CN115785459A - Preparation method of 2D ZnBDC MOFs nano lubricating material - Google Patents
Preparation method of 2D ZnBDC MOFs nano lubricating material Download PDFInfo
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- CN115785459A CN115785459A CN202210874448.0A CN202210874448A CN115785459A CN 115785459 A CN115785459 A CN 115785459A CN 202210874448 A CN202210874448 A CN 202210874448A CN 115785459 A CN115785459 A CN 115785459A
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Abstract
The invention discloses a preparation method of a 2D ZnBDC MOFs nano lubricating material, which comprises the following steps: the invention provides an MOF nano lubricating material and a preparation method thereof, and the MOF nano lubricating material has adjustable structure and function, large surface area and ultrahigh porosity, has weak interlayer molecular force action in the structure, screens and prepares 2DMOFs with excellent oil solubility as a lubricating oil additive, and has profound significance for solving a plurality of scientific problems of 2D nano materials in a lubricating agent and realizing application.
Description
Technical Field
The invention belongs to the technical field of nano lubricating materials, and particularly relates to a preparation method of a 2D ZnBDC MOFs nano lubricating material.
Background
With the rapid development of modern technology, the energy consumed by frictional contact accounts for about 23% of the total global energy consumption, of which 20% is generated by friction and 3% is related to wear, and these friction and wear are derived from various aspects of mechanical technology, transportation, aerospace and daily life. Therefore, it would be economically advantageous to reduce or even eliminate the friction and wear generated by various moving mechanical systems. The advanced lubrication technology greatly reduces the abrasion loss of a mechanical system, reduces the occurrence of malignant accidents of mechanical equipment and prolongs the service life of the machinery. Lubricants are effective materials for controlling friction and wear, lubricant additives are effective methods for improving performance, and current complex lubricants generally contain both base oils and additives. The additive is present in a minor proportion but plays a key role in imparting new properties or compensating for the disadvantages in the base oil. There is a need to develop high-end lubricant additives with low toxicity, environmental friendliness, high performance, and versatility.
Compared to traditional metal organic lubricant additives such as molybdenum dithiocarbamate (MoDTC) and zinc dialkyldithiophosphate (ZDDP), 2D inorganic nanomaterials (graphene, fluorinated graphene, boron nitride, molybdenum disulfide, etc.) have advantages in reduced friction and wear performance as well as environmental sustainability. However, the high density, easy aggregation and uncontrollable size and morphology preparation of 2D inorganic nanomaterials in base oils prevents their practical application as additives in liquid lubricants.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of a 2D ZnBDC MOFs nano lubricating material.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a 2D ZnBDC MOFs nano lubricating material comprises the following steps:
dissolving: dissolving zinc salt and terephthalic acid in a water-organic solvent;
high-temperature reaction: transferring the mixture solution prepared by dissolving into a stainless steel autoclave lined with Teflon, placing the stainless steel autoclave into a homogeneous reactor for reaction, and then collecting white precipitate through centrifugation;
purification, washing and drying: and purifying the obtained white precipitate, washing by using an organic solvent, and drying after washing to obtain the product 2D ZnBDC nanosheet.
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: in solution, the zinc salt is Zn (NO) 3 ) 2 ·6H 2 O。。
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: in the dissolution, the water-organic solvent is water and DMF.
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: in the high temperature reaction, the mixture solution was stirred at 10rpm and heated at 140 ℃ for 24 hours.
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: in the purification, washing and drying, washing with an organic solvent was performed as DMF and methanol.
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: in the purification, washing and drying, the drying conditions are as follows: drying at 60 deg.C for 12h.
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: zinc salts, by weight: terephthalic acid (H) 2 BDC)=5~5.5:1。
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: water by volume: DMF =0 to 5.
In purification, washing and drying, the DMF: methanol = 0.5-2:1, and the number of washing times is 3.
As a preferred scheme of the preparation method of the 2D ZnBDC MOFs nano lubricating material, the preparation method comprises the following steps: the prepared 2D ZnBDC nanosheet is used for preparing a lubricant containing 2D ZnBDC MOFs.
The invention provides an MOF nano lubricating material and a preparation method thereof, which can have adjustable structure and function, large surface area and ultrahigh porosity, have weak interlayer molecular force action in the structure, screen and prepare 2D MOFs with excellent oil solubility as a lubricating oil additive, and have profound significance for solving a plurality of scientific problems (dispersibility, stability, interface problems and the like) of 2D nano materials in a lubricant and realizing application.
