CN110699161A - Process method for preparing high-concentration graphene lubricating oil additive by weak agglomeration-deagglomeration method - Google Patents
Process method for preparing high-concentration graphene lubricating oil additive by weak agglomeration-deagglomeration method 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
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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
- C10M141/00—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential
- C10M141/06—Lubricating compositions characterised by the additive being a mixture of two or more compounds covered by more than one of the main groups C10M125/00 - C10M139/00, each of these compounds being essential at least one of them being an organic nitrogen-containing compound
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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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
-
- 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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/02—Well-defined aliphatic compounds
- C10M2203/022—Well-defined aliphatic compounds saturated
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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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
-
- 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/08—Amides
Abstract
The invention discloses a process method for preparing a high-concentration graphene lubricating oil additive by a weak agglomeration-deagglomeration method, which comprises the steps of forming transition phase micro-floccules by performing electrostatic adsorption or hydrogen bond adsorption on graphene substances from a graphene hydrophilic phase solution which is easy to form uniform dispersion with a flocculating agent, transferring the transition phase micro-floccules to an organic medium to form a uniform graphene organic phase, transferring the uniform graphene organic phase to an oil phase, and realizing wet transfer of the dispersed graphene from the water phase to the oil phase, so that the high-concentration graphene additive can be prepared.
Description
Technical Field
The invention belongs to the field of lubricants, and particularly relates to a preparation process of an ultrahigh-concentration graphene lubricating oil reinforcing agent.
Background
The lubricant additive is a key functional material determining the core performance of a lubricating material, and is widely applied to the fields of transportation, engineering machinery, metallurgy, industrial machine tools and the like. With the rapid development of economy, industrial equipment and fuel oil technology are continuously improved, corresponding lubricating systems and lubricating materials are synchronously upgraded and updated, and the industrial pollution emission and energy consumption are greatly increased, so that the lubricant additive faces multiple challenges: on the government level, new energy-saving, environment-friendly and emission-reduction regulations are continuously pushed out, and the fuel economy is required to be improved; in the industrial field, both in the automotive industry and in the mechanical industry, the lubricant performance is required to be improved in all directions so as to adapt to increasingly harsh operating conditions; on the terminal, users expect a more cost-effective product: long service life, low energy consumption and low equipment maintenance cost.
The above requirements and demands have a profound impact on additive formulation design. The lubricating oil additive is promoted to gradually develop towards high performance, multi-functionalization and environmental friendliness: excellent antiwear, antifriction and antioxidant performance, lower SAPS content limit values (sulfated ash, phosphorus and sulfur), reduced content of heavy metal ions (zinc, molybdenum and the like), environmental compatibility, biodegradation and reproducibility. The existing lubricant extreme pressure antiwear agent is mainly a compound containing sulfur, phosphorus, chlorine or heavy metal elements such as zinc, molybdenum and the like. At present, some novel environment-friendly products such as boron compounds, nano compounds and the like appear in the market, and become the development trend of the lubricating technology.
The nano carbon material can be used as an anti-wear and anti-friction material of lubricating oil, and has become a research hotspot in China in this few years, graphene, fullerene, carbon nano tubes and the like are widely and deeply researched by experts and scholars, and the graphene is proved to be added into the lubricating oil to obviously reduce friction and wear, thereby being beneficial to improving the fuel economy. In 2018, 20 days in 9 and 9, the Ministry of industry and communications has revised the guide catalogue of the first batch application of key new materials and the catalogue of the graphene lubricating oil inclusion, so that the application of the graphene lubricating oil in the fields of automobiles and engineering machinery is promoted. Part of graphene lubricant products and lubricating oil thereof are already in the market, and a batch of related preparation methods are also emerged. CN106811265A discloses a method for adding a graphene dispersion liquid into a base oil to form an emulsion, and then removing water to form a graphene lubricating oil, but the method can be used for preparing a lubricating oil with a low graphene concentration, but is difficult to operate, long in time consumption and difficult to produce in a large scale during large-scale oil production. CN105296053B discloses a preparation method of a graphene lubricating oil additive, which is characterized by large energy consumption, high cost and complex operation through the processes of centrifugation, drying, high temperature and high pressure and then mixing. CN107338086A discloses a preparation method of a lubricating oil additive of graphene-doped composite dispersant, wherein the modified graphene has a large sheet diameter, and is modified, dried and ultrasonically dissolved, so that the time consumption is long.
