CN112142889A - Preparation method of graphene composite material and application of graphene composite material in lubricating oil - Google Patents
Preparation method of graphene composite material and application of graphene composite material in lubricating oil Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-acryloyl morpholine
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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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
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/024—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an amido or imido group
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Abstract
The invention discloses a preparation method of a graphene composite material and application of the graphene composite material in lubricating oil, and relates to the technical field of composite materials, wherein the graphene composite material prepared by the invention has good compatibility with hydrocarbon groups in the lubricating oil, and can promote graphene to be uniformly and stably dispersed in the lubricating oil so as to solve the problem of poor dispersibility of conventional graphene and prevent the phenomenon of graphene sedimentation of the lubricating oil during preparation or after storage; and the antifriction and antiwear performance of the lubricating oil can be obviously improved, and the lubricating effect of the lubricating oil is optimized, so that the service life of a device is effectively prolonged.
Description
The technical field is as follows:
the invention relates to the technical field of composite materials, in particular to a preparation method of a graphene composite material and application of the graphene composite material in lubricating oil.
Background art:
graphene, a material consisting of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. Because of the thickness of only one layer of carbon atoms, it is the thinnest and hardest material found to date. Graphene, however, is highly susceptible to agglomeration or stacking due to the strong intermolecular van der waals forces between its layers. In addition, due to the perfect hexagonal carbon lattice structure of graphene, graphene cannot be dispersed in water or organic solvents, so that the use of graphene is severely limited.
The graphene lubricating oil is used as a carrier of lubricating oil, the graphene particles can be filled in the surface damage part of the friction pair, the friction pair is repaired, metal friction is replaced by friction between the graphene, the friction coefficient is reduced, the graphene is inlaid in the surface of the friction pair, the friction pair can be well protected, and the service life of a device is effectively prolonged.
Based on the problem of poor graphene dispersibility, the field generally adopts a method of adding a dispersant to promote uniform dispersion of graphene in the lubricating oil, but the dispersant is mostly a surfactant, is easy to foam during mixing, and still has the problem of graphene sedimentation after standing, thereby affecting the service performance of the lubricating oil.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a preparation method of a graphene composite material, wherein intercalation modified graphite is prepared by an intercalation polymerization method, and then a grinding stripping machine is adopted to prepare the graphene composite material, so that the obtained graphene composite material can be uniformly and stably dispersed in lubricating oil, and the antifriction and antiwear performances of the lubricating oil are optimized.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of a graphene composite material comprises the following preparation steps:
(1) heating N-hydroxymethyl acrylamide to 75-80 ℃, preserving heat, adding trifluoropropionic acid after the N-hydroxymethyl acrylamide is completely melted, then dropwise adding concentrated sulfuric acid, heating the reaction solution, reacting in a reflux state, adding water and stirring after the reaction is finished, filtering and precipitating, washing with water and drying to obtain a monomer;
(2) heating the monomer prepared in the step (1) to 65-70 ℃, preserving heat, adding graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment at 65-70 ℃ to obtain a mixture;
(3) adding an initiator into the mixture prepared in the step (2), and heating to 105-110 ℃ for polymerization reaction to obtain intercalation modified graphite;
(4) and (4) adding the intercalation modified graphite prepared in the step (3) into a stripping machine, and grinding to obtain the graphene composite material.
The molar ratio of the N-methylolacrylamide to the trifluoropropionic acid is 1-1.05: 1.
The concentration of the concentrated sulfuric acid is 98 wt%, and the using amount of the concentrated sulfuric acid is 2-5 wt% of the total amount of the N-hydroxymethyl acrylamide and the trifluoropropionic acid.
The reaction equation for the above monomers is as follows:
n-hydroxymethyl acrylamide and trifluoropropionic acid are subjected to esterification reaction, wherein concentrated sulfuric acid is used as a dehydrating agent to promote the forward progress of the esterification reaction.
The mass ratio of the monomer to the graphite powder is 5-15: 10-30.
The ultrasonic frequency of the ultrasonic treatment is 20KHz, and the ultrasonic power is 300-900W.
The amount of the initiator is 2-5 wt% of the amount of the monomer.
The initiator is dicumyl peroxide.
The above monomers are polymerized under the action of an initiator, and the reaction equation is as follows:
n is a natural number of 20 to 200.
The monomer enters the graphite flake layer under the action of ultrasonic waves, the coulomb force among the graphite flake layers is overcome by utilizing the heat released during polymerization, the generated polymer is compounded with the graphite flake layer in a chemical bond mode, and the prepared intercalation modified graphite is subjected to grinding action to peel off the graphite to form the graphene.
The rotation speed of the grinding is 500-.
