is improved, and when the modified graphite is prepared, metal particles are loaded on the graphite, the conductive silicon particles are further improved, the conductive particles are coated on the graphite particles, the conductive particles are uniformly, the conductive particles are coated on the surface of the expanded graphite, the expanded and the surface of the modified graphite is further, and the insulation performance is improved, and the insulation performance is guaranteed.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a three-dimensional structure of an ultra-fine copper foil wire composite wire according to the present invention;
FIG. 2 is a schematic sectional view of the ultra-fine copper foil wire composite wire according to the present invention.
In the figure, 100 parts of copper foil wire cores, 200 parts of fluorine-containing anti-corrosion layers and 300 parts of external protective layers.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the application, vinyl-terminated silicone oil is selected from divinyl-terminated polydimethylsiloxane of Lv-Biing (Jining) chemical technology Co., ltd, the viscosity (25 ℃) is 100+/-10 MPa.S, the vinyl content (molar ratio) is 2.60+/-0.20%, and the low-density polyethylene powder is selected from Dongguan Weijie plastic raw materials Co., ltd, the brand is the middle petrochemical name, the density is 0.918g/cm 3, and the melting point is 122 ℃.
Example 1
The embodiment provides a preparation method of fluorine reinforced modified resin for an ultra-fine copper foil wire composite wire, which comprises the following steps:
A1, preparing fluorine-containing resin
600G of butyl acrylate, 150g of perfluorooctyl acrylate, 100g of vinyl-terminated silicone oil, 170g of oleylamine and 5L of toluene are weighed and added into a reaction kettle protected by nitrogen, the temperature of the reaction kettle is increased to 75 ℃, 8g of azodiisobutyronitrile is added into the reaction kettle, the reaction is kept for 6 hours, the temperature of the reaction kettle is increased to 80 ℃ after the reaction is completed, and the solvent is distilled off under reduced pressure, so that the fluorine-containing resin is obtained.
A2, fluorine reinforced modified resin
Adding fluorine-containing resin and bisphenol A epoxy resin E-51 into a reaction kettle according to the weight ratio of 7:2, stirring, raising the temperature of the reaction kettle to 190 ℃, and carrying out melt mixing for 30min to obtain the fluorine-reinforced modified resin.
Example 2
The embodiment provides a preparation method of fluorine reinforced modified resin for an ultra-fine copper foil wire composite wire, which comprises the following steps:
A1, preparing fluorine-containing resin
650G of butyl acrylate, 165g of perfluorooctyl acrylate, 110g of vinyl-terminated silicone oil, 180g of oleylamine and 5L of toluene are weighed and added into a reaction kettle protected by nitrogen, the temperature of the reaction kettle is increased to 80 ℃, 10g of azodiisobutyronitrile is added into the reaction kettle, the reaction is carried out for 7 hours under heat preservation, the temperature of the reaction kettle is increased to 85 ℃ after the reaction is completed, and the solvent is distilled off under reduced pressure, so that the fluorine-containing resin is obtained.
A2, fluorine reinforced modified resin
Adding fluorine-containing resin and bisphenol A epoxy resin E-51 into a reaction kettle according to the weight ratio of 7:2.5, stirring, raising the temperature of the reaction kettle to 195 ℃, and carrying out melt mixing for 40min to obtain the fluorine-reinforced modified resin.
Example 3
The embodiment provides a preparation method of fluorine reinforced modified resin for an ultra-fine copper foil wire composite wire, which comprises the following steps:
A1, preparing fluorine-containing resin
700G of butyl acrylate, 7180g of perfluorooctyl acrylate, 120g of vinyl-terminated silicone oil, 190g of oleylamine and 5L of toluene are weighed and added into a reaction kettle protected by nitrogen, the temperature of the reaction kettle is increased to 85 ℃,12 g of azodiisobutyronitrile is added into the reaction kettle, the reaction is carried out for 8 hours under heat preservation, the temperature of the reaction kettle is increased to 90 ℃ after the reaction is completed, and the solvent is distilled off under reduced pressure, so that the fluorine-containing resin is obtained.
