CN111876223B - Modified carbon nanotube ionic liquid lamellar liquid crystal lubricant and preparation method thereof - Google Patents
Modified carbon nanotube ionic liquid lamellar liquid crystal lubricant and preparation method thereof 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
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular 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
- 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
- C10M2201/14—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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
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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
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/108—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
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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
- C10M2223/00—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions
- C10M2223/02—Organic non-macromolecular compounds containing phosphorus as ingredients in lubricant compositions having no phosphorus-to-carbon bonds
- C10M2223/04—Phosphate esters
Abstract
The scheme relates to a modified carbon nanotube ionic liquid lamellar liquid crystal lubricant and a preparation method thereof. According to the invention, the stearyl alcohol modified carbon nano tube is introduced into the ionic liquid lamellar liquid crystal, so that the dispersity and lubricity of the carbon nano tube are improved, and the problems of creeping and leakage in the use process of the lubricant are solved to a certain extent; the modified carbon nanotube ionic liquid lamellar liquid crystal lubricant prepared by the invention is a semi-liquid semi-solid lubricant, achieves better balance in antifriction, anti-wear and anti-creep properties, and can be applied to lubrication of balls, rollers, bearing rings and the like.
Description
Technical Field
The invention relates to the technical field of lubrication, in particular to a modified carbon nano tube ionic liquid lamellar liquid crystal lubricant and a preparation method thereof.
Background
Friction is ubiquitous, and most of energy consumption in the world is used for resisting friction, so that friction is reduced, and wear is an effective way for improving energy utilization rate. The use of lubricating oils and greases is a common method of reducing friction and wear. At present, the lubrication modes mainly comprise solid lubrication and liquid lubrication. Compared with liquid lubrication, solid lubrication has the defects of large friction resistance, incapability of self-repairing and the like, which are difficult to overcome, and liquid lubrication has the defects of lack of a backflow supplementing mechanism, certain volatility and easiness in creeping loss due to complex environmental factors such as microgravity, vacuum and the like. The creeping motion often affects the machining precision and the surface roughness of the machine tool, and even generates waste products or fails when the creeping motion is serious. The creeping motion is mainly related to the difference between static friction coefficients and dynamic friction coefficients of sliding guide surfaces and the magnitude of the static friction coefficient, and the creeping motion is also related to the temperature.
In recent years, semisolid lubricants formed by compounding ionic liquids and lamellar liquid crystals have the advantages of low vapor pressure, nonvolatility, incombustibility, excellent thermal stability and the like, and certain test results are obtained in research of various mechanical equipment, space environments and micro-nano electromechanical systems, but the problems of leakage, creeping and the like in the using process are still not effectively solved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to prepare the semi-solid lubricant with the anti-creeping performance by introducing the compounding of the carbon nano tube and the ionic liquid lamellar liquid crystal.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a modified carbon nanotube ionic liquid lamellar liquid crystal lubricant comprises the following steps:
s1, modification of the carbon nano tube:
1) placing the carbon nano tube in a mixed solution of sulfuric acid and nitric acid, performing ultrasonic dispersion for 1h, then refluxing in a water bath at the temperature of 80 ℃ for 4h, filtering, washing until the filtrate is neutral, drying, and grinding to obtain an acidified carbon nano tube;
2) placing the acidified carbon nanotubes in SOCl 2 Performing ultrasonic treatment for 0.5h, stirring and refluxing for 2h at 80 ℃ under the action of DMF, filtering, drying and grinding to obtain the carbon nanotube of acyl chloride;
3) placing the acyl chloride carbon nano tube in a mixed solution of DMF and stearyl alcohol, performing ultrasonic dispersion for 0.5h, stirring and refluxing for 24h at 80 ℃, filtering, washing and drying to obtain a stearyl alcohol modified carbon nano tube;
s2, dissolving a surfactant in water, adding the stearyl alcohol modified carbon nano tube, uniformly mixing, and performing ultrasonic dispersion for 2 hours to obtain a carbon nano tube dispersion liquid;
and S3, adding the surfactant, the ionic liquid and the carbon nano tube dispersion liquid into a container, uniformly stirring, and standing for 2-24h to obtain the carbon nano tube layered liquid crystal lubricant.
Preferably, in the preparation method, the volume ratio of the mixed solution of sulfuric acid and nitric acid is 3: 1.
