CN104293470A - Preparation method of ionized graphene oxide water-based lubricant additive - Google Patents
Preparation method of ionized graphene oxide water-based lubricant additive Download PDFInfo
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- CN104293470A CN104293470A CN201410524906.3A CN201410524906A CN104293470A CN 104293470 A CN104293470 A CN 104293470A CN 201410524906 A CN201410524906 A CN 201410524906A CN 104293470 A CN104293470 A CN 104293470A
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Abstract
The invention discloses a preparation method of an ionized graphene oxide water-based lubricant additive. The method comprises the following three steps: synthesis of graphene oxide, graphene oxide modification, and nano composition of ionized graphene oxide and alkyl imidazole ionic liquid. The water-based lubricant additive prepared by the method disclosed by the invention can be directly used as anti-wear additive of water or an emulsion of water; the ionized graphene oxide water-based lubricant additive is simple in process, available in raw materials and low in cost, has good lubricating property and compatibility with water, is capable of reducing friction force and surface abrasion, and effectively prolonging the service life of engineering machinery or components in water.
Description
Technical field
The present invention relates to process for modifying surface, be specifically related to a kind of preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives.
Background technology
In recent years, water base lubricant is widely used in many fields as hydraulic efficiency oil, cutting fluid, metal forming operation and oil production industry.The movable machinery worked in ocean environment and parts affect the problems such as its working efficiency, weather resistance and environment compatibility due to the existence of friction and receive much concern.Compared with mineral grease lubricant, water base lubricant has incomparable advantage, as: with low cost, environment compatibility good and thermal conductivity is high.Separately, because the frictional coefficient of water in metallic rubbing pairs is very high, and antiwear property is very poor, therefore, needs to develop high-performance additives to strengthen its water based lubrication to metallic surface.At present, carbon nanomaterial as a kind of hydrophobic material of novel strong mechanical performance by extensive concern and application and development.Because it is a kind of hydrophobic material, so need when it is used to water based lubrication material to carry out surface modification.Adopting hydrophilic treatment method to make carbon nanomaterial become water base lubricant is the comparatively simple method of one.Graphene is a kind of two-dirnentional structure of monoatomic thickness, derives from the graphite of a layering, and large-scale commercial production.Graphene, as a kind of carbon nanomaterial of low-dimensional, has important application prospect as Water-based Lubricating Additives.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of can directly as the emulsion of water or water wear preventive additive, technique is simple, raw material is easy to get, with low cost, there is the good preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives of performance reducing friction and reduce surface abrasion.
Following technical scheme is adopted for solving the problems of the technologies described above the present invention:
The preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives, comprises following processing step:
The preparation of <1> graphene oxide: graphite preoxidation in microwave is become graphene film; Graphene film is immersed in by H
2o
2and H
2sO
4oxidation and surface hydroxylation process is carried out in the Piranha solution of 3:7 preparation by volume; Add potassium permanganate at above-mentioned Piranha solution, the mass body volume concentrations of potassium permanganate and this Piranha solution is 8-20mg/mL, 70 DEG C of constant temperature 2 hours, obtains graphene oxide;
<2> graphene oxide modification: add step <1> gained graphene oxide in ethanol ultrasonic disperse, form homodisperse graphene oxide dispersion, the mass body volume concentrations of graphene oxide and ethanol is 20mg/mL, add 1 milliliter of surface-modifying agent by every gram of graphene oxide and modification is carried out to surface of graphene oxide, obtain ionized oxygen functionalized graphene;
<3> is nano combined: by step <2> gained ionized oxygen functionalized graphene and alkyl imidazo ion liquid 1:10-20 obtained Water-based Lubricating Additives after mixing in mass ratio.
In described step <1>, microwave frequency range is 2000MHz-5000MHz, and power is 2000-4000W, and the time is 5-30 minute.
In described step <1>, the mass volume ratio of graphene film and Piranha solution is 1g:50mL.
In described step <1>, oxidation and surface hydroxylation treatment temp control at 90 DEG C, and the time length is 1 hour.
In described step <2>, the power of ultrasonic disperse is 300-600W, 6-3 minutes time length.