A2, fluorine reinforced modified resin
Adding fluorine-containing resin and bisphenol A epoxy resin E-51 into a reaction kettle according to the weight ratio of 7:3, stirring, raising the temperature of the reaction kettle to 200 ℃, and carrying out melt mixing for 50min to obtain the fluorine-reinforced modified resin.
Example 4
The embodiment provides a preparation method of composite polyethylene for an ultra-fine copper foil wire composite wire, which comprises the following steps:
b1, preparing modified polyethylene
Uniformly adding low-density polyethylene powder, tea polyphenol, glycidyl methacrylate and benzoyl peroxide in a weight ratio of 100:1:5:0.5 into an internal mixer at 185 ℃, setting the rotating speed of the internal mixer to be 50r/min, and carrying out internal mixing for 10min to obtain a mixture;
transferring the mixture into a plate vulcanizing machine, raising the temperature of the plate vulcanizing machine to 190 ℃, raising the pressure to 9MPa, preserving heat and pressure for 5min, cooling, discharging, crushing, adding 1 g/200 mL of powder and dimethylbenzene into a reaction kettle according to the dosage, stirring, raising the temperature of the reaction kettle to reflux, preserving heat and stirring until the system is dissolved, lowering the temperature of the reaction kettle to room temperature, adding petroleum ether with the volume equal to that of the dimethylbenzene into the reaction kettle, precipitating a large amount of solids, carrying out suction filtration, transferring a filter cake into a drying oven with the temperature of 60 ℃, and drying to constant weight to obtain the modified polyethylene.
B2, preparing expanded graphite
Uniformly mixing potassium permanganate and 80wt% sulfuric acid according to a ratio of 1g to 7mL to obtain a modifier;
Adding flake graphite powder and a modifier into a reaction kettle according to the proportion of 1g to 8mL, stirring for 30min at room temperature, after the reaction is completed, carrying out suction filtration until no liquid drops, adding a filter cake and 20wt% hydrogen peroxide into the reaction kettle according to the proportion of 1g to 8mL, stirring, increasing the temperature of the reaction kettle to 75 ℃, stirring for 60min, reducing the temperature of the reaction kettle to room temperature, carrying out suction filtration, washing a filter cake with purified water to be neutral, carrying out suction drying, transferring the filter cake into a drying box with the temperature of 70 ℃, and carrying out vacuum drying until the weight is constant, thus obtaining activated graphite powder;
and (3) placing the activated graphite powder into a tube furnace in a nitrogen atmosphere, increasing the temperature of the tube furnace to 300 ℃, carrying out heat preservation treatment for 10min, and cooling and discharging to obtain the expanded graphite.
B3, preparing load type expanded graphite
70G of expanded graphite, 10g of pentacarbonyl iron and 5L of kerosene are weighed, added into a high-pressure reaction kettle protected by nitrogen, and stirred in a closed manner, the temperature of the high-pressure reaction kettle is increased to 260 ℃, the pressure of the high-pressure reaction kettle is controlled to be lower than 0.2MPa through a pressure release valve in the heating process, the heat preservation treatment is carried out for 90min, after the reaction is completed, the pressure of the high-pressure reaction kettle is reduced to room temperature, the high-pressure reaction kettle is centrifuged, solids are washed by acetone for 5 times and then pumped, a filter cake is transferred into a drying box with the temperature of 60 ℃, and the filter cake is dried in a vacuum manner to constant weight, so that the load type expanded graphite is obtained.
B4, preparing modified nano silicon dioxide
Weighing 50g of nano silicon dioxide, 300mL of absolute ethyl alcohol and 10g of 3-aminopropyl triethoxysilane, adding into a reaction kettle, stirring, increasing the temperature of the reaction kettle to 50 ℃, adding 50mL of 0.3mol/L sodium hydroxide solution into the reaction kettle, carrying out heat preservation reaction for 50min, reducing the temperature of the reaction kettle to room temperature after the reaction is completed, carrying out suction filtration, washing a filter cake with purified water to be neutral, then carrying out suction drying, placing the filter cake into a drying box with the temperature of 70 ℃, and carrying out vacuum drying to constant weight to obtain activated silicon dioxide powder;
Weighing 50g of activated silicon dioxide powder and 500mL of toluene, adding the activated silicon dioxide powder and the toluene into a reaction kettle protected by nitrogen, stirring, adding 20g of propyltriethoxysilane isocyanate into the reaction kettle at room temperature, stirring for 40min, after the reaction is finished, performing suction filtration, washing a filter cake with toluene for 3 times, then pumping, transferring the filter cake into a drying box with the temperature of 70 ℃, and performing vacuum drying to constant weight to obtain the modified nano silicon dioxide.
