CN105602650A - Carbon nanotube-modified nano-additive and preparation method and application thereof - Google Patents
Carbon nanotube-modified nano-additive and preparation method and application thereof Download PDFInfo
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- CN105602650A CN105602650A CN201510961886.0A CN201510961886A CN105602650A CN 105602650 A CN105602650 A CN 105602650A CN 201510961886 A CN201510961886 A CN 201510961886A CN 105602650 A CN105602650 A CN 105602650A
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
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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
- C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
- C10M107/20—Lubricating compositions characterised by the base-material being a macromolecular compound containing oxygen
- C10M107/30—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M107/32—Condensation polymers of aldehydes or ketones; Polyesters; Polyethers
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- 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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/1033—Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
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Abstract
The present invention discloses a carbon nanotube-modified nano-additive. The nano-additive is multiwalled carbon nanotube-polymer phosphate. The invention also discloses a preparation method of the nano-additive and application thereof to the polyether. The nano-additive can form a stable dispersion system in polyether, and has good thermal stability, and excellent anti-friction wear characteristics at high temperature of 150 DEG C.
Description
Technical field
The present invention relates to a kind of nanometer additive based on carbon nano tube modified and its preparation method and application.
Background technology
Along with the fast development of turbogenerator, auto industry, farm equipment and microelectron-mechanical industrial equipment etc., rightDemand in the lubricant that can effectively use under hot environment is also progressively increasing, and this hot environment has also causedLubricant based on mineral oil can not bear for a long time under this operating mode and use. In order to address these problems, many efficientSyntholube be developed to meet the demand to hot environment as polyalphaolefin (PAO) and polyethers (PAG) etc. In addition,The antiwear and friction-reducing additive that can be used in high-temperature lubricant is also little, and this has limited answering of high-temperature lubricant to a great extentWith.
Research before show by lubricant, add nano material (such as CNT, Graphene, fullerene andGraphite nano plate) can improve the tribological property of lubricant. This is a fast-developing emerging field, because nano materialMinimum size and very large specific area, make nano material be different from traditional lubriation material. In addition, in order to prepareCan polydispersion, the nano material of long-time stable existence in different solvents or oil lubricant, had good several methodBe used to polymer to be connected in nano material by covalent bond. In these methods, ATRP(ATRP) be to adopt a kind of maximum methods. For example, Pei little Wei etc. makes in this way the grafting of polymer ions liquid to carbonOn nanotube (Pei little Wei etc., J.Polym.Sci., PartA, Polym.Chem.2008,46,7225). TribologyTest result show this nano material can be in a kind of ionic liquid stable dispersion, and can significantly improve this ionThe tribological property of liquid. Except ATRP, (BenjaminKerscher, the et.al. such as KerscherMacromolecules2013,46,4395) method of modifying by ring-opening polymerisation effect and chain terminal is by tree-shaped ionLiquid polymers grafting is to Graphene. The Graphene ionic liquid nano flake of this tree-shaped functionalization can exist easilyScattered several weeks of disperseing in water and can be stable.
CNT is modified and had a lot of reports used as the research of lubricating additive. But, almostReport does not relate to polymer phosphate (PPEs) is connected on carbon nanomaterial by covalent bond, and by after this modificationCarbon nanomaterial as additive. Work before us shows that phosphate can be very under high-temperature conditionIn many lubricants grease, show excellent antifriction antiwear characteristic (Wu Xinhu etc., RSCAdv.2014,4,6074; RSCAdv., 2014,4,54760; Ind.Eng.Chem.Res.2014,53,5660), therefore by tree-shaped polymer phosphorusAcid esters (PPEs) perhaps can be highly significant on CNT (CNT) by being covalently bound to. By by PPEs and CNT bonding,The CNT-PPEs nano material that we can design should be able to have good electric conductivity, outstanding heat endurance and machineryStability, good tribological property and characteristic that can stable dispersion in lubricating oil.
Summary of the invention
The object of the present invention is to provide a kind of nanometer based on carbon nano tube modified that can use under hot environmentAdditive and its preparation method and application, this nanometer additive is bonded to CNT by covalent bond by polymer phosphateUpper, in conjunction with after nano material in lubricating oil, can disperse in a large number, and can several weeks of stable dispersion, in addition at heightThe lower anti-wear and wear-resistant performance that can significantly improve lubricating oil of temperature.
Based on carbon nano tube modified nanometer additive, it is characterized in that this nanometer additive is multi-walled carbon nano-tubes-poly-Compound phosphate (being called for short MWCNT-PPEs), its concrete structure formula is suc as formula shown in I.
