CN117535087B - Preparation method of lubricating oil additive containing single-layer or oligolayer graphene - Google Patents
Preparation method of lubricating oil additive containing single-layer or oligolayer graphene Download PDFInfo
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- CN117535087B CN117535087B CN202311401006.5A CN202311401006A CN117535087B CN 117535087 B CN117535087 B CN 117535087B CN 202311401006 A CN202311401006 A CN 202311401006A CN 117535087 B CN117535087 B CN 117535087B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 95
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 74
- 239000000654 additive Substances 0.000 title claims abstract description 41
- 230000000996 additive effect Effects 0.000 title claims abstract description 41
- 239000002356 single layer Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- -1 graphene ester Chemical class 0.000 claims abstract description 48
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 47
- 239000010439 graphite Substances 0.000 claims abstract description 47
- 239000011259 mixed solution Substances 0.000 claims abstract description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000002148 esters Chemical class 0.000 claims abstract description 15
- 239000003599 detergent Substances 0.000 claims abstract description 13
- 239000000080 wetting agent Substances 0.000 claims abstract description 12
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 17
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 claims description 16
- 229910052791 calcium Inorganic materials 0.000 claims description 12
- 239000011575 calcium Substances 0.000 claims description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 8
- 229960002317 succinimide Drugs 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 229920002367 Polyisobutene Polymers 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 claims description 4
- 229960001860 salicylate Drugs 0.000 claims description 4
- 229940044652 phenolsulfonate Drugs 0.000 claims description 3
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 2
- MAAUYFIROALKRY-UHFFFAOYSA-N 6-hydroxy-7-thiabicyclo[4.1.0]hepta-2,4-diene-1-carboxylic acid Chemical compound C1=CC=CC2(C(=O)O)C1(O)S2 MAAUYFIROALKRY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 2
- 229940049964 oleate Drugs 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000002199 base oil Substances 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- 239000007822 coupling agent Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 14
- AXAVYKPSABZLIB-UHFFFAOYSA-N C1(CCC(N1)=O)=O.CC(C)=C.CC(C)=C Chemical group C1(CCC(N1)=O)=O.CC(C)=C.CC(C)=C AXAVYKPSABZLIB-UHFFFAOYSA-N 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 6
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000010705 motor oil Substances 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003879 lubricant additive Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/02—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic oxygen-containing compound
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/2805—Esters used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/086—Imides
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/06—Thio-acids; Thiocyanates; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/64—Environmental friendly compositions
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- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention relates to the technical field of lubricating oil, in particular to a preparation method of a lubricating oil additive containing single-layer or oligolayer graphene. According to the invention, a titanate coupling agent is selected as a wetting agent of graphite, a high-efficiency ashless dispersant and a metal detergent are used as a stripping agent, and low-viscosity ester-based lubricating oil is used as a solvent, and the graphite mixed solution is obtained by mixing; and mechanically stripping the graphite mixed solution to obtain the graphene ester-based lubricating oil additive. The preparation method is simple, and graphene in the peeled graphene ester-based lubricating oil additive has strong lipophilicity and can be directly compounded with various base oils.
Description
Technical Field
The invention relates to the technical field of lubricating oil, in particular to a preparation method of a lubricating oil additive containing single-layer or oligolayer graphene.
Background
The new graphene material has excellent performance, is applied to hundreds of types around the graphene, and particularly relates to the fields of coating, cable, heating, lubricating oil, heat dissipation, environmental protection, biology, energy and the like. In 2012, the research group led by American Ab tribute laboratories Anirudha Sumant and ALI ERDEMIR found that adsorbing a layer of graphene on the contact surface of steel material greatly reduced the friction coefficient and wear rate, and effectively prevented the rust, which is known as magic. In 2016, researchers at the university of northwest mchx engineering institute of america found pleated graphene to be a very promising lubricant additive.
The current preparation methods of graphene mainly comprise an oxidation-reduction method, a chemical vapor deposition method and a mechanical stripping method. The oxidation-reduction method for preparing the graphene has serious defects, serious pollution of chemical reagents and difficult problem of waste acid treatment at present. The chemical vapor deposition method for preparing graphene has high cost and is difficult to mass production. The mechanical stripping method is the most direct method for preparing high-quality graphene, but the strong van der Waals force and the hydrophobic property between graphene sheets make the stripping efficiency of the graphene low, and the selection of a proper stripping agent and a proper solvent is critical to the quality of the graphene.
