CN116590069A - Lubricant with mechanical self-adaption as well as preparation method and application thereof - Google Patents
Lubricant with mechanical self-adaption as well as preparation method and application thereof Download PDFInfo
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- CN116590069A CN116590069A CN202310587528.2A CN202310587528A CN116590069A CN 116590069 A CN116590069 A CN 116590069A CN 202310587528 A CN202310587528 A CN 202310587528A CN 116590069 A CN116590069 A CN 116590069A
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- lubricant
- lipoic acid
- lithium
- gel
- butoxide
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- 239000000314 lubricant Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- AGBQKNBQESQNJD-UHFFFAOYSA-M lipoate Chemical compound [O-]C(=O)CCCCC1CCSS1 AGBQKNBQESQNJD-UHFFFAOYSA-M 0.000 claims abstract description 85
- 235000019136 lipoic acid Nutrition 0.000 claims abstract description 85
- 229960002663 thioctic acid Drugs 0.000 claims abstract description 85
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 53
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000004519 grease Substances 0.000 claims abstract description 30
- 239000002199 base oil Substances 0.000 claims abstract description 25
- 230000001050 lubricating effect Effects 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002562 thickening agent Substances 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 69
- LZWQNOHZMQIFBX-UHFFFAOYSA-N lithium;2-methylpropan-2-olate Chemical compound [Li+].CC(C)(C)[O-] LZWQNOHZMQIFBX-UHFFFAOYSA-N 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 238000005461 lubrication Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 229940068886 polyethylene glycol 300 Drugs 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 2
- 230000003044 adaptive effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000010687 lubricating oil Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 230000009194 climbing Effects 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 19
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 17
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 12
- 238000003756 stirring Methods 0.000 description 11
- 230000035515 penetration Effects 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 1
- 229920002556 Polyethylene Glycol 300 Polymers 0.000 description 1
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Classifications
-
- 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
- C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
- C10M117/02—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D339/00—Heterocyclic compounds containing rings having two sulfur atoms as the only ring hetero atoms
- C07D339/02—Five-membered rings
- C07D339/04—Five-membered rings having the hetero atoms in positions 1 and 2, e.g. lipoic acid
-
- 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
- C10M169/02—Mixtures of base-materials and thickeners
-
- 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
- C10M2209/1045—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only used as base material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/64—Environmental friendly compositions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/01—Emulsions, colloids, or micelles
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Lubricants (AREA)
Abstract
The invention relates to the technical field of lubricating materials, and provides a lubricant with mechanical self-adaptability, and a preparation method and application thereof. According to the invention, the gel lubricant or lubricating grease is prepared by taking the lithium lipoic acid as a gel factor or thickener, the lithium lipoic acid has the advantages of simple structure, easiness in synthesis, low cost, excellent wear resistance and antifriction property, strong bearing capacity, mechanical self-adaption and capability of capturing base oil again through rapid self-assembly in the use process, so that the problems of leakage, climbing and the like of lubricating oil are prevented. In addition, the lubricant provided by the invention is green and nontoxic, has few additive types, simple preparation method and wide application prospect.
Description
Technical Field
The invention relates to the technical field of lubricants, in particular to a lubricant with mechanical self-adaption as well as a preparation method and application thereof.
Background
Friction and wear cause a significant amount of energy and economic loss, so it is important to use advanced lubricants to reduce friction and wear. Gel lubricants are a new type of semisolid lubricant that has excellent thermoreversibility and thixotropic properties, and have been receiving great attention because of their low coefficient of friction and good antiwear properties during friction. The gel lubricant is solid like grease on the surface, but has fluidity like lubricating oil in the using process, and has the dual characteristics of lubricating oil and grease.
In the previous research, the applicant has designed and prepared a class of small molecule gelators which gel a variety of lubricating oils (1. Cai, m.; liang, y.; zhou, f.; lie, w. Journal ofMaterials Chemistry 2011,21,13399-13405.2.Yu, q.; fan, m.; li, d.; song, z.; cai, m.; zhou, f.; liu, w.acs applied materials & interfaces 2014,6,15783-94.3.Cai, m.; liang, y.; zhou, f.; lie, w. Journal of Materials Chemistry 2011,21,13399-13405.4.201810098226.8). The novel gel lubricant prepared in the literature can effectively avoid the creeping of lubricating oil, and has better antifriction and antiwear properties than basic lubricating liquid and lubricating grease. However, the above reported gel lubricants have problems in that the synthesis procedure of the gelator is complicated and the cost is expensive, which limits their application in tribology. Thus, the design and preparation of high performance, low cost supramolecular gel lubricants remains one of the research hotspots in this area.