The preparation method of nanometer additive as mentioned above, is characterized in that this preparation method comprises the following steps:
1) preparation of hydroxylating multi-walled carbon nano-tubes-poly-3-ethyl-3-methylol oxetanes (being called for short MWCNT-PEHO)
Hydroxylating multi-walled carbon nano-tubes (being called for short MWCNT-OH) is added to CH under argon shield2Cl2And BFEE（BF3·OEt2) in, ultrasonic processing 15 ~ 30min, then slowly drips 3-ethyl-3-methylol oxetanes (EHO),Stirring at room temperature reaction 40 ~ 50h under argon shield, reaction finishes the rear ethanol cancellation of using, and washing, is drying to obtain MWCNT-PEHO;
2) preparation of multi-walled carbon nano-tubes-polymer phosphate
Under argon shield, MWCNT-PEHO, phosphorus chloride diphenyl phthalate and lewis acid catalyst are added in toluene, 90 ~110 DEG C of stirring reaction 12 ~ 15h, remove by filter solvent, and washing, is drying to obtain MWCNT-PPEs.
The mass volume ratio of described hydroxylating multi-walled carbon nano-tubes and 3-ethyl-3-methylol oxetanes is 4 ~ 6mg/mL。
Described CH2Cl2With the volume ratio of BFEE be 10 ~ 30.
The mass volume ratio of described MWCNT-PEHO and phosphorus chloride diphenyl phthalate is 20 ~ 33mg/mL.
Described lewis acid catalyst is anhydrous Aluminum chloride or anhydrous magnesium chloride, and its quality used is MWCNT-PEHO quality10% ~ 30%.
The described above application of nanometer additive in polyethers, is characterized in that described nanometer additive accounts for polyethers quality0.04~0.10%。
Described nanometer additive accounts for 0.08% of polyethers quality.
MWCNT-PPEs of the present invention has good dispersiveness in polyethers (PAG), can stable dispersion several starsPhase.
MWCNT-PPEs of the present invention adds in polyethers, and at 150 DEG C, load 25N, can when addition 0.04-0.10%To significantly improve the anti-wear and wear-resistant performance of base oil PAG.
MWCNT-PPEs of the present invention adds in polyethers, and at 150 DEG C, the MWCNT-PPEs of optium concentration 0.08% existsMaximum bearing load in PAG is 100N.
Brief description of the drawings
Fig. 1 is raw material MWCNT-OH, intermediate MWCNT-PEHO in embodiment 1 and end product MWCNT-PPEs'sPyrolysis temperature curve.
Fig. 2 is that concentration is respectively 0%, 0.04%, 0.06%, 0.08%, and 0.10% embodiment 1 product (MWCNT-PPEs) addsBe added in polyethers (PAG), on the micro-vibration friction abrasion testing machine of SRV-IV in 150 DEG C, frequency 25Hz, load 25N, amplitude 1The relation curve that under the operating mode of mm, coefficient of friction changes in time.
Fig. 3 is that concentration is respectively 0%, 0.04%, 0.06%, 0.08% and 0.10% embodiment 1 product (MWCNT-PPEs)Add in polyethers (PAG), on the micro-vibration friction abrasion testing machine of SRV-IV in 150 DEG C, frequency 25Hz, load 25N, shakesWidth 1mm, the long wear volume that grinds spot under 30min operating mode that grinds.
Fig. 4 be concentration be respectively 0% and 0.08%MWCNT-PPEs add in polyethers (PAG), shake SRV-IV is micro-On dynamic friction abrasion tester in 150 DEG C, frequency 25Hz, the friction coefficient load change when load is increased to 200N from 25NRelation curve.
Detailed description of the invention
Embodiment 1
The preparation of step (1) multi-walled carbon nano-tubes-poly-3-ethyl-3-methylol oxetanes (MWCNT-PEHO): by 100MgMWCNT-OH joins 50mLCH under argon shield2Cl2With 2mL BFEE (BF3·OEt2) in, ultrasonicProcess 20min. Then by sampling pump, 20mL3-ethyl-3-methylol oxetanes (EHO) being lasted to 2h is added drop-wise toIn reaction system. Reactant mixture is stirring at room temperature reaction 48h under argon shield, has reacted the rear ethanol cancellation of using. In order to removeNot, with the PEHO of MWCNT-OH bonding, the product after filtration is not dispersed in ethanol again, filter, with ethanol washing for several times,After use CHCl3Washing once. Product is at 60 DEG C of vacuum drying 4h.