The invention also adds 1, 2-cyclohexanediol diglycidyl ether in the step (4), promotes the stripping of graphite by utilizing the wetting and penetrating action of the 1, 2-cyclohexanediol diglycidyl ether, and further improves the anti-wear and anti-friction performance of the lubricating oil by utilizing the lubricating action of the 1, 2-cyclohexanediol diglycidyl ether.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of a graphene composite material comprises the following preparation steps:
(1) heating N-hydroxymethyl acrylamide to 75-80 ℃, preserving heat, adding trifluoropropionic acid after the N-hydroxymethyl acrylamide is completely melted, then dropwise adding concentrated sulfuric acid, heating the reaction solution, reacting in a reflux state, adding water and stirring after the reaction is finished, filtering and precipitating, washing with water and drying to obtain a monomer;
(2) heating the monomer prepared in the step (1) to 65-70 ℃, preserving heat, adding graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment at 65-70 ℃ to obtain a mixture;
(3) adding an initiator into the mixture prepared in the step (2), and heating to 105-110 ℃ for polymerization reaction to obtain intercalation modified graphite;
(4) and (3) adding the intercalation modified graphite prepared in the step (3) and 1, 2-cyclohexanediol diglycidyl ether into a stripping machine, and grinding to obtain the graphene composite material.
The molar ratio of the N-methylolacrylamide to the trifluoropropionic acid is 1-1.05: 1.
The concentration of the concentrated sulfuric acid is 98 wt%, and the using amount of the concentrated sulfuric acid is 2-5 wt% of the total amount of the N-hydroxymethyl acrylamide and the trifluoropropionic acid.
The mass ratio of the monomer to the graphite powder is 5-15: 10-30.
The ultrasonic frequency of the ultrasonic treatment is 20KHz, and the ultrasonic power is 300-900W.
The amount of the initiator is 2-5 wt% of the amount of the monomer.
The initiator is dicumyl peroxide.
The rotation speed of the grinding is 500-.
The mass ratio of the intercalation modified graphite to the 1, 2-cyclohexanediol diglycidyl ether is 100: 1-5.
The graphene composite material is applied to lubricating oil.
The addition amount of the graphene composite material in the lubricating oil is 0.5-5 wt%.
The graphene composite material prepared by the two technical schemes is added into lubricating oil, so that the antifriction and antiwear performance of the lubricating oil is optimized, and the problem of poor dispersibility of the conventional graphene is solved, wherein the dispersibility comprises the instant dispersibility during the preparation of the lubricating oil and the dispersion stability during the storage of the lubricating oil.
The invention has the beneficial effects that:
(1) the graphene composite material prepared by the invention has good compatibility with hydrocarbon groups in lubricating oil, and can promote graphene to be uniformly and stably dispersed in the lubricating oil, so that the problem of poor dispersibility of conventional graphene is solved, and the phenomenon of graphene sedimentation of the lubricating oil during preparation or after storage is prevented.
(2) The graphene composite material prepared by the invention has strong use safety and environmental protection, does not damage equipment and pollute the environment, can obviously improve the antifriction and antiwear properties of lubricating oil, and optimizes the lubricating effect of the lubricating oil, thereby effectively prolonging the service life of devices.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Graphite powder was purchased from 800 mesh micropowder graphite of Qingdao morning positive graphite Co.
Lubricating oil was purchased from great wall tall L-HM 46 lubricating oil.
Example 1
(1) Heating 10.6g N-hydroxymethyl acrylamide to 80 ℃, preserving heat, adding 12.8g of trifluoropropionic acid after N-hydroxymethyl acrylamide is completely melted, dropwise adding 1g of concentrated sulfuric acid with the concentration of 98 wt%, heating the reaction solution, reacting for 5 hours under the reflux state, adding 500mL of water after the reaction is finished, stirring, filtering, precipitating, washing with water, and drying to obtain a monomer;1H NMR(DMSO-d6,400MHz),:9.38(s,1H),6.48(t,1H),6.09-6.00(m,2H),5.75(s,2H),2.77(s,2H)；ESI-MS:m/z＝212.05[M+1]+.
(2) heating 10g of the monomer prepared in the step (1) to 70 ℃, preserving heat, adding 15g of graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment for 3h at 70 ℃, wherein the ultrasonic frequency is 20KHz, and the ultrasonic power is 600W to obtain a mixture;
(3) adding 0.5g of dicumyl peroxide into the mixture prepared in the step (2), heating to 110 ℃, and carrying out polymerization reaction for 3h to obtain intercalation modified graphite;
(4) and (3) adding 100g of the intercalation modified graphite prepared in the step (3) into a stripping machine, and grinding for 5 hours at the rotating speed of 1000r/min to obtain the graphene composite material.
