CN110257142B - Preparation method of ultrasonic response type boron nitride nano gel lubricating material - Google Patents
Preparation method of ultrasonic response type boron nitride nano gel lubricating material Download PDFInfo
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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
- 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
- C10M169/04—Mixtures of base-materials and additives
- C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
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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
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
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- 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
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Abstract
The invention discloses a preparation method of an ultrasonic response type boron nitride nanogel lubricating material, which is obtained by mixing a urea-based modified boron nitride two-dimensional nanosheet serving as a gel factor with base oil in a dispersion liquid and carrying out ultrasonic treatment. The gel lubricating material has special ultrasonic response gelling property, and can form a stable gel structure under the action of ultrasonic waves under the mild condition of below 60 ℃, so that the thermal influence of a heating-cooling process in the preparation process of the thermal response gel on the material in a system is avoided. Under the condition of not adding other lubricating additives, the gel lubricating material has excellent antifriction and antiwear properties and lubricating properties within the temperature range of normal temperature to 180 ℃, and can be used in the field of industrial lubricants for bearings, gears and other transmission systems.
Description
Technical Field
The invention relates to a nano composite lubricating material based on ultrasonic response type gel, in particular to an ultrasonic response type boron nitride nano gel lubricating material and a preparation method thereof, belonging to the technical field of lubricating materials.
Background
Lubricating oil and lubricating grease are widely applied in industry as two major fluid lubricants, the lubricating oil has good fluidity, so that the lubricating oil is easy to pump and transport, has excellent lubricating capability on a narrow friction interface, and has obvious heat dissipation effect, but on the other hand, the lubricating oil is easy to run off under the action of gravity and centrifugal force and is not easy to keep on a friction surface; compared with lubricating oil, the lubricating grease has a semi-fluid characteristic, can effectively make up for the defect that the lubricating oil is easy to run off, but has relatively poor pumping performance, and is easy to cause a lean lubricating state in a narrow friction contact area. In order to combine the advantages of lubricating oils and greases, gel-type lubricants have come into play. A certain type of gel factors are added into the lubricating oil, and the lubricating oil can be converted into a gel state from a fluid state under certain external stimulation. Therefore, by utilizing the sol-gel phase change behavior of the gel lubricant to environmental stimulation, creep loss of the lubricant at a lubrication part can be effectively avoided, the shear thinning property which is more sensitive than that of lubricating grease can also effectively avoid lean lubrication of a friction interface, and the energy loss of a lubrication pumping system is further reduced. A series of researches show that certain gel factors not only have the capacity of regulating and controlling the phase change and rheological behavior of base oil, but also have obvious friction-reducing and wear-resisting effects. (1. Takahashi, K.; Shitara, Y.; Mori, S. Tribology Online 2008, 3, 131-136.2. Takahashi, K.; Shitara, Y.; Kaimai, T.; Kanno, A.; Mori, S. Tribology International, 2010, 43, 1577-1583.3. Yu, Q., Huang, G.; Cai, M.; Zhou, F.; Liu W. Tribology International, 2016, 95, 55-65.).
With the development of the gel lubricating material, the nanometer material is added to play the synergistic effect of the nanometer additive and the gel factor in the aspects of rheological behavior regulation and friction-reducing and wear-resisting performances, so that the lubricating, friction-reducing and wear-resisting performances of the gel material are improved. In addition, the dispersion stability of the nano-additive in the system can be further improved due to the immobilization of the gelator network (1. Zhang, R.; Qiao, D.; Liu, X.; Guo, Z.; Cai, M.; Shi, L. Triblology International, 2018, 118, 60-70.2. Zhang, R.; Qiao, D.; Liu, X.; Guo, Z.; Hu L.; Shi L. Industrial & Engineering Chemistry Research, 2018, 57, 10379) 10390). However, most gel-type lubricants currently employ a thermally responsive gelator, and the "sol-gel" conversion process often requires a "heating-cooling" process, for example, when gelator 1-methyl-2, 4-di (N-octadecyl urea) benzene is used, the system needs to be heated to 140 ℃ to dissolve the gelator in the base oil, and gelation occurs during cooling; the N-octadecyl-D-glucosamide gelator needs to be heated to 160 ℃. Such high processing temperatures make many temperature sensitive nanoparticles and their surface modifications susceptible to thermal oxidative decomposition, and the violent movement of the nanoparticles in the thermal base oil further aggravates the agglomeration of the nanoparticles during the cooling process. Therefore, in order to solve the application limitation of the nano-material in the thermal response gel lubricant, it is necessary to develop a novel gel system which contributes to the dispersion stability of the nano-lubricating material.
