CN101469143A - Preparation of multi-arm carbon nano-tube lubricant additive - Google Patents
Preparation of multi-arm carbon nano-tube lubricant additive Download PDFInfo
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- CN101469143A CN101469143A CN 200710308578 CN200710308578A CN101469143A CN 101469143 A CN101469143 A CN 101469143A CN 200710308578 CN200710308578 CN 200710308578 CN 200710308578 A CN200710308578 A CN 200710308578A CN 101469143 A CN101469143 A CN 101469143A
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Abstract
The invention discloses a method for preparing a multi-arm carbon nanotube lube additive. Through solid load of a chain transfer agent on the surface of a multi-arm carbon nanotube, the method carries out active polymerization on different monomers to obtain functionalized multi-arm carbon nanotubes modified by different polymers. The preparation process is simple and easy to operate; the prepared multi-arm carbon nanotube lube additive has good thermal stability and mechanical stability, and can greatly improve dispersion of the carbon nanotube in lube. The lube additive utilizes the rigid carbon nanotube as a nuclear structure and plays a role in bearing; long-chain macromolecule plays a role in abrasion reduction due to the flexibility and viscoelasticity of the macromolecule and realizes the conversion from sliding friction to rolling friction microscopically; therefore, the lube additive shows excellent abrasion resistance and is expected to solve the problem of lubrication of a mechanical material.
Description
Technical field
The present invention relates to a kind of preparation method of functionalization multi-arm carbon nano-tube lubricant additive.
Background technology
According to professor Vogelpohl of Germany measuring and calculating, the produced worldwide energy 1/3 to 1/2 because frictional wear effect and being lost, professor Jost of Britain also points out in recent years, 30～40% of the whole world consumption energy consumes to be used in frictional wear.It is lubricated fully that the lubricant of excellent property can make machinery obtain, thereby the efficient of machinery is improved, and reduces the consumption of the energy, the life-span of prolonged mechanical.Therefore improve lubricity and rub, reduce wear, prevent that to reduce sintering from having significant meaning to national economy.
It is the brand-new research field that developed recently gets up that nano material is applied to lubricating system.Characteristics such as surface-area is big because nano material has, high diffusibility and fusing point reduction, with the nano material is that the basis novel lubricant of preparation is applied in the friction system, play decompression anti-attrition effect with not only forming a film of easily shearing at friction surface, reduce frictional coefficient, and can carry out filling up and repairing to a certain degree to friction surface, play the anti-attrition effect.
A kind of novel, magical nano material-carbon nanotube (CNT) is since coming out, the people's attention extremely with its excellent physics-chem characteristic, unique tubular structure, extremely strong anti-pressure ability and wide application prospect is subjected to great restriction but its insoluble infusible characteristics further develop with application it.Good solvent energy dissolved carbon nanotube is not arranged up to now yet, thereby it is carried out chemical modification, synthesize soluble carbon nano tube derivative, significant to research and the application and development of developing carbon nanotube in more areas.
At present, CNT in the research of friction field seldom, report only limits to CNT perhaps to investigate its lubricating property by physical blending in disperse phase as solid lubricant.In view of the insoluble molten characteristic of carbon nanotube and all deficiencies of existing CNT base lubricating agent, develop and a kind ofly prepare method polymer-modified, soluble carbon nano-tube lubricant additive and have very big practical application meaning.
Summary of the invention
The objective of the invention is to improve the insoluble not molten characteristic of carbon nanotube and overcome all deficiencies of CNT base lubricating agent in the past, a kind of preparation method polymer-modified, soluble carbon nano-tube lubricant additive is provided.
The present invention realizes by following measure:
The present invention carries out living polymerization by at the immobilized chain-transfer agent in multi-arm carbon nano-tube surface to different monomers, has obtained different polymer-modified functionalization multi-arm carbon nano-tubes.