B5, preparing modified graphite
Weighing 100g of supported expanded graphite, 40g of modified nano silicon dioxide, 30g of tetraethoxysilane and 1000mL of absolute ethyl alcohol, adding into a reaction kettle, stirring after ultrasonic dispersion for 30min, raising the temperature of the reaction kettle to 50 ℃, adding 10mL of 0.3mol/L sodium hydroxide solution into the reaction kettle, carrying out heat preservation reaction for 60min, reducing the temperature of the reaction kettle to room temperature after the reaction is completed, carrying out suction filtration, washing a filter cake with purified water to be neutral, then carrying out suction drying, and placing the filter cake into a drying box with the temperature of 70 ℃ and carrying out vacuum drying to constant weight to obtain the modified graphite.
B6, preparing composite polyethylene
Weighing 100 parts by weight of low-density polyethylene, 30 parts by weight of modified polyethylene and 12 parts by weight of modified graphite, adding into a double-screw extruder, wherein the temperatures of 6 temperature sections from a feeding end to a discharging end of the double-screw extruder are 190 ℃, 195 ℃ and 200 ℃ in sequence, and the main shaft rotating speed of the double-screw extruder is 15r/min, and crushing after melt extrusion to obtain a polyethylene mixture;
weighing 100 parts by weight of polyethylene mixture and 10 parts by weight of bisphenol A epoxy resin E-51 parts by weight, adding into a reaction kettle, stirring, raising the temperature of the reaction kettle to 190 ℃, and carrying out melt mixing for 30 minutes to obtain the composite polyethylene.
Example 5
The embodiment provides a preparation method of composite polyethylene for an ultra-fine copper foil wire composite wire, which comprises the following steps:
b1, preparing modified polyethylene
Uniformly adding low-density polyethylene powder, tea polyphenol, glycidyl methacrylate and benzoyl peroxide in a weight ratio of 100:1:6:0.5 into an internal mixer at 190 ℃, setting the rotating speed of the internal mixer to be 55r/min, and carrying out internal mixing for 13min to obtain a mixture;
Transferring the mixture into a plate vulcanizing machine, raising the temperature of the plate vulcanizing machine to 195 ℃, raising the pressure to 9.5MPa, preserving heat and pressure for 8min, reducing the temperature and discharging, crushing, adding the powder and the dimethylbenzene into a reaction kettle according to the dosage of 1g to 200mL, stirring, raising the temperature of the reaction kettle to reflux, preserving heat and stirring until the system is dissolved, reducing the temperature of the reaction kettle to room temperature, adding petroleum ether with the volume of the petroleum ether equal to that of the dimethylbenzene into the reaction kettle, precipitating a large amount of solids, carrying out suction filtration, transferring the filter cake into a drying box with the temperature of 65 ℃, and drying to constant weight to obtain the modified polyethylene.
B2, preparing expanded graphite
Uniformly mixing potassium permanganate and 80-90wt% sulfuric acid according to a ratio of 1g to 7mL to obtain a modifier;
Adding flake graphite powder and a modifier into a reaction kettle according to the proportion of 1g to 10mL, stirring for 35min at room temperature, after the reaction is completed, carrying out suction filtration until no liquid drops, adding a filter cake and 25wt% hydrogen peroxide into the reaction kettle according to the proportion of 1g to 9mL, stirring, increasing the temperature of the reaction kettle to 80 ℃, stirring for 70min, reducing the temperature of the reaction kettle to room temperature, carrying out suction filtration, washing a filter cake with purified water to be neutral, carrying out suction drying, transferring the filter cake into a drying box with the temperature of 75 ℃, and carrying out vacuum drying until the weight is constant, thus obtaining activated graphite powder;
And (3) placing the activated graphite powder into a tube furnace in a nitrogen atmosphere, increasing the temperature of the tube furnace to 330 ℃, carrying out heat preservation treatment for 15min, and cooling and discharging to obtain the expanded graphite.
