CN116130142A - High-conductivity, anti-corrosion and anti-aging electric power composite grease and preparation method thereof - Google Patents
High-conductivity, anti-corrosion and anti-aging electric power composite grease and preparation method thereof Download PDFInfo
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- CN116130142A CN116130142A CN202211696163.9A CN202211696163A CN116130142A CN 116130142 A CN116130142 A CN 116130142A CN 202211696163 A CN202211696163 A CN 202211696163A CN 116130142 A CN116130142 A CN 116130142A
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- 239000004519 grease Substances 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 64
- 238000005260 corrosion Methods 0.000 title claims abstract description 34
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 68
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 56
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052709 silver Inorganic materials 0.000 claims abstract description 41
- 239000004332 silver Substances 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 40
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 35
- 239000002134 carbon nanofiber Substances 0.000 claims abstract description 32
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011231 conductive filler Substances 0.000 claims abstract description 31
- 150000001875 compounds Chemical class 0.000 claims abstract description 26
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 230000032683 aging Effects 0.000 claims abstract description 13
- 230000007797 corrosion Effects 0.000 claims abstract description 13
- 229920002545 silicone oil Polymers 0.000 claims description 43
- 238000000227 grinding Methods 0.000 claims description 36
- 239000011248 coating agent Substances 0.000 claims description 28
- 238000000576 coating method Methods 0.000 claims description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 230000004048 modification Effects 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 15
- 239000005662 Paraffin oil Substances 0.000 claims description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 14
- 125000000217 alkyl group Chemical group 0.000 claims description 14
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 14
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 14
- -1 methyl trifluoropropyl Chemical group 0.000 claims description 14
- 229920000570 polyether Polymers 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 230000004913 activation Effects 0.000 claims description 11
- 239000000440 bentonite Substances 0.000 claims description 11
- 229910000278 bentonite Inorganic materials 0.000 claims description 11
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 11
- 229910021485 fumed silica Inorganic materials 0.000 claims description 11
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 11
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 11
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 11
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 11
- 230000004927 fusion Effects 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 6
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002562 thickening agent Substances 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 5
- 238000000498 ball milling Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 3
- 239000002199 base oil Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229940099259 vaseline Drugs 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a high-conductivity, anti-corrosion and anti-aging electric power compound grease which comprises the following components in percentage by mass: 60% -70% of composite conductive filler, 20% -30% of base grease and 5% -10% of mixing auxiliary agent; the composite conductive filler comprises: 4-10 parts of graphene flakes, 8-20 parts of graphite powder, 60-80 parts of silver-coated copper powder and 6-12 parts of carbon nanofiber powder. The invention also discloses a preparation method of the high-conductivity, anti-corrosion and aging-resistant electric power composite grease. The high-conductivity, corrosion-resistant and aging-resistant power compound grease and the preparation method thereof can solve the problems of poor conductivity and low drop point of the traditional power compound grease, and have the advantages of aging resistance and corrosion resistance.
Description
Technical Field
The invention relates to the technical field of composite grease, in particular to high-conductivity, corrosion-resistant and aging-resistant electric power composite grease and a preparation method thereof.
Background
The composite grease for electric power is also called conductive paste, is a neutral conductive dressing with good electric contact performance, and is widely applied to installation, overhaul and maintenance of power transformation, transmission and distribution equipment. When the electric power compound grease is used, the electric power compound grease is coated on the contact surface of the conductor which is electrically connected, and has the functions of reducing contact resistance, reducing heating and improving through-flow capacity.
The main components of the electric power composite grease comprise oils and conductive fillers, the oils are mostly single base oil, such as vaseline and the like, the conductive fillers are mainly single metal powder, and the metal powder is mixed with the base oil to prepare the electric power composite grease. However, the electric power composite grease has low dropping point, is easy to flow at high temperature, has unsatisfactory electric conductivity and has great potential safety hazard.