The application report of graphene in lubricating oil is very many, and generally comprises preparation of graphene, modification of graphene, blending of lubricating oil and addition of graphene, but the process is very complex and not environment-friendly. Therefore, a high-efficiency, low-cost and environment-friendly method for preparing graphene for lubricating oil is very necessary. The technical method for preparing the monolayer or oligolayer graphene for the lubricating oil by using the low-viscosity ester-based lubricating oil as a dispersing solvent, compounding an ashless dispersing agent and a metal detergent as a stripping agent and using a titanate coupling agent as a wetting agent is not disclosed at present. The graphene ester-based lubricating oil additive prepared in this way can be directly added into lubricating oil.
Disclosure of Invention
The invention aims to provide a preparation method of a lubricating oil additive containing single-layer or oligolayer graphene, which aims to solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a lubricating oil additive containing single-layer or oligolayer graphene comprises the following steps:
Step 1: adding an ashless dispersant and a metal detergent into low-viscosity ester-based lubricating oil, and mechanically stirring to obtain uniform mixed solution;
Step 2: adding graphite into the mixed solution, mechanically stirring, and dropwise adding a wetting agent in the stirring process to obtain a graphite mixed solution;
step 3: and mechanically stripping the graphite mixed solution to obtain the graphene ester-based lubricating oil additive.
Further, in step 1, the ashless dispersant is one or a mixture of more of mono-polyisobutylene succinimide, di-polyisobutylene succinimide, boronated polyisobutylene succinimide and high molecular weight succinimide.
Further, in step 1, the ashless dispersant is preferably diisobutylene succinimide.
Further, in step1, the metal detergent is one or a mixture of more of calcium alkyl salicylate, calcium alkyl salicylate sulfide detergent, calcium alkyl phenolsulfonate and magnesium alkyl salicylate.
Further, in step1, the metal detergent is preferably calcium alkyl phenolsulfonate.
Further, in the step 1, the low-viscosity ester-based lubricating oil is one or a mixture of more than one of neopentyl glycol complex ester, dipentaerythritol ester, epoxy pentaerythritol tetrasoybean oleate, trimethylolpropane complex ester and monoglyceride.
Further, in step 1, the low-viscosity ester-based lubricating oil is preferably dipentaerythritol ester.
Further, in step 2, the graphite is any one of scaly graphite, spherical graphite and expanded graphite.
In step 2, the graphite is preferably expanded graphite having a particle size of 325 to 15000 mesh and a volume of 200 to 300 times that of the original graphite.
Further, in step 2, the expansion ratio of graphite is 300.
Further, in step 2, the wetting agent is one or a mixture of more of isopropyl tri (dioctyl-phosphoryloxy) titanate, monoalkoxy phosphate titanate, monoalkoxy titanate and di-fatty acyl titanate ethylene glycol.
Further, in step 2, the wetting agent is preferably isopropyl tris (dioctyl-phosphoryloxy) titanate.
In step 3, the mechanical stripping method is one or more of high-speed shearing, high-pressure homogenizing and micro-jet.
In step 3, the mechanical stripping method is preferably high-pressure homogenization, the pressure is 300MPa, and the homogenization time is 2-10 h.
In the step 3, the content of the ashless dispersant is 0.5 to 2 percent, the content of the metal detergent is 0.2 to 1 percent, the content of the graphene is 0.01 to 0.5 percent, the content of the wetting agent is 0.1 to 0.5 percent, and the balance is low-viscosity ester-based lubricating oil.
In step 3, the thickness of the graphene sheet layer in the graphene ester-based lubricating oil additive is 0.33-2 nm, and the particle size D50 is 0.1-1 mu m.
Compared with the prior art, the invention has the following beneficial effects:
The first object of the invention is to provide a preparation method of single-layer or oligolayer graphene for lubricating oil, which is characterized in that titanate coupling agent is selected as a wetting agent of graphite, efficient ashless dispersant and metal detergent are used as stripping agents, low-viscosity ester-based lubricating oil is used as a solvent, stripping efficiency of graphene is greatly improved, and the obtained graphene has complete structure and few defects.