Example 2
(1) Heating 10.6g N-hydroxymethyl acrylamide to 80 ℃, preserving heat, adding 12.8g of trifluoropropionic acid after N-hydroxymethyl acrylamide is completely melted, dropwise adding 1g of concentrated sulfuric acid with the concentration of 98 wt%, heating the reaction solution, reacting for 5 hours under the reflux state, adding 500mL of water after the reaction is finished, stirring, filtering, precipitating, washing with water, and drying to obtain a monomer;
(2) heating 8g of the monomer prepared in the step (1) to 70 ℃, preserving heat, adding 15g of graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment for 3h at 70 ℃, wherein the ultrasonic frequency is 20KHz and the ultrasonic power is 600W to obtain a mixture;
(3) adding 0.5g of dicumyl peroxide into the mixture prepared in the step (2), heating to 110 ℃, and carrying out polymerization reaction for 3h to obtain intercalation modified graphite;
(4) and (3) adding 100g of the intercalation modified graphite prepared in the step (3) into a stripping machine, and grinding for 5 hours at the rotating speed of 1000r/min to obtain the graphene composite material.
Example 3
Example 3 the procedure for preparing a graphene composite material was the same as in example 1 except that 5g of 1, 2-cyclohexanediol diglycidyl ether was added in step (4).
(1) Heating 10.6g N-hydroxymethyl acrylamide to 80 ℃, preserving heat, adding 12.8g of trifluoropropionic acid after N-hydroxymethyl acrylamide is completely melted, dropwise adding 1g of concentrated sulfuric acid with the concentration of 98 wt%, heating the reaction solution, reacting for 5 hours under the reflux state, adding 500mL of water after the reaction is finished, stirring, filtering, precipitating, washing with water, and drying to obtain a monomer;
(2) heating 10g of the monomer prepared in the step (1) to 70 ℃, preserving heat, adding 15g of graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment for 3h at 70 ℃, wherein the ultrasonic frequency is 20KHz, and the ultrasonic power is 600W to obtain a mixture;
(3) adding 0.5g of dicumyl peroxide into the mixture prepared in the step (2), heating to 110 ℃, and carrying out polymerization reaction for 3h to obtain intercalation modified graphite;
(4) and (3) adding 100g of the intercalation modified graphite prepared in the step (3) and 5g of 1, 2-cyclohexanediol diglycidyl ether into a stripping machine, and grinding for 5 hours at the rotating speed of 1000r/min to obtain the graphene composite material.
Comparative example 1
Comparative example 1 the graphene composite material was prepared according to the same procedure as in example 1, except that the monomer in the step (2) was replaced with a silane coupling agent KH 560.
(1) Heating 10g of silane coupling agent KH560 to 70 ℃, adding 15g of graphite powder, and carrying out ultrasonic treatment for 3h at 70 ℃, wherein the ultrasonic frequency is 20KHz, and the ultrasonic power is 600W, so as to obtain a mixture;
(2) adding 0.5g of dicumyl peroxide into the mixture prepared in the step (1), heating to 110 ℃, and carrying out polymerization reaction for 3h to obtain intercalation modified graphite;
(3) and (3) adding 100g of the intercalation modified graphite prepared in the step (2) into a stripping machine, and grinding for 5 hours at the rotating speed of 1000r/min to obtain the graphene composite material.
Comparative example 2
Comparative example 2 the operation procedure for preparing a graphene composite material was the same as in example 1, except that trifluoropropionic acid in step (1) was replaced with propionic acid.
(1) Heating 10.6g N-hydroxymethyl acrylamide to 80 ℃, preserving heat, adding 7.4g of propionic acid after N-hydroxymethyl acrylamide is completely melted, then dropwise adding 1g of concentrated sulfuric acid with the concentration of 98 wt%, heating the reaction solution, reacting for 5 hours under the reflux state, adding 500mL of water after the reaction is finished, stirring, filtering, precipitating, washing with water, and drying to obtain a monomer;
(2) heating 10g of the monomer prepared in the step (1) to 70 ℃, preserving heat, adding 15g of graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment for 3h at 70 ℃, wherein the ultrasonic frequency is 20KHz, and the ultrasonic power is 600W to obtain a mixture;
(3) adding 0.5g of dicumyl peroxide into the mixture prepared in the step (2), heating to 110 ℃, and carrying out polymerization reaction for 3h to obtain intercalation modified graphite;
(4) and (3) adding 100g of the intercalation modified graphite prepared in the step (3) into a stripping machine, and grinding for 5 hours at the rotating speed of 1000r/min to obtain the graphene composite material.