Preferably, in the preparation method, the mass ratio of the modified carbon nanotube, the surfactant and the water is (0.05-0.1): (0.1-1): 100.
preferably, in the preparation method, the surfactant is selected from one or more of Brij30, Tween-80 and Triton X-100.
Preferably, in the preparation method, the mass ratio of the surfactant, the ionic liquid and the carbon nanotube dispersion liquid is (40-55): (7-12): (25-33).
Preferably, in the preparation method, the ionic liquid is dibutyl-1- (2-propylbenzimidazolyl) phosphate (BP 304).
The modified carbon nanotube ionic liquid lamellar liquid crystal lubricant prepared by the preparation method of any one of the above.
The tube wall of the carbon nano tube has some defects, the end can be opened by using a strong oxidant and oxidized into carboxyl, and then the aim of modifying the carbon nano tube can be achieved by connecting different chemical substances and groups. According to the invention, the carbon nano tube is acidified by using a mixed solution of nitric acid and sulfuric acid, and then converted into acyl chloride, and further reacted with stearyl alcohol to obtain the modified carbon nano tube.
The lamellar liquid crystal is usually composed of a surfactant/co-surfactant/water three-component system, and formed bilayers and water layers are arranged at intervals and in parallel to form a long-range ordered and short-range unordered lamellar structure. Just because the long layers of the lamellar liquid crystals are orderly arranged, the layers can slide relatively, and therefore, the lubricating property is better than that of a common lubricant. Dibutyl-1- (2-propyl benzimidazolyl) phosphate ionic liquid is considered as a novel green solvent, and the novel green solvent is introduced into a lamellar liquid crystal system instead of a cosurfactant, so that the prepared lamellar liquid crystal lubricant has the advantages of difficult volatilization, no pollution, recycling and the like. Meanwhile, the lamellar liquid crystal finally formed by compounding the modified carbon nano tubes in the lamellar liquid crystal lubricant is a semi-liquid semi-solid lubricant, and compared with solid lubricating oil and liquid lubricating oil, the lamellar liquid crystal lubricant has good friction-reducing and wear-resisting properties and effectively reduces creeping motion in the using process.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the stearyl alcohol modified carbon nano tube is introduced into the ionic liquid lamellar liquid crystal, so that the dispersity and the lubricity of the carbon nano tube are improved, and the problems of creeping and leakage existing in the use process of the lubricant are reduced to a certain extent; the modified carbon nanotube ionic liquid lamellar liquid crystal lubricant prepared by the invention is a semi-liquid semi-solid lubricant, achieves better balance in antifriction, anti-wear and anti-creep properties, and can be applied to lubrication of balls, rollers, bearing rings and the like.
Drawings
FIG. 1 is a graph of 0.05% S-CNT/Brij30/BP304/H prepared in example 2 of the present invention 2 A polarizing micrograph of an O-system layered liquid crystal.
FIG. 2 is a graph of 0.05% S-CNT/Brij30/BP304/H prepared in example 2 of the present invention 2 Small angle X-scattering diagram of O-system lamellar liquid crystals.
FIG. 3 shows S-CNT/Brij30/BP304/H prepared by examples 2 to 7 of the present invention 2 A friction coefficient map of the O-system lamellar liquid crystal lubricant.
FIG. 4 shows S-CNT/Brij30/BP304/H prepared by examples 2 to 7 of the present invention 2 A graph of the coefficient of friction of the O-system lamellar liquid crystal lubricant versus the S-CNT content.
FIG. 5 shows S-CNT/Brij30/BP304/H prepared by examples 2 to 7 of the present invention 2 Graph of wear volume versus S-CNT content for O-system lamellar liquid crystalline lubricants.