B3, preparing load type expanded graphite
70G of expanded graphite, 10g of pentacarbonyl iron and 5L of kerosene are weighed, added into a high-pressure reaction kettle protected by nitrogen, and stirred in a closed manner, the temperature of the high-pressure reaction kettle is increased to 270 ℃, the pressure of the high-pressure reaction kettle is controlled to be lower than 0.2MPa through a pressure release valve in the heating process, the heat preservation treatment is carried out for 105 minutes, after the reaction is completed, the pressure of the high-pressure reaction kettle is reduced to room temperature, the high-pressure reaction kettle is centrifuged, solids are washed by acetone for 5 times and then pumped, a filter cake is transferred into a drying box with the temperature of 65 ℃, and the filter cake is dried in a vacuum manner to constant weight, so that the load type expanded graphite is obtained.
B4, preparing modified nano silicon dioxide
Weighing 50g of nano silicon dioxide, 300mL of absolute ethyl alcohol and 10g of 3-aminopropyl triethoxysilane, adding into a reaction kettle, stirring, increasing the temperature of the reaction kettle to 50-60 ℃, adding 50mL of 0.4mol/L sodium hydroxide solution into the reaction kettle, carrying out heat preservation reaction for 55min, reducing the temperature of the reaction kettle to room temperature after the reaction is completed, carrying out suction filtration, washing a filter cake with purified water to be neutral, then pumping, placing the filter cake into a drying box with the temperature of 75 ℃, and carrying out vacuum drying to constant weight to obtain activated silicon dioxide powder;
Weighing 50g of activated silicon dioxide powder and 500mL of toluene, adding the activated silicon dioxide powder and the toluene into a reaction kettle protected by nitrogen, stirring, adding 20g of propyltriethoxysilane isocyanate into the reaction kettle at room temperature, stirring for 45min, after the reaction is completed, performing suction filtration, washing a filter cake with toluene for 3 times, then pumping, transferring the filter cake into a drying box with the temperature of 75 ℃, and performing vacuum drying to constant weight to obtain the modified nano silicon dioxide.
B5, preparing modified graphite
Weighing 100g of supported expanded graphite, 40g of modified nano silicon dioxide, 30g of tetraethoxysilane and 1000mL of absolute ethyl alcohol, adding into a reaction kettle, stirring after ultrasonic dispersion for 30-50min, raising the temperature of the reaction kettle to 50-60 ℃, adding 10mL of 0.4mol/L sodium hydroxide solution into the reaction kettle, carrying out heat preservation reaction for 75min, reducing the temperature of the reaction kettle to room temperature after the reaction is completed, carrying out suction filtration, washing a filter cake with purified water to be neutral, then pumping the filter cake, placing the filter cake into a drying box with the temperature of 75 ℃, and carrying out vacuum drying to constant weight to obtain the modified graphite.
B6, preparing composite polyethylene
Weighing 100 parts by weight of low-density polyethylene, 35 parts by weight of modified polyethylene and 14 parts by weight of modified graphite, adding into a double-screw extruder, wherein the temperatures of 6 temperature sections from a feeding end to a discharging end of the double-screw extruder are 190 ℃, 195 ℃ and 200 ℃ in sequence, and the main shaft rotating speed of the double-screw extruder is 15r/min, and crushing after melt extrusion to obtain a polyethylene mixture;
Weighing 100 parts by weight of polyethylene mixture and 13 parts by weight of bisphenol A epoxy resin E-51 parts by weight, adding into a reaction kettle, stirring, raising the temperature of the reaction kettle to 195 ℃, and carrying out melt mixing for 40min to obtain the composite polyethylene.