The preparation of step (2) multi-walled carbon nano-tubes-polymer phosphate (MWCNT-PPEs): under argon shield by 100MgMWCNT-PEHO, 3.5mL phosphorus chloride diphenyl phthalate and 20mg anhydrous Aluminum chloride join in 50mL toluene. InsteadAnswer mixture at 110 DEG C of stirring reaction 15h. Remove by filter solvent, then use toluene wash three times. After dry, be again dispersed inIn ionized water, filter, washing for several times, is finally washed three times with ethanol again. 60 DEG C of dried overnight of vacuum.
Embodiment 2
Step (1) is identical with embodiment 1.
The preparation of step (2) multi-walled carbon nano-tubes-polymer phosphate (MWCNT-PPEs): under argon shield by 100MgMWCNT-PEHO, 3.5mL phosphorus chloride diphenyl phthalate and 20mg anhydrous magnesium chloride join in 50mL toluene. InsteadAnswer mixture at 110 DEG C of stirring reaction 15h. Remove by filter solvent, then use toluene wash three times. After dry, be again dispersed inIn ionized water, filter, washing for several times, is finally washed three times with ethanol again. 60 DEG C of dried overnight of vacuum.
Embodiment 3
Step (1) is identical with embodiment 1.
The preparation of step (2) multi-walled carbon nano-tubes-polymer phosphate (MWCNT-PPEs): under argon shield by 100MgMWCNT-PEHO, 3.5mL phosphorus chloride diphenyl phthalate and 20mg aluminum trichloride (anhydrous) join in 50mL toluene. InsteadAnswer mixture at 90 DEG C of stirring reaction 15h. Remove by filter solvent, then use toluene wash three times. After dry, be again dispersed in fromIn sub-water, filter, washing for several times, is finally washed three times with ethanol again. 60 DEG C of dried overnight of vacuum.
Evaluation of Thermal Stability
Heat endurance is to measure by STA449CJupitersimultaneousTG-DSC. By the raw material in embodiment 1MWCNT-OH, intermediate product MWCNT-PEHO, the each 5mg of product MWCNT-PPEs puts into sample cell, and probe temperature is from 20 ~ 800DEG C, it is 10 DEG C/min that temperature is advanced the speed, and under nitrogen environment, measures. Result as shown in Figure 1. The thermal decomposition of MWCNT-PPEsTemperature is 369 DEG C, be higher than raw material MWCNT-PEHO(272 DEG C). From accompanying drawing 1, also can find out product MWCNT-PPEs simultaneouslyIn no longer contain intermediate MWCNT-PEHO.
The tribological property evaluation of product:
MWCNT-PPEs prepared by embodiment 1 adds in polyethers (PAG), and being mixed with concentration is 0%, 0.04%, 0.06%,0.08% and 0.10% dispersion, its tribological property of overall merit:
1. the micro-vibration friction abrasion testing machine test concentrations of SRV-IV that the German Optimol grease of employing company produces is respectively0%, 0.04%, 0.06%, 0.08% and 0.10% embodiment 1 product (MWCNT-PPEs) join in polyethers (PAG), 150DEG C, frequency 25Hz, amplitude 1mm, the coefficient of friction f under the operating mode of load 25N when long mill 30min, test steel ball used and be Φ=The GCr15 bearing steel of 10mm, the GCr15 bloom that lower sample is Φ 24 × 7.9mm. The results are shown in accompanying drawing 2. As seen from the figure, exist150 DEG C of temperature, this compound can well lubricate steel-steel-steel pair as additive, and coefficient of friction significantly reduces, antifrictionEffect is very obvious.
2. adopt the non-contacting surface test instrument of MicroXAM3D test concentrations to be respectively 0%, 0.04%, 0.06%,0.08% and 0.10% embodiment 1 product (MWCNT-PPEs) joins in polyethers (PAG), at 150 DEG C, and frequency 25Hz, amplitude1mm, the wear volume under the operating mode of load 25N after long mill 30min. Test result as shown in Figure 3, adds after this additive,The wear volume of mill spot obviously reduces. Show that this additive has good anti-wear effect.