The invention also has the following effects:
(1) The application provides a 2D ZnBDC MOFs nanosheet prepared by using deionized water as a modulator and through a novel surfactant from bottom to top in a mediated manner, and the preparation method is simple, environment-friendly and cost-saving.
(2) Compared with other 2D nano materials, the 2D ZnBDC MOFs nanosheet prepared by taking deionized water as a modulator through a novel surfactant from bottom to top in a mediated mode has the advantages that the 2D MOFs nanosheet not only has a graphene-like periodic network structure, but also has an organic composition similar to a lubricant, a natural organic interface exists between the 2D MOFs nanosheet and lubricating oil, and the 2D MOFs nanosheet has good performance as a lubricant adding material.
(3) The application provides a 2D ZnBDC MOFs nanosheet prepared by taking deionized water as a modulator and through a novel surfactant from bottom to top in a mediated mode, when the nanosheet is added as a lubricant addition material, the average friction coefficient and the wear loss are respectively reduced by 16.7% and 20%.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a chemical equation for the synthesis of 2D ZnBDC nanoplates of the present invention;
FIG. 2 is SEM and TEM images of ZnBDC products of examples 1-6 of the present invention;
FIG. 3 shows (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (λ ex =340 nm) of ZnBDC product of examples 1-6 of the present invention;
FIG. 4 is an AFM analysis of ZnBDC as a product of example 3 of the invention;
FIG. 5 is a graph of the time-dependent dispersion of (A) 2D ZnBDC-base oil (100 SN) in example 10 of the present invention; (B) 2D ZnBDC (1.00 wt.%) -concentration change in base oil;
FIG. 6 is the COF curve (A), average COF and average wear volume (B) at 8N for 2D ZnBDC base oils in examples 7-10 of the invention; base oil and 2D ZnBDC-COF curve (C), average COF and Average Wear Scar Diameter (AWSD) (D) at 100N for base oil;
FIG. 7 is the average COF and average wear volume (or AWSD) for 2D ZnBDC base oils at different loads (ball-to-slider mode (A, B) and ball-to-ball mode (C, D)) in examples 7-10 of the invention;
FIG. 8 is the average COF and average wear volume (or AWSD) of neat oil and 2D ZnBDC-base oil at different frequencies (or speeds) with the base oil (ball-to-slipper mode (A, B) and ball-to-ball mode (C, D)) in example 8 of this invention;
fig. 9 is an optical profile of wear marks, a depth cross-section plot and a 3D profile of the base oil (a), 2D ZnBDC (0.05 wt.%) -base oil (B), 2D ZnBDC (0.10 wt.%) -base oil (C), 2D ZnBDC (0.50 wt.%) -base oil (D) and 2D ZnBDC (1.00 wt.%) -base oil (E) rubbed at a frequency of 2Hz and a load of 10N in examples 7-10 of the present invention;
FIG. 10 is a cross-sectional plot of the optical profile and depth of the wear scar rubbed at 1200r/min and 150N load for base oil (A) and 2D ZnBDC (0.1 wt.%) -base oil (B) in example 8 of the present invention;
FIG. 11 is a Raman spectrum of (A) the wear surfaces of 2D ZnBDC and GGr15 bearing steel balls in examples 7-10 of the present invention; (B) Raman spectra of base oil and 2D ZnBDC-base oil on the wear surface of a GGr15 bearing steel ball; (C) Base oil (100 SN) and 2D ZnBDC-contact angle of base oil on 304 stainless steel.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
2.6774g Zn (NO) 3 ) 2 ·6H 2 O and 0.4980g terephthalic acid (H) 2 BDC) was dissolved in the mixed solvent (0 mL H) 2 O and 80mL DMF).
The mixture solution was transferred to a teflon-lined stainless autoclave and placed in a homogeneous reactor at 10 r.p.m. and 140 ℃ for 24 hours, and then centrifuged at 3000rpm for 10min to collect a white precipitate.
The white precipitate was purified and washed by at least 3 washes by immersion in DMF (25 mL each) followed by methanol (MeOH, 25mL each). Finally, the washed nanoplatelets were dried at 60 ℃ for 12h. And obtaining the product 2D ZnBDC nanosheet. The chemical equation for the synthesis of the product is shown in FIG. 1, and the SEM and TEM images are shown in FIG. 2, and (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (. Lamda.ex =340 nm) are shown in FIG. 3.