At present, a simple and fast method for adding graphene into oil to form a long-term stable dispersion system is still lacked, the problems of complex modification process, high cost, difficult large-scale production and yield and the like exist, and a preparation method of a high-concentration graphene lubricant additive which is simple in process, can be produced in large-scale production and is stable for a long time needs to be developed in the field.
Disclosure of Invention
The invention aims to provide a preparation process of a high-concentration graphene lubricant additive, and the high-concentration graphene lubricant additive which is stably dispersed for a long time is prepared.
The purpose of the invention is realized by the following technical scheme:
a process method for preparing a high-concentration graphene lubricating oil additive by a weak agglomeration-deagglomeration method mainly comprises the following steps:
1) dissolving graphene materials in a soluble medium, and forming a uniform solution in one or more modes of stirring, ultrasound or homogenization and the like;
2) preparing a graphene flocculant solution: the graphene flocculant is selected from alkali metal solution, organic ammonium salt, metal cations, polyacrylamide copolymer, alkylamine, stearic acid amide, N-dimethylethanolamine, dodecanol, hexadecanol and other substance solutions capable of forming electrostatic adsorption or hydrogen bonds with graphene surface groups, the solvent is selected from one or a combination of water, petroleum ether, ethanol, N-heptane and other solvents, and the concentration of the flocculant is 1-30%.
3) Dropping the flocculant solution into the graphene substance solution, separating floccules from a hydrophilic medium by adopting one or more of filtration, centrifugation, extraction and desiccant water absorption methods, transferring wet graphene substance floccules into an organic solvent, and dispersing floccules by using one or more of ultrasound, homogenization and stirring to form a homogeneous graphene substance organic solution;
4) adding base oil into the graphene organic solution, adding a dispersing agent, and uniformly stirring at the speed of 100-5000 rpm;
5) and removing the volatile organic solvent by using reduced pressure distillation modes such as rotary evaporation and the like to obtain the 1-10% high-concentration stably-dispersed graphene lubricating oil additive.
Preferably, the graphene-like substance is graphene with a transverse sheet diameter of 100 nm-10 μm, 1-5 layers, an oxygen content of 0-50%, an epoxy group and a hydroxyl group on the surface, and a carboxyl functional group on the edge, and derivatives or combinations thereof.
Preferably, wherein the hydrophilic medium includes, but is not limited to, water, ethanol, isopropanol or a combination thereof.
Preferably, the dispersant is one or a combination of more of silane coupling agent, titanate coupling agent, mono-alkenyl succinimide, bis-alkenyl succinimide, poly-isobutylene succinimide, oleic acid, stearic acid, cetyl trimethyl ammonium bromide and the like.
Preferably, the base oil is one or a combination of more of group I, group II, group III base oils, finished oil or vegetable oil, and the addition amount of the base oil is 10-100 times (weight ratio) of the graphene-like substances.
Preferably, with the dropping of the flocculant solution, molecules of the flocculant and graphene oxide form weak agglomeration through electrostatic adsorption or hydrogen bonds, the dropping amount of the flocculant is controlled, the dropping is stopped when a micro-flocculation state occurs, and the ratio of graphene substances to the flocculant is 1: 10-10: 1.
Preferably, the concentration of the graphene-like substance in the solvent is 1-10% (weight percentage).
Preferably, a commercially available graphene aqueous phase stabilizing solution can be directly used.
Preferably, the organic solvent includes one or a combination of weak polar volatile organic solvents such as petroleum ether, isopropanol, ethanol, n-heptane and the like.
The invention also protects the high-concentration graphene lubricating oil additive prepared by the process method.