Disclosure of Invention
In view of this, the present invention provides a lubricant with mechanical adaptivity, and a preparation method and application thereof. According to the invention, the lithium lipoic acid is used as a gel factor or a thickener, the preparation method of the lithium lipoic acid is simple, the cost is low, and the obtained lubricant (gel lubricant or lubricating grease) has excellent tribological performance and mechanical self-adaptability.
In order to achieve the above object, the present invention provides the following technical solutions:
application of lithium lipoic acid as a gel factor or thickener in a lubricant; the structure of the lithium lipoic acid is shown as a formula I:
the invention also provides a lubricant with mechanical self-adaption, which comprises base oil and lithium lipoic acid; the base oil is polyethylene glycol; the lubricant is gel lubricant or lubricating grease.
Preferably, the mass fraction of the lithium lipoic acid in the lubricant with mechanical self-adaption is 1-20%.
Preferably, the polyethylene glycol includes one or more of polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, and polyethylene glycol 600.
The invention also provides a preparation method of the lubricant with mechanical self-adaption, when the lubricant is a gel lubricant, the preparation method comprises the following steps:
(1) Mixing lipoic acid, methanol and lithium tert-butoxide for reaction to obtain lipoic acid lithium gel factor;
(2) Heating, mixing and cooling the lithium lipoic acid gel factor and base oil to obtain the gel lubricant;
when the lubricant is grease, the preparation method comprises the following steps:
(a) Heating and mixing lipoic acid and base oil to obtain a mixture;
(b) And mixing the mixture with a methanol solution of lithium tert-butoxide for reaction, and sequentially carrying out heat preservation, cooling and grinding after the reaction is finished to obtain the lubricating grease.
Preferably, the molar ratio of the lipoic acid to the lithium tert-butoxide in the step (1) is 1-1.2:1; the molar ratio of the lipoic acid in the step (a) to the lithium tert-butoxide in the step (b) is 1-1.2:1.
Preferably, in the step (1), the method for mixing lipoic acid, methanol and lithium tert-butoxide comprises the following steps: lipoic acid is added into methanol, stirred at 30-42 ℃ until dissolved, and then lithium tert-butoxide is added.
Preferably, the reaction temperature in the step (1) is 48-55 ℃ and the reaction time is 3-6 h; the heating and mixing temperature in the step (2) is 60-80 ℃.
Preferably, the temperature of the reaction in the step (b) is 70-80 ℃ and the time is 10-20 min; the temperature of the heat preservation is 110-130 ℃, and the heat preservation time is 5-15 min.
The invention also provides the lubricant with mechanical self-adaption according to the scheme or the application of the lubricant with mechanical self-adaption prepared by the preparation method according to the scheme in the field of lubrication of mechanical parts.
The invention provides application of lithium lipoic acid as a gel factor or a thickener in a lubricant, and the invention prepares the lubricant by using the lithium lipoic acid as the gel factor or the thickener, and has simple structure, easy synthesis, low cost and wide application prospect in the field of lubricants.
The invention also provides a lubricant with mechanical self-adaption, and the lubricant comprises base oil and lithium lipoic acid, and can be divided into gel lubricant and lubricating grease according to different preparation methods. The lithium lipoic acid contains dynamic covalent bonds, and the gel lubricant prepared by the lithium lipoic acid has both the stimulus response of physical gel and the stability of chemical gel, can obviously improve the tribological performance of lubricating oil, and has very excellent antifriction and antiwear performances and extremely high bearing capacity (more than 1000N). The lubricant provided by the invention has good heat stability, mechanical stability and self-recovery performance, has the advantages of faster self-recovery and stronger mechanical performance compared with the conventional supermolecule gel lubricant, has excellent antifriction and wear-resistant performance, and also has mechanical self-adaptability, and can recapture base oil through rapid self-assembly in the use process, thereby preventing the problems of leakage, climbing and the like of lubricating oil. In addition, the lubricant provided by the invention is green and nontoxic, has few additive types, simple preparation method and low cost, and has wide application prospect.
