CN111004665A - Preparation method of graphite-based nano titanium dioxide lubricating oil - Google Patents
Preparation method of graphite-based nano titanium dioxide lubricating oil Download PDFInfo
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- CN111004665A CN111004665A CN201911160010.0A CN201911160010A CN111004665A CN 111004665 A CN111004665 A CN 111004665A CN 201911160010 A CN201911160010 A CN 201911160010A CN 111004665 A CN111004665 A CN 111004665A
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- graphite
- titanium dioxide
- lubricating oil
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- nano titanium
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
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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
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/102—Aliphatic fractions
- C10M2203/1025—Aliphatic fractions used as base material
Abstract
The invention discloses a preparation method of graphite-based nano titanium dioxide lubricating oil, which is characterized by comprising the following steps: a. pulverizing graphite into micropowder with particle size of 4-10 μm; b. adding potassium permanganate, sulfuric acid, nitric acid and titanium tetrachloride into the micro-powder graphite, reacting for 100-; c. pulverizing again to particle size of 1-4 μm; d. and (3) carrying out surface modification by using oleic acid, adding the modified product into the lubricating oil base oil, and carrying out ultrasonic homogenization at 30-50 ℃. The invention has the beneficial effects that: the graphite is crushed to 1-4 mu m by adopting a physical method and a chemical method, and meanwhile, titanium dioxide is attached to the micron graphite base in a nano form to form the graphite-based nano titanium dioxide composite material, so that the pressure reduction and wear resistance and the self-repairing performance of the lubricating oil and the stability of the graphite in the lubricating oil are improved.
Description
Technical Field
The invention belongs to the technical field of nano lubricating oil, and relates to a preparation method of graphite-based nano titanium dioxide lubricating oil.
Background
In an automobile engine, the loss caused by mechanical friction accounts for 15% of the total power of the engine, and each 10% increase of mechanical loss results in 1.5% of additional fuel consumption, so that the additional emission pollution is more striking. The friction wear mainly occurs on the surface of a friction part, and the addition of the nano solid lubricant in the lubricating oil of an automobile engine is one of important methods for reducing the friction wear of the surface.
In recent years, the application of advanced carbon materials in the field of friction is greatly concerned, particularly the high-quality performance of graphite and composite materials thereof, and the application research of carbon materials in tribology enters a new hot trend. The graphite has excellent self-moistening performance, pressure reducing, wear resisting and self repairing performance owing to its special layered structure.
TiO2There are 3 crystal structures of the crystal structure,rutile, orchitian and ruthenian respectively. The basic composition structure of each ore is TiO2The lubricating oil is characterized in that octahedrons or different types of ores form a skeleton by sharing vertexes or sharing edges, the scale is 10-degree on the mohs hardness scale, the rutile type titanium dioxide is 6-6.5, and the anatase type titanium dioxide is 5-6.0, so that the pressure reduction and wear resistance of the lubricating oil can be improved, and the lubricating oil is non-toxic, harmless and good in stability.
The self-repairing capability of the existing graphite lubricating oil is insufficient, and the sulfur/phosphorus-containing pressure-reducing anti-wear additive is easy to corrode mechanical equipment, influences the use effect of the lubricating oil and causes damage to machinery.
Disclosure of Invention
The invention aims to solve the problem that the existing lubricating oil for automobile engines is not strong in pressure reduction wear resistance and self-repairing performance, and provides a preparation method of graphite-based nano titanium dioxide lubricating oil.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of graphite-based nano titanium dioxide lubricating oil is characterized by comprising the following steps:
a. adding high-purity graphite with carbon content of 99-99.999% into a jet mill at the speed of 0.4-0.6g/s, and crushing in high-pressure airflow of 0.7-1.0Mpa to obtain graphite with particle size of 4-10 μm;
b. adding potassium permanganate, sulfuric acid, nitric acid and titanium tetrachloride into the micro powder graphite obtained in the step a, and controlling the micro powder graphite: potassium permanganate: sulfuric acid: nitric acid: the mass ratio of titanium tetrachloride is 1: 1: 5: 1: 5, reacting at 25-28 ℃ for 140min, washing with deionized water, filtering, drying at 50-70 ℃ for 6-8h, and then expanding at high temperature in a muffle furnace (600-900 ℃) for 3-5s to obtain graphite-based nano titanium dioxide expanded graphite;
c. b, adding the graphite-based nano titanium dioxide expanded graphite obtained in the step b into a jet mill again at the speed of 0.4-0.6g/s, and crushing in high-pressure airflow of 0.7-1.0Mpa to obtain graphite-based nano titanium dioxide micro powder with the particle size of 1-4 mu m;
d. and c, performing surface modification on the graphite-based nano titanium dioxide micropowder obtained in the step c by using oleic acid, controlling the mass ratio of the graphite-based nano titanium dioxide micropowder to the oleic acid to be 1:2, stirring for 30min, adding the graphite-based nano titanium dioxide micropowder subjected to surface modification by using oleic acid into lubricating oil base oil (250 SN base oil), and controlling the volume ratio of the graphite-based nano titanium dioxide micropowder to the lubricating oil base oil to be 1: and (3) uniformly dispersing the mixture by ultrasonic at the temperature of 20 ℃ to 30-50 ℃ to obtain the graphite-based nano titanium dioxide lubricating oil.