Disclosure of Invention
The invention aims to provide a high-conductivity, corrosion-resistant and aging-resistant electric power compound grease, which solves the problems of poor conductivity and low dropping point of the traditional electric power compound grease. The invention further aims to provide a preparation method of the high-conductivity, corrosion-resistant and aging-resistant electric power composite grease.
In order to achieve the purpose, the invention provides a high-conductivity, anti-corrosion and anti-aging electric power compound grease which comprises the following components in percentage by mass: 60% -70% of composite conductive filler, 20% -30% of base grease and 5% -10% of mixing auxiliary agent; the composite conductive filler comprises: 4-10 parts of graphene flakes, 8-20 parts of graphite powder, 60-80 parts of silver-coated copper powder and 6-12 parts of carbon nanofiber powder.
Preferably, the thickness of the graphene flake is 30-400nm, the particle size of the graphite powder is 1000 meshes, and the particle size of the silver-coated copper powder is 2 mu m; the diameter of the carbon nano fiber powder is 50-200nm, and the length is 50-100um.
Preferably, the base lipid is a polyether: paraffin oil: methyl trifluoropropyl silicone oil: methyl long chain alkyl silicone oil: benzyl silicone oil = 3:2:1:1:1 mixture; the viscosity of the polyether was 300, the viscosity of the paraffin oil was 500, the viscosity of the methyltrifluoropropyl silicone oil was 1000, the viscosity of the methyl long-chain alkyl silicone oil was 5000, and the viscosity of the benzyl silicone oil was 10000.
Preferably, the mixing auxiliary agent comprises 2-4 parts of dispersing agent sodium polyacrylate, 4-6 parts of thickener fumed silica, 2-4 parts of antioxidant tris (2, 4-di-tert-butylphenyl) phosphite, 8-12 parts of bentonite and 2-6 parts of molybdenum disulfide.
The preparation method of the high-conductivity, anti-corrosion and anti-aging power compound grease comprises the following steps:
s1, preparing silver-coated copper powder, namely adding ultrafine copper powder into an activation solution, stirring for 10min at normal temperature, standing, and carrying out solid-liquid separation to obtain copper powder suspension; dropwise adding a mixed solution of silver nitrate and tetraisopropyl di (dioctyl phosphite acyloxy) titanate in a constant temperature environment of 50 ℃, adding a reducing agent disodium ethylenediamine tetraacetate, stirring uniformly, standing until solid-liquid separation is achieved, and vacuum drying to obtain compact silver-coated copper powder;
s2, preparing a composite conductive filler, namely respectively adding graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder into a ball-type grinding machine, and grinding for 2 hours to obtain composite powder; adding the composite powder into a fusion coating machine, carrying out coating modification, coating a graphite layer and a graphene layer on the surface of silver-coated copper powder, and grafting carbon nanofibers;
s3, preparing base grease, namely mixing polyether with the viscosity of 300 Pa.s, paraffin oil with the viscosity of 500 Pa.s, methyltrifluoropropyl silicone oil with the viscosity of 1000 Pa.s, methyl long-chain alkyl silicone oil with the viscosity of 5000 Pa.s and benzyl silicone oil with the viscosity of 10000 Pa.s in a stirrer according to the mass ratio of 3:2:1:1:1 for 0.5h to obtain the base grease;
s4, preparing a mixed auxiliary agent, namely adding 2-4 parts of sodium polyacrylate, 4-6 parts of fumed silica, 2-4 parts of tris (2, 4-di-tert-butylphenyl) phosphite ester, 8-12 parts of bentonite and 2-6 parts of molybdenum disulfide into a vacuum shearing, dispersing and grinding device for grinding, homogenizing and stirring for 0.5h to obtain the mixed auxiliary agent;
s5, adding the composite conductive filler and the base grease into a three-roller grinder for constant-temperature grinding, and standing for 5-10 min to obtain a mixed matrix; adding the mixed auxiliary agent into the mixed matrix at a constant speed, stirring uniformly for 0.5h in a vacuum deaeration machine, and cooling to room temperature to obtain the electric power composite grease.