Drawings
FIG. 1 is a graph showing the results of the load carrying capacity test of PEG400 and gel lubricant A1;
FIG. 2 shows the trend of the modulus of the gel lubricant A1 when the stress gradually increases and decreases;
FIG. 3 shows the trend of the modulus change of the gel lubricant A1 when the stress is alternated;
fig. 4 is a thermogram of gel lubricants A1-A3 and base oil PEG 400.
Detailed Description
The invention provides an application of lithium lipoic acid as a gel factor or a thickening agent in a lubricant; the structure of the lithium lipoic acid is shown as a formula I:
in the present invention, the lubricant includes a gel lubricant and grease, and when the gel lubricant is prepared using the lithium lipoic acid, the lithium lipoic acid functions as a gel factor, and when the grease is prepared using the lithium lipoic acid, the lithium lipoic acid functions as a thickener. The lithium lipoic acid is used as a gel factor or a thickening agent to prepare gel lubricant or grease, and the obtained gel lubricant and grease have good mechanical properties, excellent tribological properties, good stability and lower cost.
The invention also provides a lubricant with mechanical self-adaption, which comprises base oil and lithium lipoic acid; the base oil is polyethylene glycol (PEG); the lubricant is gel lubricant or lubricating grease.
In the present invention, the PEG preferably includes one or more of PEG200, PEG300, PEG400, and PEG 600.
In the present invention, the mass fraction of lithium lipoic acid in the lubricant having mechanical adaptivity is preferably 1 to 20%, more preferably 3 to 15%, and the balance is base oil.
The invention also provides a preparation method of the lubricant with mechanical self-adaption, and the lubricant provided by the invention is divided into gel lubricant and lubricating grease, and the preparation method is respectively described below.
In the present invention, when the lubricant is a gel lubricant, the preparation method includes the steps of:
(1) Mixing lipoic acid, methanol and lithium tert-butoxide for reaction to obtain lipoic acid lithium gel factor;
(2) And heating, mixing and cooling the lithium lipoic acid gel factor and the base oil to obtain the gel lubricant.
The method mixes lipoic acid, methanol and lithium tert-butoxide for reaction (marked as first reaction) to obtain the lipoic acid lithium gel factor. In the present invention, the molar ratio of the lipoic acid to the lithium tert-butoxide is preferably 1 to 1.2:1, more preferably 1 to 1.1:1; the mass ratio of the lipoic acid to the methanol is preferably 1:50; the method of mixing lipoic acid, methanol and lithium t-butoxide preferably comprises: adding lipoic acid into methanol, stirring at 30-42 ℃ until the lipoic acid is dissolved, and then adding lithium tert-butoxide; the temperature of the first reaction is preferably 48-55 ℃, more preferably 50-52 ℃, and the reaction time is preferably 3-6 h, more preferably 4-5 h; in the specific embodiment of the invention, the temperature of the reaction system is preferably raised to 48-55 ℃ after the lithium tert-butoxide is added, and the reaction system is stirred until the lithium tert-butoxide is completely dissolved and then is subjected to heat preservation reaction for 3-6 hours. After the reaction is finished, the obtained product liquid is preferably subjected to rotary evaporation and then dried to obtain the lithium lipoic acid gel factor.
After the lithium lipoic acid gel factor is obtained, the lithium lipoic acid gel factor and the base oil are heated and mixed (marked as first heating and mixing) and then cooled, so that the gel lubricant is obtained. In the present invention, the temperature of the first heated mixing is preferably 60 to 80 ℃, more preferably 65 to 75 ℃, and the first heated mixing is preferably performed under stirring conditions; the invention has no special requirement on the time of the first heating and mixing, and the stirring is stopped after the lithium lipoic acid gel factor is completely dissolved, and the stirring is stopped, and the temperature is cooled to the room temperature.
In the preparation of the gel lubricant, lithium lipoic acid powder is synthesized in methanol solution, and then the lithium lipoic acid powder and base oil are heated and mixed, and the gel lubricant is obtained after cooling.