Example 6
The embodiment provides a preparation method of composite polyethylene for an ultra-fine copper foil wire composite wire, which comprises the following steps:
b1, preparing modified polyethylene
Uniformly adding low-density polyethylene powder, tea polyphenol, glycidyl methacrylate and benzoyl peroxide in a weight ratio of 100:1:7:0.5 into an internal mixer at a temperature of 195 ℃, setting the rotating speed of the internal mixer to be 60r/min, and carrying out internal mixing for 15min to obtain a mixture;
Transferring the mixture into a plate vulcanizing machine, raising the temperature of the plate vulcanizing machine to 200 ℃, raising the pressure to 10MPa, preserving heat and pressure for 10min, cooling, discharging, crushing, adding 1 g/200 mL of powder and dimethylbenzene into a reaction kettle according to the dosage, stirring, raising the temperature of the reaction kettle to reflux, preserving heat and stirring until the system is dissolved, lowering the temperature of the reaction kettle to room temperature, adding petroleum ether with the volume equal to that of the dimethylbenzene into the reaction kettle, precipitating a large amount of solids, carrying out suction filtration, transferring a filter cake into a drying oven with the temperature of 70 ℃, and drying to constant weight to obtain the modified polyethylene.
B2, preparing expanded graphite
Uniformly mixing potassium permanganate and 90wt% sulfuric acid according to a ratio of 1g to 7mL to obtain a modifier;
Adding flake graphite powder and a modifier into a reaction kettle according to the proportion of 1g to 12mL, stirring for 40min at room temperature, after the reaction is completed, carrying out suction filtration until no liquid drops, adding a filter cake and 30wt% hydrogen peroxide into the reaction kettle according to the proportion of 1g to 10mL, stirring, increasing the temperature of the reaction kettle to 85 ℃, stirring for 80min, reducing the temperature of the reaction kettle to room temperature, carrying out suction filtration, washing a filter cake with purified water to be neutral, carrying out suction drying, transferring the filter cake into a drying box with the temperature of 80 ℃, and carrying out vacuum drying until the weight is constant, thus obtaining activated graphite powder;
And (3) placing the activated graphite powder into a tube furnace in a nitrogen atmosphere, increasing the temperature of the tube furnace to 350 ℃, carrying out heat preservation treatment for 20min, and cooling and discharging to obtain the expanded graphite.
B3, preparing load type expanded graphite
70G of expanded graphite, 10g of pentacarbonyl iron and 5L of kerosene are weighed, added into a high-pressure reaction kettle protected by nitrogen, and stirred in a closed manner, the temperature of the high-pressure reaction kettle is increased to 280 ℃, the pressure of the high-pressure reaction kettle is controlled to be lower than 0.2MPa through a pressure release valve in the heating process, the heat preservation treatment is carried out for 120min, after the reaction is completed, the pressure of the high-pressure reaction kettle is reduced to room temperature, the high-pressure reaction kettle is centrifuged, solids are washed by acetone for 5 times and then pumped, a filter cake is transferred into a drying box with the temperature of 70 ℃, and the filter cake is dried in a vacuum manner to constant weight, so that the load type expanded graphite is obtained.
B4, preparing modified nano silicon dioxide
Weighing 50g of nano silicon dioxide, 300mL of absolute ethyl alcohol and 10g of 3-aminopropyl triethoxysilane, adding into a reaction kettle, stirring, heating the reaction kettle to 60 ℃, adding 50mL of 0.5mol/L sodium hydroxide solution into the reaction kettle, carrying out heat preservation reaction for 60min, reducing the temperature of the reaction kettle to room temperature after the reaction is completed, carrying out suction filtration, washing a filter cake with purified water to be neutral, then carrying out suction drying, placing the filter cake into a drying box with the temperature of 80 ℃, and carrying out vacuum drying to constant weight to obtain activated silicon dioxide powder;
weighing 50g of activated silicon dioxide powder and 500mL of toluene, adding the activated silicon dioxide powder and the toluene into a reaction kettle protected by nitrogen, stirring, adding 20g of propyltriethoxysilane isocyanate into the reaction kettle at room temperature, stirring for 50min, after the reaction is completed, performing suction filtration, washing a filter cake with toluene for 3 times, then pumping, transferring the filter cake into a drying box with the temperature of 80 ℃, and performing vacuum drying to constant weight to obtain the modified nano silicon dioxide.