The second object of the present invention is to provide a low-viscosity graphene ester-based lubricating oil additive which can be easily blended with various base oils to obtain a graphene-based lubricating oil having high stability and excellent performance.
(1) According to the graphene-based high-quality lubricating oil, the special ashless dispersant and the metal detergent are used as the stripping agent, the low-viscosity ester-based lubricating oil is used as the dispersing solvent, the titanate coupling agent is used as the wetting agent, and the graphene for high-quality lubricating oil can be stripped out efficiently and green with low cost through high-pressure homogenization.
(2) The prepared graphene ester-based lubricating oil additive can be directly compounded with various base oils to obtain various high-quality graphene-based lubricating oils through blending, and is simpler and more convenient than the traditional method.
(3) Graphene in the peeled graphene ester-based lubricating oil additive has strong lipophilicity and is more stable in dispersion in other base oils.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a high power transmission electron microscopy image of graphene in a graphene ester-based lubricating oil additive of example 1 of the present invention;
FIG. 2 is an atomic force microscope image of graphene in the graphene ester-based lubricating oil additive of example 1 of the present invention;
FIG. 3 is a graph showing the laser particle size of graphene in the graphene ester-based lubricating oil additive of example 1 of the present invention;
Fig. 4 is a graph of comparative stability of graphene lubricating oil for vehicles and graphene ester-based lubricating oil for vehicles.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but 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.
The materials used in the invention and the sources thereof: the flake graphite is from Qingdao Huatai lubrication sealing technology Co., ltd, model ht; the expanded graphite is from Qingdao source Cheng Run graphite New Material Co., ltd, model 99100300; the base oil 100N is from Jinan Xin resplendent chemical industry Co., ltd; 5w-30 motor oil from BMW/BMW; model Longlife-01.
Example 1:
500g of dipentaerythritol ester, 5g of diisobutylene succinimide and 2.5g of calcium alkylphenol sulfonate are weighed into a flask, heated and mechanically stirred at 80 ℃ for 30min at 500rpm to obtain a mixed solution.
300G of mixed solution is weighed, 0.75g of expanded graphite (with the mesh number of 500 meshes) is added into the mixed solution, the stirring time is 10min, the rotating speed is 500rpm, 1.2g of isopropyl tri (dioctyl-phosphoryloxy) titanate is dropwise added during stirring, the stirring time is 30min, and the rotating speed is 500rpm, so that the graphite mixed solution is obtained.
200G of graphite mixed solution is weighed, placed in a high-pressure homogenizer, circularly homogenized under 300MPa for 10 hours, and the graphene ester-based lubricating oil additive is obtained.
The graphene in the graphene ester-based lubricating oil additive is obtained by using a high-power transmission electron microscope, an atomic force microscope and a laser particle size analyzer for analysis, and the average graphene sheet layer of the graphene obtained by the method is 2.8 layers, the thickness is 1nm, and the particle size D50 is 1.5 mu m as shown in a graph (1), a graph (2) and a graph (3).
Example 2: base oil 100N was used instead of dipentaerythritol ester in example 1.
500G of base oil 100N,5g of diisobutylene succinimide and 2.5g of calcium alkylphenol sulfonate are weighed into a flask, heated and mechanically stirred at 80 ℃ for 30min at 500rpm to obtain a mixed solution.
300G of mixed solution is weighed, 0.75g of expanded graphite (with the mesh number of 500 meshes) is added into the mixed solution, the stirring time is 10min, the rotating speed is 500rpm, 1.2g of isopropyl tri (dioctyl-phosphoryloxy) titanate is dropwise added during stirring, the stirring time is 30min, and the rotating speed is 500rpm, so that the graphite mixed solution is obtained.
200G of graphite lubricating oil is weighed and placed in a high-pressure homogenizer for circular homogenization under 300MPa for 10 hours, so as to obtain graphene lubricating oil slurry.
And (3) analyzing the graphene in the graphene lubricating oil slurry by using a high-power transmission electron microscope, an atomic force microscope and a laser particle size analyzer, wherein the average lamellar layer of the graphene is 5.2 layers, the thickness is 1.7nm, and the particle size D50 is 1.8 mu m.