The invention has the following beneficial effects:
the weak agglomeration method disclosed by the invention is mainly characterized in that slight adsorption is generated between a compound and a graphene substance (comprising graphene and graphene oxide with different oxidation degrees, wherein the oxygen content is 0-50%) through electrostatic coulomb force and hydrogen bonds, so that the organic phase formed by the graphene substance and the adsorbed compound is conveniently separated from a water phase, and the graphene substance adsorbate is easily redispersed in an ultrasonic oscillation or shearing stirring mode after an oil phase is added, so that a high-concentration graphene oil phase additive is formed. The method is simple and convenient to operate, few in required reagents and equipment, high in production speed, high in product concentration and capable of realizing large-scale production, the small amount of high-concentration graphene additive can be diluted in a large amount of lubricating oil, the method is completely carried out in a wet method state, the problems that the powdered graphene substance and the modified and dried powder thereof are difficult to disperse and unstable when being directly dissolved in the lubricating oil are solved, and the wet method transfer of the graphene substance from a soluble water phase medium to the lubricating oil is realized.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
The key point of the method is that graphene substances form transition phase micro-floccules through electrostatic adsorption or hydrogen bond adsorption with a flocculating agent from a graphene hydrophilic phase solution which is easy to form uniform dispersion, then the transition phase micro-floccules are transferred to an organic medium to form a uniform graphene organic phase, and then the uniform graphene organic phase is transferred to an oil phase, so that the method for wet transfer of the dispersed graphene from the water phase to the oil phase is realized, and the high-concentration graphene additive can be prepared.
The main technical scheme of the invention is as follows:
the preparation method comprises the following steps of dissolving a graphene substance, optionally the graphene substance has the transverse sheet diameter of 100 nm-10 mu m, 1-5 layers and the oxygen content of 0-50%, wherein the surface of the graphene substance has epoxy groups and hydroxyl groups, and the edge of the graphene substance has carboxyl functional groups, derivatives or combinations thereof in a soluble medium, such as one or more of hydrophilic media such as a water phase, ethanol, isopropanol and the like, and forming a uniform solution in one or more modes such as stirring, ultrasound or homogenization, wherein the concentration of the graphene substance in a solvent is 1-10% (weight percentage). Aqueous phase stabilizing solutions of, for example, commercially available graphene, which are directly available, may also be used.
Preparing a graphene flocculant solution: the solution can be alkali metal solution (PH regulator), organic ammonium salt, metal cation, polyacrylamide copolymer, substance solution which can form electrostatic adsorption or hydrogen bond with graphene surface groups such as alkylamine, stearic acid amide, N-dimethylethanolamine, dodecanol and hexadecanol, the solvent can be one or combination of water, petroleum ether, ethanol, N-heptane and other solvents, and the concentration of the flocculating agent is 1-30%.
And (3) dropwise adding a flocculant solution into the graphene hydrophilic medium solution. With the dropping of the flocculant solution, flocculant molecules and graphene oxide form weak agglomeration through electrostatic adsorption or hydrogen bonds, the dropping amount of the flocculant is controlled, the dropping is stopped when a micro-flocculation state occurs, and the ratio of graphene substances to the flocculant is 1: 10-10: 1 generally. Separating floccule from hydrophilic medium by one of filtration, centrifugation, extraction and drying agent water absorption methods, transferring wet graphene substance floccule into organic solvent, wherein the organic solvent can adopt one or combination of weak-polarity volatile organic solvents such as petroleum ether, isopropanol, ethanol, n-heptane and the like, and dispersing the floccule by one or more of ultrasonic, homogenization and stirring to form homogeneous graphene substance organic solution.
Adding base oil into the graphene organic solution, wherein the base oil is selected from one or a combination of more of I-type, II-type and III-type base oil, finished oil or vegetable oil, and the addition amount of the base oil is 10-100 times (weight ratio) of the graphene. Adding a dispersing agent, wherein the dispersing agent is selected from one or a combination of more of silane coupling agent, titanate coupling agent, mono-alkenyl succinimide, bis-butyl imide, polyisobutenyl succinimide, oleic acid, stearic acid, cetyl trimethyl ammonium bromide and the like. Stirring uniformly at the speed of 100-5000 rpm to avoid emulsification.
