CN107523381A - A kind of preparation method of graphene carbon nanometer tube composite materials load nano copper particle lubriation material - Google Patents
A kind of preparation method of graphene carbon nanometer tube composite materials load nano copper particle lubriation material Download PDFInfo
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- CN107523381A CN107523381A CN201710914808.4A CN201710914808A CN107523381A CN 107523381 A CN107523381 A CN 107523381A CN 201710914808 A CN201710914808 A CN 201710914808A CN 107523381 A CN107523381 A CN 107523381A
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Classifications
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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
- C10M163/00—Lubricating compositions characterised by the additive being a mixture of a compound of unknown or incompletely defined constitution and a non-macromolecular compound, each of these compounds being essential
-
- 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
- C10M2201/05—Metals; Alloys
-
- 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
- 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
Abstract
A kind of preparation method of graphene carbon nanometer tube composite materials load nano copper particle lubriation material.Graphene oxide and CNT are distributed in Tris HCl cushioning liquid, dopamine hydrochloride is added after being uniformly dispersed, by poly-dopamine functional graft to graphene oxide and carbon nano tube surface.Then functional graphene oxide/carbon nano tube compound material is distributed in ethanol, adds soluble copper salt, reducing agent reaction is added after dissolving completely, mantoquita is converted into Nanometer Copper original position and loads to Graphene/carbon nanotube composite material surface.The present invention carries out biomimetic modification with poly-dopamine to graphene oxide and CNT, and preparation technology is simple, and poly-dopamine can not only organically combine graphene oxide and CNT, and abundant active group is provided on its surface.The material uniform and stable can not only be distributed in polarity base oil, but also has excellent antiwear and antifriction effect.
Description
Technical field
The invention belongs to nano composite material preparing technical field, and in particular to a kind of graphene-carbon nano tube composite wood
The preparation method of material load nano copper particle lubriation material.
Background technology
Nano-carbon material has being widely present from zero dimension to two dimension, such as the fullerene of zero dimension, one-dimensional CNT, and two
Graphene oxide of dimension etc..These carbon materials have research in tribological field, usually as lubricating additive or polymerization
Thing inserts, play antiwear and antifriction effect.Cu nano particle preparation process is simple, cheap, has self lubricity, as profit
Oil additive extensive application.With the rapid development of science and technology, single nanometer lubricating additive will slowly can not meet
The demand of people, therefore the research and preparation of novel nanocomposite materials will be trends of the times.
The Chinese invention patent of Application No. 201410002980.9 discloses a kind of hydro-thermal of graphene/copper composite material
Salzburg vitriol, nickel sulfate, citric acid, boric acid are configured to mixed solution by preparation method, this method, then add oxidation stone
Black alkene, graphene/copper nano composite material is prepared under the reduction of sodium hypophosphite reducing agent.Application No.
201510632643.2 Chinese invention patent disclose a kind of metal nanoparticle/graphene/carbon nano-tube material of preparing
Method.The invention by metal salt solution, graphite oxide and CNT by being dispersed in water, ethanol, DMF
Irradiated in equal solvent, it is nano combined to prepare metal nanoparticle/graphene/carbon nano-tube with low infrared emissivity
Material.The Chinese invention patent of Application No. 201710000439.8 discloses a kind of graphene/carbon nanometer of mercapto modification
Pipe composite and preparation method.Acetic acid, acetone, 3- mercaptopropyl trimethoxysilanes are configured to mixed solution by this method, so
Graphene/carbon nano-tube is scattered wherein afterwards, is passed through nitrogen protection, is filtered after reaction, mercapto modification is obtained after vacuum drying
Graphene/carbon nanotube composite material.
However, copper nano particles in combination product prepared by the above method uniformly can not be grown in good distribution
On carbon nanomaterial matrix, though some have being uniformly distributed for Cu nano particles, experimental procedure is complicated or needs to use costliness
Instrument.So that the cost of composite is more high-leveled and difficult with popularization and application.
