CN105419906A - Complex lithium grease - Google Patents
Complex lithium grease Download PDFInfo
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- CN105419906A CN105419906A CN201510955403.6A CN201510955403A CN105419906A CN 105419906 A CN105419906 A CN 105419906A CN 201510955403 A CN201510955403 A CN 201510955403A CN 105419906 A CN105419906 A CN 105419906A
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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
- C10M121/00—Lubricating compositions characterised by the thickener being a compound of unknown or incompletely defined constitution
- C10M121/04—Reaction products
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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
- C10M123/00—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential
- C10M123/02—Lubricating compositions characterised by the thickener being a mixture of two or more compounds covered by more than one of the main groups C10M113/00 - C10M121/00, each of these compounds being essential at least one of them being a non-macromolecular 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
- C10M113/00—Lubricating compositions characterised by the thickening agent 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
- 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
- C10M117/04—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 containing hydroxy groups
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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
- C10M117/00—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof
- C10M117/06—Lubricating compositions characterised by the thickener being a non-macromolecular carboxylic acid or salt thereof having more than one carboxyl group bound to an acyclic carbon atom or cycloaliphatic carbon atom
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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
- C10M169/06—Mixtures of thickeners 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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/087—Boron oxides, acids or salts
- C10M2201/0876—Boron oxides, acids or salts used as thickening agent
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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
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base 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
- 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
- C10M2203/108—Residual fractions, e.g. bright stocks
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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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/0206—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers used as base 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
- C10M2207/1276—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as thickening agent
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/2805—Esters used as base 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
- C10M2207/2835—Esters of polyhydroxy compounds used as base 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
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
- C10M2215/064—Di- and triaryl amines
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- 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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- 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
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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- 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
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Abstract
The invention relates to complex lithium grease. The complex lithium grease comprises a thickening agent which is formed by compounding 12 hydroxy fatty acid lithium soap and binary acid lithium soap, and then combining with a compound formed by lithium salt borate, wherein the molar ratio of 12-hydroxy fatty acid to boracic acid is 1 to (0.2 to 0.5). According to the complex lithium grease provided by the invention, the problems that complex lithium grease of a traditional preparation process is not high in dropping point, and an additive is needed to be additionally added to realize antifriction and anti-wear properties, and under the condition of not adding antifriction and anti-wear agents, through changing the addition technology of the boracic acid, the dropping point and the antifriction and anti-wear properties of the complex lithium grease are improved, so as to enable the complex lithium grease to meet the requirement of lubrication under the severe conditions that the using temperature is higher than 260 DEG C, and the PB value is larger than 980N.
Description
The divisional application that the present invention is original applying number is 201310736769.5, original application day is on December 30th, 2013, former denomination of invention is " a kind of preparation method of complex lithium grease ".
Technical field
The present invention relates to a kind of complex lithium grease, particularly relating to when not adding low friction compound, improve the complex lithium grease comprising this viscosifying agent of dropping point and anti-wear and wear-resistant performance.
Background technology
Along with the development of modern industrial technology, iron and steel, automobile, the industries such as weaving, to the high temperature performance of lubricating grease, anti-wear and wear-resistant performance is had higher requirement, current lithium soap grease can not meet high temperature, at a high speed, the harsh working condition of heavy loading, common complex lithium grease is in the process used, although there is certain advantage compared with lithium soap grease, but because dropping point is not high, antifriction antiwear is not good, be difficult to reach service requirements, in order to the requirement of satisfied harsh operating mode, need in complex lithium grease, add multiple abrasion resistant extreme-pressure additive.
