CN112920880A - Preparation method of 2D MOFs nanosheet-based lubricant - Google Patents
Preparation method of 2D MOFs nanosheet-based lubricant Download PDFInfo
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- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
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Abstract
The invention relates to a preparation method of a 2D MOFs nanosheet-based lubricant, which comprises the following steps: preparing 2D MOFs nano-sheets by a liquid-liquid interface synthesis method; preparing the 2D MOFs nanosheet-based lubricant by grinding, stirring or ultrasonic dispersion. The invention overcomes the defect that the prior dispersity and stability of the 2D inorganic nano material in the lubricant are insufficient and industrial application is difficult to realize, the 2D MOFs consisting of organic compounds and metal ions or metal clusters has a natural organic interface, and weak molecular force action between layers of the 2D inorganic nano material is realized, so that high dispersion and stability of molecular size can be realized without modification, and the 2D inorganic nano material has the effects of friction reduction and wear resistance. The liquid/liquid interface adopted by the invention is a deionized water/base oil interface to prepare the 2D MOFs, and the synthesis condition is simple, the operation is easy, the cost is low and the quality is controllable.
Description
Technical Field
The invention relates to the technical field of preparation of nano materials, in particular to a preparation method of a 2D MOFs nanosheet-based lubricant.
Background
It is statistical that about one-third to one-half of the energy worldwide per year is consumed in various forms of frictional wear, and lubrication technology is one of the most effective ways to solve this problem. Zinc dialkyldithiophosphates (ZDDP) as antiwear additives for lubricating oils are no longer permitted to be used and added in large quantities due to the presence of harmful elements, and therefore a green lubricating oil additive capable of replacing it must be sought. With the rapid development of graphene research, other 2D nano sheet Materials with graphene-like structure, such as boron nitride, graphite oxide, and transition metal sulfides, are also receiving more and more attention [ Chen Z, Liu XW, Liu YH, et al scientific Reports,2015,5:1-7.Kumari S, Sharma OP, Gusain R, et al acs Applied Materials & Interfaces,2015,7:3708-3716 ]. These materials have excellent interlaminar shear properties, long-range order of structure and ultra-thin properties, and are candidates for excellent lubricant additives. For example, Liang et al, in-situ exfoliated graphene can improve the tribological properties of deionized water, i.e., the friction coefficient and the wear scar diameter are respectively reduced by 81.3% and 61.8% compared with deionized water [ Liang SS, Shen ZG, Yi M, et al. However, the practical application of the 2D inorganic nanosheets (graphene, boron nitride and the like) in the lubricant is seriously hindered due to aggregation or deposition of the inorganic nanosheets and natural poor interface problems with organic molecules, and the inorganic nanosheets cannot be transparently and long-term present in the lubricant even through surface organic modification, and simultaneously cause uncontrollable modification and difficult scale-up, and cannot meet the actual requirements of the lubricant on the stability and dispersibility of the additive. For example, 3, 5-di-tert-butyl-4-hydroxybenzaldehyde functionalized graphene prepared by Chouhan et al not only promotes the dispersibility in base oil, but also improves the friction-reducing and wear-resisting properties of the base oil, but is difficult to realize the mass production and the transparent long-term existence of 3, 5-di-tert-butyl-4-hydroxybenzaldehyde functionalized graphene in lubricant [ Chouhan A, Mungse HP, Sharma OP, et al. journal of color and interface science,2018,513:666 676 ]. Thus, there is a need for a two-dimensional material that can be stably dispersed in a lubricant for a long period of time without modification.
The 2D MOFs nanosheet not only has the excellent physical and chemical properties of the 2D nanosheet, but also has a natural excellent organic interface which is inevitably one of the candidates of the lubricant additive. The existing method for preparing the 2D MOFs nanosheet mainly comprises the following steps: "bottom-up" and "top-down" approaches. The 2D MOFs nanosheet prepared by the top-down method cannot avoid the limitations of complex preparation process, harsh conditions, low yield and the like. Such as Peng Y, Li YS, Ban YJ, et al, Angewandte Chemie-International Edition,2017,56: 9757-. The 2D MOFs nanosheet prepared by the bottom-up method has the problems of high cost, environmental pollution and the like which cannot be avoided. Such as Bai WS, Li SJ, Ma JP, et al, Journal of Materials Chemistry A,2019,7: 9086-.
Disclosure of Invention
The invention aims to provide a preparation method of a 2D MOFs nanosheet-based lubricant.