Surface-modifying agent in described step <2> is: 1-ethyl-3-3 Ethoxysilane hexafluoro phosphatization imidazoles, 1-ethyl-3-3 Ethoxysilane limidazolium, 1-ethyl-3-3 Ethoxysilane tetrafluoro boron imidazoles, 1-ethyl-3-3 Ethoxysilane sulfuration imidazoles or 1-methyl-3-3 Ethoxysilane imidazolitm chloride.
Described alkyl imidazo ion liquid is Methylimidazole, ethyl imidazol(e), propyl imidazole, octylimidazole or octadecyl imidazoles, and carbochain is 1-18 carbon.
Compared with prior art, the invention has the advantages that:
1, the Water-based Lubricating Additives prepared of the present invention can directly as the wear preventive additive of the emulsion of water or water;
2, technique is simple, and raw material is easy to get, with low cost;
3, the Water-based Lubricating Additives that prepared by the present invention has good oilness and the consistency of water, can reduce friction and reduce surface abrasion, effectively extends engineering machinery or the working life of parts in water.
Embodiment:
Embodiment 1:
By 1 gram of graphite frequency be 2000MHz, power is 2000W, in the microwave of 30 minutes time, preoxidation becomes graphene film; Again graphene film is immersed in by H
2o
2with dense H
2sO
4carry out oxidation and surface hydroxylation process in 50 milliliters of Piranha solution of 3:7 preparation by volume, temperature controls at 90 DEG C, and the time length is 1 hour; And then the potassium permanganate of 1 gram is added at above-mentioned Piranha solution, 70 DEG C of constant temperature 2 hours, obtain graphene oxide; Graphene oxide is added in 50 milliliters of ethanol again and carries out ultrasonic disperse, the power of ultrasonic disperse is 600W, 3 minutes time length, form homodisperse graphene oxide dispersion, add 1 milliliter of 1-ethyl-3-3 Ethoxysilane hexafluoro phosphatization imidazoles and modification is carried out to graphenic surface obtain ionized oxygen functionalized graphene.By ionized oxygen functionalized graphene and methyl imidazole ion liquid 1:20 obtained Water-based Lubricating Additives after mixing in mass ratio.
Embodiment 2:
By 1 gram of graphite frequency be 2500MHz, power is 2500W, in the microwave of 20 minutes time, preoxidation becomes graphene film; Graphene film is immersed in by H
2o
2with dense H
2sO
4carry out oxidation and surface hydroxylation process in 50 milliliters of Piranha solution of 3:7 preparation by volume, temperature controls at 90 DEG C, and the time length is 1 hour; And then the potassium permanganate of 0.8 gram is added at above-mentioned Piranha solution, 70 DEG C of constant temperature 2 hours, obtain graphene oxide; Graphene oxide is added in 50 milliliters of ethanol again and carries out ultrasonic disperse, the power of ultrasonic disperse is 500W, 4 minutes time length, form homodisperse graphene oxide dispersion, add 1 milliliter of 1-ethyl-3-3 Ethoxysilane limidazolium and modification is carried out to graphenic surface obtain ionized oxygen functionalized graphene.By ionized oxygen functionalized graphene and propyl imidazole ion liquid 1:18 obtained Water-based Lubricating Additives after mixing in mass ratio.
Embodiment 3:
By 1 gram of graphite frequency be 3000MHz, power is 2800W, in the microwave of 15 minutes time, preoxidation becomes graphene film; Graphene film is immersed in by H
2o
2with dense H
2sO
4carry out oxidation and surface hydroxylation process in 50 milliliters of Piranha solution of 3:7 preparation by volume, temperature controls at 90 DEG C, and the time length is 1 hour; And then the potassium permanganate of 0.6 gram is added at above-mentioned Piranha solution, 70 DEG C of constant temperature 2 hours, obtain graphene oxide; Graphene oxide is added in 50 milliliters of ethanol again and carries out ultrasonic disperse, the power of ultrasonic disperse is 400W, 5 minutes time length, form homodisperse graphene oxide dispersion, add 1 milliliter of 1-ethyl-3-3 Ethoxysilane sulfuration imidazoles and modification is carried out to graphenic surface obtain ionized oxygen functionalized graphene.By ionized oxygen functionalized graphene and ethyl group imidazole ion liquid 1:16 obtained Water-based Lubricating Additives after mixing in mass ratio.
