CN102051257B - Complex lithium-base lubricating grease and production technique thereof - Google Patents
Complex lithium-base lubricating grease and production technique thereof Download PDFInfo
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Abstract
The invention relates to a complex lithium-base lubricating grease and a production technique thereof. The complex lithium-base lubricating grease comprises the following components in parts by weight: 9-13.5 parts of 12 hydroxystearic acid, 3-4.5 parts of decanedioic acid, 2.6-3.9 parts of lithium hydroxide, 5-50 parts of compound calcium sulfonate lubricating grease, 22.8-78.3 parts of base oil, 0.5-1 part of thickener, 1-3 parts of multifunctional agent, 0.5-1 part of antioxidant and 0.1-0.3 part of metal deactivator. The production technique comprises the following steps: converting superhigh-base-number calcium sulfonate with a conversion agent at 60-100 DEG C for 20-60 minutes until the superhigh-base-number calcium sulfonate becomes obviously thickened, and heating to 140-180 DEG Cto remove water, thereby obtaining the complex calcium sulfonate lubricating grease. The invention has the advantages of long service life in the occasions of long grease-complementation period under long-term heavy load, slight oxidative stain at high temperature, excellent anti-rusting property in damp or sea occasions, and low loss in the occasions of substantive water flushing; and the invention has favorable lubricating property and can prolong the service life of the bearing in the occasions of dampness and heavy load.
Description
Technical field
The present invention relates to a kind of lubricating grease and production technique thereof.
Background technology
Complex lithium grease is a kind of high-quality high temperature grease, is widely used in the lubricated of the field devices bearings such as mine, metallurgy, steel rolling, automobile, chemical industry, machinery, boats and ships.Its advantage is that dropping point is high, broad application temperature range; Colloid stability and anti-shear performance are better than common lithium soap grease, and work-ing life is longer than common lithium soap grease; Wastage is little, is difficult for running off in bearing, saves the consumption of lubricating grease.
But under some severe condition, use also Shortcomings, show following aspect:
In long-term operation, mend long occasion of fat cycle, the bearing life of complex lithium grease can not meet the demands fully, and during especially with heavy load conditions (such as some large-size axis parts cushion cap frame tests), bearing life is not long.
At long term high temperature, mend long occasion of fat cycle, the complex lithium grease color obviously deepens, and oxidation rate is accelerated.
In the occasion of humidity many water, especially seawater, its rustproof property is not ideal enough.
In the occasion that large water gaging washes away, its number of dropouts can increase, and is unfavorable to bearing lubrication and sealing.
In the occasion of many water heavy loading, its extreme pressure property can decline to a great extent, and wearing and tearing can be accelerated, and bearing reduces work-ing life.
Summary of the invention
The purpose of this invention is to provide the extensive complex lithium grease of a kind of adaptability and production technique thereof, be characterized in: the occasion of mending fat cycle length in long-term heavy loading is longer work-ing life; Lighter in the oxidation stain of high temperature occasion; Occasion rust-preventing characteristic at the many water of humidity or seawater is outstanding; The occasion of washing away at large water gaging runs off little; Occasion lubricity in many water heavy loading is good, prolongs bearing life.
The base oil aspect adopts high viscosity Dormant oils or synthetic oil, and vaporization at high temperature is little, to adapt to the requirement of high temperature.
The viscosifying agent aspect is take lithium hydroxide and composite calcium sulfonate grease lubricant as viscosifying agent.The soap fiber uniform and smooth of lithium hydroxide, colloid stability is good.The shallow good in oxidation resistance of composite calcium sulfonate grease lubricant high-temperature discoloration.
Calcium sulphonate wherein be viscosifying agent also be excellent rust-preventive agent; calcium sulphonate can wrap up water the formation micella on the one hand; prevent metallic corrosion or corrosion by the contact probability that reduces water and metal; calcium sulphonate itself also has stronger adsorptive power to metal on the other hand; occasion at many water or seawater also can form protective membrane in the metallic surface by active adsorption; under duplicate protection, rustless property is other lubricating grease head and shoulders above.
Calcium sulphonate and nano-calcium carbonate can form special stable soap structure, add the polar end adsorptive power stronger to metal of calcium sulphonate molecule, non-polar end has preferably avidity to grease soap body system, make whole lubricating grease system keep continuity, the anti-water performance of flushing of composite calcium sulfonate grease lubricant is 3 to 4 times of complex lithium grease.