The invention for realizing the aim comprises the following steps:
the method comprises the following steps: under milling and ultrasonic conditions, the zinc salt is dissolved in the base oil to obtain an oil phase. Under magnetic stirring, dissolving an organic ligand in a mixed solution of an organic solvent and deionized water in a volume ratio of 1: 2-6 respectively to obtain a water phase. Dripping an oil phase into the upper layer of the water phase solution to obtain a mixed solution with obviously layered two-phase interface, reacting zinc ions in the oil phase with organic ligands in the water phase at the interface for 6-12h at 25-30 ℃, forming one or more layers of white substances at the interface, and filtering and drying the white products at the interface to obtain 2D MOFs nano-sheets; the zinc salt is zinc nitrate hexahydrate and/or zinc acetate dihydrate; the organic ligand is one of benzimidazole, 2-methylimidazole and terephthalic acid; the organic solvent is one of ethanol, N, N-dimethylformamide and methanol;
step two: and step two, preparing the 2D MOFs nanosheet-based lubricant by grinding, stirring and/or ultrasonic dispersion. Adding 0.2 wt.% to 1.0 wt.% 2D MOFs nanoplates to a base oil, vegetable oil, or grease.
In the present invention, since the metal salt and the organic ligand have different solubilities in water and an organic solvent, in order to obtain a homogeneous two-phase solution, the reactants should be completely dissolved in the solvent to prepare corresponding solutions in advance.
In the invention, because the oil phase is above the water phase in the interface synthesis process, the oil phase is added in the order of dripping into the upper layer of the water phase, and meanwhile, in order to avoid the generation of a multi-layer interface of the two phases, the oil phase is dripped along the cup wall.
In the first step of the invention, zinc nitrate hexahydrate or zinc acetate dihydrate is used as a metal source, is dissolved in an oil phase and is subjected to coordination reaction with an organic ligand in a lower water phase under the action of gravity and an interface, and a white flaky product with several layers of thickness is formed at the interface of the two phases and exists stably.
Preferably, the zinc salt in step one is zinc nitrate hexahydrate or zinc acetate dihydrate.
Preferably, the organic ligand and the organic solvent are fixed and matched in combination in the first step, namely benzimidazole/ethanol, 2-methylimidazole/methanol and terephthalic acid/N, N-dimethylformamide. The organic ligand can be dissolved in the organic solvent matched with the organic ligand.
Preferably, the volume ratio of the organic solvent to the deionized water in the reaction liquid in the first step is 1: 2-6. The primary liquid/liquid interface in the interfacial synthesis process is the water/base oil interface.
Preferably, the molar ratio of the zinc ions to the organic ligands in the reaction liquid in the first step is 1-2: 6.
Preferably, the drying temperature in the first step is 80-100 ℃, and the drying time is 16-20 h.
Preferably, the grinding time in the second step is 5min, the stirring speed is 400r/min, the stirring time is 30-60min, the ultrasonic power is 30-40kHz, and the ultrasonic time is 40-70 min.
In addition, the invention also provides research on the dispersion performance of the 2D MOFs nanosheet in base oil or vegetable oil.
The invention adopts a water/oil interface synthesis method to prepare the 2D MOFs nanosheet by adjusting the volume ratio of the organic solvent in the aqueous solution, and compared with the prior art, the method has the following advantages:
1. the problem that the 2D inorganic nano material is difficult to realize industrial application due to insufficient inherent dispersibility and stability in a lubricant is solved, the 2D MOFs consisting of organic compounds and metal ions or metal clusters has a natural organic interface, and weak molecular force action among 2D inorganic nano material layers is realized, so that high dispersion and stability of molecular size can be realized without modification, and the 2D inorganic nano material has the effects of reducing friction and resisting wear;
2. the liquid/liquid interface adopted by the invention is a deionized water/base oil interface to prepare the 2D MOFs, and the synthesis condition is simple, the operation is easy, the cost is low and the quality is controllable.
Drawings
FIG. 1 is an SEM photograph of Zn (Bim) (OAc) nanoplates obtained in example 1.
FIG. 2 shows photographs of the lubricant dispersion and Tyndall phenomenon obtained in example 1, wherein (A) is a base oil and (B) is a vegetable oil.
Fig. 3 is a TEM photograph of the 2D ZnBDC nanoplatelets obtained in example 5.