In view of disadvantages described above, it is necessary to which a kind of preparation method simple to operate, cheap and economic and environment-friendly is provided.
The content of the invention
The defects of in order to overcome above-mentioned preparation method, it is an object of the invention to provide a kind of graphene-carbon nano tube to answer
Condensation material loads the preparation method of nano copper particle lubriation material, and graphene-carbon nano tube composite material prepared by this method is born
The antiwear and antifriction effect of base oil can effectively be improved by carrying nano copper particle, and graphene-carbon nano tube composite material surface
The poly-dopamine of functionalization can not only stability of composite materials structure, and abundant active group contributes to composite in base
Scattered in plinth oil and stably, graphene-carbon nano tube composite material load nano copper particle has performance as lubriation material
It is good, the advantages such as cost is low.
To achieve the above object, the present invention is to be achieved through the following technical solutions：
A kind of preparation method of graphene-carbon nano tube composite material load nano copper particle lubriation material, specific steps include：
1）Graphene oxide, CNT are distributed in enough Tris-HCl cushioning liquid, it is 0.2- then to add concentration
0.5 wt.% dopamine hydrochlorides, are reacted at 20-25 DEG C, and poly-dopamine is grafted into graphene oxide and CNT
Surface, obtain functional graphene oxide/carbon nano tube compound material；
2）By step 1）Product is distributed in enough ethanol, adds soluble copper salt, and excessive reductant is added after dissolving completely,
Reacted at 75-95 DEG C, mantoquita is converted into Nanometer Copper original position and load to Graphene/carbon nanotube composite material surface, obtain
Nano copper particle lubriation material is loaded to graphene-carbon nano tube composite material.
Further improve of the invention is that the mass ratio of described graphene oxide and CNT is 1:1~1:5.
Further improve of the invention is that the pH value of described Tris-HCl cushioning liquid is 8.5.
Further improve of the invention is that described mantoquita is copper sulphate, copper chloride, copper nitrate or copper acetate.Its
The concentration of middle mantoquita is 0.01 ~ 0.1 mol/L.
Further improve of the invention is that described reducing agent is sodium borohydride or sodium hypophosphite, and its concentration is copper
2 ~ 3 times of salinity.
Further improve of the invention is that the temperature of described reduction reaction is 75-95 DEG C, reaction time 10-30
min。
Further improve of the invention is, before adding reducing agent, dispersion liquid is quiet after being completely dissolved soluble copper salt
Put, remove clear liquid, rejoin enough ethanol, be configured to dispersion liquid.
Compared with prior art, the present invention has following beneficial effect：
The present invention carries out surface modification using poly-dopamine to graphene oxide and CNT, not only by graphene and carbon nanometer
Pipe is organically combined with each other, and graphene oxide-carbon nano tube compound material surface can be made to possess the function of more horn of plenty
Group, so as to its superficial growth size is single, equally distributed Cu nano particles.In addition, poly-dopamine functionalization composite
Surface contain that abundant active group contributes to it in base oil it is scattered with stably.Graphene, CNT and Nanometer Copper
Combination be beneficial to composite lubrication cooperative effect produced in friction process, improve the friction and abrasion of lubricating oil
Energy.
Brief description of the drawings
Fig. 1 is that the EDS of graphene-carbon nano tube composite material load nano copper particle lubriation material prepared by the present invention is surveyed
Test result；
Fig. 2 is the TEM photos of graphene-carbon nano tube composite material load nano copper particle lubriation material prepared by the present invention；
Fig. 3 is that graphene-carbon nano tube composite material prepared by the present invention loads nano copper particle lubriation material in soya-bean oil
Scattered photo；
Fig. 4 is that graphene-carbon nano tube composite material prepared by the present invention loads nano copper particle as soya-bean oil lubricating additive
Coefficient of friction and wear scar diameter curve.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be the present invention explanation without
It is to limit.