At present, complex lithium grease is very fast in China's development, substantially instead of lithium soap grease, and the document of report complex lithium grease is a lot of both at home and abroad, patent about complex lithium grease constantly occurs, as U.S. Patent Application Publication US3681242, US3711407, US3929651, the open CN1052890A of Chinese patent application, CN1052891A, the composition of these complex lithium greases is substantially the same, there are 12 oxystearic acids and diprotic acid (nonane diacid, sebacic acid) form two components, also have and add Whitfield's ointment, boric acid composition three components, material adds to generate mixture with lithium hydroxide reaction by preparation method together, the complex lithium grease dropping point of such preparation is not high, only reach about 260-280 DEG C, anti-wear and wear-resistant performance is not also given prominence to, PB value is failed more than 980N, and the industrial equipments in modern times is proposed higher requirement to use temperature and anti-wear and wear-resistant performance, by 12 oxystearic acids, sebacic acid, the conventional preparation techniques that the materials such as boric acid once add simultaneously will reach service requirements just to be needed to add antifriction and antiwear agents.In order to improve dropping point and the anti-wear and wear-resistant performance of complex lithium grease, not adding antifriction and antiwear agents again simultaneously, with regard to needing, necessary improvement being made to the process of preparing of complex lithium grease.
Summary of the invention
For the problems referred to above, in order to improve dropping point and the anti-wear and wear-resistant performance of complex lithium grease, not adding antifriction and antiwear agents again simultaneously, with regard to needing, necessary improvement being made to the process of preparing of complex lithium grease.The invention provides a kind of preparation method of complex lithium grease.
The invention discloses a kind of preparation method of complex lithium grease, comprise the steps:
/ 3rd, 12 oxystearic acids of base oil or synthetic oil total amount, diprotic acid, lithium hydroxide and water are added in autoclave, airtight, stir and the pressurization that heats up, carry out saponification reaction;
After saponification reaction completes, pressure release, adds boric acid, stir;
Add base oil or synthetic oil total amount three/stir intensification in the lump, carry out constant temperature refining;
Add residue base oil or synthetic oil cooling, adjustment denseness, adds oxidation inhibitor and rust-preventive agent, after circulation shear or mechanical mill, is finished product.
Under the condition not adding antifriction and antiwear agents, by changing the adding technology of boric acid, improve dropping point and the anti-wear and wear-resistant performance of complex lithium grease, can in use temperature higher than 260 DEG C, PB value meets the requirement of lubrication under being greater than the severe condition of 980N.
According to one preferred embodiment, described saponification reaction completes when experiencing the treatment step of heat up pressurization and maintenance constant temperature and pressure successively, the interpolation of described boric acid includes pressure release cooling, add boric acid and keep the treatment step of constant temperature, and described constant temperature refining stirs to heat up and complete after keeping the treatment step of constant temperature under experience successively adds base oil or synthetic oil dilution, normal pressure.
According to one preferred embodiment, described saponification reaction to heat up through 1-3.5 hour at described autoclave, and pressurization, described pressurization temperature in the kettle reach 130-150 DEG C, pressure reaches 0.3-0.6Mpa and complete after keeping constant temperature and pressure 0.5-2 hour.This technique can make saponification reaction complete in the short period of time, and makes 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound cocrystallization, forms two component mixtures.
According to one preferred embodiment, described boric acid after described saponification reaction completes, described autoclave pressure release to normal pressure and described pressurization temperature in the kettle is 110--150 DEG C time add, after described boric acid adds described autoclave, described pressurization temperature in the kettle is made to reach 130-150 DEG C and keep constant temperature 0.5-1 hour at ambient pressure.
The adding technology of this boric acid can make boric acid fully be reacted into lithium borate salt and the abundant compound cocrystallization of two component mixtures formed with 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap, now, in sebacic acid molecule carbonyl the Sauerstoffatom of electron rich first with 12 hydroxy acid molecules hydroxyls in there is unoccupied orbital hydrogen atom form hydrogen bond, then in 12 hydroxy acid molecules carbonyls the Sauerstoffatom of electron rich again with boric acid molecule in there is unoccupied orbital boron atom form coordinate bond, new three components mixture can be formed like this.This new three components mixture is different from the three components mixture 12 oxystearic acids, sebacic acid, boric acid once being added simultaneously autoclave formation, this new three components mixture compound molecule structure is slightly long, the fibrous texture intensity of overlap joint is high, firm, thus the dropping point of complex lithium grease and resistance to abrasion can be increased substantially.
According to one preferred embodiment, constant temperature refining be add in described autoclave base oil or synthetic oil total amount 1/3rd, be warming up to 210-260 DEG C under normal pressure and keep constant temperature to complete after 0.5 hour.