A kind of preparation method of multi-arm carbon nano-tube lubricant additive is characterized in that this method specifically may further comprise the steps:
A, multi-arm carbon nano-tube (MWCNT) after acidifying with SOCl
270 ℃ of reactions, boil off remaining SOCl
2, solids reacted 48 hours at 120 ℃ with no water glycol; Obtain MWCNT-OH through centrifugal, drying; MWCNT-OH and chain-transfer agent 4-(isopropyl cyanide acid) dithiobenzoic acid ester (CPAD) are dissolved in methylene dichloride, add a small amount of dicyclohexylcarbodiimide (DCC), centrifugal drying obtains MWCNT-SC (S) Ph behind this mixture lucifuge reaction at room temperature certain hour;
B, MWCNT-SC (S) Ph, vinylbenzene and Diisopropyl azodicarboxylate (AIBN) are joined a certain amount of N, N diformamide (DMF) solution, this mixture through vacuumize, behind the logical nitrogen in 100 ℃ of stirring reactions; Reaction finishes, and obtains product through centrifugal, washing, drying.
The product that the present invention obtains is that structural formula is as follows:
Wherein R represents COOCH
2CH
2COOCH
2CH
2C (CH
3) (CN)
The preparation of the said chain-transfer agent CPAD of the present invention is achieved in that
After dithiobenzoic acid and a spot of iodine is dissolved in ethyl acetate, slowly splash into methyl-sulphoxide.This mixture lucifuge reaction added the ethyl acetate solution of Diisopropyl azodicarboxylate acid after 10 hours, and back flow reaction is 18 hours again, removes and desolvates, and crude product separates through silica gel column chromatography, ethyl acetate: normal hexane=make eluent at 1: 2, product is the bright red solid.The mol ratio of dithiobenzoic acid and methyl-sulphoxide, Diisopropyl azodicarboxylate acid is 2: 1: 1.5.
The mol ratio of (S) Ph of MWCNT-SC among the present invention and vinylbenzene, Diisopropyl azodicarboxylate is 4: 2000:1.
The polymer-modified carbon nano-tube lubricant additive of the present invention's preparation is because the sterically hindered effect of polymer molecular chain, can effectively avoid the reunion of carbon nanotube in lubricating oil, utilize rigidity CNT to play the carrying effect for nuclear structure, the long-chain polymer is then owing to its flexibility, visco-elasticity will play the anti-attrition effect, realize becoming on the microcosmic sliding friction and be rolling resistance, thereby show good abrasion resistance.
Preparation process of the present invention is simple to operation, prepared multi-arm carbon nano-tube lubricant additive thermostability, good mechanical stability; Can greatly improve the dispersiveness of carbon nanotube in lubricating oil.This lubricating oil additive utilizes the rigidity carbon nanotube to play the carrying effect for nuclear structure, the long-chain polymer is then owing to its flexibility, visco-elasticity will play the anti-attrition effect, realize becoming on the microcosmic sliding friction and be rolling resistance, thereby show good abrasion resistance, be expected to solve the lubrication problem of mechanical material.This method is significant to research and the application and development of developing carbon nanotube in tribological field.
Compare with existing C NT base lubricating agent, the prepared carbon nano-tube lubricant additive of this preparation method has following characteristics:
1, can greatly improve dispersiveness and the solvability of CNT in lubricating oil.
2, Zhi Bei carbon nano-tube lubricant additive character is very stable, and high temperature is difficult for down decomposing.
3, can significantly improve the abrasion resistance of lubricating oil.
Embodiment
Now be illustrated for example in order to understand the present invention better.
Embodiment
The carbon nano-tube lubricant additive that polystyrene is modified:
1,2 gram MWCNT are distributed in the 30ml concentrated nitric acid, the backflow acidifying is after 20 hours, and washing to neutral, drying obtains 1.3 gram MWCNT-COOH.1 gram MWCNT-COOH is added 25ml SOCl
2In 70 ℃ of reactions 24 hours, boil off remaining SOCl
2, residuum immediately with the ethylene glycol of 40ml purifying 120 ℃ of reactions 48 hours.Obtain 0.9 gram MWCNT-OH through centrifugal, drying.0.6 gram MWCNT-OH and 2.8g chain-transfer agent CPAD are dissolved in the 25ml anhydrous methylene chloride, add 2.3g DCC, the lucifuge reaction at room temperature of this mixture is centrifugal after 24 hours, the washing drying obtains 0.6 gram MWCNT-SC (S) Ph.