The ultrasonic response gel is a novel environment sensitive gel which can generate sol-gel phase change under the action of ultrasonic waves, the dependence of the gel forming process on temperature is small, and a stable gel structure can be formed at the temperature below 60 ℃, so that the thermal oxidation of materials in a system is avoided. Meanwhile, for an ultrasonic response gel system containing the nano material, ultrasonic waves can induce the system to generate sol-gel conversion on one hand, and can improve the dispersibility of the nano material in the system on the other hand, so that the unification of the dispersion process and the gelling process is realized. Therefore, the development of the nano composite lubricating material of the ultrasonic response type gel has very important significance.
Disclosure of Invention
The invention aims to provide a preparation method of an ultrasonic response type boron nitride nanogel lubricating material.
Preparation of boron nitride nano gel lubricating material
The ultrasonic response type boron nitride nanogel lubricating material is obtained by mixing a urea-based modified boron nitride two-dimensional nanosheet serving as a gel factor and base oil in a dispersion liquid and carrying out ultrasonic treatment. The specific preparation method of the ultrasonic response type boron nitride nanogel lubricating material comprises the following steps:
(1) preparation of gelator-base oil dispersion: stirring and dispersing the carbamido modified boron nitride gel factor in a low-boiling point solvent to obtain gel factor dispersion liquid with the concentration of 10-15 mg/mL; and adding the gelator dispersion liquid into the base oil, stirring and dispersing uniformly, and then distilling under reduced pressure to remove the solvent to obtain the uniformly dispersed gelator-base oil dispersion liquid.
The carbamido modified boron nitride two-dimensional nanosheet has an inorganic/organic composite structure with an inorganic nanomaterial as a core, wherein the inorganic core is a layered boron nitride nanosheet, the surface of the nanosheet is modified with a diurea organic molecule, the diurea organic molecule is connected with the boron nitride nanosheet through a urea bond, and the structural formula is as follows:
the size of the boron nitride two-dimensional nano-sheet is 50-300 nm, and the thickness is 3-20 nm.
The R is1Is an aryl functional group containing 6 to 15 carbon atoms, R2Is one of aryl, cycloalkyl, straight-chain alkyl or branched-chain alkyl functional groups containing 6-20 carbon atoms.
The low boiling point solvent is a solvent with a boiling point lower than 80 ℃ and comprises: petroleum ether, diethyl ether, acetone, methanol and ethanol.
The base oil is one or the combination of synthetic hydrocarbon oil and ester oil; the content of gelator in gelator-base oil dispersion is 5-40 wt. -%)
The relative vacuum degree of the reduced pressure distillation is-80 to-90 kPa, and the temperature is 40 to 60 ℃.
(2) Preparing a nanogel lubricating material: and carrying out ultrasonic treatment on the gelator-base oil dispersion liquid to obtain the boron nitride-based nano gel lubricating material. Ultrasonic treatment conditions are as follows: the power is 40-120W, the ultrasonic frequency is 20-80 kHz, the temperature is 0-60 ℃, and the treatment time is 5-30 minutes.
Performance of boron nitride nano gel lubricating material
1. Appearance of gel
The formed boron nitride nanogel is an opaque gelatinous semi-solid with certain structure retentivity, as shown in figure 1. The color of the gel depends on the color of the base oil, and when the base oil is colorless and transparent, the formed gel is white and has smooth and fine touch.