Lubricating oil is mechanical nutrient solution, can ensure the normal operation of machinery, reduces the injury. Graphite and titanium dioxide have excellent pressure-reducing and wear-resisting properties in lubricating oil due to their own properties. The compounding of the graphite and the titanium dioxide can enhance the pressurizing and wear-resisting performance of the composite material, and is more convenient for modification and lubricating oil blending.
The invention has the beneficial effects that: the graphite is crushed to 1-4 microns by a physical method and a chemical method, and meanwhile, titanium dioxide is attached to the micron graphite base in a nano form to form the graphite-based nano titanium dioxide composite material, so that the pressure reduction and wear resistance and the self-repairing performance of the lubricating oil are improved to a great extent, and the stability of the graphite in the lubricating oil is improved.
Detailed Description
Example 1
A preparation method of graphite-based nano titanium dioxide lubricating oil comprises the following specific implementation steps:
1. adding natural crystalline flake graphite (carbon content 99.9%) into jet mill (high pressure air flow 0.8 Mpa) at 0.5g/s to jet mill, repeating the operation for ten times to twenty times to obtain micropowder graphite with particle size of 5 μm;
2. adding 5g of potassium permanganate, 25g of sulfuric acid, 5g of nitric acid and 25g of titanium tetrachloride into 5g of micro-powder graphite, reacting at room temperature for 120min, washing with deionized water, filtering to remove redundant acid, drying at 70 ℃ for 6h, and then expanding at high temperature in a muffle furnace (900 ℃) for 3-5s to obtain graphite-based nano titanium dioxide expanded graphite;
3. b, adding the graphite-based nano titanium dioxide expanded graphite obtained in the step b into a jet mill again at the speed of 0.5g/s, and crushing in a high-pressure air flow of 0.8MPa to obtain graphite-based nano titanium dioxide micro powder with the particle size of 3 microns;
4. weighing 5g of graphite-based nano titanium dioxide micro powder, adding 10g of oleic acid, stirring in a 60r/s magnetic stirrer for 30min, adding 10mL of graphite-based nano titanium dioxide micro powder subjected to surface modification by the oleic acid into 100mL of 250SN base oil, and performing ultrasonic dispersion uniformly at 40 ℃ to obtain the graphite-based nano titanium dioxide lubricating oil.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (1)
1. A preparation method of graphite-based nano titanium dioxide lubricating oil is characterized by comprising the following steps:
a. adding high-purity graphite with carbon content of 99-99.999% into a jet mill, and pulverizing in high-pressure air flow of 0.7-1.0Mpa to obtain graphite with particle size of 4-10 μm;
b. adding potassium permanganate, sulfuric acid, nitric acid and titanium tetrachloride into the micro powder graphite obtained in the step a, and controlling the micro powder graphite: potassium permanganate: sulfuric acid: nitric acid: the mass ratio of titanium tetrachloride is 1: 1: 5: 1: 5, reacting at 25-28 ℃ for 140min for 100-;
c. b, adding the graphite-based nano titanium dioxide expanded graphite obtained in the step b into the jet mill again, and crushing in high-pressure air flow of 0.7-1.0Mpa to obtain graphite-based nano titanium dioxide micro powder with the particle size of 1-4 mu m;
d. and c, performing surface modification on the graphite-based nano titanium dioxide micropowder obtained in the step c by using oleic acid, controlling the mass ratio of the graphite-based nano titanium dioxide micropowder to the oleic acid to be 1:2, stirring for 30min, adding the graphite-based nano titanium dioxide micropowder subjected to surface modification by using oleic acid into lubricating oil base oil, and controlling the volume ratio of the graphite-based nano titanium dioxide micropowder to the lubricating oil base oil to be 1: and (3) uniformly dispersing the mixture by ultrasonic at the temperature of 20 ℃ to 30-50 ℃ to obtain the graphite-based nano titanium dioxide lubricating oil.
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| CN111004665A true CN111004665A (en) | 2020-04-14 |
| CN111004665B CN111004665B (en) | 2022-05-17 |
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Citations (6)
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| CN101077988A (en) * | 2007-06-29 | 2007-11-28 | 燕山大学 | Method for preparing nano expanded graphite lubricating oil additive |
| CN104017628A (en) * | 2014-06-18 | 2014-09-03 | 中国人民解放军装甲兵工程学院 | Method for preparing composite anti-friction and anti-wear additive of graphene-loaded nanoparticles |
| CN104556221A (en) * | 2014-12-05 | 2015-04-29 | 常州轻工职业技术学院 | TiO2/lamellar graphite nano composite material as well as preparation method thereof |
| CN106190432A (en) * | 2016-07-07 | 2016-12-07 | 重庆德领科技有限公司 | A kind of modified graphene lubricating oil of polymolecularity and preparation method thereof |
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2019
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| CN104556221A (en) * | 2014-12-05 | 2015-04-29 | 常州轻工职业技术学院 | TiO2/lamellar graphite nano composite material as well as preparation method thereof |
| CN106190432A (en) * | 2016-07-07 | 2016-12-07 | 重庆德领科技有限公司 | A kind of modified graphene lubricating oil of polymolecularity and preparation method thereof |
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