Preferably, in the step S1, the activating solution is a suspension of 2% 1,4 butynediol and 4% ammonium chloride.
Preferably, in the S1, the mass ratio of the silver nitrate to the tetraisopropyl di (dioctyl phosphite acyloxy) titanate is 1:1, and the concentration is 0.4mol/L.
Preferably, in the step S2, the temperature of the coating modification is 100-220 ℃ and the time is 5-7 h.
Preferably, in the step S5, the grinding temperature of the grinder is 60-80 ℃ and the grinding time is 1h.
The high-conductivity, anti-corrosion and anti-aging electric power compound grease and the preparation method thereof have the advantages and positive effects that:
1. the graphene flake, the graphite powder, the silver-coated copper powder and the carbon nanofiber are used as the composite conductive filler, the graphene flake has excellent electrical property, high elastic modulus and very good heat conductivity, the graphite powder has good heat resistance and conductivity, and the carbon nanofiber is inserted between the coated copper powder by utilizing the large length-diameter ratio and the high specific surface area of the carbon nanofiber to construct a high-efficiency conductive and heat-conductive network, so that the heat resistance and the conductivity of the composite conductive filler can be further improved. And the graphite powder has good lubricating property, so that graphene flakes, carbon nanofiber powder and graphite powder can be uniformly coated on the silver-coated copper powder, and the wear resistance of the composite conductive filler is improved.
2. The closest packing of the composite powder is realized by adopting a ball milling mode, more powder can be added into the homogeneous base grease, a high-efficiency electric conduction and heat conduction network is constructed, and the electric conductivity and the heat conductivity of the electric composite grease are improved.
Detailed Description
The high-conductivity, anti-corrosion and anti-aging power compound grease comprises the following components in percentage by mass: 60% -70% of composite conductive filler, 20% -30% of base grease and 5% -10% of mixing auxiliary agent; the composite conductive filler comprises: 4-10 parts of graphene flakes, 8-20 parts of graphite powder, 60-80 parts of silver-coated copper powder and 6-15 parts of carbon nanofiber powder.
The thickness of the graphene flake is 30-400nm, the particle size of the graphite powder is 1000 meshes, and the particle size of the silver-coated copper powder is 2 mu m; the diameter of the carbon nano fiber powder is 50-200nm, and the length is 50-100um.
The base grease is polyether: paraffin oil: methyl trifluoropropyl silicone oil: methyl long chain alkyl silicone oil: benzyl silicone oil = 3:2:1:1:1 mixture; the viscosity of the polyether was 300, the viscosity of the paraffin oil was 500, the viscosity of the methyltrifluoropropyl silicone oil was 1000, the viscosity of the methyl long-chain alkyl silicone oil was 5000, and the viscosity of the benzyl silicone oil was 10000.
The mixing auxiliary agent comprises 2-4 parts of dispersing agent sodium polyacrylate, 4-6 parts of thickener fumed silica, 2-4 parts of antioxidant tris (2, 4-di-tert-butylphenyl) phosphite, 8-12 parts of bentonite and 2-6 parts of molybdenum disulfide.
The preparation method of the high-conductivity, anti-corrosion and anti-aging power compound grease comprises the following steps:
s1, preparing silver-coated copper powder, namely adding ultrafine copper powder into an activation solution, stirring for 10min at normal temperature, standing, and carrying out solid-liquid separation to obtain copper powder suspension; dropwise adding a mixed solution of silver nitrate and tetraisopropyl di (dioctyl phosphite acyloxy) titanate in a constant temperature environment of 50 ℃, adding a reducing agent disodium ethylenediamine tetraacetate, stirring uniformly, standing until solid-liquid separation, and vacuum drying to obtain compact silver-coated copper powder.