In the composite calcium sulfonate grease lubricant calcium carbonate of contained nano-scale be viscosifying agent also be a kind of inert extreme pressure anti-wear additives, occasion at high temperature or many water still has excellent extreme pressure and antiwear behavior, its principle is that nano-calcium carbonate contacts under the high temperature that causes with friction pair microcosmic projection at water, can partly freely out directly friction pair be separated lubricate, or be deposited on the metallic surface, form deposited film or reaction film lubricate, such performance is very rare to the prolongation of high temperature or many water occasion bearing life, and other extreme pressure anti-wear additives are difficult to have such performance.
Mostly general extreme pressure anti-wear additives is the fluid cpds of the elements such as sulfur-bearing, phosphorus, nitrogen, molybdenum, by physical adsorption, chemisorption or chemical reaction at the metallic surface lubricate.Its shortcoming is that flash-point is lower, and high-temperature volatile is large, obviously reduces in the effect of many water occasion.This has the reason of physics and chemistry two aspects, and physical cause is can vapor away at high-temperature field unification partially liq extreme pressure anti-wear additives, because the extreme pressure and antiwear behavior that the minimizing of extreme-pressure anti-wear dosage causes decline.On the other hand, molecular thermalmotion increases under the high temperature, and the physics of the wear-resistant molecule of extreme pressure agent and chemisorption rate reduce and cause that extreme pressure property descends.Chemical principle forms softer chemical reaction film because being the elements such as sulphur, phosphorus, nitrogen, molybdenum under the TRANSIENT HIGH TEMPERATURE that the contact of friction pair microcosmic projection causes, reduces the surface of friction pair roughness, enlarge active surface, the pressure of reduction contact site and lubricate.Chemical reaction film is actually a kind of slight controlled useful corrosion, but when the application site long term high temperature, this corrosion meeting is developed into the metallic corrosion of whole system by the metallic corrosion of microcosmic point of contact, can cause like this bearing surface metal hardness to descend, the bearing wear amount can increase, thereby affects bearing life.The polarity of water is stronger, in that the occasion of water is arranged, in the metallic surface, water and liquid extreme pressure anti-wear additives are the competitive adsorption relations, the existence of water can reduce the adsorption rate of extreme pressure anti-wear additives, thereby can cause extreme pressure anti-wear to decline to a great extent, and causes that wearing and tearing increase and bearing life shortens.Water also can cause the hydrolysis of extreme pressure anti-wear additives, produces the acidic substance corroding metal.
The tackifier aspect take high molecular polymer type tackifier as main, mainly is the adhesivity of strengthening lubricating grease, improves colloid stability and the sealing property of lubricating grease.
Multi-functional dose of aspect cooperates with zinc dialkyl dithiocarbamate and methylene-bis Keywords dibutyl dithiocarbamate, has excellent antioxygen, anticorrosive, metallicity and extreme-pressure anti-wear, antifriction performance.
The oxidation inhibitor aspect take high-temperature antioxidant as main, improves lubricating grease antioxidant property at high temperature.
The metal passivator aspect, but the katalysis of adding efficient metal passivator establishment metal pair lubricating grease oxidation suppresses high temperature corrosion.
Complex lithium grease is characterized in that wherein the weight part proportioning of each composition is as follows:
12 oxystearic acids: 9-13.5
Sebacic acid: 3-4.5
Lithium hydroxide: 2.6-3.9
Composite calcium sulfonate grease lubricant: 5-50
Base oil: 22.8-78.3
Tackifier: 0.5-1
Multi-functional dose: 1-3
Oxidation inhibitor: 0.5-1
Metal passivator: 0.1-0.3
Described 12 oxystearic acids, sebacic acid, lithium hydroxide are technical pure, and market is on sale.
Described composite calcium sulfonate grease lubricant refers to that take overbased calcium sulphonate as raw material under the effect of transforming agent, transforming agent accounts for the 4-10% of calcium sulphonate weight; The calcium carbonate that the inside is contained is converted into nano-scale by unformed state, and with the lubricating grease of the contained calcium sulphonate in the inside by associating and forming, this lubricating grease adds in the product of the present invention in the mode of mixing, and becomes an integral part of product of the present invention again.The method for making of described composite calcium sulfonate grease lubricant is: overbased calcium sulphonate and transforming agent are transformed 20-60 minute at 60-100 ℃, until the apparition retrogradation, be heated to 140-180 ℃ and slough moisture and get final product.