Example 3: the difference from example 1 is that example 3 does not add a stripping agent.
300G of dipentaerythritol ester is weighed, 0.75g of expanded graphite (with the mesh number of 500 meshes) is added into the mixed solution, the stirring time is 10min under mechanical stirring, the rotating speed is 500rpm, 1.2g of isopropyl tri (dioctyl-phosphoryloxy) titanate is dropwise added during stirring, the stirring time is continued for 30min, and the rotating speed is 500rpm, so that the graphite mixed solution is obtained.
200G of graphite mixed solution is weighed, placed in a high-pressure homogenizer, circularly homogenized under 300MPa for 10 hours, and the graphene ester-based lubricating oil additive is obtained.
And (3) analyzing the graphene in the graphene ester-based lubricating oil additive by using a high-power transmission electron microscope, an atomic force microscope and a laser particle size analyzer, wherein the average lamellar layer of the graphene is 15.8 layers, the thickness is 5.2nm, and the particle size D50 is 1.85 mu m.
Example 4: the difference from example 1 is that example 4 does not add a wetting agent.
500G of dipentaerythritol ester, 5g of diisobutylene succinimide and 2.5g of calcium alkylphenol sulfonate are weighed into a flask, heated and mechanically stirred at 80 ℃ for 30min at 500rpm to obtain a mixed solution.
300G of mixed solution is weighed, 0.75g of expanded graphite (with the mesh number of 500 meshes) is added into the mixed solution, and the mixed solution is mechanically stirred for 10min at the rotating speed of 500rpm to obtain the graphite mixed solution.
200G of graphite mixed solution is weighed, placed in a high-pressure homogenizer, circularly homogenized under 300MPa for 10 hours, and the graphene ester-based lubricating oil additive is obtained.
And (3) analyzing the graphene in the graphene ester-based lubricating oil additive by using a high-power transmission electron microscope, an atomic force microscope and a laser particle size analyzer, wherein the average lamellar layer of the graphene is 8.9 layers, the thickness is 3.1nm, and the particle size D50 is 1.8 mu m.
Example 5: the difference from example 1 is that the graphite of example 5 is selected from the group consisting of flake graphite.
500G of dipentaerythritol ester, 5g of diisobutylene succinimide and 2.5g of calcium alkylphenol sulfonate are weighed into a flask, heated and mechanically stirred at 80 ℃ for 30min at 500rpm to obtain a mixed solution.
300G of mixed solution is weighed, 0.75g of flake graphite (with the mesh number of 500 meshes) is added into the mixed solution, the stirring time is 10min, the rotating speed is 500rpm, 1.2g of isopropyl tri (dioctyl-phosphoryloxy) titanate is dropwise added during stirring, the stirring time is 30min, and the rotating speed is 500rpm, so that the graphite mixed solution is obtained.
200G of graphite mixed solution is weighed, placed in a high-pressure homogenizer, circularly homogenized under 300MPa for 10 hours, and the graphene ester-based lubricating oil additive is obtained.
And (3) analyzing the graphene in the graphene ester-based lubricating oil additive by using a high-power transmission electron microscope, an atomic force microscope and a laser particle size analyzer, wherein the average lamellar layer of the graphene is 32.1 layers, the thickness is 11nm, and the particle size D50 is 2.1um.
Example 6: the difference from example 1 is that example 6 mechanical peel selects ultra-high shear.
500G of dipentaerythritol ester, 5g of diisobutylene succinimide and 2.5g of calcium alkylphenol sulfonate are weighed into a flask, heated and mechanically stirred at 80 ℃ for 30min at 500rpm to obtain a mixed solution.
300G of mixed solution is weighed, 0.75g of expanded graphite (with the mesh number of 500 meshes) is added into the mixed solution, the stirring time is 10min, the rotating speed is 500rpm, 1.2g of isopropyl tri (dioctyl-phosphoryloxy) titanate is dropwise added during stirring, the stirring time is 30min, and the rotating speed is 500rpm, so that the graphite mixed solution is obtained.
200G of graphite mixed solution is weighed and placed in an ultra-high speed shearing machine for high-speed shearing, the linear speed reaches 23m/s, and the time is 10 hours, so that the graphene ester-based lubricating oil additive is obtained.