The activation solution is a suspension of 2% 1,4 butynediol and 4% ammonium chloride.
The mass ratio of the silver nitrate to the tetraisopropyl di (dioctyl phosphite acyloxy) titanate is 1:1, and the concentration is 0.4mol/L.
S2, preparing a composite conductive filler, namely respectively adding graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder into a ball-type grinding machine, and grinding for 2 hours to obtain composite powder; and adding the composite powder into a fusion coating machine, coating and modifying, coating a graphite layer and a graphene layer on the surface of the silver-coated copper powder, and grafting carbon nanofibers.
The temperature of coating modification is 100-220 ℃ and the time is 5-7 h.
The stripping of graphene scales is realized through high temperature and shearing force generated by ball milling to obtain thin-layer graphene with the thickness of 30-400nm, and the closest packing and surface activation of the composite powder of graphene, graphite powder, silver coated copper powder and carbon nanofiber powder are realized by means of the ball milling mechanical force shaping effect.
Cladding fusion is to inlay one material on another material by adopting external mechanical force, and combine to form a new material with two material characteristics. According to the invention, graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder are used as composite conductive filler, the graphene and the graphite powder are fused on the surface of the copper powder, and carbon nanofibers are inserted into the composite conductive filler, so that a novel substance which not only has the magnetism of a metal material, but also has the ultrahigh conductivity and toughness of the graphene and the graphite is obtained.
The graphene flake has excellent electrical property, high elastic modulus and very good heat conduction performance, and the graphene flake and the graphite powder mutually promote the electric conduction and heat conduction performance under the action of the carbon nanofiber, and meanwhile, the heat resistance, the wear resistance, the ageing resistance and the corrosion resistance of the silver-coated copper powder are improved. The closest packing of the composite powder is realized by adopting a ball milling mode, more powder can be added into the homogeneous base grease, a high-efficiency electric conduction and heat conduction network is constructed, and the electric conductivity and the heat conductivity of the electric composite grease are improved.
S3, preparing base grease, namely mixing polyether with the viscosity of 300 Pa.s, paraffin oil with the viscosity of 500 Pa.s, methyl trifluoropropyl silicone oil with the viscosity of 1000 Pa.s, methyl long-chain alkyl silicone oil with the viscosity of 5000 Pa.s and benzyl silicone oil with the viscosity of 10000 Pa.s in a stirrer according to the mass ratio of 3:2:1:1:1 for 0.5h to obtain the base grease.
S4, preparing a mixed auxiliary agent, namely adding 2-4 parts of sodium polyacrylate, 4-6 parts of fumed silica, 2-4 parts of tris (2, 4-di-tert-butylphenyl) phosphite, 8-12 parts of bentonite and 2-6 parts of molybdenum disulfide into a vacuum shearing, dispersing and grinding device for grinding, homogenizing and stirring for 0.5h to obtain the mixed auxiliary agent.
S5, adding the composite conductive filler and the base grease into a three-roller grinder for constant-temperature grinding, and standing for 5-10 min to obtain a mixed matrix; adding the mixed auxiliary agent into the mixed matrix at a constant speed, stirring uniformly for 0.5h in a vacuum deaeration machine, and cooling to room temperature to obtain the electric power composite grease. The grinding temperature of the grinder is 60-80 ℃ and the grinding time is 1h.