2. Ultrasonic responsiveness
The free-flowing gelator-base oil dispersion is placed in an ultrasonic dispersion device, and under the mild condition of below 60 ℃, the dispersion can be converted into a semi-solid gel state and fixed at the bottom of an inverted sample bottle without flowing, as shown in figure 1. When the applied force is higher than the yield strength of the gel material, the colloid can generate shearing deformation and can be converted into fluid under the action of continuous shearing, and the formed fluid can be repeatedly converted into a gel form under the action of ultrasonic waves. Rheological tests show that the yield strength of the boron nitride nanogel formed under ultrasonic induction is related to the concentration of the gelator, the yield strength of the gel is 20.3 Pa when the concentration of the gelator is 5wt%, and the yield strength of the gel is 30.8 Pa when the concentration of the gelator is 9 wt%.
3. Testing of antifriction and antiwear Properties
Testing the lubricating property of the prepared boron nitride nanogel by using an SRV-IV reciprocating friction tester, wherein the friction pair adopts a ball-disk contact form, the material is GCr15 bearing steel, and the diameter of the steel ball is 10 mm; under the condition of applying a certain normal load, the steel ball slides back and forth according to the set frequency and amplitude, and the lubricating performance of the lubricant is represented by measuring the friction coefficient and the wear rate in the relative sliding process of the ball and the disc. The specific experimental conditions are as follows: the reciprocating sliding frequency is 25 Hz, the amplitude is 1 mm, the normal phase load is 50N, the temperature is 20 ℃, the test is carried out for 30 minutes, the lubricant is PAO10 and boron nitride nanogel taking PAO10 as base oil respectively, and the gel factor content is 5wt%, 7wt% and 9wt% respectively. The average friction coefficient and the wear volume are shown in fig. 2, and under the same test conditions, compared with PAO10, boron nitride nanogels with three concentrations show better friction reduction and wear resistance, wherein the friction coefficient is reduced by more than 30%, and the wear volume of the material is reduced by more than 45%.
4. High temperature lubricity test
The testing machine and the friction pair configuration which are the same as the friction reducing and wear resisting performance test are adopted, and the specific test conditions are as follows: the reciprocating sliding frequency is 25 Hz, the amplitude is 1 mm, the normal phase load is 50N, the test temperature is 180 ℃, the test time is 30 minutes, the lubricants are PAO10 and boron nitride nanogel taking PAO10 as base oil respectively, and the gel factor content is 7 wt%. The experimental results show that: under the condition of 180 ℃, the boron nitride nanogel still maintains excellent lubricating property, the friction coefficient is stabilized to be about 0.14, and compared with PAO10, the boron nitride nanogel can reduce the friction coefficient of a friction pair by 25 percent and reduce the abrasion by 35 percent, as shown in figure 3.
5. Bearing capacity test
The testing machine and the friction pair configuration which are the same as the friction reducing and wear resisting performance test are adopted, and the specific experimental conditions are as follows: the reciprocating sliding frequency is 25 Hz, the amplitude is 1 mm, the test temperature is 20 ℃, the load is increased from 100N to 800N in a step mode, each time the load is increased by 100N, the stability test is carried out for 300 seconds under each load, the lubricant is PAO10 and boron nitride nanogel taking PAO10 as base oil respectively, and the gel factor content is 5 wt%. As shown in fig. 4, it can be seen that under the same test conditions, the boron nitride nanogel has a lower and more stable friction coefficient than PAO10, within 400N, the friction coefficient of PAO10 is above 0.2, while the friction coefficient of boron nitride nanogel is around 0.12. When the load is increased to 500N, the friction coefficient of the PAO base oil is greatly increased, the testing machine is locked and stopped at 600N, and the friction coefficient of the boron nitride nanogel is always maintained at about 0.16 until the load is 800N.