In the present invention, when the lubricant is grease, the preparation method includes the steps of:
(a) Heating and mixing lipoic acid and base oil to obtain a mixture;
(b) And mixing the mixture with a methanol solution of lithium tert-butoxide for reaction, and sequentially carrying out heat preservation, cooling and grinding after the reaction is finished to obtain the lubricating grease.
The lipoic acid and the base oil are heated and mixed (marked as second heating and mixing) to obtain the mixture. In the present invention, the temperature of the second heated mixing is preferably 40 to 50 ℃, and the second heated mixing is preferably performed under stirring conditions; the invention has no special requirement on the time of the second heating and mixing, and the lipoic acid is stirred until the lipoic acid is completely dissolved.
After the obtained mixture is obtained, the mixture is mixed with a methanol solution of lithium tert-butoxide for reaction (marked as a second reaction), and after the reaction is finished, heat preservation, cooling and grinding are sequentially carried out to obtain the lubricating grease. In the present invention, the molar ratio of the lipoic acid to the lithium tert-butoxide is preferably 1 to 1.2:1, more preferably 1 to 1.1:1; in the methanol solution of the lithium tert-butoxide, the dosage ratio of the lithium tert-butoxide to the methanol is preferably 1:50; in the invention, preferably, the methanol solution of the lithium tert-butoxide is dropwise added to the mixture; the temperature of the second reaction is preferably 70-80 ℃ and the time is preferably 10-20 min, and the time of the second reaction is counted from the beginning of the dropwise addition of the lithium tert-butoxide; the temperature of the heat preservation is preferably 110-130 ℃, more preferably 115-125 ℃, and the time of the heat preservation is preferably 5-15 min, more preferably 10min; the cooling is preferably natural cooling to room temperature; the grinding is preferably performed by three-roll grinding, and the number of grinding is preferably 3.
In the preparation of the grease, lipoic acid and lithium tert-butoxide directly react in a base oil system to generate lithium lipoic acid, and then the semisolid grease is obtained through cooling and grinding.
The invention also provides the lubricant with mechanical self-adaption according to the scheme or the application of the lubricant with mechanical self-adaption prepared by the preparation method according to the scheme in the field of lubrication of mechanical parts. The invention is not particularly limited to the particular method of application described, as it is known to those skilled in the art.
The following description of the embodiments of the present invention will clearly and fully describe the technical solutions of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Lipoic acid (0.01 mol) is added into 20mL of methanol, heated (40 ℃) and stirred until the lipoic acid is dissolved, then lithium tert-butoxide (0.01 mol) is added, the mixture is continuously heated to 50 ℃, the mixture is stirred until the lipoic acid is completely dissolved, the mixture is maintained for 4 hours, and after the reaction is complete, the mixture is distilled to dryness and dried, and then the gel factor (lithium lipoic acid) is obtained.
After adding 0.3g of a gel factor (lithium lipoic acid) to 9.7g of PEG400 and stirring the mixture to complete dissolution by heating (60 ℃), the heating and stirring are stopped, and the mixture is cooled to room temperature to obtain a lithium lipoic acid supermolecule gel lubricant, which is denoted as A1.
Example 2
The lithium lipoic acid was prepared in the same manner as in example 1.
After adding 0.5g of a gel factor (lithium lipoic acid) to 9.5g of PEG400 and stirring the mixture to be completely dissolved by heating (60 ℃), the heating and stirring are stopped, and the mixture is cooled to room temperature to obtain a lithium lipoic acid supermolecule gel lubricant, which is denoted as A2.
Example 3
The lithium lipoic acid was prepared in the same manner as in example 1.
After adding 0.7g of a gel factor (lithium lipoic acid) to 9.3g of PEG400 and stirring the mixture to complete dissolution by heating (60 ℃), the heating and stirring are stopped, and the mixture is cooled to room temperature to obtain a lithium lipoic acid supermolecule gel lubricant, which is denoted as A3.