Add the base oil of normal temperature or 1/3rd of synthetic oil total amount can dilute the high soap content material formed, be conducive to heat transfer, be beneficial to the heat temperature raising of material.Be warming up to 210-260 DEG C under normal pressure and keep constant temperature 0.5 hour, soap can be made to divide and at high temperature form oily true solution, each moiety fully contacts, and constant temperature certain hour makes the effect of each component high temperature compound cocrystallization best.
According to one preferred embodiment, mediation still is proceeded to after adding 1/3rd of the base oil of normal temperature or synthetic oil total amount, 130 DEG C are cooled at mediation still internal recycle, 110 DEG C are trimmed to by mechanical pump, oxidation inhibitor and rust-preventive agent is added when 105-110 DEG C, stir simultaneously and adjust denseness, degassed.
Add the base oil of normal temperature or 1/3rd of synthetic oil total amount can make material at high temperature cool rapidly, reaching the temperature forming necessary structure, is also the growth being conducive to cocrystallization.
According to one preferred embodiment, described diprotic acid is sebacic acid or nonane diacid.
According to one preferred embodiment, the mol ratio of described 12 oxystearic acids and described diprotic acid is 1: 0.2-0.8.
According to one preferred embodiment, the mol ratio of described 12 hydroxy fatty acids and described boric acid is 1: 0.2-0.5.
According to one preferred embodiment, the mass ratio of described lithium hydroxide and water is 1: 5.
According to one preferred embodiment, described base oil is made up of bright stock, 500N, 150N, and weight percent shared by it is respectively 28%, 50%, 22%.
According to one preferred embodiment, described synthetic oil is polyalphaolefin or synthetic ester.
According to one preferred embodiment, described oxidation inhibitor is alkyl diphenylamine.
According to one preferred embodiment, described rust-preventive agent is one or more in barium mahogany sulfonate, synthetic sodium sulfonate, zinc naphthenate, alkylbenzotriazole.
The complex lithium grease that a kind of above-mentioned preparation method obtains.
The complex lithium grease not adding antifriction and antiwear agents that a kind of above-mentioned preparation method obtains.
According to one preferred embodiment, described complex lithium grease comprises base oil or synthetic oil, the viscosifying agent be made up of the mixture formed with boric acid after 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound and the additive be made up of oxidation inhibitor and rust-preventive agent, and the weight percentage that described base oil or synthetic oil, described viscosifying agent and described additive account for described complex lithium grease is respectively 75 ~ 90%, 10 ~ 20%, 0.05 ~ 5%.
A kind of above-mentioned preparation method obtains and is added with the complex lithium grease of antifriction and antiwear agents.
According to one preferred embodiment, described complex lithium grease comprises base oil or synthetic oil, the viscosifying agent be made up of the mixture formed with boric acid after 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound, the additive that is made up of oxidation inhibitor, rust-preventive agent and antifriction and antiwear agents, and the weight percentage that described base oil or synthetic oil, described viscosifying agent and described additive account for described complex lithium grease is respectively 75 ~ 90%, 10 ~ 20%, 0.05 ~ 5%.
According to one preferred embodiment, described antifriction and antiwear agents is any one in aminothio ester, dialkyl dithiocarbamate.
Beneficial effect of the present invention is:
1. the complex lithium grease dropping point that instant invention overcomes conventional preparation techniques is not high, the outer additivated problem of antifriction antiwear sexual needs, under the condition not adding antifriction and antiwear agents, by changing the adding technology of boric acid, improve dropping point and the anti-wear and wear-resistant performance of complex lithium grease, can in use temperature higher than 260 DEG C, PB value meets the requirement of lubrication under being greater than the severe condition of 980N.
2. the harsh degree that the preparation method of complex lithium grease of the present invention can require according to product performance makes formula more flexible, according to the different requirements of different working conditionss to product performance, selection adds and does not add wear-resistant friction reducer, and operational condition and temperature, pressure control more wide in range, more easy to operate.
