CN107557110A - A kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material - Google Patents
A kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material Download PDFInfo
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Abstract
A kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material.Molybdenum disulfide nano sheet is distributed in Tris HCl cushioning liquid, dopamine hydrochloride is added after being uniformly dispersed, poly-dopamine is grafted to molybdenum disulfide nano sheet surface.Then functionalization molybdenum disulfide nano sheet 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 molybdenum disulfide nano sheet surface.The present invention carries out biomimetic modification with poly-dopamine to molybdenum disulfide nano sheet, and preparation technology is simple, and poly-dopamine can not only organically combine molybdenum disulfide nano sheet and Nanometer Copper, and abundant active group is provided on its surface.The Nanometer Copper obtained after in-situ reducing is uniformly adhered to molybdenum disulfide nano sheet surface so that the composite 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, is related to molybdenum disulfide nano sheet load nano copper particle profit
The preparation method of sliding material.
Background technology
For molybdenum disulfide as typical transistion metal compound, its specific surface area is big, and adsorption capacity is strong, is widely used
In absorption, catalysis and the field such as electrochemistry, while MoS2Preparation method is easy, cost is cheap, has special layer structure,
Transfer membrane is formed with regard to sliding can occur under low stress load, therefore has very big Research Significance in lubricating area, in recent years, with
Molybdenum disulfide is carrier, and preparing the more excellent novel nanocomposite materials of greasy property becomes an important research side
To.
The Chinese invention patent of application number 201410212428.2 discloses a kind of water-based graphite alkene-molybdenum disulfide nano tube
The preparation method of lubricating additive, the preparation of this method including water-soluble graphene, the preparation of water-soluble molybdenum disulfide nano tube,
Three processes of preparation of water-based graphite alkene-molybdenum disulfide nano tube lubricating additive.The China of application number 201310589309.4
Patent of invention discloses a kind of preparation method of the nanometer lubricating additive of cadmium doping molybdenum disulfide, and this method is existed by hydro-thermal method
260 DEG C of reaction 24h prepare the Cd doping MoS2 nanometer sheets that flower-like structure is assembled into by nanometer sheet.Meng et al. passes through in-situ chemical
The precipitation method are successfully prepared Cu-GO composites, characterize and find that the copper nano particles uniform load of particle diameter 5-10 nanometers is aoxidizing
The surface of graphene, the lubricating oil for finding to prepare as paraffin wax additives research have remarkable antifriction and abrasion resistance.
In spite of a small amount of Chinese invention patent for preparing molybdenum disulfide based nano composite material, but on molybdenum disulfide
The preparation method of nanometer sheet load nano copper particle lubriation material yet there are no relevant report.
The content of the invention
In order to make up the blank of above-mentioned preparation method, it is an object of the invention to provide a kind of load of molybdenum disulfide nano sheet
The preparation method of nano copper particle lubriation material, molybdenum disulfide nano sheet load nano copper particle prepared by this method can be effective
Raising base oil antiwear and antifriction effect, and the surface-functionalized poly-dopamine of molybdenum disulfide nano sheet can not only stablize it is compound
The structure of material, and abundant active group contributes to scattered in base oil of composite and stably, and molybdenum disulfide is received
Rice piece load nano copper particle load nano copper particle has that performance is good as lubriation material, 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 molybdenum disulfide nano sheet load nano copper particle lubriation material, specific steps include：
1）Molybdenum disulfide nano sheet is distributed in enough Tris-HCl cushioning liquid, it is 0.2-0.5 then to add concentration
Wt.% dopamine hydrochloride, reacted at 20-25 DEG C DEG C, reaction is complete, by poly-dopamine functional graft to two sulphur
Change molybdenum nanometer sheet surface；
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 molybdenum disulfide nano sheet surface, obtains
Molybdenum disulfide nano sheet loads nano copper particle lubriation material.
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.
Of the invention further improve be, described reducing agent is sodium borohydride or sodium hypophosphite, its molar concentration
For 1/3 ~ 1/2 times of mantoquita concentration.
Further improve of the invention is that the temperature of described reduction reaction is 75-95 DEG C, reaction time 10-30
min。
Compared with prior art, the present invention has following beneficial effect：
The present invention carries out surface modification using poly-dopamine to molybdenum disulfide nano sheet, gathers around oxidation molybdenum disulfide nano sheet surface
There is the functional group of more horn of plenty, so as to its superficial growth size is single, equally distributed Cu nano particles.In addition, poly- DOPA
Amino-functionalization composite material surface contain that abundant active group contributes to it in base oil it is scattered with stably.Molybdenum disulfide
The combination of nanometer sheet and Nanometer Copper is beneficial to composite and lubrication cooperative effect is produced in friction process, improves lubrication
The friction and wear behavior of oil.