And (3) analyzing the graphene in the graphene ester-based lubricating oil additive by using a high-power transmission electron microscope, an atomic force microscope and a laser particle size analyzer, wherein the average lamellar layer of the graphene is 3.4 layers, the thickness is 1.1nm, and the particle size D50 is 1.9 mu m.
Experiment:
The graphene ester-based lubricating oil additive in example 1 and the graphene lubricating oil slurry in example 2 are respectively blended with 5w-30 of commercially available shell car engine oil, and the blending method is as follows: 500g of shell 5w-30 car engine oil is taken and stirred on a dispersing machine, 25g of graphene ester-based lubricating oil additive is added, stirring is carried out for 30min, ultrasonic dispersing is carried out for 20min, standing is carried out for 2h, the example 1 is marked as the car graphene ester-based lubricating oil additive, and the example 2 is marked as the car graphene lubricating oil.
Conclusion:
As shown in fig. 4, the graphene ester-based lubricating oil additive for vehicles prepared in example 1 and the graphene lubricating oil for vehicles prepared in example 2 are respectively taken and placed in a test tube, and after 6 months of standing, observation shows that the graphene ester-based lubricating oil additive for vehicles has no layering condition, and the graphene lubricating oil for vehicles has a slight layering condition, which indicates that the stability of the graphene ester-based lubricating oil additive is better.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A preparation method of a lubricating oil additive containing single-layer or oligolayer graphene is characterized by comprising the following steps: the method comprises the following steps:
Step 1: adding an ashless dispersant and a metal detergent into ester-based lubricating oil, and mechanically stirring to obtain a mixed solution; the ashless dispersant is one or more of single polyisobutene succinimide, double polyisobutene succinimide, boronated polyisobutene succinimide and succinimide; the metal detergent is one or more of calcium alkyl salicylate, calcium alkyl salicylate sulfide detergent, calcium alkyl phenol sulfonate and magnesium alkyl salicylate; the ester-based lubricating oil is one or more of neopentyl glycol complex ester, dipentaerythritol ester, epoxy pentaerythritol tetrasoybean oleate, trimethylolpropane complex ester and monoglyceride;
Step 2: adding graphite into the mixed solution, mechanically stirring, and dropwise adding a wetting agent in the stirring process to obtain a graphite mixed solution; the wetting agent is one or more of isopropyl tri (dioctyl-phosphoryloxy) titanate, monoalkoxy phosphate titanate, monoalkoxy titanate and di-fatty acyl titanate ethylene glycol;
step 3: mechanically stripping the graphite mixed solution to obtain a graphene ester-based lubricating oil additive; the mechanical stripping method is high-pressure homogenization, the pressure is 200-300 MPa, and the homogenization time is 2-10 h.
2. The method for preparing the lubricating oil additive containing single-layer or oligolayer graphene according to claim 1, which is characterized by comprising the following steps: in the step 2, the graphite is any one of flake graphite, spherical graphite and expanded graphite.
3. The method for preparing the lubricating oil additive containing single-layer or oligolayer graphene according to claim 2, which is characterized in that: the particle size of the expanded graphite is 325-15000 meshes, and the expansion multiple of the expanded graphite is 200-300.
4. The method for preparing the lubricating oil additive containing single-layer or oligolayer graphene according to claim 1, which is characterized by comprising the following steps: in the step 3, the content of the ashless dispersant in the graphene ester-based lubricating oil additive is 0.5-2%, the content of the metal detergent is 0.2-1%, the content of the graphene is 0.01-0.5%, the content of the wetting agent is 0.1-0.5% by weight, and the balance is ester-based lubricating oil.
5. The method for preparing the lubricating oil additive containing single-layer or oligolayer graphene according to claim 1, which is characterized by comprising the following steps: in the step 3, in the graphene ester-based lubricating oil additive, the thickness of graphene sheets is 0.33-2 nm, and the particle size D50 is 0.1-1 mu m.
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| CN101812351A (en) * | 2010-04-01 | 2010-08-25 | 江苏工业学院 | Lubricating oil additive based on single-layer or more-layer graphene |
| CN111073751A (en) * | 2019-12-09 | 2020-04-28 | 上海烯望材料科技有限公司 | Application of lubricating oil detergent dispersant in preparation of graphene |
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