3. the complex lithium grease obtained according to the preparation method of complex lithium grease of the present invention, while raising dropping point and anti-wear and wear-resistant performance, has good high temperature performance and mechanical stability, colloid stability.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the preparation method of complex lithium grease of the present invention.
Embodiment
The present invention is illustrated below in conjunction with drawings and Examples.Those skilled in the art should understand, embodiment cited is here that the present invention is understood in help, should not be considered as concrete restriction of the present invention.Various starting material in embodiment are domestic market buying, applied in actual production.
Fig. 1 is the process flow sheet of the preparation method of complex lithium grease of the present invention.Under Fig. 1 shows a kind of condition not adding antifriction and antiwear agents, by changing the adding technology of boric acid, improve the preparation method of the dropping point of complex lithium grease and the complex lithium grease of anti-wear and wear-resistant performance, it comprises the steps:
1) water of 1/3rd, 12 oxystearic acids of base oil or synthetic oil total amount, diprotic acid, lithium hydroxide and 5 times of lithium hydroxides is added in autoclave, airtight, stir.
2) heat up pressurization, through 1-3.5 hour, when pressurization temperature in the kettle reach 130-150 DEG C, pressure reaches 0.3-0.6Mpa, stops heating, keep constant temperature and pressure 0.5-2 hour in autoclave, carry out saponification reaction.
This technique can make saponification reaction complete in the short period of time, and makes 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound cocrystallization, forms two component mixtures.
3), after saponification reaction completes, the pressure in release autoclave becomes atmospheric pressure state, adds boric acid when temperature is 110-150 DEG C.
4) heat up stirring, makes temperature keep 0.5-1 hour at 130-150 DEG C, then add the base oil of normal temperature or 1/3rd of synthetic oil total amount under normal pressure.
The adding technology of this boric acid can make boric acid fully be reacted into lithium borate salt and the abundant compound cocrystallization of two component mixtures formed with 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap, now, in sebacic acid molecule carbonyl the Sauerstoffatom of electron rich first with 12 hydroxy acid molecules hydroxyls in there is unoccupied orbital hydrogen atom form hydrogen bond, then in 12 hydroxy acid molecules carbonyls the Sauerstoffatom of electron rich again with boric acid molecule in there is unoccupied orbital boron atom form coordinate bond, new three components mixture can be formed like this.This new three components mixture is different from the three components mixture 12 oxystearic acids, sebacic acid, boric acid once being added simultaneously autoclave formation, this new three components mixture compound molecule structure is slightly long, the fibrous texture intensity of overlap joint is high, firm, thus the dropping point of complex lithium grease and resistance to abrasion can be increased substantially.Add the base oil of normal temperature or 1/3rd of synthetic oil total amount can dilute the high soap content material formed, be conducive to heat transfer, be beneficial to the heat temperature raising of material.
5) continue the stirring that heats up, stop heat temperature raising when temperature rises to 210-260 DEG C under normal pressure, constant temperature 0.5 hour, then add the base oil of normal temperature or 1/3rd of synthetic oil total amount, proceed to mediation still.
Be warming up to 210-260 DEG C under normal pressure and keep constant temperature 0.5 hour, soap can be made to divide and at high temperature form oily true solution, each moiety fully contacts, and constant temperature certain hour makes the effect of each component high temperature compound cocrystallization best.Add the base oil of normal temperature or 1/3rd of synthetic oil total amount can make material at high temperature cool rapidly, reaching the temperature forming necessary structure, is also make each component compound cocrystallization.
6) be cooled to 130 DEG C at mediation still internal recycle, be trimmed to 110 DEG C by mechanical pump, add oxidation inhibitor, rust-preventive agent at 105-110 DEG C, stir and adjust denseness, after degassed, being finished product.
By the preparation method of the complex lithium grease shown in Fig. 1, the complex lithium grease dropping point that can overcome conventional preparation techniques is not high, the outer additivated problem of antifriction antiwear sexual needs, under the condition not adding antifriction and antiwear agents, by changing the adding technology of boric acid, form new three components mixture.This new three components mixture is different from the three components mixture 12 oxystearic acids, sebacic acid, boric acid once being added simultaneously autoclave formation, this new three components mixture compound molecule structure is slightly long, the fibrous texture intensity of overlap joint is high, firm, thus the dropping point of complex lithium grease and resistance to abrasion can be increased substantially, can in use temperature higher than 260 DEG C, PB value meets the requirement of lubrication under being greater than the severe condition of 980N.