In conclusion, the carbamido modified boron nitride two-dimensional nanosheet is taken as a gel factor, is mixed with base oil in a dispersion liquid and is subjected to ultrasonic treatment, the gel system has special ultrasonic response gelling characteristics, and can form a stable gel structure under the mild condition below 60 ℃ under the action of ultrasonic waves, so that the thermal influence of a heating-cooling process in the preparation process of the thermal response gel on materials in the system is avoided. Under the condition of not adding other lubricating additives, the material has excellent antifriction and antiwear properties and lubricating properties within the temperature range of normal temperature to 180 ℃, and can be used in the field of industrial lubricants for bearings, gears and other transmission systems.
Drawings
FIG. 1 is an appearance of a boron nitride nanogel according to the invention.
FIG. 2 shows the average friction coefficient and wear volume of steel friction pairs lubricated with PAO10 and boron nitride nanogel based on PAO 10.
FIG. 3 is the friction coefficient curve and wear volume of steel friction pair at 180 deg.C under PAO10 and boron nitride nanogel lubrication with PAO10 as base oil.
FIG. 4 is a friction coefficient change curve of a steel friction pair under normal load of 100-800N under lubrication by using PAO10 and boron nitride nanogel using PAO10 as base oil.
Detailed Description
Example 1
Preparation of the gelator: mixing 1 g of hexagonal boron nitride raw material, 60 g of urea and 450 g of steel ball, ball-milling for 20 h in nitrogen atmosphere, standing and cooling, washing with water, collecting precipitate, adding 100 mL of concentrated hydrochloric acid to wash out trace iron in the precipitate, washing the precipitate to be neutral with deionized water, centrifuging at 2000 rpm for 30 min to remove large-size boron nitride particles, and collecting an upper aminated boron nitride nanosheet; dispersing 0.15 g of aminated boron nitride nanosheet in 100 mL of anhydrous ether, dropwise and slowly adding the aminated boron nitride nanosheet into 20 mL of ether solution containing 7.4 mL of toluene-2, 4-diisocyanate within 5 h under high-speed stirring, continuously stirring and reacting for 12 h under the normal temperature condition, filtering, and washing with ether and cyclohexane for multiple times to remove excessive toluene-2, 4-diisocyanate; drying the filter cake, dispersing the filter cake into 50 mL of toluene solution, dropwise adding the filter cake into toluene solution containing 1.5 g of octadecylamine, stirring at a high speed at 40 ℃ for reaction for 12 h, filtering out a product, washing for 5 times by using 50 mL of mixed solvent (V n-butyl alcohol: V petroleum ether =1: 1), removing unreacted octadecylamine, and centrifuging at 9000 rpm for 15 min to obtain the ureido-modified boron nitride two-dimensional nanosheet, namely the gel factor. The structure of the gelator is as follows:
r1 is tolyl containing 7 carbon atoms, R2 is n-octadecyl containing 18 carbon atoms.
Preparing boron nitride nanogel: 0.26g of gelator is weighed and stirred and dispersed in 20 mL of petroleum ether to obtain the concentration of 13 mg.mL-1The gelator dispersion of (1); respectively measuring 8.1 mL, 11.5 mL and 19.8 mL of gel factor dispersion liquid, adding the gel factor dispersion liquid into 2 g of PAO10 base oil, uniformly stirring, and removing petroleum ether in the mixed liquid by reduced pressure distillation (-85 kPa, 50 ℃) to respectively obtain base oil dispersion liquid with the gel factor contents of 5wt%, 7wt% and 9 wt%; will be provided withPlacing the base oil dispersion in an ultrasonic water bath with power of 60W and frequency of 40 kHz, and performing ultrasonic treatment at 50 ℃ for 20 min to obtain boron nitride nanogels with gel factor concentrations of 5wt%, 7wt% and 9 wt%. The gel appearance is shown in fig. 1, and the average friction coefficient and wear volume of the gel are shown in fig. 2; the high-temperature lubricating property is shown in figure 3; the load bearing capacity is shown in figure 4.