FIG. 6 is a graph of 0.20% S-CNT/Brij30/BP30 prepared in examples 5 and 7 of the present invention4/H 2 A creep speed curve diagram of the O-system lamellar liquid crystal lubricant under the temperature gradient.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: preparation of modified carbon nanotubes
Weighing 0.5g of carbon nano tube, placing the carbon nano tube in 50mL of mixed solution of sulfuric acid/nitric acid (v/v 3:1), performing ultrasonic dispersion for 1h, refluxing in water bath at 80 ℃ for 4h, filtering, repeatedly washing with a large amount of deionized water and acetone until the filtrate is neutral, drying and grinding; placing the ground carbon nanotubes in 50mL of SOCl 2 Performing ultrasonic treatment for 0.5h, using DMF as a catalyst, stirring and refluxing for 2h at 80 ℃, filtering, drying and grinding for later use; according to the carbon nano tube: and (2) weighing the treated carbon nano tube and stearyl alcohol respectively according to the mass ratio of 1:5, placing the carbon nano tube and the stearyl alcohol into a DMF solution, ultrasonically dispersing for 0.5h, stirring and refluxing for 24h at 80 ℃, filtering, washing and drying to obtain the stearyl alcohol modified carbon nano tube.
Example 2: preparation of 0.05% S-CNT Ionic liquid lamellar liquid Crystal Lubricant
Weigh 0.1g Brij30 in a 100mL beaker to give a 0.1 wt% aqueous solution of Brij 30; then, 50mg of the modified carbon nanotube of example 1 was added to the solution, and the mixture was sonicated in a sonicator for 24 hours, to finally obtain a uniform black dispersion. According to the mass ratio Brij30/BP304/H 2 Weighing the carbon nanotube dispersion liquid instead of water, uniformly mixing at about 70 ℃, centrifuging, stirring, and repeating the two steps to fully and uniformly mix the sample. Placing the mixture in a constant temperature box (25 +/-0.1) DEG C for more than two weeks to reach balance, and preparing to obtain the carbon nano tube ionic liquid lamellar liquid crystal lubricant.
Example 3: preparation of 0.1% S-CNT Ionic liquid lamellar liquid Crystal Lubricant
Weigh 0.1g Brij30 in a 100mL beaker to give a 0.1 wt% aqueous solution of Brij 30; then, 100mg of the modified carbon nanotube of example 1 was added to the solution, and the mixture was sonicated in a sonicator for 24 hours, to finally obtain a uniform black dispersion. According to the mass ratio Brij30/BP304/H 2 The procedure of example 2 was repeated except that the carbon nanotube dispersion was weighed with O55: 13:32 instead of water.
Example 4: preparation of 0.15% S-CNT Ionic liquid lamellar liquid Crystal Lubricant
Weigh 0.1g Brij30 in a 100mL beaker to give a 0.1 wt% aqueous solution of Brij 30; then 150mg of the modified carbon nanotube of example 1 was added to the solution, and the mixture was sonicated in a sonicator for 24h to finally obtain a uniform black dispersion. According to the mass ratio Brij30/BP304/H 2 The procedure of example 2 was repeated except that the carbon nanotube dispersion was weighed with O55: 13:32 instead of water.
Example 5: preparation of 0.20% S-CNT Ionic liquid lamellar liquid Crystal Lubricant
Weigh 0.1g Brij30 in a 100mL beaker to give a 0.1 wt% aqueous solution of Brij 30; then, 200mg of the modified carbon nanotube of example 1 was added to the solution, and the mixture was sonicated in a sonicator for 24 hours, to finally obtain a uniform black dispersion. According to the mass ratio Brij30/BP304/H 2 The procedure of example 2 was repeated except that the carbon nanotube dispersion was weighed with O55: 13:32 instead of water.
Example 6: preparation of 0.25% S-CNT Ionic liquid lamellar liquid Crystal Lubricant
Weigh 0.1g Brij30 in a 100mL beaker to give a 0.1 wt% aqueous solution of Brij 30; then, 250mg of the modified carbon nanotube of example 1 was added to the solution, and the mixture was sonicated in a sonicator for 24 hours, to finally obtain a uniform black dispersion. According to the mass ratio Brij30/BP304/H 2 The procedure of example 2 was repeated except that the carbon nanotube dispersion was weighed with O55: 13:32 instead of water.
Example 7:
according to the mass ratio Brij30/BP304/H 2 Weighing each of the materials with a weight ratio of 55:13:32The components are evenly mixed at about 70 ℃, centrifuged and stirred, and the two steps are repeatedly carried out, so that the sample is fully and evenly mixed. Placing the mixture in a constant temperature box (25 +/-0.1) DEG C for more than two weeks to balance the mixture, and preparing the carbon nano tube ionic liquid lamellar liquid crystal lubricant.