Specific embodiment and comparative example.
Embodiment 1
A preparation method for complex lithium grease, it comprises the steps:
1) base oil 380 kilograms formed by the 150N by the bright stock of 28%, the 500N of 50% and 22%, 12 oxystearic acid 120 kilograms, sebacic acid 35 kilograms, lithium hydroxide 30 kilograms and 150 kilograms, water add volume 1.5M
3autoclave pressure in, airtight, stir.
2) heat up pressurization, through 1-3.5 hour, when pressurization temperature in the kettle reaches 130-150 DEG C, when pressure reaches 0.3-0.6Mpa, stops heating, keep constant temperature and pressure 0.5-2 hour in autoclave, carry out saponification reaction.
3), after saponification reaction completes, the pressure in release autoclave, becomes atmospheric pressure state, adds 6 kilograms of boric acid when temperature is 110-150 DEG C.
4) heat up stirring, makes temperature keep 0.5-1 hour at 130-150 DEG C, then add the base oil 380 kilograms be made up of the 150N of the bright stock of 28%, the 500N of 50% and 22% under normal pressure.
5) continue the stirring that heats up, stop heat temperature raising when temperature rises to 210-260 DEG C under normal pressure, constant temperature 0.5 hour, then add the base oil 380 kilograms be made up of the 150N of the bright stock of 28%, the 500N of 50% and 22%, proceed to mediation still.
6) be cooled to 130 DEG C at mediation still internal recycle, be trimmed to 110 DEG C by mechanical pump, add 2.5 kilograms of alkyl diphenylamines and 0.8 kilogram of barium mahogany sulfonate at 105-110 DEG C, stir and adjust denseness, after degassed, being finished product.
The determination data of embodiment 1 is in table 1.
Embodiment 2
Adopt polyalphaolefin as production base oil, except base oil is different, other proportioning raw materials of complex lithium grease is consistent with embodiment 1 with technological process.The determination data of embodiment 2 is in table 1.
Embodiment 3
Adopt polyol ester and mineral base oil mixed base oil to make production base oil, except base oil is different, other proportioning raw materials of compositing lithio ester is consistent with embodiment 1 with technological process.The determination data of embodiment 3 is in table 1.
Comparative example 1
Comparative example 1 is compared with embodiment 1, and its difference is only that the adding technology of mixture boric acid is different.It comprises the steps:
1) base oil 380 kilograms formed by the 150N by the bright stock of 28%, the 500N of 50% and 22%, 12 oxystearic acid 120 kilograms, sebacic acid 35 kilograms, lithium hydroxide 30 kilograms, 150 kilograms, water and boric acid 6 kilograms add volume 1.5M
3autoclave pressure in, airtight, stir.
2) heat up pressurization, through 1-3.5 hour, when pressurization temperature in the kettle reaches 130-150 DEG C, when pressure reaches 0.3-0.6Mpa, stops heating, keep constant temperature and pressure 0.5-2 hour in autoclave, carry out saponification reaction.
3), after saponification reaction completes, the pressure in release autoclave, becomes atmospheric pressure state, adds the base oil 380 kilograms be made up of the 150N of the bright stock of 28%, the 500N of 50% and 22%.
4) continue the stirring that heats up, stop heat temperature raising when temperature rises to 210-260 DEG C under normal pressure, constant temperature 0.5 hour, then add the base oil 380 kilograms be made up of the 150N of the bright stock of 28%, the 500N of 50% and 22%, proceed to mediation still.
5) be cooled to 130 DEG C at mediation still internal recycle, be trimmed to 110 DEG C by mechanical pump, add 2.5 kilograms of alkyl diphenylamines and 0.8 kilogram of barium mahogany sulfonate at 105-110 DEG C, stir and adjust denseness, after degassed, being finished product.