Example 2
2.6774g Zn (NO) 3 ) 2 ·6H 2 O and 0.4980g terephthalic acid (H) 2 BDC) was dissolved in the mixed solvent (10 mL H) 2 O and 70mL DMF).
The mixture solution was transferred to a teflon-lined stainless steel autoclave and placed in a homogeneous reactor at 10 r.p.m. and 140 c for reaction for 24 hours, and then centrifuged at 3000rpm for 10min to collect a white precipitate.
The white precipitate was purified and washed by at least 3 washes by immersion in DMF (25 mL each) followed by methanol (MeOH, 25mL each). Finally, the washed nanoplatelets were dried at 60 ℃ for 12h. And obtaining the product 2D ZnBDC nanosheet. The chemical equation of the synthesis of the product is shown in FIG. 1, and the SEM and TEM images are shown in FIG. 2, and (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (. Lamda.ex =340 nm) are shown in FIG. 3.
Example 3
2.6774g Zn (NO) 3 ) 2 ·6H 2 O and 0.4980g terephthalic acid (H) 2 BDC)(H 2 BDC) was dissolved in the mixed solvent (20 mL H) 2 O and 60mL DMF).
The mixture solution was transferred to a teflon-lined stainless steel autoclave and placed in a homogeneous reactor at 10 r.p.m. and 140 c for reaction for 24 hours, and then centrifuged at 3000rpm for 10min to collect a white precipitate.
The white precipitate was purified and washed by at least 3 washes by immersion in DMF (25 mL each) followed by methanol (MeOH, 25mL each). Finally, the washed nanoplatelets were dried at 60 ℃ for 12h. And obtaining the product 2D ZnBDC nanosheet. The chemical equation for the synthesis of the product is shown in FIG. 1, the SEM and TEM images are shown in FIG. 2, (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (. Lamda.ex =340 nm) are shown in FIG. 3, and the AFM analysis is shown in FIG. 4.
Example 4
2.6774g Zn (NO) 3 ) 2 ·6H 2 O and 0.4980g terephthalic acid (H) 2 BDC) was dissolved in the mixed solvent (30 mL H) 2 O and 50mL DMF).
The mixture solution was transferred to a teflon-lined stainless steel autoclave and placed in a homogeneous reactor at a rotation speed of 10 r.p.m. and a temperature of 140 ℃ for reaction for 24 hours, and then centrifuged at 3000rpm for 10min to obtain a white precipitate.
The white precipitate was purified and washed by at least 3 washes by immersion in DMF (25 mL each) followed by methanol (MeOH, 25mL each). Finally, the washed nanoplatelets were dried at 60 ℃ for 12h. And obtaining the product 2D ZnBDC nanosheet. The chemical equation for the synthesis of the product is shown in FIG. 1, and the SEM and TEM images are shown in FIG. 2, and (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (. Lamda.ex =340 nm) are shown in FIG. 3.
Example 5
2.6774g Zn (NO) 3 ) 2 ·6H 2 O and 0.4980g terephthalic acid (H) 2 BDC) was dissolved in the mixed solvent (40 mL H) 2 O and 40mL DMF).
The mixture solution was transferred to a teflon-lined stainless steel autoclave and placed in a homogeneous reactor at a rotation speed of 10 r.p.m. and a temperature of 140 ℃ for reaction for 24 hours, and then centrifuged at 3000rpm for 10min to obtain a white precipitate.
The white precipitate was purified and washed at least 3 times with DMF (25 mL each) and methanol (MeOH, 25mL each) in that order. Finally, the washed nanoplatelets were dried at 60 ℃ for 12h. And obtaining the product 2D ZnBDC nanosheet. The chemical equation for the synthesis of the product is shown in FIG. 1, and the SEM and TEM images are shown in FIG. 2, and (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (. Lamda.ex =340 nm) are shown in FIG. 3.
Example 6
2.6774g Zn (NO) 3 ) 2 ·6H 2 O and 0.4980g terephthalic acid (H) 2 BDC) was dissolved in the mixed solvent (50 mL H) 2 O and 30mL DMF).