B5, preparing modified graphite
Weighing 100g of supported expanded graphite, 40g of modified nano silicon dioxide, 30g of tetraethoxysilane and 1000mL of absolute ethyl alcohol, adding into a reaction kettle, stirring after ultrasonic dispersion for 50min, raising the temperature of the reaction kettle to 60 ℃, adding 10mL of 0.5mol/L sodium hydroxide solution into the reaction kettle, carrying out heat preservation reaction for 90min, reducing the temperature of the reaction kettle to room temperature after the reaction is completed, carrying out suction filtration, washing a filter cake with purified water to be neutral, then carrying out suction drying, and placing the filter cake into a drying box with the temperature of 80 ℃ and carrying out vacuum drying to constant weight to obtain the modified graphite.
B6, preparing composite polyethylene
Weighing 100 parts by weight of low-density polyethylene, 40 parts by weight of modified polyethylene and 16 parts by weight of modified graphite, adding the low-density polyethylene, 40 parts by weight of modified polyethylene and 16 parts by weight of modified graphite into a double-screw extruder, wherein the temperatures of 6 temperature sections from a feeding end to a discharging end of the double-screw extruder are 190 ℃, 195 ℃ and 200 ℃ in sequence, and the main shaft rotating speed of the double-screw extruder is 15r/min, and crushing after melt extrusion to obtain a polyethylene mixture;
weighing 100 parts by weight of polyethylene mixture and 15 parts by weight of bisphenol A epoxy resin E-51 parts by weight, adding into a reaction kettle, stirring, raising the temperature of the reaction kettle to 200 ℃, and carrying out melt mixing for 50 minutes to obtain the composite polyethylene.
Example 7
Referring to fig. 1-2, the embodiment provides a method for preparing an ultra-fine copper foil wire composite wire, which comprises the following steps:
S1, adding the fluorine-reinforced modified resin prepared in the embodiment 1 into a smelting furnace with the temperature of 190 ℃, and heating the mixture at a constant temperature until the fluorine-reinforced modified resin is melted to obtain fluid fluorine-reinforced modified resin coating liquid;
S2, adding the composite polyethylene prepared in the embodiment 4 into a smelting furnace with the temperature of 190 ℃, and heating the composite polyethylene in a heat preservation manner until the composite polyethylene is melted to obtain fluid composite polyethylene coating liquid;
S3, selecting a copper foil wire with the diameter of 0.02mm as a copper foil wire core 100, heating the copper foil wire core 100 to 500 ℃, carrying out heat preservation treatment for 2min, passing the copper foil wire core 100 through a smelting furnace filled with fluorine-reinforced modified resin coating liquid, then passing through a forming hole, carrying out water cooling, cooling and solidifying, forming a fluorine-containing anticorrosive layer 200 with the thickness of 0.008mm on the surface of the copper foil wire core 100, and arranging a plurality of grooves parallel to the copper foil wire core 100 on the fluorine-containing anticorrosive layer 200 to obtain a composite wire blank;
S4, the composite conductor blank passes through a smelting furnace filled with composite polyethylene coating liquid without drying, passes through a forming hole, is cooled and solidified, and forms an outer protective layer 300 with the thickness of 0.015mm on the surface of the composite conductor blank, so that the composite conductor with the insulating layer coating the wire core is obtained.
Example 8
Referring to fig. 1-2, the embodiment provides a method for preparing an ultra-fine copper foil wire composite wire, which comprises the following steps:
S1, adding the fluorine-reinforced modified resin prepared in the embodiment 2 into a smelting furnace with the temperature of 195 ℃, and heating the mixture at a constant temperature until the fluorine-reinforced modified resin is melted to obtain fluid fluorine-reinforced modified resin coating liquid;
S2, adding the composite polyethylene prepared in the embodiment 5 into a smelting furnace with the temperature of 195 ℃, and heating the composite polyethylene in a heat preservation manner until the composite polyethylene is melted to obtain fluid composite polyethylene coating liquid;
S3, selecting a copper foil wire with the diameter of 0.03mm as a copper foil wire core 100, heating the copper foil wire core 100 to 600 ℃, carrying out heat preservation treatment for 2.5min, passing the copper foil wire core 100 through a smelting furnace filled with fluorine-reinforced modified resin coating liquid, then passing through a forming hole, carrying out water cooling and cooling solidification, forming a fluorine-containing anticorrosive layer 200 with the thickness of 0.010mm on the surface of the copper foil wire core 100, and arranging a plurality of grooves parallel to the copper foil wire core 100 on the fluorine-containing anticorrosive layer 200 to obtain a composite wire blank;
S4, the composite conductor blank passes through a smelting furnace filled with composite polyethylene coating liquid without drying, passes through a forming hole, is cooled and solidified, and forms an outer protective layer 300 with the thickness of 0.017mm on the surface of the composite conductor blank, so that the composite conductor with the insulating layer coating the wire core is obtained.