FIGS. 1 and 2 are a polarization micrograph and a small angle X-ray diffraction pattern, respectively, of a 0.05% S-CNT ionic liquid crystalline lubricant, showing Maltese crosses and oil streaks as seen in FIG. 1, indicating that the sample produced is a lamellar liquid crystalline single phase. In FIG. 2, the scattering factor ratio corresponding to the small-angle X scattering peak is 1:2, which is a typical characteristic of the lamellar liquid crystal, and further confirms that the ionic liquid lamellar liquid crystal containing the modified carbon nanotube is successfully prepared in the scheme.
It can be observed from FIG. 3 that the coefficient of friction of the pure lamellar liquid crystal is around 0.12, and the coefficient of friction is reduced by the addition of the S-CNT, and it can be seen from the combination of FIG. 3 and FIG. 4 that the coefficient of friction is gradually reduced as the content of the S-CNT is increased.
It can be observed from fig. 5 that the wear volume of the lamellar liquid crystal is reduced after the addition of S-CNT compared to the pure lamellar liquid crystal, and the wear volume is gradually reduced as the content of S-CNT is increased. Fig. 4 and fig. 5 both show that the ionic liquid lamellar liquid crystal lubricant prepared by the invention has good friction-reducing and wear-resisting properties.
FIG. 6 is a graph of creep rate of the lubricant at 50-70 deg.C, 2 deg.C per liter, from which it can be seen that the creep rate of the lubricant with S-CNT addition is significantly less than the lubricant without S-NCT addition. Moreover, the temperature is increased, so that the influence on the lubricant added with the S-CNT is much less, and the S-CNT is proved to be added to effectively reduce the creeping motion generated in the using process of the lubricant.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (6)
1. The preparation method of the modified carbon nanotube ionic liquid lamellar liquid crystal lubricant is characterized by comprising the following steps of:
s1: modification of carbon nanotubes:
a) placing the carbon nano tube in a mixed solution of sulfuric acid and nitric acid, performing ultrasonic dispersion for 1h, then refluxing in a water bath at the temperature of 80 ℃ for 4h, filtering, washing until the filtrate is neutral, drying, and grinding to obtain an acidified carbon nano tube;
b) placing the acidified carbon nanotubes in SOCl 2 Performing ultrasonic treatment for 0.5h, stirring and refluxing for 2h at 80 ℃ under the action of DMF, filtering, drying and grinding to obtain the carbon nanotube of acyl chloride;
c) placing the acyl chloride carbon nano tube in a mixed solution of DMF and stearyl alcohol, performing ultrasonic dispersion for 0.5h, stirring and refluxing for 24h at 80 ℃, filtering, washing and drying to obtain a stearyl alcohol modified carbon nano tube;
s2: dissolving a surfactant in water, adding the stearyl alcohol modified carbon nano tube, uniformly mixing, and performing ultrasonic dispersion for 2 hours to obtain a modified carbon nano tube dispersion liquid;
s3: adding a surfactant, an ionic liquid and the carbon nano tube dispersion liquid into a container, uniformly stirring, and standing for 2-24h to obtain a modified carbon nano tube ionic liquid lamellar liquid crystal lubricant;
the mass ratio of the modified carbon nano tube to the surfactant to the water is (0.01-0.05) to (0.1-0.5) to 100.
2. The method according to claim 1, wherein the mixed solution of sulfuric acid and nitric acid has a solution volume ratio of 3: 1.
3. The method according to claim 1, wherein the surfactants are selected from Brij30, Tween-80, Triton X-100.
4. The method according to claim 1, wherein the surfactant, the ionic liquid, and the modified carbon nanotube dispersion liquid are present in a mass ratio of (40-55) to (7-12) to (25-33).
5. The method according to claim 1, wherein the ionic liquid is dibutyl-1- (2-propylbenzimidazolyl) phosphate.
6. A modified carbon nanotube ionic liquid lamellar liquid crystal lubricant prepared by the preparation method of any one of claims 1 to 5.
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| CN113181436A (en) * | 2021-05-07 | 2021-07-30 | 扬州大学 | Hydroxyapatite/layered liquid crystal lubricant, preparation method and application thereof in dynamic drug release test |
| CN114015491B (en) * | 2021-11-23 | 2022-06-10 | 中国科学院宁波材料技术与工程研究所 | Lubricating oil additive containing modified nano carbon material and preparation method thereof |
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