And removing the volatile organic solvent by using reduced pressure distillation modes such as rotary evaporation and the like to obtain the 1-10% high-concentration stably-dispersed graphene lubricating oil additive.
The following is detailed by way of specific embodiments:
example 1
(1) Taking 50g of graphene aqueous solution with the concentration of 1%, and adding 5g of petroleum ether solution of 1% cetyl trimethyl ammonium bromide to generate micro flocculation;
(2) filtering out a water layer by using a coarse net, immediately transferring the micro-floccule into petroleum ether for ultrasonic treatment, and deflocculating;
(3) adding the uniform deflocculated graphene petroleum ether solution into 50g of 150SN base oil, performing rotary distillation at 50 ℃ for 2h, and removing volatile petroleum ether to obtain a 1% graphene oil concentrated solution;
(4) and (3) diluting the graphene oil concentrated solution by 100 times into HM46 hydraulic oil, and performing common stirring to obtain the graphene hydraulic oil.
Example 2
(1) Taking 50g of 5% graphene oxide aqueous solution, adding 25g of 1% stearic acid amide ethanol solution, and performing micro-flocculation;
(2) placing into CaCl2 wrapped by dialysis bag, removing most water, transferring the rest micro-floccule into ethanol, and performing ultrasonic treatment to deflocculate;
(3) adding the uniform deflocculated graphene ethanol solution into 50g of SN 5W-40 fully-synthesized gasoline engine oil, performing rotary distillation at 60 ℃ for 2h, and removing volatile ethanol to obtain 5% graphene oil concentrated solution;
(4) and (3) diluting the graphene oil concentrated solution by 250 times into SN 5W-40 fully-synthesized gasoline engine oil, and carrying out common stirring to obtain the graphene gasoline engine oil.
The graphene lube friction test data in examples 1 and 2 are as follows:
| coefficient of friction | Abrasive grain diameter/mm | The improvement rate% | ||
| Example 1 | Hydraulic oil | 0.13 | 0.55 | / |
| Example 2 | Gasoline engine oil | 0.12 | 0.53 | / |
| Example 1 | Graphene hydraulic oil | 0.08 | 0.38 | 31％ |
| Example 2 | Graphene gasoline engine oil | 0.09 | 0.40 | 24.5％ |
Therefore, compared with the existing products, the graphene hydraulic oil and the graphene gasoline oil provided by the invention have the advantages that the improvement rate reaches 31% and 24.5%, and the efficiency is very excellent.
In addition, the high-concentration graphene additive prepared by the method can be stably stored for more than 1 year without any agglomeration and precipitation. The graphene high-concentration additive prepared by the method is dissolved in lubricating oil through common stirring, and the prepared oil product is placed for two years without any agglomeration and precipitation and can be smoothly filtered through 5-micron and 10-micron filter membranes.
According to the invention, graphene substances form transition phase micro-floccules through electrostatic adsorption or hydrogen bond adsorption with a flocculating agent from a graphene hydrophilic phase solution which is easy to form uniform dispersion, then the transition phase micro-floccules are transferred to an organic medium to form a uniform graphene organic phase, and then the uniform graphene organic phase is transferred to an oil phase, so that the dispersed graphene is transferred from a water phase to the oil phase in a wet state, and the high-concentration graphene additive can be prepared. Compared with the prior art, the method has the advantages that the complex steps of organic modification, washing and drying and oil redissolution due to the fact that graphene is difficult to dissolve in oil are skipped, energy consumption and time consumption are avoided, the risk that the water phase-oil phase emulsion of graphene is difficult to completely separate and oil deterioration is easy to cause is avoided, the transfer of the water phase-organic phase-oil phase of graphene in a wet state is realized, the preparation time is short, the prepared graphene additive is high in concentration, large-scale operation is facilitated, and the process for industrially preparing a large amount of lubricating oil simply and conveniently by using the graphene concentrated additive is realized.