Example 1
The high-conductivity, anti-corrosion and anti-aging electric power compound grease comprises the following components in parts by weight:
graphite powder | 8 |
Graphene flake | 4 |
Carbon nanofiber powder | 6 |
Silver-coated copper powder | 60 |
Sodium polyacrylate | 2 |
Fumed silica | 4 |
Bentonite clay | 8 |
Tris (2, 4-di-tert-butylphenyl) phosphite | 2 |
Molybdenum disulfide | 2 |
Polyether | 6 |
Paraffin oil | 4 |
Methyl trifluoropropyl silicone oil | 2 |
Methyl long-chain alkyl silicone oil | 2 |
Benzyl silicone oil | 2 |
The preparation method of the high-conductivity, anti-corrosion and anti-aging power compound grease comprises the following steps:
s1, preparing silver-coated copper powder, namely adding ultrafine copper powder into an activation solution, stirring for 10min at normal temperature, standing, and carrying out solid-liquid separation to obtain copper powder suspension; dropwise adding a mixed solution of silver nitrate and tetraisopropyl di (dioctyl phosphite acyloxy) titanate in a constant temperature environment of 50 ℃, adding a reducing agent disodium ethylenediamine tetraacetate, stirring uniformly, standing until solid-liquid separation, and vacuum drying to obtain compact silver-coated copper powder. The activation solution is a suspension of 2% 1,4 butynediol and 4% ammonium chloride. The mass ratio of the silver nitrate to the tetraisopropyl di (dioctyl phosphite acyloxy) titanate is 1:1, and the concentration is 0.4mol/L.
S2, preparing a composite conductive filler, namely adding graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder into a ball-type grinding machine respectively, and grinding for 2 hours to obtain composite powder with the thickness of the graphene flakes being 30-400nm, the particle size of the graphite powder being 1000 meshes, the particle size of the silver-coated copper powder being 2 mu m and the diameter of the carbon nanofiber powder being 50-200 nm. And adding the composite powder into a fusion coating machine for coating modification, wherein the coating modification temperature is 100-220 ℃ and the coating modification time is 5-7 h. And coating a graphite layer and a graphene layer on the surface of the silver-coated copper powder, and grafting carbon nanofibers to obtain the composite conductive filler.
S3, preparing base grease, namely mixing polyether with the viscosity of 300 Pa.s, paraffin oil with the viscosity of 500 Pa.s, methyl trifluoropropyl silicone oil with the viscosity of 1000 Pa.s, methyl long-chain alkyl silicone oil with the viscosity of 5000 Pa.s and benzyl silicone oil with the viscosity of 10000 Pa.s in a stirrer according to the mass ratio of 3:2:1:1:1 for 0.5h to obtain the base grease.
S4, preparing a mixing auxiliary agent, namely adding sodium polyacrylate, fumed silica, tris (2, 4-di-tert-butylphenyl) phosphite, bentonite and molybdenum disulfide into a vacuum shearing, dispersing and grinding device for grinding, homogenizing and stirring for 0.5h to obtain the mixing auxiliary agent.
S5, adding the composite conductive filler and the base grease into a three-roller grinder, grinding for 1h in a constant temperature environment of 60-80 ℃, and standing for 5-10 min to obtain a mixed matrix; adding the mixed auxiliary agent into the mixed matrix at a constant speed, stirring uniformly for 0.5h in a vacuum deaeration machine, and cooling to room temperature to obtain the electric power composite grease.
Example 2
The high-conductivity, anti-corrosion and anti-aging electric power compound grease comprises the following components in parts by weight:
graphite powder | 12 |
Graphene flake | 6 |
Carbon nanofiber powder | 9 |
Silver-coated copper powder | 70 |
Sodium polyacrylate | 3 |
Fumed silica | 5 |
Bentonite clay | 10 |
Tris (2, 4-di-tert-butylphenyl) phosphite | 3 |
Molybdenum disulfide | 4 |
Polyether | 9 |
Paraffin oil | 6 |
Methyl trifluoropropyl silicone oil | 3 |
Methyl long-chain alkyl silicone oil | 3 |
Benzyl silicone oil | 3 |
The preparation method of the high-conductivity, anti-corrosion and anti-aging power compound grease comprises the following steps:
s1, preparing silver-coated copper powder, namely adding ultrafine copper powder into an activation solution, stirring for 10min at normal temperature, standing, and carrying out solid-liquid separation to obtain copper powder suspension; dropwise adding a mixed solution of silver nitrate and tetraisopropyl di (dioctyl phosphite acyloxy) titanate in a constant temperature environment of 50 ℃, adding a reducing agent disodium ethylenediamine tetraacetate, stirring uniformly, standing until solid-liquid separation, and vacuum drying to obtain compact silver-coated copper powder. The activation solution is a suspension of 2% 1,4 butynediol and 4% ammonium chloride. The mass ratio of the silver nitrate to the tetraisopropyl di (dioctyl phosphite acyloxy) titanate is 1:1, and the concentration is 0.4mol/L.