The determination data of comparative example 1 is in table 1.
Comparative example 2
Comparative example 2, compared with comparative example 1, adds wear-resistant friction reducer.It comprises the steps:
1) base oil 380 kilograms formed by the 150N by the bright stock of 28%, the 500N of 50% and 22%, 12 oxystearic acid 120 kilograms, sebacic acid 35 kilograms, lithium hydroxide 30 kilograms, 150 kilograms, water and boric acid 6 kilograms add volume 1.5M
3autoclave pressure in, airtight, stir.
2) heat up pressurization, through 1-3.5 hour, when pressurization temperature in the kettle reaches 130-150 DEG C, when pressure reaches 0.3-0.6Mpa, stops heating, keep constant temperature and pressure 0.5-2 hour in autoclave, carry out saponification reaction.
3), after saponification reaction completes, the pressure in release autoclave, becomes atmospheric pressure state, adds the base oil 380 kilograms be made up of the 150N of the bright stock of 28%, the 500N of 50% and 22%.
4) continue the stirring that heats up, stop heat temperature raising when temperature rises to 210-260 DEG C under normal pressure, constant temperature 0.5 hour, then add the base oil 380 kilograms be made up of the 150N of the bright stock of 28%, the 500N of 50% and 22%, proceed to mediation still.
5) 130 DEG C are cooled at mediation still internal recycle, 110 DEG C are trimmed to by mechanical pump, add 2.5 kilograms of alkyl diphenylamines and 0.8 kilogram of barium mahogany sulfonate and 4.5 kilograms of dialkyl dithiocarbamates at 105-110 DEG C, stir and adjust denseness, after degassed, being finished product.
The determination data of comparative example 2 is in table 1.
Table 1
As can be seen from Table 1, the dropping point of the embodiment 1 of preparation method of the present invention, embodiment 2 and the complex lithium grease obtained by embodiment 3 is adopted all to be greater than 300 DEG C, PB value is all greater than 980N, also has good high temperature performance and mechanical stability, colloid stability.
In addition, the harsh degree that the preparation method of complex lithium grease of the present invention can require according to product performance makes formula more flexible, according to the different requirements of different working conditionss to product performance, selection adds and does not add wear-resistant friction reducer, and operational condition and temperature, pressure control more wide in range, more easy to operate.
A kind of complex lithium grease can be obtained by the preparation method of complex lithium grease of the present invention.This complex lithium grease comprises base oil or synthetic oil, the viscosifying agent be made up of the mixture formed with boric acid after 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound, the additive that is made up of oxidation inhibitor, rust-preventive agent, and the weight percentage that described base oil or synthetic oil, described viscosifying agent and described additive account for described complex lithium grease is respectively 75 ~ 90%, 10 ~ 20%, 0.05 ~ 5%.
Also a kind of complex lithium grease not adding wear-resistant friction reducer can be obtained by the preparation method of complex lithium grease of the present invention.This complex lithium grease comprises base oil or synthetic oil, the viscosifying agent be made up of the mixture formed with boric acid after 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound, the additive that is made up of oxidation inhibitor, rust-preventive agent, and the weight percentage that described base oil or synthetic oil, described viscosifying agent and described additive account for described complex lithium grease is respectively 75 ~ 90%, 10 ~ 20%, 0.05 ~ 5%.
A kind of complex lithium grease being added with wear-resistant friction reducer can also be obtained by the preparation method of complex lithium grease of the present invention.Wear-resistant friction reducer can adopt aminothio ester, dialkyl dithiocarbamate etc.Wear-resistant friction reducer and oxidation inhibitor, rust-preventive agent form together with additive and add.This complex lithium grease comprises base oil or synthetic oil, the viscosifying agent be made up of the mixture formed with boric acid after 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound, the additive that is made up of oxidation inhibitor, rust-preventive agent and antifriction and antiwear agents, and the weight percentage that described base oil or synthetic oil, described viscosifying agent and described additive account for described complex lithium grease is respectively 75 ~ 90%, 10 ~ 20%, 0.05 ~ 5%.