Embodiment 1
Step 1：0.025g GO and 0.05gCNTs is distributed in 200 mL Tris-HCl buffer solutions under ultrasonication
(pH=8.5).0.4 g dopamine hydrochlorides are added, are reacted 12 hours under strong magnetic agitation effect.With distilled water and
The repeated multiple times centrifuge washing of ethanol, to remove the impurity such as free PDA.Finally it is dried with freeze drying box just available
PDA/GO-CNTs sample powders.
Step 2：0.02 g PDA/GO-CNTs are dispersed in 50mL ethanol solution under ultrasonication, then added
Enter 0.15 g copper acetates, stirring is allowed to dissolve.Another beaker is taken 0.12g sodium hypophosphites to be dissolved into 40mL ethanol solution
In.Above two liquid is added in flask, in temperature constant magnetic stirring water-bath under stirring action 80 DEG C react 20 minutes.
Flask is taken out, carries out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained Cu/PDA/GO-CNTs sample powders.
It refer to shown in Fig. 1, it is as the graphene-carbon nano tube composite material prepared by the inventive method embodiment 1
Load the EDS figures of nano copper particle.As seen from Figure 1：Graphene-carbon nano tube composite material load prepared by the present invention
Nano copper particle contains the elements such as C, O, N, Cu.
It refer to shown in Fig. 2, it is as the graphene-carbon nano tube composite material prepared by the inventive method embodiment 1
Load the TEM figures of nano copper particle.As seen from Figure 2：CNT is compounded in graphene nanometer sheet surface, copper nano particles
It is evenly distributed on graphene-carbon nano tube composite material surface.
It refer to shown in Fig. 3, it is as the graphene-carbon nano tube composite material prepared by the inventive method embodiment 1
Load photo of the nano copper particle in soybean basis oil dispersed.As seen from Figure 3：Graphene-carbon prepared by the present invention is received
Nano copper particle is uniform and stable is distributed in base oil for the load of mitron composite, and after static 10 days, composite remains to surely
Fixed is scattered.
It refer to shown in Fig. 4, it is as the graphene-carbon nano tube composite material prepared by the inventive method embodiment 1
Load nano copper particle concentration and coefficient of friction and the relation picture of abrasion size in soybean oil.As seen from Figure 4：This hair
Bright prepared graphene-carbon nano tube composite material load nano copper particle effectively reduce soybean oil coefficient of friction and
Wear-life.
Embodiment 2
Step 1：0.01g GO and 0.05gCNTs is distributed in 200 mL Tris-HCl buffer solutions under ultrasonication
(pH=8.5).0.4 g dopamine hydrochlorides are added, are reacted 12 hours under strong magnetic agitation effect.With distilled water and
The repeated multiple times centrifuge washing of ethanol, to remove the magazines such as free PDA.Finally it is dried with freeze drying box just available
PDA/GO-CNTs sample powders.
Step 2：0.02 g PDA/GO-CNTs are dispersed in 50 mL ethanol solution under ultrasonication, then
0.15 g copper sulphate is added, stirring is allowed to dissolve.Another beaker is taken 0.1g sodium hypophosphites to be dissolved into 40 mL ethanol solution
In.Above two liquid is added in flask, in temperature constant magnetic stirring water-bath under stirring action 80 DEG C react 20 minutes.
Flask is taken out, carries out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained Cu/PDA/GO-CNTs sample powders.
Embodiment 3
Step 1：0.01g GO and 0.05gCNTs is distributed in 200 mL Tris-HCl buffer solutions under ultrasonication
(pH=8.5).0.4 g dopamine hydrochlorides are added, are reacted 12 hours under strong magnetic agitation effect.With distilled water and
The repeated multiple times centrifuge washing of ethanol, to remove the magazines such as free PDA.Finally it is dried with freeze drying box just available
PDA/GO-CNTs sample powders.
Step 2：0.02 g PDA/GO-CNTs are dispersed in 50 mL ethanol solution under ultrasonication, then
0.2 g copper nitrates are added, stirring is allowed to dissolve.Another beaker is taken 0.1g sodium borohydrides to be dissolved into 40 mL ethanol solution.