The mixture solution was transferred to a teflon-lined stainless steel autoclave and placed in a homogeneous reactor at 10 r.p.m. and 140 ℃ for reaction for 24 hours, followed by centrifugation at 3000rpm for 10min to give a white precipitate.
The white precipitate was purified and washed by at least 3 washes by immersion in DMF (25 mL each) followed by methanol (MeOH, 25mL each). Finally, the washed nanosheets were dried at 60 ℃ for 12h. And obtaining the product 2D ZnBDC nanosheet. The chemical equation for the synthesis of the product is shown in FIG. 1, and the SEM and TEM images are shown in FIG. 2, and (A) XRD spectrum, (B) FT-IR spectrum, (C) Raman spectrum and (D) PL spectrum (. Lamda.ex =340 nm) are shown in FIG. 3.
Example 7
For the processes of the 2D ZnBDC nanoplates prepared in examples 1-6, the solvent is fundamentally an important factor affecting the nucleation and growth rate of the 2D MOFs particles. Therefore, the ratio of H2O to DMF is typically used to adjust the particle size of MOFs, as H2O affects the degree of deprotonation of the acid ligands. The morphology of ZnBDC (0:8) shows a bulk structure with a multilayer structure and consists of randomly stacked nanosheets. However, as the proportion of water increases, the morphology of ZnBDC has significant changes, namely the disappearance of the multilayer structure and the presence of few-layer nanoplatelets. The few-layered nanoplatelets have an irregular shape and a more transparent degree than ZnBDC (0:8). With further increase in water ratio, the rapid nucleation due to the higher polarity of water and morphology of small crystalline poly ZnBDC (5:3) restored the multilayer structure. Atomic force microscopy results showed that +2D ZnBDC (2:6) had few layers of nanoplatelet character, a thickness of about 5nm, and a yield of 54%. Has advantages over other ratios.
In summary, the greater the proportion of 2D ZnBDC in the oil, the thinner its thickness, the longer the settling time required.
The product 2D ZnBDC nanosheet obtained in example 3 was taken and placed in 100SN mineral oil, and the addition amount of the 2D ZnBDC nanosheet was (0.05 wt.%).
And (3) putting the mixed oil into a water bath container for ultrasonic dispersion treatment, wherein the ultrasonic treatment parameter is 300W for 4h, and taking out for later use after the ultrasonic treatment is finished.
And performing friction test by a reciprocating slide block tester. The friction pair adopts a GGr15 bearing steel ball with the diameter of 6mm and a 304 stainless steel slide block (with the length of 30mm, the width of 15mm and the height of 4 mm), and petroleum ether and ethanol are used for 300W ultrasonic cleaning for 10min before the friction test.
The coefficient of friction (COF) was obtained by a relative reciprocal sliding test on a friction pair with a one-way stroke length of 1.5mm and a load of 10N for 30min. Repeating for three times. The coefficients of friction are shown in FIGS. 6-7.
After the friction test, a detailed topography map of the macroscopic surface morphology (wear scar width and wear depth) of the steel ball and the slide block was measured using a 3D laser scanning microscope as shown in fig. 9.
A four-ball friction tester was used to determine the relative wear resistance of the lubricant in ball-ball mode. The friction tester consists of four balls, namely three fixed steel balls and one rotating ball. AISI GGr15 steel balls of 12.7 mm diameter were used. The top ball (fourth ball) was rotated at 1200rpm for 6 hours at room temperature. Each test was repeated three times. After the test is finished, the diameter of the grinding crack is measured by an optical microscope, and the Raman spectrum and the contact angle of the lubricating oil on 304 stainless steel are shown in FIG. 11.
Example 8
The product 2D ZnBDC nanosheet obtained in example 3 was taken and placed in 100SN mineral oil, and the addition amount of the 2D ZnBDC nanosheet was (0.10 wt.%).
And (3) putting the mixed oil into a water bath container for ultrasonic dispersion treatment, wherein the ultrasonic treatment parameter is 300W for 4h, and taking out for later use after the ultrasonic treatment is finished.
And performing friction test by a reciprocating slide block tester. The friction pair adopts a GGr15 bearing steel ball with the diameter of 6mm and a 304 stainless steel slide block (with the length of 30mm, the width of 15mm and the height of 4 mm), and petroleum ether and ethanol are used for 300W ultrasonic cleaning for 10min before the friction test.