Example 4
To the beaker was added 0.24g of lipoic acid and 9.69g of PEG400, heated to 45℃and stirred until the lipoic acid was completely dissolved. 0.08g of lithium t-butoxide was dissolved in 10mL of methanol, and a solution of lithium t-butoxide was added dropwise to PEG 400. After reacting at 75 ℃ for 15min, heating to 120 ℃, preserving heat for 10min, cooling to room temperature, and grinding for three times by a three-roller mill to obtain lubricating grease, which is denoted as B1.
Example 5
To the beaker was added 0.40g of lipoic acid and 9.48g of PEG400, heated to 45℃and stirred until the lipoic acid was completely dissolved. 0.13g of lithium t-butoxide was dissolved in 10mL of methanol, and a solution of lithium t-butoxide was added dropwise to PEG 400. After reacting at 75 ℃ for 15min, heating to 120 ℃, preserving heat for 10min, cooling to room temperature, and grinding for three times by a three-roller mill to obtain lubricating grease, which is denoted as B2.
Example 6
To the beaker was added 0.56g of lipoic acid and 9.27g of PEG400, heated to 45℃and stirred until the lipoic acid was completely dissolved. 0.19g of lithium t-butoxide was dissolved in 10mL of methanol, and a solution of lithium t-butoxide was added dropwise to PEG 400. After reacting at 75 ℃ for 15min, heating to 120 ℃, preserving heat for 10min, cooling to room temperature, and grinding for three times by a three-roller mill to obtain lubricating grease, which is denoted as B3.
Performance testing
1. Coefficient of friction test
The frictional wear properties of the lithium lipoic acid supermolecule gel lubricant and the lubricating grease were evaluated by using an SRV-V micro-vibration frictional wear testing machine manufactured by German optimol grease company, and compared with PEG 400. The test conditions were: the load is 200N, the temperature is 25 ℃, the frequency is 25Hz, the amplitude is 1mm, the experimental time is 30min, the experimental test ball is AISI 52100 steel ball, and the lower sample is AISI 52100 steel block.
The test results are shown in Table 1.
TABLE 1 average coefficient of friction of PEG400, gel lubricants A1-A3, greases B1-B3
Sample numbering | PEG400 | A1 | A2 | A3 |
Average coefficient of friction | 0.1546 | 0.1057 | 0.1078 | 0.1034 |
Sample numbering | B1 | B2 | B3 | / |
Average coefficient of friction | 0.1103 | 0.1068 | 0.1031 | / |
As can be seen from the data in Table 1, the gel lubricants A1 to A3 and the greases B1 to B3 prepared according to the present invention each have a low friction coefficient.
2. Load bearing capability test
The load carrying capacity of the base oil PEG400 and the gel lubricant A1 prepared in example 1 were tested under the following conditions: the load is 100-1100N, the frequency is 25Hz, the amplitude is 1mm, the experimental time is 50min, the temperature is 25 ℃, the diameter of an experimental test ball is 10mm, and the lower sample is a steel block with the hardness of 700 HV.
The test results are shown in Table 2 and FIG. 1, and 3% gel in FIG. 1 represents the gel lubricant A1 prepared in example 1.
Table 2PEG400 and highest carrying capacity of example 1
From the results in table 2 and fig. 1, it can be seen that the gel lubricants provided by the present invention have significantly improved load bearing capacity compared to the base oil. The experimental result shows that the antifriction and antiwear performance of the lithium lipoic acid supermolecule gel lubricant is far better than that of the base oil PEG, and the lithium lipoic acid supermolecule gel lubricant has extremely low friction coefficient and extremely high bearing capacity. Further, the lubricants A2, A3 and B1, B2 and B3 were subjected to the load bearing capacity test, and the results showed that each lubricant had an excellent load bearing capacity.
3. Drop point and cone penetration test of grease
The drop point and cone penetration test results of the greases B1 to B3 prepared in examples 4 to 6 are shown in Table 3, the drop point test method is GB/T3498, and the working cone penetration test method is GB/T3498-2008.
TABLE 3 penetration and drop Point of greases B1 to B3
Sample numbering | B1 | B2 | B3 |
Drop point (DEG C) | 144 | 162 | 164 |
Work cone penetration (0.1 mm) | 390 | 360 | 308 |
According to the data in Table 3, the lubricating grease provided by the invention has higher high-temperature resistance and higher consistency, and can meet the use requirements.