Above two liquid is added in flask, in temperature constant magnetic stirring water-bath under stirring action 80 DEG C react 20 minutes.Take
Go out flask, carry out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained Cu/PDA/GO-CNTs sample powders.
Embodiment 4
Step 1：0.01g GO and 0.01gCNTs is distributed in 200 mL Tris-HCl buffer solutions under ultrasonication
(pH=8.5).0.4 g dopamine hydrochlorides are added, are reacted 12 hours under strong magnetic agitation effect.With distilled water and
The repeated multiple times centrifuge washing of ethanol, to remove the magazines such as free PDA.Finally it is dried with freeze drying box just available
PDA/GO-CNTs sample powders.
Step 2：0.02 g PDA/GO-CNTs are dispersed in 50 mL ethanol solution under ultrasonication, then
0.15 g copper acetates are added, stirring is allowed to dissolve.Another beaker is taken 0.2g sodium hypophosphites to be dissolved into 40 mL ethanol solution
In.Above two liquid is added in flask, in temperature constant magnetic stirring water-bath under stirring action 95 DEG C react 10 minutes.
Flask is taken out, carries out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained Cu/PDA/GO-CNTs sample powders.
Embodiment 5
Step 1：0.01g GO and 0.03gCNTs is distributed in 200 mL Tris-HCl buffer solutions under ultrasonication
(pH=8.5).0.4 g dopamine hydrochlorides are added, are reacted 12 hours under strong magnetic agitation effect.With distilled water and
The repeated multiple times centrifuge washing of ethanol, to remove the magazines such as free PDA.Finally it is dried with freeze drying box just available
PDA/GO-CNTs sample powders.
Step 2：0.02 g PDA/GO-CNTs are dispersed in 50 mL ethanol solution under ultrasonication, then
0.15 g copper chlorides are added, stirring is allowed to dissolve.Take another beaker 0.15g sodium hypophosphites are dissolved into 40 mL ethanol it is molten
In liquid.Above two liquid is added in flask, 70 DEG C of 30 points of reactions under stirring action in temperature constant magnetic stirring water-bath
Clock.Flask is taken out, carries out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained Cu/PDA/GO-CNTs sample powders.
Claims (9)
- A kind of 1. preparation method of graphene-carbon nano tube composite material load nano copper particle lubriation material, it is characterised in that Specific steps include：1）Graphene oxide, CNT are distributed in enough Tris-HCl cushioning liquid, it is 0.2- then to add concentration 0.5 wt.% dopamine hydrochlorides, are reacted at 20-25 DEG C, and reaction is complete, by poly-dopamine functional graft to oxidation Graphene and carbon nano tube surface, obtain functional graphene oxide/carbon nano tube compound material；2）By step 1）Product is distributed in enough ethanol, adds soluble copper salt, and excessive reductant is added after dissolving completely, Reacted at 75-95 DEG C, reaction is complete, mantoquita is converted into Nanometer Copper original position and loads to graphene/carbon nano-tube composite wood Expect surface, obtain graphene-carbon nano tube composite material load nano copper particle lubriation material.
- 2. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that described graphene oxide and the mass ratio of CNT are 1:1~1:5.
- 3. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that the pH value of described Tris-HCl cushioning liquid is 8.5.
- 4. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that described mantoquita is copper sulphate, copper chloride, copper nitrate or copper acetate.
- 5. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that when adding soluble copper salt, be formulated as the mantoquita that mantoquita concentration is 0.01 ~ 0.1 mol/L Ethanol solution.
- 6. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that described reducing agent is sodium borohydride or sodium hypophosphite.
- 7. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that before adding reducing agent, be formulated as the ethanol solution of reducing agent, make the mole dense of the solution Spend the ethanol solution for mantoquita 2 ~ 3 times.