Beneficial effect of the present invention is:
1. the complex lithium grease dropping point that instant invention overcomes conventional preparation techniques is not high, the outer additivated problem of antifriction antiwear sexual needs, under the condition not adding antifriction and antiwear agents, by changing the adding technology of boric acid, forms new three components mixture.This new three components mixture is different from the three components mixture 12 oxystearic acids, sebacic acid, boric acid once being added simultaneously autoclave formation, this new three components mixture compound molecule structure is slightly long, the fibrous texture intensity of overlap joint is high, firm, thus the dropping point of complex lithium grease and resistance to abrasion can be increased substantially, can in use temperature higher than 260 DEG C, PB value meets the requirement of lubrication under being greater than the severe condition of 980N.
2. the harsh degree that the preparation method of complex lithium grease of the present invention can require according to product performance makes formula more flexible, according to the different requirements of different working conditionss to product performance, selection adds and does not add wear-resistant friction reducer, and operational condition and temperature, pressure control more wide in range, more easy to operate.
3. the complex lithium grease obtained according to the preparation method of complex lithium grease of the present invention, while raising dropping point and anti-wear and wear-resistant performance, has good high temperature performance and mechanical stability, colloid stability.
Above embodiment is only preferred part of the present invention; be not limited to the present invention; although the example described above is to invention has been specific description; but the technician of the industry still can modify to the technical scheme of described embodiment; or to the replacement that technical characteristic is wherein equal to; all carry out within content of the present invention and engineering philosophy amendment, equivalent replacement, improvement etc., all should belong within protection of the present invention.
Claims (10)
1. a complex lithium grease, is characterized in that, described complex lithium grease comprises the viscosifying agent be made up of the mixture formed with boric acid after 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap compound,
Wherein said viscosifying agent is formed by following steps: by 1/3rd, 12 oxystearic acids of base oil or synthetic oil total amount, diprotic acid, lithium hydroxide and water are carried out saponification reaction, generates 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap and compound cocrystallization forms two component mixtures; After saponification reaction completes, add boric acid, make acid reaction generate lithium borate salt and form three components mixture with the two component mixture cocrystallization that 12 hydroxy fatty acid lithium soaps and diprotic acid lithium soap are formed.
2. complex lithium grease as claimed in claim 1, it is characterized in that, the mol ratio of wherein said 12 hydroxy fatty acids and described boric acid is 1: 0.2 ~ 0.5.
3. complex lithium grease as claimed in claim 2, it is characterized in that, the mass ratio of described lithium hydroxide and water is 1: 5.
4. complex lithium grease as claimed in claim 3, is characterized in that, described complex lithium grease is not containing antifriction and antiwear agents.
5. complex lithium grease as claimed in claim 4, it is characterized in that, the dropping point of described complex lithium grease is greater than 300 DEG C, and PB value is greater than 980N.
6. complex lithium grease as claimed in claim 5, it is characterized in that, described boric acid after described saponification reaction completes, autoclave pressure release to normal pressure and the temperature in the kettle that pressurizes is 110 ~ 150 DEG C time add, after described boric acid adds described autoclave, make described pressurization temperature in the kettle reach 130 ~ 150 DEG C at ambient pressure and keep constant temperature 0.5 ~ 1 hour to form described viscosifying agent.
7. complex lithium grease as claimed in claim 6, it is characterized in that, described saponification reaction adds in autoclave by 1/3rd of base oil or synthetic oil total amount and 12 oxystearic acids, diprotic acid, lithium hydroxide and water, and the pressurization that heated up through 1 ~ 3.5 hour, described pressurization temperature in the kettle reach 130 ~ 150 DEG C, pressure reaches 0.3 ~ 0.6MPa and keep constant temperature and pressure to complete after 0.5 ~ 2 hour.
8. complex lithium grease as claimed in claims 6 or 7, it is characterized in that, described complex lithium grease is formed after described viscosifying agent is formed after constant temperature refining, described constant temperature refining process comprises: add the base oil of normal temperature or 1/3rd of synthetic oil total amount to dilute the high soap content material formed, be warming up to 210 ~ 260 DEG C and keep constant temperature 0.5 hour under normal pressure.