3. the micro-vibration friction abrasion testing machine test concentrations of SRV-IV that the German Optimol grease of employing company produces is dividedBe not that 0% and 0.08% embodiment 1 product (MWCNT-PPEs) adds in polyethers PAG, at 150 DEG C, frequency 25Hz, amplitude1mm, under the operating mode of load 25 ~ 200N, coefficient of friction f is with the relation curve of load change, and testing steel ball used is Φ=10mm'sGCr15 bearing steel, the GCr15 bloom that lower sample is Φ 24 × 7.9mm. The results are shown in accompanying drawing 4. As seen from the figure, when load fromWhen 25N is increased to 100N, the coefficient of friction of embodiment 1 product (MWCNT-PPEs) significantly reduces. Show example 1 productMaximum bearing load at 150 DEG C is 100N.
Claims (8)
1. the nanometer additive based on carbon nano tube modified, is characterized in that this nanometer additive is multi-walled carbon nano-tubes-polymerizationThing phosphate (being called for short MWCNT-PPEs), its concrete structure formula is suc as formula shown in I.
2. the preparation method of nanometer additive as claimed in claim 1, is characterized in that this preparation method comprises the following steps:
1) preparation of hydroxylating multi-walled carbon nano-tubes-poly-3-ethyl-3-methylol oxetanes
Hydroxylating multi-walled carbon nano-tubes is added to CH under argon shield2Cl2In BFEE, ultrasonic processing 15 ~ 30Min, then slowly drips 3-ethyl-3-methylol oxetanes, and under argon shield, stirring at room temperature reaction 40 ~ 50h, anti-Should finish the rear ethanol cancellation of using, washing, is drying to obtain MWCNT-PEHO;
2) preparation of multi-walled carbon nano-tubes-polymer phosphate
Under argon shield, MWCNT-PEHO, phosphorus chloride diphenyl phthalate and lewis acid catalyst are added in toluene, 90 ~110oC stirring reaction 12 ~ 15h, removes by filter solvent, and washing, is drying to obtain MWCNT-PPEs.
3. preparation method as claimed in claim 2, is characterized in that described hydroxylating multi-walled carbon nano-tubes and 3-ethyl-3-hydroxylThe mass volume ratio of methyl oxetanes is 4 ~ 6mg/mL.
4. preparation method as claimed in claim 2, is characterized in that described CH2Cl2With the volume ratio of BFEE be 10~30。
5. preparation method as claimed in claim 2, is characterized in that the matter of described MWCNT-PEHO and phosphorus chloride diphenyl phthalateAmount volume ratio is 20 ~ 33mg/mL.
6. preparation method as claimed in claim 2, is characterized in that described lewis acid catalyst is anhydrous Aluminum chloride or nothingAqueous magnesium chloride, its quality used is 10% ~ 30% of MWCNT-PEHO quality.
7. the application of nanometer additive in polyethers as claimed in claim 1, is characterized in that described nanometer additive accounts for polyethers0.04 ~ 0.10% of quality.
8. application as claimed in claim 7, is characterized in that described nanometer additive accounts for 0.08% of polyethers quality.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108163838A (en) * | 2017-12-30 | 2018-06-15 | 武汉工程大学 | A kind of Schiff 's base copper complex is carbon nano-tube modified and its preparation method and application |
| CN112080329A (en) * | 2020-09-21 | 2020-12-15 | 中国科学院兰州化学物理研究所 | Multi-wall carbon nanotube nano friction reducer and application thereof |
| CN114045184A (en) * | 2021-11-05 | 2022-02-15 | 中国科学院兰州化学物理研究所 | Carbon-silicon composite nanofluid antifriction and antiwear additive and application thereof |
| CN115491242A (en) * | 2022-09-01 | 2022-12-20 | 兰州空间技术物理研究所 | Organic phosphate modified graphene oxide powder and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108163838A (en) * | 2017-12-30 | 2018-06-15 | 武汉工程大学 | A kind of Schiff 's base copper complex is carbon nano-tube modified and its preparation method and application |
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| CN114045184A (en) * | 2021-11-05 | 2022-02-15 | 中国科学院兰州化学物理研究所 | Carbon-silicon composite nanofluid antifriction and antiwear additive and application thereof |
| CN114045184B (en) * | 2021-11-05 | 2022-12-06 | 中国科学院兰州化学物理研究所 | Carbon-silicon composite nanofluid antifriction and antiwear additive and application thereof |
| CN115491242A (en) * | 2022-09-01 | 2022-12-20 | 兰州空间技术物理研究所 | Organic phosphate modified graphene oxide powder and application thereof |
| CN115491242B (en) * | 2022-09-01 | 2023-04-21 | 兰州空间技术物理研究所 | Organic phosphate modified graphene oxide powder and application thereof |
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