2,0.08 gram MWCNT-SC (S) Ph, 1 gram vinylbenzene and AIBN (the DMF solution of 0.1mL0.5M) are joined among the 4ml DMF, this mixture through vacuumize, behind the logical nitrogen in 100 ℃ of stirring reactions 24 hours.Reaction is finished, and obtains the carbon nano-tube lubricant additive (MWCNT-PS) that final product-polystyrene is modified through centrifugal, washing, drying.
Claims (2)
1, a kind of preparation method of multi-arm carbon nano-tube lubricant additive is characterized in that this method specifically may further comprise the steps:
A, multi-arm carbon nano-tube (MWCNT) after acidifying with SOCl
270 ℃ of reactions, boil off remaining SOCl
2, solids reacted 48 hours at 120 ℃ with no water glycol; Obtain MWCNT-OH through centrifugal, drying; MWCNT-OH and chain-transfer agent 4-(isopropyl cyanide acid) dithiobenzoic acid ester are dissolved in methylene dichloride, add a small amount of dicyclohexylcarbodiimide, centrifugal drying obtains MWCNT-SC (S) Ph behind this mixture lucifuge reaction at room temperature certain hour;
B, MWCNT-SC (S) Ph, vinylbenzene and Diisopropyl azodicarboxylate are joined a certain amount of N, N diformamide (DMF) solution, this mixture through vacuumize, behind the logical nitrogen in 100 ℃ of stirring reactions; Reaction finishes, and obtains product through centrifugal, washing, drying.
2, the method for claim 1, the mol ratio that it is characterized in that MWCNT-SC (S) Ph and vinylbenzene, Diisopropyl azodicarboxylate is 4:2000: 1.
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| CN 200710308578 CN101469143A (en) | 2007-12-25 | 2007-12-25 | Preparation of multi-arm carbon nano-tube lubricant additive |
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| CN 200710308578 CN101469143A (en) | 2007-12-25 | 2007-12-25 | Preparation of multi-arm carbon nano-tube lubricant additive |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602650A (en) * | 2015-12-18 | 2016-05-25 | 中国科学院兰州化学物理研究所 | Carbon nanotube-modified nano-additive and preparation method and application thereof |
| CN105602649A (en) * | 2015-12-21 | 2016-05-25 | 中国科学院兰州化学物理研究所 | Graphene oxide modified nano additive and application thereof to lubricating oil |
| CN106381207A (en) * | 2016-08-31 | 2017-02-08 | 东营市昊铭润滑科技有限公司 | Diesel engine lubricating oil with long replacing period and preparation method thereof |
| CN110511519A (en) * | 2019-09-27 | 2019-11-29 | 陕西科技大学 | With the double-deck shell-core structure carbosphere/polymethyl methacrylate/polyethylene imine nanometer composite material preparation method |
| 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 |
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2007
- 2007-12-25 CN CN 200710308578 patent/CN101469143A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602650A (en) * | 2015-12-18 | 2016-05-25 | 中国科学院兰州化学物理研究所 | Carbon nanotube-modified nano-additive and preparation method and application thereof |
| CN105602650B (en) * | 2015-12-18 | 2018-09-25 | 中国科学院兰州化学物理研究所 | It is a kind of based on carbon nano tube modified nanometer additive and its preparation method and application |
| CN105602649A (en) * | 2015-12-21 | 2016-05-25 | 中国科学院兰州化学物理研究所 | Graphene oxide modified nano additive and application thereof to lubricating oil |
| CN105602649B (en) * | 2015-12-21 | 2018-02-27 | 中国科学院兰州化学物理研究所 | A kind of nanometer additive based on graphene oxide modification and its application in lubricating oil |
| CN106381207A (en) * | 2016-08-31 | 2017-02-08 | 东营市昊铭润滑科技有限公司 | Diesel engine lubricating oil with long replacing period and preparation method thereof |
| CN110511519A (en) * | 2019-09-27 | 2019-11-29 | 陕西科技大学 | With the double-deck shell-core structure carbosphere/polymethyl methacrylate/polyethylene imine nanometer composite material preparation method |
| CN110511519B (en) * | 2019-09-27 | 2021-08-31 | 陕西科技大学 | Preparation method of carbon microsphere/polymethyl methacrylate/polyethyleneimine nanocomposite with double-layer shell-core structure |
| 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 |
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