9. complex lithium grease as claimed in claim 8, it is characterized in that, described complex lithium grease is after constant temperature has been refined, add the residue base oil of normal temperature or 1/3rd of synthetic oil total amount make material at high temperature rapidly cooling be beneficial to the growth of cocrystallization, proceed to mediation still afterwards, be cooled to 130 DEG C at mediation still internal recycle, be trimmed to 110 DEG C by mechanical pump, add oxidation inhibitor and rust-preventive agent when 105-110 DEG C, stir simultaneously and adjust denseness degassed rear formation.
10. complex lithium grease as claimed in claim 9, it is characterized in that, the additive that described complex lithium grease comprises base oil or synthetic oil, viscosifying agent and is made up of oxidation inhibitor and rust-preventive agent, wherein, the weight percentage that described base oil or synthetic oil, described viscosifying agent and described additive account for described complex lithium grease is respectively 75 ~ 90%, 10 ~ 20%, 0.05 ~ 5%, and the percentage composition sum of described base oil or synthetic oil, described viscosifying agent and described additive is 100%.
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| CN106929126B (en) * | 2015-12-31 | 2019-12-10 | 中国石油天然气股份有限公司 | Composite lithium-based bearing lubricating grease composition |
| CN105779084A (en) * | 2016-03-17 | 2016-07-20 | 上海摩克润滑油技术有限公司 | Bearing grease for squeezing machine of cane sugar factory and preparation method of bearing grease |
| CN108117916A (en) * | 2016-11-28 | 2018-06-05 | 徐承东 | Superhigh temperature special greases and preparation method |
| CN110205179B (en) * | 2019-06-11 | 2021-08-17 | 中山华明泰科技股份有限公司 | Preparation method and application of hydroxy fatty acid lithium |
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| US4189387A (en) * | 1978-08-31 | 1980-02-19 | King James P | Lubricant compositions based on zirconium polymers |
| CN101200670A (en) * | 2006-12-12 | 2008-06-18 | 中国石油天然气集团公司 | Composite lithium-base grease and method for making same |
| CN101921650A (en) * | 2010-08-04 | 2010-12-22 | 中国海洋石油总公司 | Complex lithium grease and preparation method thereof |
| CN102977978A (en) * | 2012-11-27 | 2013-03-20 | 无锡意格尔润滑科技股份有限公司 | Bearing lubricating grease and preparation method thereof |
| CN103450978A (en) * | 2013-09-05 | 2013-12-18 | 江苏龙蟠石化有限公司 | Lubricating grease for hub bearing of heavy load truck and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3535713C1 (en) * | 1985-10-05 | 1987-04-02 | Texaco Technologie Europa Gmbh | Grease for high application temperatures |
| KR100716474B1 (en) * | 2006-05-19 | 2007-05-15 | 조길래 | Lithium complex soap clear grease composition |
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2013
- 2013-12-30 CN CN201510955845.0A patent/CN105542904B/en active Active
- 2013-12-30 CN CN201310736769.5A patent/CN103773580B/en active Active
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4189387A (en) * | 1978-08-31 | 1980-02-19 | King James P | Lubricant compositions based on zirconium polymers |
| CN101200670A (en) * | 2006-12-12 | 2008-06-18 | 中国石油天然气集团公司 | Composite lithium-base grease and method for making same |
| CN101921650A (en) * | 2010-08-04 | 2010-12-22 | 中国海洋石油总公司 | Complex lithium grease and preparation method thereof |
| CN102977978A (en) * | 2012-11-27 | 2013-03-20 | 无锡意格尔润滑科技股份有限公司 | Bearing lubricating grease and preparation method thereof |
| CN103450978A (en) * | 2013-09-05 | 2013-12-18 | 江苏龙蟠石化有限公司 | Lubricating grease for hub bearing of heavy load truck and preparation method thereof |
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| CN103773580A (en) | 2014-05-07 |
| CN105542904A (en) | 2016-05-04 |
| CN105419906B (en) | 2018-07-27 |
| CN105542904B (en) | 2018-04-03 |
| CN103773580B (en) | 2016-01-20 |
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