Embodiment 4:
By 1 gram of graphite frequency be 5000MHz, power is 4000W, in the microwave of 5 minutes time, preoxidation becomes graphene film; Graphene film is immersed in by H
2o
2with dense H
2sO
4carry out oxidation and surface hydroxylation process in 50 milliliters of Piranha solution of 3:7 preparation by volume, temperature controls at 90 DEG C, and the time length is 1 hour; And then the potassium permanganate of 0.4 gram is added at above-mentioned Piranha solution, 70 DEG C of constant temperature 2 hours, obtain graphene oxide; Again this graphene oxide is added in 50 milliliters of ethanol and carries out ultrasonic disperse, the power of ultrasonic disperse is 300W, 3 minutes time length, form homodisperse graphene oxide dispersion, add 1 milliliter of 1-ethyl-3-3 Ethoxysilane imidazolitm chloride and modification is carried out to graphenic surface obtain ionized oxygen functionalized graphene.By ionized oxygen functionalized graphene and octyl imidazole ion liquid 1:10 obtained Water-based Lubricating Additives after mixing in mass ratio.
After tested, the frictional coefficient of Water-based Lubricating Additives in distilled water that embodiment 1 to 4 is obtained is 0.06 ~ 0.08.This ionized oxygen functionalized graphene Water-based Lubricating Additives is applied to stainless steel surface in water, and its frictional coefficient is only 0.6 (when not adding any additive, stainless steel surface frictional coefficient is 3.0), and its antifriction effect is remarkable.
Claims (7)
1. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives, is characterized in that, comprises following processing step:
The preparation of <1> graphene oxide: graphite preoxidation in microwave is become graphene film; Graphene film is immersed in by H
2o
2and H
2sO
4oxidation and surface hydroxylation process is carried out in the Piranha solution of 3:7 preparation by volume; Add potassium permanganate at above-mentioned Piranha solution, the mass body volume concentrations of potassium permanganate and this Piranha solution is 8-20mg/mL, 70 DEG C of constant temperature 2 hours, obtains graphene oxide;
<2> graphene oxide modification: add step <1> gained graphene oxide in ethanol ultrasonic disperse, form homodisperse graphene oxide dispersion, the mass body volume concentrations of graphene oxide and ethanol is 20mg/mL, add 1 milliliter of surface-modifying agent by every gram of graphene oxide and modification is carried out to surface of graphene oxide, obtain ionized oxygen functionalized graphene;
<3> is nano combined: by step <2> gained ionized oxygen functionalized graphene and alkyl imidazo ion liquid 1:10-20 obtained Water-based Lubricating Additives after mixing in mass ratio.
2. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives according to claim 1, it is characterized in that: in described step <1>, microwave frequency range is 2000MHz-5000MHz, power is 2000-4000W, and the time is 5-30 minute.
3. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives according to claim 1, is characterized in that: in described step <1>, the mass volume ratio of graphene film and Piranha solution is 1g:50mL.
4. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives according to claim 1, it is characterized in that: in described step <1>, oxidation and surface hydroxylation treatment temp control at 90 DEG C, and the time length is 1 hour.
5. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives according to claim 1, is characterized in that: in described step <2>, the power of ultrasonic disperse is 300-600W, 6-3 minutes time length.
6. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives according to claim 1, is characterized in that: the surface-modifying agent in described step <2> is: 1-ethyl-3-3 Ethoxysilane hexafluoro phosphatization imidazoles, 1-ethyl-3-3 Ethoxysilane limidazolium, 1-ethyl-3-3 Ethoxysilane tetrafluoro boron imidazoles, 1-ethyl-3-3 Ethoxysilane sulfuration imidazoles or 1-methyl-3-3 Ethoxysilane imidazolitm chloride.