S2, preparing a composite conductive filler, namely respectively adding graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder into a ball-type grinding machine, and grinding for 2 hours to obtain composite powder with the thickness of the graphene flakes being 30-400nm, the particle size of the graphite powder being 1000 meshes, the particle size of the silver-coated copper powder being 2 mu m and the diameter of the carbon nanofiber powder being 50-200 nm. And adding the composite powder into a fusion coating machine for coating modification, wherein the coating modification temperature is 100-220 ℃ and the coating modification time is 5-7 h. And coating a graphite layer and a graphene layer on the surface of the silver-coated copper powder, and grafting carbon nanofibers to obtain the composite conductive filler.
S3, preparing base grease, namely mixing polyether with the viscosity of 300 Pa.s, paraffin oil with the viscosity of 500 Pa.s, methyl trifluoropropyl silicone oil with the viscosity of 1000 Pa.s, methyl long-chain alkyl silicone oil with the viscosity of 5000 Pa.s and benzyl silicone oil with the viscosity of 10000 Pa.s in a stirrer according to the mass ratio of 3:2:1:1:1 for 0.5h to obtain the base grease.
S4, preparing a mixing auxiliary agent, namely adding sodium polyacrylate, fumed silica, tris (2, 4-di-tert-butylphenyl) phosphite, bentonite and molybdenum disulfide into a vacuum shearing, dispersing and grinding device for grinding, homogenizing and stirring for 0.5h to obtain the mixing auxiliary agent.
S5, adding the composite conductive filler and the base grease into a three-roller grinder, grinding for 1h in a constant temperature environment of 60-80 ℃, and standing for 5-10 min to obtain a mixed matrix; adding the mixed auxiliary agent into the mixed matrix at a constant speed, stirring uniformly for 0.5h in a vacuum deaeration machine, and cooling to room temperature to obtain the electric power composite grease.
Example 3
The high-conductivity, anti-corrosion and anti-aging electric power compound grease comprises the following components in parts by weight:
the preparation method of the high-conductivity, anti-corrosion and anti-aging power compound grease comprises the following steps:
s1, preparing silver-coated copper powder, namely adding ultrafine copper powder into an activation solution, stirring for 10min at normal temperature, standing, and carrying out solid-liquid separation to obtain copper powder suspension; dropwise adding a mixed solution of silver nitrate and tetraisopropyl di (dioctyl phosphite acyloxy) titanate in a constant temperature environment of 50 ℃, adding a reducing agent disodium ethylenediamine tetraacetate, stirring uniformly, standing until solid-liquid separation, and vacuum drying to obtain compact silver-coated copper powder. The activation solution is a suspension of 2% 1,4 butynediol and 4% ammonium chloride. The mass ratio of the silver nitrate to the tetraisopropyl di (dioctyl phosphite acyloxy) titanate is 1:1, and the concentration is 0.4mol/L.
S2, preparing a composite conductive filler, namely respectively adding graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder into a ball-type grinding machine, and grinding for 2 hours to obtain composite powder with the thickness of the graphene flakes being 30-400nm, the particle size of the graphite powder being 1000 meshes, the particle size of the silver-coated copper powder being 2 mu m and the diameter of the carbon nanofiber powder being 50-200 nm. And adding the composite powder into a fusion coating machine for coating modification, wherein the coating modification temperature is 100-220 ℃ and the coating modification time is 5-7 h. And coating a graphite layer and a graphene layer on the surface of the silver-coated copper powder, and grafting carbon nanofibers to obtain the composite conductive filler.