FIG. 4 is an SEM photograph of 2D ZIF-8 nanoplates obtained in example 8.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
Preparation of Zn (bim) (OAc) nanoplates
Grinding 0.657g of zinc acetate dihydrate into powder and dissolving in 30mL of base oil under ultrasonic conditions to obtain an oil phase, dissolving 2.124g of benzimidazole in 10mL of ethanol and 20mL of deionized water in a volume ratio of 1:2 to 30mL of the mixed solution to obtain an aqueous phase. Then, the oil phase solution is dripped into the upper layer of the water phase to obtain a layered reaction solution, and the layered reaction solution is stood to react for 10 hours at the temperature of 25 ℃. After the reaction, a white film was formed at the interface between the two phases, and a white film was obtained as the intermediate layer by filtration, dried in an air-blast drying oven at 85 ℃ for 17 hours, and ground to collect a white powder.
As shown in the SEM photograph of FIG. 1, the thickness of the Zn (Bim) (OAc) nanosheets obtained by the preparation is about 3-4 nm.
0.08g of Zn (Bim) (OAc) nanosheets are weighed into 20g of 150SN base oil, and the base oil is placed in an ultrasonic cleaner with ultrasonic power of 40kHz for ultrasonic 45min to obtain the Zn (Bim) (OAc) nanosheet-base oil lubricant. Weighing 0.08g of Zn (Bim) (OAc) nanosheets, adding the nanosheets into 20g of vegetable oil, pouring the mixture into a mortar for grinding for 5min, then magnetically stirring for 35min under the condition that the stirring speed is 300-400r/min, and finally placing the lubricant into an ultrasonic cleaner with the ultrasonic power of 40kHz for ultrasonic treatment for 45min to obtain the Zn (Bim) (OAc) nanosheet-vegetable oil lubricant. Weighing 0.08g of Zn (bim) (OAc) nanosheet, adding into 20g of lubricating grease, pouring into a mortar, and grinding for 5min to obtain Zn (bim) (OAc) nanosheet-lubricating grease lubricant. So as to obtain various uniformly dispersed lubricants, and finally, carrying out a friction and wear test on a multifunctional friction and wear testing machine under the test conditions of 3Hz frequency and 30N load.
As shown in the lubricant dispersion photograph of fig. 2, it is known that zn (bim) (oac) nanosheets can be stably dispersed in the base oil for 150 days.
Examples 2 to 3
0.657g of zinc acetate dihydrate was ground into a powder and dissolved in 30mL of base oil under ultrasonic conditions to obtain an oil phase, and 2.124g of benzimidazole was dissolved in ethanol and deionized water at a volume ratio of 1:3 and 1: 6 to 30mL of the mixed solution to obtain an aqueous phase. Then, the oil phase solution is dripped into the upper layer of the water phase to obtain a layered reaction solution, and the layered reaction solution is stood to react for 10 hours at the temperature of 25 ℃. After the reaction, a white film was formed at the interface between the two phases, and a white film was obtained as the intermediate layer by filtration, dried in an air-blast drying oven at 85 ℃ for 17 hours, and ground to collect a white powder.
A Zn (Bim) (OAc) nanoplatelet lubricant was prepared as in example 1.
In examples 2 and 3, Zn (Bim) (OAc) nanoplatelets base lubricant can be stably dispersed in base oil for 100-120 days, and can be stably dispersed in vegetable oil for only 20-30 days.
Comparative example 1
0.657g of zinc acetate dihydrate was ground into a powder and dissolved in 30mL of base oil under sonication to obtain an oil phase, and 2.124g of benzimidazole was dissolved in 30mL of deionized water to obtain an aqueous phase. Then, the oil phase solution is dripped into the upper layer of the water phase to obtain a layered reaction solution, and the layered reaction solution is stood to react for 10 hours at the temperature of 25 ℃. After the reaction, no white film was formed at the interface between the two phases.
The following table shows the effect of the volume ratio of ethanol to water on zn (bim) (oac) nanoplate thickness, dispersibility, stability and friction performance.
From the above table, it can be seen that the thickness of the zn (bim) (oac) nanosheet prepared at a volume ratio of ethanol to deionized water of 1:2 is the thinnest, the dispersion stability in the base oil is the best (stable dispersion for 150 days) and the antifriction effect is the best.
Examples 4 to 6:
preparation of 2D ZnBDC nanosheet
0.595g of zinc nitrate hexahydrate is ground into powder and dissolved in 30mL of base oil under ultrasonic conditions to obtain an oil phase, and 1.992g of terephthalic acid is dissolved in N, N-dimethylformamide and deionized water according to the volume ratio of 1: 2. 1:3 and 1: 6 to 30mL of the mixed solution to obtain an aqueous phase. Then, the oil phase solution is dripped into the upper layer of the water phase to obtain a layered reaction solution, and the layered reaction solution is stood to react for 10 hours at the temperature of 25 ℃. And after the reaction is finished, generating a white film at the interface of two phases, filtering to obtain a white film in the middle layer, drying for 17 hours in an air drying oven at 85 ℃, and collecting the white powder 2D ZnBDC nanosheet after grinding.