The above embodiments can be locally adjusted in different ways by those skilled in the art without departing from the principles and purposes of the present invention, for example, as an optimization, in order to achieve better anti-wear and anti-friction effects, specific modification of graphene can be performed in the aqueous phase link of graphene-based materials or the organic phase link after deflocculation, and functional groups helpful for improving the performance of lubricating oil are grafted, so as to realize high performance and multiple functions of graphene additives. Instead, in the technical scheme, the deflocculated graphene substances can be transferred into a complexing agent to be removed by rotary distillation of an organic solvent, so that the lubricant complexing agent added with graphene is obtained and is used for oil product production. The scope of the invention is indicated by the appended claims and is not limited to the foregoing detailed description, but rather is limited to the specific embodiments within the scope thereof.
Claims (10)
1. A process method for preparing a high-concentration graphene lubricating oil additive by a weak agglomeration-deagglomeration method mainly comprises the following steps:
1) dissolving graphene materials in a soluble medium, and forming a uniform solution in one or more modes of stirring, ultrasound or homogenization and the like;
2) preparing a graphene flocculant solution: the graphene flocculant is selected from alkali metal solution, organic ammonium salt, metal cations, polyacrylamide copolymer, alkylamine, stearic acid amide, N-dimethylethanolamine, dodecanol, hexadecanol and other substance solutions capable of forming electrostatic adsorption or hydrogen bonds with graphene surface groups, the solvent is selected from one or a combination of water, petroleum ether, ethanol, N-heptane and other solvents, and the concentration of the flocculant is 1-30%;
3) dropping the flocculant solution into the graphene substance solution, separating floccules from a hydrophilic medium by adopting one or more of filtration, centrifugation, extraction and desiccant water absorption methods, transferring the wet graphene substance floccules into an organic solvent, and dispersing the floccules by using one or more of ultrasound, homogenization and stirring to form a homogeneous graphene substance organic solution.
4) Adding base oil into the graphene organic solution, adding a dispersing agent, and uniformly stirring at the speed of 100-5000 rpm;
5) and removing the volatile organic solvent by using reduced pressure distillation modes such as rotary evaporation and the like to obtain the 1-10% high-concentration stably-dispersed graphene lubricating oil additive.
2. The process method according to claim 1, wherein the graphene-like material is graphene with a transverse sheet diameter of 100nm to 10 μm, 1 to 5 layers, an oxygen content of 0 to 50%, an epoxy group and a hydroxyl group on the surface, and a carboxyl functional group on the edge, and derivatives or combinations thereof.
3. A process as claimed in claim 1 or 2 wherein said hydrophilic medium includes but is not limited to water, ethanol, isopropanol or combinations thereof.
4. The process of claim 3, wherein the dispersant is one or more selected from silane coupling agent, titanate coupling agent, mono-alkenyl succinimide, di-butyl imide, poly-isobutylene succinimide, oleic acid, stearic acid, cetyl trimethyl ammonium bromide, etc.
5. The process method according to claim 4, wherein the base oil is one or more of group I, group II, group III base oil, finished oil or vegetable oil, and the base oil is added in an amount of 10-100 times (by weight) that of the graphene-based material.
6. The process method according to claim 5, wherein with the dropwise addition of the flocculant solution, molecules of the flocculant and graphene form weak agglomeration through electrostatic adsorption or hydrogen bonds, the dropwise addition amount of the flocculant is controlled, the dropwise addition is stopped when a micro-flocculation state occurs, and the ratio of the graphene substances to the flocculant is 1: 10-10: 1.
7. The process according to claim 1 or 2, wherein the concentration of the graphene-like substance in the solvent is 1-10% (by weight).
8. The process according to claim 1, wherein the aqueous stabilizing solution of graphene is commercially available.
9. The process of claim 1 or 2, wherein the organic solvent is selected from the group consisting of petroleum ether, isopropanol, ethanol, n-heptane, and combinations thereof.
10. A high concentration graphene lubricant additive prepared according to the process of any one of claims 1 to 9.
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Application publication date: 20200117 |