S3, preparing base grease, namely mixing polyether with the viscosity of 300 Pa.s, paraffin oil with the viscosity of 500 Pa.s, methyl trifluoropropyl silicone oil with the viscosity of 1000 Pa.s, methyl long-chain alkyl silicone oil with the viscosity of 5000 Pa.s and benzyl silicone oil with the viscosity of 10000 Pa.s in a stirrer according to the mass ratio of 3:2:1:1:1 for 0.5h to obtain the base grease.
S4, preparing a mixing auxiliary agent, namely adding sodium polyacrylate, fumed silica, tris (2, 4-di-tert-butylphenyl) phosphite, bentonite and molybdenum disulfide into a vacuum shearing, dispersing and grinding device for grinding, homogenizing and stirring for 0.5h to obtain the mixing auxiliary agent.
S5, adding the composite conductive filler and the base grease into a three-roller grinder, grinding for 1h in a constant temperature environment of 60-80 ℃, and standing for 5-10 min to obtain a mixed matrix; adding the mixed auxiliary agent into the mixed matrix at a constant speed, stirring uniformly for 0.5h in a vacuum deaeration machine, and cooling to room temperature to obtain the electric power composite grease.
The electric power complex grease obtained in examples 1 to 3 was subjected to performance test, and the test results are shown in Table 1:
TABLE 1 examples 1-3 electric Power Complex lipid Properties
As can be seen from table 1, the electric power compound grease prepared in examples 1-3 is an ointment with uniform appearance, no obvious particle impurities, fine product, and soft and hard degree and cone penetration degree all meet the standard requirements; the PH value is neutral, the copper sheet and the aluminum sheet are not corroded, and the corrosion resistance and the aging resistance are excellent; the acceleration stability is good, and the phenomena of precipitation, layering and wall hanging are avoided. And the drop points are all more than 300 ℃, so that the electric composite grease prepared by using the traditional single conductive filler and single silicone oil as the base grease is broken through, and the electric composite grease has excellent conductivity and good corrosion resistance, heat resistance and wear resistance.
Therefore, the high-conductivity, corrosion-resistant and aging-resistant power compound grease and the preparation method thereof can solve the problems of poor conductivity and low dropping point of the traditional power compound grease, and have the advantages of aging resistance and corrosion resistance.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (9)
1. The high-conductivity, anti-corrosion and anti-aging electric power composite grease is characterized by comprising the following components in percentage by mass: 60% -70% of composite conductive filler, 20% -30% of base grease and 5% -10% of mixing auxiliary agent; the composite conductive filler comprises: 4-10 parts of graphene flakes, 8-20 parts of graphite powder, 60-80 parts of silver-coated copper powder and 6-12 parts of carbon nanofiber powder.
2. The highly conductive, corrosion resistant, aging resistant electrical complex grease of claim 1, wherein: the thickness of the graphene flake is 30-400nm, the particle size of the graphite powder is 1000 meshes, and the particle size of the silver-coated copper powder is 2 mu m; the diameter of the carbon nano fiber powder is 50-200nm, and the length is 50-100um.
3. A highly conductive, corrosion resistant, aging resistant electrical complex grease as defined in claim 2, wherein: the base grease is polyether: paraffin oil: methyl trifluoropropyl silicone oil: methyl long chain alkyl silicone oil: benzyl silicone oil = 3:2:1:1:1 mixture; the viscosity of the polyether was 300, the viscosity of the paraffin oil was 500, the viscosity of the methyltrifluoropropyl silicone oil was 1000, the viscosity of the methyl long-chain alkyl silicone oil was 5000, and the viscosity of the benzyl silicone oil was 10000.