As shown in the TEM photograph of fig. 3, the thickness of the 2D ZnBDC nanosheets obtained from example 5 was about 3-4 nm.
0.08g of 2D ZnBDC nanosheet is weighed and added into 20g of 150SN base oil, and then the base oil is placed in an ultrasonic cleaner with ultrasonic power of 40kHz and subjected to ultrasonic treatment for 45min to obtain the 2D ZnBDC nanosheet-base oil lubricant. Weighing 0.08g of 2D ZnBDC nanosheet, adding the 2D ZnBDC nanosheet into 20g of vegetable oil, pouring the mixture into a mortar for grinding for 5min, then magnetically stirring for 35min under the condition that the stirring speed is 300-400r/min, and finally placing the lubricant into an ultrasonic cleaner with the ultrasonic power of 40kHz for ultrasonic treatment for 45min to obtain the 2D ZnBDC nanosheet-vegetable oil lubricant. 0.08g of 2D ZnBDC nanosheet is weighed and added into 20g of lubricating grease, and the mixture is poured into a mortar to be ground for 5min, so that the 2D ZnBDC nanosheet-lubricating grease lubricant is obtained. So as to obtain various uniformly dispersed lubricants, and finally, carrying out a friction and wear test on a multifunctional friction and wear test machine under the test conditions of 3Hz frequency and 30N load.
In example 5, the 2D ZnBDC nanosheet has the best dispersibility in the base oil and can be stably dispersed for 150 days.
The following table shows the effect of the volume ratio of N, N-dimethylformamide to deionized water on the 2D ZnBDC nanoplatelets and the tribological properties.
As can be seen from the table above, the thickness of the 2D ZnBDC nanosheet prepared when the volume ratio of the N, N-dimethylformamide to the deionized water is 1:3 can reach 3-4nm, and the 2D ZnBDC nanosheet has the best dispersion stability (stable dispersion for 150 days) and friction reduction effect in the base oil.
Examples 7 to 9:
preparation of 2D ZIF-8 nanosheets
0.891g of zinc nitrate hexahydrate is ground into powder and dissolved in 30mL of base oil under ultrasonic conditions to obtain an oil phase, and 1.476g of 2-methylimidazole is dissolved in methanol and deionized water at a volume ratio of 1: 2. 1:3 and 1: 6 to 30mL of the mixed solution to obtain an aqueous phase. Then, the oil phase solution is dripped into the upper layer of the water phase to obtain a layered reaction solution, and the layered reaction solution is stood to react for 10 hours at the temperature of 25 ℃. And after the reaction is finished, generating a white film at the interface of the two phases, filtering to obtain a white film at the middle layer, drying for 17 hours in an air drying oven at 85 ℃, and collecting white powder 2D ZIF-8 after grinding.
As shown in the SEM photograph of fig. 4, the thickness of the 2D ZIF-8 nanosheets obtained from example 8 was about 8-10 nm.
0.08g of 2D ZIF-8 nanosheet is weighed and added into 20g of 150SN base oil, and then the mixture is placed in an ultrasonic cleaner with ultrasonic power of 40kHz and subjected to ultrasonic treatment for 45min to obtain the 2D ZIF-8 nanosheet-base oil lubricant. Weighing 0.08g of 2D ZIF-8 nanosheet, adding the 2D ZIF-8 nanosheet into 20g of vegetable oil, pouring the mixture into a mortar for grinding for 5min, then magnetically stirring for 35min under the condition that the stirring speed is 300-400r/min, and finally placing the lubricant in an ultrasonic cleaner with the ultrasonic power of 40kHz for ultrasonic 45min to obtain the 2D ZIF-8 nanosheet-vegetable oil lubricant. 0.08g of 2D ZIF-8 nanosheet is weighed and added into 20g of lubricating grease, and the mixture is poured into a mortar to be ground for 5min, so that the 2D ZIF-8 nanosheet-lubricating grease lubricant is obtained. So as to obtain various uniformly dispersed lubricants, and finally, carrying out a friction and wear test on a multifunctional friction and wear testing machine under the test conditions of 3Hz frequency and 30N load.
In example 7, the 2D ZIF-8 nanosheet has the best dispersibility in the base oil and can be stably dispersed for 150 days.