Brief description of the drawings
Fig. 1 is the EDS test results of molybdenum disulfide nano sheet load nano copper particle lubriation material prepared by the present invention；
Fig. 2 is the TEM photos of molybdenum disulfide nano sheet load nano copper particle lubriation material prepared by the present invention；
Fig. 3 is that molybdenum disulfide nano sheet prepared by the present invention loads scattered photo of the nano copper particle lubriation material in soya-bean oil；
Fig. 4 is that molybdenum disulfide nano sheet prepared by the present invention loads nano copper particle lubriation material 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：The thioacetamide of 0.12g sodium molybdate and 0.24g is added in 80 milliliters of deionized water simultaneously ultrasound 0.5
Homogeneous transparent liquid is prepared in h, transfers the solution into afterwards in 100 ml polytetrafluoroethyllining lining stainless steel cauldron, with
Reactor is put into convection oven afterwards, reaction temperature is arranged to 240 DEG C, the reaction time is 24 hours.Natural cooling afterwards
To room temperature, by the absolute ethyl alcohol centrifuge washing of the product in reactor, then black product is placed in vacuum drying oven and dried, is obtained
To molybdenum disulfide nano sheet.
Step 2：0.04g molybdenum disulfide is distributed in 100 ml Tris-HCL (pH=8.5) cushioning liquid and surpassed
Black liquor is prepared in sound 2h, and 0.2g Dopamine hydrochloride is added in above-mentioned solution afterwards and is stirred vigorously 12 h, is used
Product, is then distributed in 100 ml ethanol, 0.5g copper acetate by distilled water and the repeated multiple times centrifuge washing product of ethanol
It is distributed to by magnetic agitation in above-mentioned solution.Take another beaker 0.445g sodium hypophosphites are dissolved into 30 mL ethanol it is molten
In liquid.Above two liquid is added in flask, 80 DEG C of 20 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 molybdenum disulfide nano sheet load Nanometer Copper
Particle.
It refer to shown in Fig. 1, it is to load Nanometer Copper as the molybdenum disulfide nano sheet prepared by the inventive method embodiment 1
The EDS figures of particle.As seen from Figure 1：Molybdenum disulfide nano sheet load nano copper particle prepared by the present invention contains Mo,
The elements such as S, O, C, N, Cu.
It refer to shown in Fig. 2, it is to load Nanometer Copper as the molybdenum disulfide nano sheet prepared by the inventive method embodiment 1
The TEM figures of particle.As seen from Figure 2：Copper nano particles are evenly distributed on molybdenum disulfide nano sheet surface.
It refer to shown in Fig. 3, it is to load nanometer as the stone molybdenum disulfide nano sheet prepared by the inventive method embodiment 1
Photo of the copper particle in soybean basis oil dispersed.As seen from Figure 3：Molybdenum disulfide nano sheet load prepared by the present invention is received
Copper particle is uniform and stable is distributed in base oil for rice, and after static 10 days, composite remains to stable scattered.
It refer to shown in Fig. 4, it is to load Nanometer Copper as the molybdenum disulfide nano sheet prepared by the inventive method embodiment 1
Particle is as the concentration of soybean oil lubricating additive and the graph of a relation of coefficient of friction.As seen from Figure 4, molybdenum disulfide nano sheet
Load nano copper particle effectively reduces the coefficient of friction of base oil.
Embodiment 2
Step 1：The thioacetamide of 0.12g sodium molybdate and 0.24g is added in 80 milliliters of deionized water simultaneously ultrasound 0.5
Homogeneous transparent liquid is prepared in h, transfers the solution into afterwards in 100 ml polytetrafluoroethyllining lining stainless steel cauldron, with
Reactor is put into convection oven afterwards, reaction temperature is arranged to 240 DEG C, the reaction time is 24 hours.Natural cooling afterwards
To room temperature, by the absolute ethyl alcohol centrifuge washing of the product in reactor, then black product is placed in vacuum drying oven and dried, is obtained
To molybdenum disulfide nano sheet.
Step 2：0.04g molybdenum disulfide is distributed in 100 ml Tris-HCL (pH=8.5) cushioning liquid and surpassed
Black liquor is prepared in sound 2h, and 0.2g Dopamine hydrochloride is added in above-mentioned solution afterwards and is stirred vigorously 12 h, is used
Product, is then distributed in 100 ml ethanol, 0.5g copper nitrate by distilled water and the repeated multiple times centrifuge washing product of ethanol
It is distributed to by magnetic agitation in above-mentioned solution.Take another beaker 0.445g sodium hypophosphites are dissolved into 30 mL ethanol it is molten
In liquid.Above two liquid is added in flask, 80 DEG C of 20 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 molybdenum disulfide nano sheet load Nanometer Copper
Particle.