4. Mechanical adaptivity test
The rheological properties of the gel lubricant prepared in example 1 were tested using an RS6000 rheometer manufactured by sameira to confirm its mechanical adaptivity. The test results are shown in FIGS. 2 to 3.
FIG. 2 shows the trend of the modulus of the gel lubricant A1 (test conditions: 5Hz,20 ℃ C.) when the stress gradually increases and decreases again; as can be seen from fig. 2, the gel lubricant A1 is changed from the gel state to the sol state during the gradual increase of the stress from 1Pa to 1000Pa, and fluidity occurs; when the stress was gradually reduced to 1Pa again, the gel state was gradually recovered.
FIG. 3 shows the trend of the modulus change of the gel lubricant A1 (test condition: 5Hz,20 ℃ C.) when the stress is alternated; as can be seen from fig. 3, the gel lubricant A1 has G' lower than G "under high shear stress, and the gel structure is broken to be converted into a sol state; under the condition of low shear stress, G 'is higher than G', and the lithium lipoic acid gradually self-assembles to recover to gel state.
In addition, mechanical self-adaptability tests are carried out on the lubricants A2, A3 and B1, B2 and B3, and the results show that the gel lubricant provided by the invention has better self-adaptability to mechanical force.
5. Thermal stability test
Thermal gravimetric tests were performed on the gel lubricants A1 to A3 and the base oil PEG400 prepared in examples 1 to 3, and the results are shown in fig. 4. As can be seen from fig. 4, the gel lubricant provided by the present invention has excellent thermal stability.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. Application of lithium lipoic acid as a gel factor or thickener in a lubricant; the structure of the lithium lipoic acid is shown as a formula I:
2. a lubricant with mechanical adaptivity, which is characterized by comprising base oil and lithium lipoic acid; the base oil is polyethylene glycol; the lubricant is gel lubricant or lubricating grease.
3. The lubricant with mechanical adaptivity according to claim 2, wherein the mass fraction of lithium lipoic acid in the lubricant with mechanical adaptivity is 1-20%.
4. The mechanically adaptive lubricant of claim 2, wherein the polyethylene glycol comprises one or more of polyethylene glycol 200, polyethylene glycol 300, polyethylene glycol 400, and polyethylene glycol 600.
5. The method for producing a lubricant having mechanical adaptivity according to any one of claims 2 to 4, characterized in that when the lubricant is a gel lubricant, the method comprises the steps of:
(1) Mixing lipoic acid, methanol and lithium tert-butoxide for reaction to obtain lipoic acid lithium gel factor;
(2) Heating, mixing and cooling the lithium lipoic acid gel factor and base oil to obtain the gel lubricant;
when the lubricant is grease, the preparation method comprises the following steps:
(a) Heating and mixing lipoic acid and base oil to obtain a mixture;
(b) And mixing the mixture with a methanol solution of lithium tert-butoxide for reaction, and sequentially carrying out heat preservation, cooling and grinding after the reaction is finished to obtain the lubricating grease.
6. The method according to claim 5, wherein the molar ratio of lipoic acid to lithium t-butoxide in the step (1) is 1-1.2:1; the molar ratio of the lipoic acid in the step (a) to the lithium tert-butoxide in the step (b) is 1-1.2:1.
7. The method of preparing according to claim 5, wherein in the step (1), the method of mixing lipoic acid, methanol and lithium t-butoxide comprises: lipoic acid is added into methanol, stirred at 30-42 ℃ until dissolved, and then lithium tert-butoxide is added.
8. The preparation method according to claim 5, wherein the reaction temperature in the step (1) is 48-55 ℃ and the reaction time is 3-6 hours; the heating and mixing temperature in the step (2) is 60-80 ℃.
9. The process according to claim 5, wherein the reaction in step (b) is carried out at a temperature of 70 to 80℃for a period of 10 to 20 minutes; the temperature of the heat preservation is 110-130 ℃, and the heat preservation time is 5-15 min.
10. Use of a lubricant with mechanical adaptivity according to any one of claims 2 to 4 or a lubricant with mechanical adaptivity prepared by a method according to any one of claims 5 to 9 in the field of lubrication of mechanical parts.
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