The following table shows the effect of the volume ratio of methanol to deionized water on the 2D ZIF-8 nanosheet and friction performance.
As can be seen from the above table, the thickness of the 2D ZIF-8 nanosheet prepared when the volume ratio of ethanol to deionized water is 1:2 is the thinnest, the dispersion stability in the base oil is the best (stable dispersion for 150 days) and the friction reduction effect is the best.
The invention conception and principle of the invention are: an interface formed by two immiscible fluids is used as an incoherent reaction environment formed by the 2D MOFs nano-sheets, so that the reaction is essentially limited to the interface to form the 2D MOFs nano-sheets. And simultaneously, in order to solve the problem of an interface between the 2D MOFs nanosheet and lubricating oil and synthesize the 2D MOFs nanosheet with oil solubility, base oil is selected as oil in an oil phase. Firstly, dissolving a metal source in oil to form an oil phase, and dissolving an organic ligand which is not dissolved in water through an organic solvent to form a water phase; and then placing the oil phase on the water phase, and enabling the metal source to diffuse at the interface of the oil phase and the water phase to contact with the organic ligand to perform a coordination reaction to form a continuous and uniform 2D MOFs nano-sheet. And finally, adding the 2D MOFs nanosheets into base oil or vegetable oil or lubricating grease for a dispersion stability test and a friction performance test to obtain the 2D MOFs nanosheet base lubricant with excellent stable dispersibility.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (8)
1. A preparation method of a 2D MOFs nanoplatelet-based lubricant is characterized by comprising the following steps:
step one, preparing 2D MOFs nano-sheets by a liquid-liquid interface synthesis method; firstly, dissolving zinc salt ground into powder in base oil through ultrasound to form an oil phase, then dissolving an organic ligand in a mixed solution of organic solvents and deionized water with different volume ratios through magnetic stirring to form a water phase, and then dropping the oil phase into the upper layer of the water phase solution, wherein the water phase and the oil phase have an obvious boundary line; reacting zinc ions in an oil phase and an organic ligand in a water phase at the temperature of 25-30 ℃ at an interface for 6-12h to form one or more layers of white substances at the interface, and filtering and drying a white product at the interface to obtain a 2D MOFs nano-sheet;
step two, preparing the 2D MOFs nanosheet-based lubricant by grinding, stirring or ultrasonic dispersion; adding 0.2 wt.% to 1.0 wt.% 2D MOFs nanoplates to a base oil, vegetable oil, or grease.
2. The method of claim 1, wherein in step one, the zinc salt is zinc nitrate hexahydrate or zinc acetate dihydrate.
3. The method for preparing a 2D MOFs nanoplatelet lubricant according to claim 1, wherein in the first step, the volume ratio of the oil phase to the water phase is 1: 1.
4. The method of claim 1, wherein in the first step, the fixed combination of organic ligand and organic solvent is benzimidazole/ethanol, 2-methylimidazole/methanol or terephthalic acid/N, N-dimethylformamide.
5. The method for preparing a 2D MOFs nanoplatelet-based lubricant according to claim 1, wherein in the first step, the volume ratio of the organic solvent to the deionized water in the reaction solution is 1: 2-6.
6. The method for preparing a 2D MOFs nanoplatelet lubricant according to claim 1, wherein in the first step, the molar ratio of zinc ions to organic ligands in the reaction solution is 1-2: 6.
7. The method for preparing a 2D MOFs nanoplatelet lubricant according to claim 1, wherein in the first step, the drying temperature is 80-100 ℃ and the drying time is 16-20 h.
8. The method for preparing 2D MOFs nanoplatelet-based lubricant according to claim 1, wherein in the second step, the grinding time is 5min, the stirring speed is 300-400r/min, the stirring time is 30-60min, the ultrasonic power is 30-40kHz, and the ultrasonic time is 40-70 min.
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| CN111500341A (en) * | 2020-04-12 | 2020-08-07 | 西北工业大学 | Preparation method of DDP modified zirconium-based metal organic framework lubricating oil additive |
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| CN115386408A (en) * | 2022-07-21 | 2022-11-25 | 扬州大学 | ZIF-7/2D Ni-BDC nano composite lubricating material and preparation method thereof |
| CN115537247A (en) * | 2022-10-08 | 2022-12-30 | 晏翔 | Wear-resistant additive, wear-resistant lubricating oil and preparation method |
| CN115785459A (en) * | 2022-07-22 | 2023-03-14 | 扬州大学 | Preparation method of 2D ZnBDC MOFs nano lubricating material |
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