4. A highly conductive, corrosion resistant, aging resistant electrical complex grease as claimed in claim 3, wherein: the mixing auxiliary agent comprises 2-4 parts of dispersing agent sodium polyacrylate, 4-6 parts of thickener fumed silica, 2-4 parts of antioxidant tris (2, 4-di-tert-butylphenyl) phosphite, 8-12 parts of bentonite and 2-6 parts of molybdenum disulfide.
5. The preparation method of the high-conductivity, anti-corrosion and anti-aging power compound grease based on the method of claim 4 is characterized by comprising the following steps:
s1, preparing silver-coated copper powder, namely adding ultrafine copper powder into an activation solution, stirring for 10min at normal temperature, standing, and carrying out solid-liquid separation to obtain copper powder suspension; dropwise adding a mixed solution of silver nitrate and tetraisopropyl di (dioctyl phosphite acyloxy) titanate in a constant temperature environment of 50 ℃, adding a reducing agent disodium ethylenediamine tetraacetate, stirring uniformly, standing until solid-liquid separation is achieved, and vacuum drying to obtain compact silver-coated copper powder;
s2, preparing a composite conductive filler, namely respectively adding graphene flakes, graphite powder, silver-coated copper powder and carbon nanofiber powder into a ball-type grinding machine, and grinding for 2 hours to obtain composite powder; adding the composite powder into a fusion coating machine, carrying out coating modification, coating a graphite layer and a graphene layer on the surface of silver-coated copper powder, and grafting carbon nanofibers;
s3, preparing base grease, namely mixing polyether with the viscosity of 300 Pa.s, paraffin oil with the viscosity of 500 Pa.s, methyltrifluoropropyl silicone oil with the viscosity of 1000 Pa.s, methyl long-chain alkyl silicone oil with the viscosity of 5000 Pa.s and benzyl silicone oil with the viscosity of 10000 Pa.s in a stirrer according to the mass ratio of 3:2:1:1:1 for 0.5h to obtain the base grease;
s4, preparing a mixed auxiliary agent, namely adding 2-4 parts of sodium polyacrylate, 4-6 parts of fumed silica, 2-4 parts of tris (2, 4-di-tert-butylphenyl) phosphite ester, 8-12 parts of bentonite and 2-6 parts of molybdenum disulfide into a vacuum shearing, dispersing and grinding device for grinding, homogenizing and stirring for 0.5h to obtain the mixed auxiliary agent;
s5, adding the composite conductive filler and the base grease into a three-roller grinder for constant-temperature grinding, and standing for 5-10 min to obtain a mixed matrix; adding the mixed auxiliary agent into the mixed matrix at a constant speed, stirring uniformly for 0.5h in a vacuum deaeration machine, and cooling to room temperature to obtain the electric power composite grease.
6. The method for preparing the high-conductivity, anti-corrosion and anti-aging power compound grease according to claim 5, which is characterized in that: in the step S1, the activating solution is a suspension of 2% 1, 4-butynediol and 4% ammonium chloride.
7. The method for preparing the high-conductivity, anti-corrosion and anti-aging power compound grease according to claim 5, which is characterized in that: in the S1, the mass ratio of the silver nitrate to the tetraisopropyl di (dioctyl phosphite acyloxy) titanate is 1:1, and the concentrations are 0.4mol/L.
8. The method for preparing the high-conductivity, anti-corrosion and anti-aging power compound grease according to claim 5, which is characterized in that: in the step S2, the coating modification temperature is 100-220 ℃ and the coating modification time is 5-7 h.
9. The method for preparing the high-conductivity, anti-corrosion and anti-aging power compound grease according to claim 5, which is characterized in that: in the step S5, the grinding temperature of the grinder is 60-80 ℃ and the grinding time is 1h.
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TW202007725A (en) * | 2018-07-23 | 2020-02-16 | 帝利科技有限公司 | An innovative single liquuid type conductive composition and its preparation method and its some application technology in printed circuit board. |
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