Embodiment 3
Step 1：The thioacetamide of 0.12 g sodium molybdate and 0.24g is added in 80 milliliters of deionized water simultaneously ultrasound
Homogeneous transparent liquid is prepared in 0.5 h, transfers the solution into 100 ml polytetrafluoroethyllining lining stainless steel cauldron afterwards
In, then reactor is put into convection oven, reaction temperature is arranged to 240 DEG C, the reaction time is 24 hours.It is natural afterwards
Room temperature is cooled to, by the absolute ethyl alcohol centrifuge washing of the product in reactor, then black product is placed in vacuum drying oven and done
It is dry, obtain molybdenum disulfide nano sheet.
Step 2：0.1g molybdenum disulfide is distributed in 100 ml Tris-HCL (pH=8.5) cushioning liquid and ultrasonic
Black liquor is prepared in 2h, and 0.2g Dopamine hydrochloride is added in above-mentioned solution afterwards and is stirred vigorously 12 h, with steaming
Product, is then distributed in 100 ml ethanol, 0.3g copper nitrate leads to by distilled water and the repeated multiple times centrifuge washing product of ethanol
Magnetic agitation is crossed to be distributed in above-mentioned solution.Another beaker is taken 0.6g sodium hypophosphites to be dissolved into 30 mL ethanol solution.
Above two liquid is added in flask, in temperature constant magnetic stirring water-bath under stirring action 70 DEG C react 30 minutes.Take
Go out flask, carry out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained molybdenum disulfide nano sheet load nano copper particle.
Embodiment 4
Step 1：The thioacetamide of 0.12 g sodium molybdate and 0.24g is added in 80 milliliters of deionized water simultaneously ultrasound
Homogeneous transparent liquid is prepared in 0.5 h, transfers the solution into 100 ml polytetrafluoroethyllining lining stainless steel cauldron afterwards
In, then reactor is put into convection oven, reaction temperature is arranged to 240 DEG C, the reaction time is 24 hours.It is natural afterwards
Room temperature is cooled to, by the absolute ethyl alcohol centrifuge washing of the product in reactor, then black product is placed in vacuum drying oven and done
It is dry, obtain molybdenum disulfide nano sheet.
Step 2：0.1 g molybdenum disulfide is distributed in 100 ml Tris-HCL (pH=8.5) cushioning liquid and surpassed
Black liquor is prepared in sound 2h, and 0.2g Dopamine hydrochloride is added in above-mentioned solution afterwards and is stirred vigorously 12 h, is used
Product, is then distributed in 100 ml ethanol, 0.3g copper acetate by distilled water and the repeated multiple times centrifuge washing product of ethanol
It is distributed to by magnetic agitation in above-mentioned solution.Another beaker is taken 0.4g sodium borohydride to be dissolved into 30 mL ethanol solution
In.Above two liquid is added in flask, in temperature constant magnetic stirring water-bath under stirring action 70 DEG C react 30 minutes.
Flask is taken out, carries out centrifuge washing after being cooled to room temperature, vacuum drying has just obtained molybdenum disulfide nano sheet load Nanometer Copper
Grain.
Embodiment 5
Step 1：The thioacetamide of 0.12 g sodium molybdate and 0.24g is added in 80 milliliters of deionized water simultaneously ultrasound
Homogeneous transparent liquid is prepared in 0.5 h, transfers the solution into 100 ml polytetrafluoroethyllining lining stainless steel cauldron afterwards
In, then reactor is put into convection oven, reaction temperature is arranged to 240 DEG C, the reaction time is 24 hours.It is natural afterwards
Room temperature is cooled to, by the absolute ethyl alcohol centrifuge washing of the product in reactor, then black product is placed in vacuum drying oven and done
It is dry, obtain molybdenum disulfide nano sheet.
Step 2：0.1 g molybdenum disulfide is distributed in 100 ml Tris-HCL (pH=8.5) cushioning liquid and surpassed
Black liquor is prepared in sound 2h, and 0.2g Dopamine hydrochloride is added in above-mentioned solution afterwards and is stirred vigorously 12 h, is used
Product, is then distributed in 100 ml ethanol, 0.3g copper acetate by distilled water and the repeated multiple times centrifuge washing product of ethanol
It is distributed to by magnetic agitation in above-mentioned solution.Another beaker is taken 0.4g sodium borohydride to be dissolved into 30 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 molybdenum disulfide nano sheet load Nanometer Copper
Grain.