7. the preparation method of ionized oxygen functionalized graphene Water-based Lubricating Additives according to claim 1, it is characterized in that: described alkyl imidazo ion liquid is Methylimidazole, ethyl imidazol(e), propyl imidazole, octylimidazole or octadecyl imidazoles, carbochain is 1-18 carbon.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104830413A (en) * | 2015-05-13 | 2015-08-12 | 南京欧美加新材料有限公司 | Preparation method of lubricating oil composition containing ionic liquid, modified nano-tin powder and graphene |
| CN104830404A (en) * | 2015-05-13 | 2015-08-12 | 南京欧美加新材料有限公司 | Preparation method of lubricating oil composition containing ionic liquid, modified nano-zinc powder and graphene |
| CN105154170A (en) * | 2015-09-21 | 2015-12-16 | 西南石油大学 | Preparation method of nanometer boehmite composite oxidized graphene antiwear lubricant |
| CN105479255A (en) * | 2016-01-18 | 2016-04-13 | 济南大学 | Nanometer additive cutting fluid dispersion and atomization circulating device based on ultrasonic vibration |
| JP2016098279A (en) * | 2014-11-19 | 2016-05-30 | 国立大学法人 岡山大学 | Aqueous lubricant composition |
| CN106085549A (en) * | 2016-06-07 | 2016-11-09 | 山东源根石油化工有限公司 | The preparation of a kind of extreme pressure anti-wear additives and the energy saving environment protection engine oil containing this extreme pressure anti-wear additives |
| CN108048936A (en) * | 2017-12-30 | 2018-05-18 | 杭州高烯科技有限公司 | A kind of preparation method of high-performance PP fibers |
| CN108085767A (en) * | 2017-12-30 | 2018-05-29 | 杭州高烯科技有限公司 | A kind of preparation method of multifunction polyacrylonitrile-graphene oxide composite fibre |
| CN109576047A (en) * | 2019-01-14 | 2019-04-05 | 西南交通大学 | A method of high lubricating property graphene is prepared with ionic liquid |
| CN114437858A (en) * | 2022-02-09 | 2022-05-06 | 沈阳建筑大学 | Graphene oxide lubricating oil and preparation method thereof |
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2014
- 2014-09-30 CN CN201410524906.3A patent/CN104293470A/en active Pending
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| YUFEI MO，ET AL.: "Graphene/Ionic Liquid Composite Films and Ion Exchange", 《SCI. REP.》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2016098279A (en) * | 2014-11-19 | 2016-05-30 | 国立大学法人 岡山大学 | Aqueous lubricant composition |
| CN104830404A (en) * | 2015-05-13 | 2015-08-12 | 南京欧美加新材料有限公司 | Preparation method of lubricating oil composition containing ionic liquid, modified nano-zinc powder and graphene |
| CN104830404B (en) * | 2015-05-13 | 2018-09-07 | 南京林业大学 | A kind of preparation method of the lubricant oil composite containing ionic liquid, modified Nano zinc powder and graphene |
| CN104830413A (en) * | 2015-05-13 | 2015-08-12 | 南京欧美加新材料有限公司 | Preparation method of lubricating oil composition containing ionic liquid, modified nano-tin powder and graphene |
| CN105154170B (en) * | 2015-09-21 | 2018-04-17 | 西南石油大学 | A kind of preparation method of nm boehmite combined oxidation graphene antifriction lubricant |
| CN105154170A (en) * | 2015-09-21 | 2015-12-16 | 西南石油大学 | Preparation method of nanometer boehmite composite oxidized graphene antiwear lubricant |
| CN105479255A (en) * | 2016-01-18 | 2016-04-13 | 济南大学 | Nanometer additive cutting fluid dispersion and atomization circulating device based on ultrasonic vibration |
| CN106085549A (en) * | 2016-06-07 | 2016-11-09 | 山东源根石油化工有限公司 | The preparation of a kind of extreme pressure anti-wear additives and the energy saving environment protection engine oil containing this extreme pressure anti-wear additives |
| CN106085549B (en) * | 2016-06-07 | 2020-07-17 | 山东源根石油化工有限公司 | Preparation of extreme pressure anti-wear agent and energy-saving environment-friendly engine oil containing extreme pressure anti-wear agent |
| CN108048936A (en) * | 2017-12-30 | 2018-05-18 | 杭州高烯科技有限公司 | A kind of preparation method of high-performance PP fibers |
| CN108085767A (en) * | 2017-12-30 | 2018-05-29 | 杭州高烯科技有限公司 | A kind of preparation method of multifunction polyacrylonitrile-graphene oxide composite fibre |
| CN109576047A (en) * | 2019-01-14 | 2019-04-05 | 西南交通大学 | A method of high lubricating property graphene is prepared with ionic liquid |
| CN109576047B (en) * | 2019-01-14 | 2021-06-15 | 西南交通大学 | Method for preparing graphene with high lubricating property by using ionic liquid |
| CN114437858A (en) * | 2022-02-09 | 2022-05-06 | 沈阳建筑大学 | Graphene oxide lubricating oil and preparation method thereof |
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Application publication date: 20150121 |