Example 2
The preparation of gelator was the same as in example 1;
0.26g of gelator is weighed and stirred and dispersed in 20 mL of petroleum ether to obtain the gelator with the concentration of 13 mg.mL-1The petroleum ether dispersion of (1); measuring 8.1 mL of dispersion, adding the dispersion into 2 g of bis (2-ethylhexyl) sebacate, uniformly stirring, carrying out reduced pressure distillation to remove petroleum ether in the mixed solution to obtain a base oil dispersion with the gel factor content of 5%, placing the dispersion in an ultrasonic water bath with the power of 100W and the frequency of 20 kHz, and carrying out ultrasonic treatment for 15 min at 50 ℃ to obtain the boron nitride-based nanogel with the bis (2-ethylhexyl) sebacate as the base oil, wherein the appearance of the gel is shown in figure 1. The antifriction and antiwear performance, high-temperature lubricating performance and bearing capacity of the lubricating oil are basically similar to those of the embodiment.
Example 3
The preparation of gelator was the same as in example 1;
0.26g of gelator is weighed and stirred and dispersed in 20 mL of petroleum ether to obtain the gelator with the concentration of 13 mg.mL-1The petroleum ether dispersion of (1); measuring 8.1 mL of dispersion, adding the dispersion into 2 g of n-dodecane, uniformly stirring, carrying out reduced pressure distillation to remove petroleum ether in the mixed solution to obtain a base oil dispersion with the gel factor content of 5%, placing the dispersion in an ultrasonic water bath with the power of 100W and the frequency of 80kHz, and carrying out ultrasonic treatment for 20 min at 50 ℃ to obtain the boron nitride-based nanogel with dodecane as the base oil, wherein the appearance of the gel is shown in figure 1. The antifriction and antiwear performance, high-temperature lubricating performance and bearing capacity of the lubricating oil are basically similar to those of the embodiment.
Claims (4)
1. A preparation method of an ultrasonic response type boron nitride nanogel lubricating material comprises the following steps:
(1) preparation of gelator-base oil dispersion: stirring and dispersing the carbamido modified boron nitride gel factor in a low-boiling point solvent to obtain gel factor dispersion liquid with the concentration of 10-15 mg/mL; adding the gelator dispersion liquid into base oil, stirring and dispersing uniformly, and then distilling under reduced pressure to remove the solvent to obtain a uniformly dispersed gelator-base oil dispersion liquid, wherein the content of gelators in the gelator-base oil dispersion liquid is 5-40 wt%; the structural formula of the ureido modified boron nitride two-dimensional nanosheet is as follows:
R1is an aryl functional group containing 6 to 15 carbon atoms, R2Is one of linear alkyl or branched alkyl functional groups containing 6-20 carbon atoms;
(2) preparing a nanogel lubricating material: carrying out ultrasonic treatment on the gelator-base oil dispersion liquid to obtain the boron nitride-based nano gel lubricating material; ultrasonic treatment conditions are as follows: the power is 40-120W, the ultrasonic frequency is 20-80 kHz, the temperature is 0-60 ℃, and the treatment time is 5-30 minutes.
2. The method for preparing an ultrasonic-responsive boron nitride nanogel lubricating material as claimed in claim 1, wherein the method comprises the following steps: the low boiling point solvent is petroleum ether, diethyl ether, acetone, methanol or ethanol.
3. The method for preparing an ultrasonic-responsive boron nitride nanogel lubricating material as claimed in claim 1, wherein the method comprises the following steps: the base oil is one or the combination of synthetic hydrocarbon oil and ester oil.
4. The method for preparing an ultrasonic-responsive boron nitride nanogel lubricating material as claimed in claim 1, wherein the method comprises the following steps: the relative vacuum degree of the reduced pressure distillation is-80 to-90 kPa, and the temperature is 40 to 60 ℃.
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