Example 4
And (3) adding 1g of the graphene composite material prepared in the example 1 into 100g of lubricating oil, and mixing at the rotating speed of 500r/min for 10min to obtain the graphene lubricating oil.
Example 5
And (3) adding 1g of the graphene composite material prepared in the example 2 into 100g of lubricating oil, and mixing at the rotating speed of 500r/min for 10min to obtain the graphene lubricating oil.
Example 6
And (3) adding 1g of the graphene composite material prepared in the example 3 into 100g of lubricating oil, and mixing at the rotating speed of 500r/min for 10min to obtain the graphene lubricating oil.
Comparative example 3
1g of the graphene composite material prepared in comparative example 1 was added to 100g of lubricating oil, and mixed at a rotation speed of 500r/min for 10min to obtain graphene lubricating oil.
Comparative example 4
And (3) adding 1g of the graphene composite material prepared in the comparative example 2 into 100g of lubricating oil, and mixing at the rotating speed of 500r/min for 10min to obtain the graphene lubricating oil.
Comparative example 5
0.6g of graphene and 0.4g of monoalkenyl succinimide (the amounts of graphene and monoalkenyl succinimide are converted from the amounts of the monomer and graphite powder used in example 1) were added to 100g of the lubricating oil, and mixed at a rotation speed of 500r/min for 10min to obtain a graphene lubricating oil. Wherein, the mono alkenyl succinimide is used as a dispersant to promote the dispersion of the graphene in the lubricating oil.
The graphene lubricating oils prepared in examples 4 to 6 and comparative examples 3 to 5 were tested for anti-friction and anti-wear properties, and the lubricating oil without added graphene was set as a blank example, and the results are shown in table 1.
The abrasion wear diameter is tested according to the standard NB/SH/T0189-2017, and the test conditions are as follows: and (3) condition C.
The test of the maximum non-clamping load is based on the standard GB/T3142-2019, and the test conditions are as follows: the temperature is 25 ℃, and the rotating speed is 1450 r/min.
TABLE 1
| Group number | Abrasive grain diameter/mm | Maximum no-seize load/N |
| Example 4 | 0.16 | 285 |
| Example 5 | 0.18 | 273 |
| Example 6 | 0.12 | 302 |
| Comparative example 3 | 0.30 | 258 |
| Comparative example 4 | 0.48 | 221 |
| Comparative example 5 | 0.40 | 239 |
| Blank example | 0.65 | 170 |
As can be seen from Table 1, the anti-friction and anti-wear properties of the lubricating oil can be remarkably improved by the preparation of the intercalated modified graphite and the addition of the 1, 2-cyclohexanediol diglycidyl ether.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A preparation method of a graphene composite material is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) heating N-hydroxymethyl acrylamide to 75-80 ℃, preserving heat, adding trifluoropropionic acid after the N-hydroxymethyl acrylamide is completely melted, then dropwise adding concentrated sulfuric acid, heating the reaction solution, reacting in a reflux state, adding water and stirring after the reaction is finished, filtering and precipitating, washing with water and drying to obtain a monomer;
(2) heating the monomer prepared in the step (1) to 65-70 ℃, preserving heat, adding graphite powder after the monomer is completely melted, and carrying out ultrasonic treatment at 65-70 ℃ to obtain a mixture;
(3) adding an initiator into the mixture prepared in the step (2), and heating to 105-110 ℃ for polymerization reaction to obtain intercalation modified graphite;
(4) and (4) adding the intercalation modified graphite prepared in the step (3) into a stripping machine, and grinding to obtain the graphene composite material.
2. The method for preparing the graphene composite material according to claim 1, wherein: the molar ratio of the N-methylolacrylamide to the trifluoropropionic acid is 1-1.05: 1.
3. The method for preparing the graphene composite material according to claim 1, wherein: the concentration of the concentrated sulfuric acid is 98 wt%, and the using amount of the concentrated sulfuric acid is 2-5 wt% of the total amount of the N-hydroxymethyl acrylamide and the trifluoropropionic acid.
4. The method for preparing the graphene composite material according to claim 1, wherein: the mass ratio of the monomer to the graphite powder is 5-15: 10-30.
5. The method for preparing the graphene composite material according to claim 1, wherein: the ultrasonic frequency of the ultrasonic treatment is 20KHz, and the ultrasonic power is 300-900W.
6. The method for preparing the graphene composite material according to claim 1, wherein: the amount of the initiator is 2-5 wt% of the amount of the monomer.
7. The method for preparing the graphene composite material according to claim 1, wherein: the initiator is dicumyl peroxide.
8. The method for preparing the graphene composite material according to claim 1, wherein: the rotation speed of the grinding is 500-.
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