Claims (8)
1. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material, it is characterised in that including following
Step：
1）Molybdenum disulfide nano sheet is distributed in enough Tris-HCl cushioning liquid, it is 0.2-0.5 then to add concentration
Wt.% dopamine hydrochlorides, reacted at 20-25 DEG C, reaction is complete, by poly-dopamine functional graft to molybdenum disulfide
Nanometer sheet surface；
2）By step 1）Product is distributed in enough ethanol, adds soluble copper salt, and excessive reduction is added after dissolving completely
Agent, to be reacted at 75-95 DEG C, reaction is complete, mantoquita is converted into Nanometer Copper original position and loads to molybdenum disulfide nano sheet surface,
Obtain molybdenum disulfide nano sheet 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 the pH value of described Tris-HCl cushioning liquid is 8.5.
3. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material according to claim 1,
Characterized in that, described mantoquita is copper sulphate, copper chloride, copper nitrate or copper acetate.
4. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material according to claim 1,
Characterized in that, when adding soluble copper salt, the ethanol solution for the mantoquita that concentration is 0.01 ~ 0.1 mol/L is configured to.
5. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material according to claim 1,
Characterized in that, described reducing agent is sodium borohydride or sodium hypophosphite.
6. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material according to claim 1,
Characterized in that, before adding reducing agent, the ethanol solution of reducing agent is formulated as, the molar concentration for making the solution is mantoquita
1/3 ~ 1/2 times of ethanol solution.
7. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material according to claim 1,
Characterized in that, the temperature of described reduction reaction is 75-95 DEG C, the reaction time is 10-30 min.
8. a kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material according to claim 1,
Characterized in that, the preparation method of the molybdenum disulfide nano sheet is, by sodium molybdate and thioacetamide in mass ratio 1:2 dissolvings
In enough deionized waters, it is placed in the high-pressure reactor with stainless steel inner lining, hydro-thermal reaction is carried out at 240 DEG C, obtains two
Molybdenum sulfide nanometer sheet.
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| CN108478597A (en) * | 2018-03-12 | 2018-09-04 | 南京邮电大学 | A kind of molybdenum disulfide compound silver nanometer particle antiseptic and preparation method thereof of poly-dopamine modification |
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| CN111117746A (en) * | 2020-01-06 | 2020-05-08 | 北京科技大学 | Preparation of nano MoS by dopamine polymerization2-Al2O3Method for compounding rolling lubricant |
| CN113041847A (en) * | 2021-02-05 | 2021-06-29 | 中国科学院城市环境研究所 | Molybdenum disulfide oxide composite film and preparation method thereof |
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| CN113647411A (en) * | 2021-08-03 | 2021-11-16 | 江南大学 | Copper nanoparticle/molybdenum disulfide composite material and preparation method and application thereof |
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| CN108478597A (en) * | 2018-03-12 | 2018-09-04 | 南京邮电大学 | A kind of molybdenum disulfide compound silver nanometer particle antiseptic and preparation method thereof of poly-dopamine modification |
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| CN109735200A (en) * | 2018-12-10 | 2019-05-10 | 华南理工大学 | A kind of corrosion-resistant epoxy paint composition and its preparation method and application |
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| CN109943310B (en) * | 2019-04-02 | 2022-05-24 | 侯吉瑞 | Modified MoS2Nano material and preparation method thereof |
| CN111117746A (en) * | 2020-01-06 | 2020-05-08 | 北京科技大学 | Preparation of nano MoS by dopamine polymerization2-Al2O3Method for compounding rolling lubricant |
| CN113041847A (en) * | 2021-02-05 | 2021-06-29 | 中国科学院城市环境研究所 | Molybdenum disulfide oxide composite film and preparation method thereof |
| CN113621420A (en) * | 2021-07-29 | 2021-11-09 | 清华大学 | Preparation method of composite lubricating material |
| CN113647411A (en) * | 2021-08-03 | 2021-11-16 | 江南大学 | Copper nanoparticle/molybdenum disulfide composite material and preparation method and application thereof |
| CN114984309A (en) * | 2022-05-30 | 2022-09-02 | 四川大学 | Preparation method and application of amphoteric ion polymer modified nanosheet |
| CN115505439A (en) * | 2022-09-22 | 2022-12-23 | 中国科学院兰州化学物理研究所 | Surface modification method of universal micro-nano powder material |
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| CN117887257A (en) * | 2024-01-15 | 2024-04-16 | 淮北师范大学 | Preparation method of N- (hydroxyethyl) oleamide hybridized MoS 2/Ag/polydopamine nano composite particles |
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