Example 9
Referring to fig. 1-2, the embodiment provides a method for preparing an ultra-fine copper foil wire composite wire, which comprises the following steps:
s1, adding the fluorine-reinforced modified resin prepared in the embodiment 3 into a smelting furnace with the temperature of 200 ℃, and heating the mixture at a constant temperature until the fluorine-reinforced modified resin is melted to obtain fluid fluorine-reinforced modified resin coating liquid;
s2, adding the composite polyethylene prepared in the embodiment 6 into a smelting furnace with the temperature of 200 ℃, and heating the composite polyethylene in a heat preservation way until the composite polyethylene is melted to obtain fluid composite polyethylene coating liquid;
S3, selecting a copper foil wire with the diameter of 0.05mm as a copper foil wire core 100, heating the copper foil wire core 100 to 700 ℃, carrying out heat preservation treatment for 3min, passing the copper foil wire core 100 through a smelting furnace filled with fluorine-reinforced modified resin coating liquid, then passing through a forming hole, carrying out water cooling, cooling and solidifying, forming a fluorine-containing anticorrosive layer 200 with the thickness of 0.012mm on the surface of the copper foil wire core 100, and arranging a plurality of grooves parallel to the copper foil wire core 100 on the fluorine-containing anticorrosive layer 200 to obtain a composite wire blank;
s4, the composite conductor blank passes through a smelting furnace filled with composite polyethylene coating liquid without drying, passes through a forming hole, is cooled and solidified, and forms an outer protective layer 300 with the thickness of 0.018mm on the surface of the composite conductor blank, so that the composite conductor with the insulating layer coating the wire core is obtained.
Comparative example 1
This comparative example differs from example 9 in that example 3 was prepared without adding bisphenol a epoxy resin in step A2.
Comparative example 2
This comparative example differs from example 9 in that in example 6, in the preparation of the composite polyethylene, step B6 was carried out in the preparation of the polyethylene mixture without adding the modified polyethylene.
Comparative example 3
This comparative example differs from example 9 in that in example 6, step B5 was omitted and the modified graphite in step B6 was replaced with the supported expanded graphite in step B3 when preparing the composite polyethylene.
Comparative example 4
This comparative example differs from example 9 in that in example 6, step B3 was omitted and the expanded graphite in step B2 was used instead of the supported expanded graphite in step B6 in the preparation of the composite polyethylene.
Performance test:
The tensile strength, elongation at break, maximum bending degree and volume resistivity at 20 ℃ of the composite wires prepared in examples 7 to 9 and comparative examples 1 to 4 were measured with reference to the standard GB/T11016.2-2009 section 2 of Plastic-insulated and rubber-insulated telephone cord;
The shielding effectiveness of the composite wires prepared in examples 7 to 9 and comparative examples 1 to 4 was measured with reference to the standard GB/T30842-2014 electromagnetic shielding effectiveness requirement and measurement method in high voltage laboratory, and the specific test results are shown in Table 1 below.
TABLE 1 Performance test data sheet for samples
Data analysis:
The data in the table are compared and analyzed, the tensile strength of the composite wire prepared by the application is 32.5MPa, the elongation at break is 375%, the maximum bending degree is 15mm, the shielding effectiveness is 37.2dB, the volume resistivity is 1.71 multiplied by 10 17 omega-m, and all performance data are better than those of the comparative example.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
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