The coefficient of friction (COF) was obtained by a relative reciprocal sliding test on a friction pair with a one-way stroke length of 1.5mm and a load of 10N for 30min. Repeating for three times. The coefficients of friction are shown in FIGS. 6-7, and the COF at different frequencies is shown in FIG. 8.
After the friction test, a detailed topography map of the macroscopic surface morphology (wear scar width and wear depth) of the steel ball and the slider was measured using a 3D laser scanning microscope as shown in fig. 9.
A four-ball friction tester was used to determine the relative wear resistance of the lubricant in ball-ball mode. The friction tester consists of four balls, namely three fixed steel balls and one rotating ball. AISI GGr15 steel balls 12.7 mm in diameter were used. The top ball (fourth ball) was rotated at 1200rpm for 6 hours at room temperature. Each test was repeated three times. After the test is finished, the diameter of the grinding mark is measured by an optical microscope, the optical appearance and the depth cross section curve chart of the grinding mark are shown in figure 10, and the Raman spectrum and the contact angle of the lubricating oil on 304 stainless steel are shown in figure 11.
Example 9
The product 2D ZnBDC nanosheet obtained in example 3 was taken and placed in 100SN mineral oil, and the addition amount of the 2D ZnBDC nanosheet was (0.50 wt.%).
And (3) putting the mixed oil into a water bath container for ultrasonic dispersion treatment, wherein the ultrasonic treatment parameter is 300W for 4h, and taking out for later use after the ultrasonic treatment is finished.
And performing friction test by a reciprocating slide block tester. The friction pair adopts a GGr15 bearing steel ball with the diameter of 6mm and a 304 stainless steel slide block (with the length of 30mm, the width of 15mm and the height of 4 mm), and petroleum ether and ethanol are used for 300W ultrasonic cleaning for 10min before the friction test.
The coefficient of friction (COF) was obtained by a relative reciprocating sliding test on a friction pair with a one-way stroke length of 1.5mm and a load of 10N for 30min. Repeating for three times. The coefficients of friction are shown in FIGS. 6-7.
After the friction test, a detailed topography map of the macroscopic surface morphology (wear scar width and wear depth) of the steel ball and the slide block was measured using a 3D laser scanning microscope as shown in fig. 9.
A four-ball friction tester was used to determine the relative wear resistance of the lubricant in ball-ball mode. The friction tester consists of four balls, namely three fixed steel balls and one rotating ball. AISI GGr15 steel balls 12.7 mm in diameter were used. The top ball (fourth ball) was rotated at 1200rpm for 6 hours at room temperature. Each test was repeated three times. After the test is finished, the diameter of the grinding crack is measured by an optical microscope, and the Raman spectrum and the contact angle of the lubricating oil on 304 stainless steel are shown in FIG. 11.
Example 10
The product 2D ZnBDC nanosheet obtained in example 3 was placed in 100SN mineral oil with the 2D ZnBDC nanosheet added in an amount of (1.00 wt.%).
And (3) putting the mixed oil into a water bath container for ultrasonic dispersion treatment, wherein the ultrasonic treatment parameter is 300W for 4h, taking out for later use after the ultrasonic treatment is finished, and the dispersion picture is shown as 5.
And performing friction test by a reciprocating slide block tester. The friction pair adopts a GGr15 bearing steel ball with the diameter of 6mm and a 304 stainless steel slide block (with the length of 30mm, the width of 15mm and the height of 4 mm), and petroleum ether and ethanol are used for 300W ultrasonic cleaning for 10min before the friction test.
The coefficient of friction (COF) was obtained by a relative reciprocal sliding test on a friction pair with a one-way stroke length of 1.5mm and a load of 10N for 30min. Repeating for three times. The coefficients of friction are shown in FIGS. 6-7.
After the friction test, a detailed topography map of the macroscopic surface morphology (wear scar width and wear depth) of the steel ball and the slide block was measured using a 3D laser scanning microscope as shown in fig. 9.
A four-ball friction tester was used to determine the relative wear resistance of the lubricant in ball-ball mode. The friction tester consists of four balls, namely three fixed steel balls and one rotating ball. AISI GGr15 steel balls 12.7 mm in diameter were used. The top ball (fourth ball) was rotated at 1200rpm for 6 hours at room temperature. Each test was repeated three times. After the test is finished, the diameter of the grinding crack is measured by an optical microscope, and the Raman spectrum and the contact angle of the lubricating oil on 304 stainless steel are shown in FIG. 11.