- 8. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that the temperature of described reduction reaction is 75-95 DEG C, and the reaction time is 10-30 min.
- 9. a kind of graphene-carbon nano tube composite material load nano copper particle lubriation material according to claim 1 Preparation method, it is characterised in that after being completely dissolved soluble copper salt, before adding reducing agent, dispersion liquid is stood, removes clear liquid, Enough ethanol is rejoined, is configured to dispersion liquid.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108795539A (en) * | 2018-08-06 | 2018-11-13 | 黑龙江科技大学 | A kind of preparation method of carbon nanomaterial lubricating oil |
| CN109012595A (en) * | 2018-09-06 | 2018-12-18 | 苏州佰锐生物科技有限公司 | A kind of preparation method of modified carbon nano-tube adsorbent for heavy metal |
| CN109052541A (en) * | 2018-09-06 | 2018-12-21 | 苏州佰锐生物科技有限公司 | A method of removal heavy metal in waste water nickel ion |
| CN109052542A (en) * | 2018-09-06 | 2018-12-21 | 苏州佰锐生物科技有限公司 | A kind of preparation method for the modified carbon nano-tube removing mercury ions in waste water |
| CN111151765A (en) * | 2020-01-20 | 2020-05-15 | 西安稀有金属材料研究院有限公司 | Preparation method of three-dimensional structure nano carbon material reinforced copper-based composite material |
| CN111440653A (en) * | 2020-04-17 | 2020-07-24 | 清华大学 | Application of polydopamine nanoparticles in water-based lubricating fluid |
| CN112316979A (en) * | 2020-09-30 | 2021-02-05 | 山东大学 | Polydopamine-modified carbon black-graphene oxide composite microsphere and preparation method and application thereof |
| CN112961721A (en) * | 2020-12-30 | 2021-06-15 | 徐州振峰新材料科技有限公司 | Graphene-containing lubricating protection additive for lubricating oil |
| CN113981481A (en) * | 2021-09-27 | 2022-01-28 | 西安电子科技大学 | Preparation method and application of copper nanoparticle-loaded one-dimensional carbon-based nano material |
| 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 |
| CN117004448A (en) * | 2023-08-04 | 2023-11-07 | 上海应用技术大学 | Cu@ alpha-Zrp nano composite material lubricating oil additive and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108795539A (en) * | 2018-08-06 | 2018-11-13 | 黑龙江科技大学 | A kind of preparation method of carbon nanomaterial lubricating oil |
| CN109012595A (en) * | 2018-09-06 | 2018-12-18 | 苏州佰锐生物科技有限公司 | A kind of preparation method of modified carbon nano-tube adsorbent for heavy metal |
| CN109052541A (en) * | 2018-09-06 | 2018-12-21 | 苏州佰锐生物科技有限公司 | A method of removal heavy metal in waste water nickel ion |
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| CN111440653A (en) * | 2020-04-17 | 2020-07-24 | 清华大学 | Application of polydopamine nanoparticles in water-based lubricating fluid |
| CN112316979A (en) * | 2020-09-30 | 2021-02-05 | 山东大学 | Polydopamine-modified carbon black-graphene oxide composite microsphere and preparation method and application thereof |
| CN112961721A (en) * | 2020-12-30 | 2021-06-15 | 徐州振峰新材料科技有限公司 | Graphene-containing lubricating protection additive for lubricating oil |
| CN113981481A (en) * | 2021-09-27 | 2022-01-28 | 西安电子科技大学 | Preparation method and application of copper nanoparticle-loaded one-dimensional carbon-based nano material |
| CN113981481B (en) * | 2021-09-27 | 2022-10-14 | 西安电子科技大学 | Preparation method and application of copper nanoparticle-loaded one-dimensional carbon-based nano material |
| 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 |
| CN117004448A (en) * | 2023-08-04 | 2023-11-07 | 上海应用技术大学 | Cu@ alpha-Zrp nano composite material lubricating oil additive and preparation method and application thereof |
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