The active principle of overbased calcium sulphonate wherein is greater than 70%, and wherein calcium carbonate is greater than 35%, and calcium sulphonate is greater than 35%, and thinning oil is mineral oil, and 40 ℃ of kinematic viscosity are greater than 25mm
2/ s.Described transforming agent is the mixture of low-carbon alcohol, organic acid and water, and the part by weight of low-carbon alcohol, organic acid and water is (1-2): 1: 1; Low-carbon alcohol is one or both or the two or more composition in methyl alcohol, ethanol, propyl alcohol, Virahol or the butanols, and organic acid is one or both or the two or more composition in formic acid, acetic acid, the phenylformic acid.
Described base oil refers to one or more and the alkylbenzene mixing oil among 500SN, 150BS, PAO10, the PAO40, and this mixing oil has good consistency to soap fiber and additive, improve aspect the lubricating grease over-all properties useful.
Described tackifier refer to that the polybutene drc is 10% with the solvent high molecular polybutene of thinning oil.
Described multi-functional dose of mixture that refers to zinc dialkyl dithiocarbamate and methylene-bis Keywords dibutyl dithiocarbamate, the part by weight of zinc dialkyl dithiocarbamate and methylene-bis Keywords dibutyl dithiocarbamate is (2-4): 7.Have excellent antioxygen, corrosion resistance and extreme-pressure anti-wear, antifriction performance.
Described oxidation inhibitor refers to the phenyl αnaphthylamine.
Described metal passivator refers to thiadiazoles derivative T561.
The production technique of complex lithium grease comprises the steps:
1) base oil of the described weight of adding in the saponification still is opened and is stirred, and rotating speed 30-60 rev/min, add whole 12 oxystearic acids, be warmed up to 90-100 ℃, 12 oxystearic acids are all dissolved;
2) 1/2 part of lithium hydroxide getting described weight is dissolved in 6-10 times of 95-100 ℃ of hot water, slowly adds and carries out saponification reaction, and the joining day is no less than 30 minutes, and saponification time is no less than 1 hour; Slowly be warming up to 120-150 ℃;
3) add sebacic acid, stirred 20 minutes, 1/2 of weight part of lithium hydroxide is dissolved in 6-10 times of 95-100 ℃ of hot water under the remainder, slowly adds and reacts, and the joining day is no less than 30 minutes, then is incubated;
4) heat up dehydration to 150 ℃ of 1/2 oxidation inhibitor that add described weight, continue to be warming up to 200-220 ℃, be incubated 10-30 minute;
5) with material pumping to blending kettle, be cooled to 120-100 ℃ of 1/2 oxidation inhibitor that adds remaining weight, adds multi-functional dose and metal passivator, usefulness circulation shear and dispersed with stirring 20 minutes;
6) above-mentioned material is uniformly dispersed with high pressure homogenizer, is pumped to blending kettle, add tackifier, stirred 20 minutes, for subsequent use;
7) composite calcium sulfonate grease lubricant is added in the above-mentioned material, be uniformly dispersed by stirring and circulation shear, namely obtain complex lithium grease.
Embodiment
Embodiment 1
Complex lithium grease is characterized in that wherein the weight part proportioning of each composition is as follows:
12 oxystearic acids: 9
Sebacic acid: 3
Lithium hydroxide: 2.6
Composite calcium sulfonate grease lubricant: 5
Base oil: 78.3
Tackifier: 0.5
Multi-functional dose: 1
Oxidation inhibitor: 0.5
Metal passivator: 0.1
The production technique of complex lithium grease is: prefabricated A product is added in the B product, be uniformly dispersed by stirring and circulation shear, get product.