In conclusion, the 2D ZnBDC MOFs nanosheet is successfully prepared by using deionized water as a modulating agent and using a surfactant modulating method, and the frictional wear behavior of the prepared lubricant in reciprocating ball-slide block and ball-ball modes is comprehensively researched.
(1) 2D ZnBDC (2:6) MOFs nanosheets with the thickness of about 5nm are successfully synthesized through characteristics such as SEM, TEM, XRD, FT-IR, raman, PL spectrum and AFM, and deprotonation of H2O is proposed to adjust longitudinal size change of ZnBDC MOFs.
(2) The dispersion and stability performance of 2D ZnBDC in base oil was tested by weighing method, and the results showed that the better natural dispersion of 2D ZnBDC in oil could be attributed to the interfacial interaction between the organic surface of 2D ZnBDC and the oil molecules.
(3) In the ball-sliding block friction mode, the friction coefficient of the 2D ZnBDC-base oil is higher than that of the base oil in the addition amount range, and the abrasion loss is lower than that of the base oil. With the increase of the addition amount, the friction coefficient of the 2D ZnBDC-base oil firstly decreases and then increases, the optimal addition amount is 0.05wt.%, and the abrasion loss continuously decreases until the abrasion loss decreases to 29%.
(4) In the ball-and-ball friction mode, the friction coefficient and the wear amount of the 2D ZnBDC-base oil were decreased and then increased as the addition amount was increased, and the average friction coefficient and the wear amount were decreased by 16.7% and 20% respectively at the optimum addition amount of 0.05 wt.%.
Different 2D ZnBDC nanosheets adopted in examples 7-10 have different sedimentation properties at different proportions, partial sedimentation is achieved within two days of 2D ZnBDC (0.05 wt.%), and complete sedimentation is achieved after seven days; partial sedimentation was achieved within two days of 2D ZnBDC (0.10 wt.%), and complete sedimentation was achieved seven days later, with slightly longer sedimentation times than described above; no sedimentation was achieved within two days of 2D ZnBDC (0.50 wt.%), and after seven days; no sedimentation was achieved within two days of 2D ZnBDC (1.00 wt.%), and after seven days; in summary, the greater the proportion of 2D ZnBDC in the oil, the thinner its thickness, the longer the settling time required.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a 2D ZnBDC MOFs nano lubricating material is characterized by comprising the following steps: the method comprises the following steps:
dissolving: dissolving zinc salt and terephthalic acid in a water-organic solvent;
high-temperature reaction: transferring the mixture solution prepared by dissolving into a stainless steel autoclave lined with Teflon, placing the stainless steel autoclave into a homogeneous reactor for reaction, and then collecting white precipitate through centrifugation;
purification, washing and drying: and purifying the obtained white precipitate, washing by using an organic solvent, and drying after washing to obtain the product 2D ZnBDC nanosheet.
2. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1, characterized in that: in the dissolving, the zinc salt is Zn (NO) 3 ) 2 ·6H 2 O。
3. The process for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1 or 2, characterized in that: in the dissolving, the water-organic solvent is water and DMF.
4. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1, characterized in that: in the high-temperature reaction, the mixture solution was stirred at 10rpm and heated at 140 ℃ for 24 hours.
5. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1, characterized in that: in the purification, washing and drying, the washing with an organic solvent is DMF and methanol.
6. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1, characterized in that: in the purification, washing and drying, the drying conditions are: drying at 60 deg.C for 12h.
7. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1, characterized in that: the zinc salt is selected from the following components in percentage by weight: terephthalic acid (H) 2 BDC)=5~5.5:1。
8. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 3, characterized in that: by volume, the water: DMF =0 to 5.
9. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 5, wherein the method comprises the following steps: in the purification, washing and drying, the DMF: methanol = 0.5-2:1, and the number of washing times is 3.
10. The method for preparing 2D ZnBDC MOFs nano-lubricating material according to claim 1, wherein the method comprises the following steps: the prepared 2D ZnBDC nanosheet is used for preparing a lubricant containing 2DZnBDC MOFs.
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CN112920880A (en) * | 2020-12-04 | 2021-06-08 | 扬州大学 | Preparation method of 2D MOFs nanosheet-based lubricant |
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