The A Manufacturing Method of Products: overbased calcium sulphonate and transforming agent are transformed 20-60 minute at 60-100 ℃, until obviously retrogradation is heated to 140-180 ℃ and sloughs moisture, for subsequent use; Transforming agent accounts for the 4-10% of calcium sulphonate weight.Described transforming agent is the mixture of low-carbon alcohol, organic acid and water, and the part by weight of low-carbon alcohol, organic acid and water is (1-2): 1: 1; Low-carbon alcohol is one or both or the two or more composition in methyl alcohol, ethanol, propyl alcohol, Virahol or the butanols, and organic acid is one or both or the two or more composition in formic acid, acetic acid, the phenylformic acid.
B Manufacturing Method of Products: in the saponification still, add whole base oils, open and stir (rotating speed 30-60 rev/min), add whole 12 oxystearic acids, be warmed up to 90-100 ℃, 12 oxystearic acids are all dissolved.Get 1/2 part of lithium hydroxide and be dissolved in 6-10 times of 95-100 ℃ of hot water, slowly add and carry out saponification reaction, the joining day is no less than 30 minutes, and saponification time is no less than 1 hour.Slowly be warming up to 120-150 ℃, add sebacic acid, stirred 20 minutes, 1/2 part of lithium hydroxide under the remainder is dissolved in 6-10 times of 95-100 ℃ of hot water, slowly adds and reacts, and the joining day is no less than 30 minutes, then be incubated, soaking time is no less than 30 minutes.Heat up dehydration to 150 ℃ of adding 1/2 oxidation inhibitor.Continue to be warming up to 200-220 ℃, be incubated 10-30 minute.Material pumping to blending kettle, is cooled to 120-100 ℃ and adds 1/2 remaining oxidation inhibitor, add multi-functional dose and metal passivator, use circulation shear and dispersed with stirring 20 minutes.Material is uniformly dispersed with high pressure homogenizer, is pumped to blending kettle, add tackifier, stirred 20 minutes, for subsequent use.
Embodiment 2:
Complex lithium grease is characterized in that wherein the weight part proportioning of each composition is as follows:
12 oxystearic acids: 11.2
Sebacic acid: 3.8
Lithium hydroxide: 3.2
Composite calcium sulfonate grease lubricant: 30
Base oil: 47.3
Tackifier: 0.8
Multi-functional dose: 2.7
Oxidation inhibitor: 0.8
Metal passivator: 0.2
The production technique of complex lithium grease is with embodiment 1.
Embodiment 3:
Complex lithium grease is characterized in that wherein the weight part proportioning of each composition is as follows:
12 oxystearic acids: 13.5
Sebacic acid: 4.5
Lithium hydroxide: 3.9
Composite calcium sulfonate grease lubricant: 50
Base oil: 22.8
Tackifier: 1
Multi-functional dose: 3
Oxidation inhibitor: 1
Metal passivator: 0.3
The production technique of complex lithium grease is with embodiment 1.
Claims (1)
1. complex lithium grease is characterized in that, wherein the weight part proportioning of each material composition is as follows:
12 oxystearic acids: 9-13.5
Sebacic acid: 3-4.5
Lithium hydroxide: 2.6-3.9
Composite calcium sulfonate grease lubricant: 5-50
Base oil: 22.8-78.3
Tackifier: 0.5-1
Multi-functional dose: 1-3
Oxidation inhibitor: 0.5-1
Metal passivator: 0.1-0.3
The method for making of described composite calcium sulfonate grease lubricant is: overbased calcium sulphonate and transforming agent are transformed 20-60 minute at 60-100 ℃, until the apparition retrogradation, be heated to 140-180 ℃ and slough moisture and get final product; Wherein transforming agent accounts for the 4-10% of overbased calcium sulphonate weight; The alkyl carbon number of described overbased calcium sulphonate is greater than 20; Described transforming agent is the mixture of low-carbon alcohol, organic acid and water, low-carbon alcohol is one or both or the two or more composition in methyl alcohol, ethanol, propyl alcohol, Virahol or the butanols, and organic acid is one or both or the two or more composition in formic acid, acetic acid, the phenylformic acid;
Described base oil refers to one or more and the mixing oil of dialkyl benzene among 500SN, 150BS, PAO10 or the PAO40, and dialkyl benzene kinematic viscosity in the time of 40 ℃ is 20-22mm
2/ s, viscosity index is greater than 110, and pour point is lower than-50 ℃;
Described tackifier refer to the solvent molecular weight of thinning oil to be 1,100,000 to 2,000,000 high molecular polybutene, and the polybutene drc is 10%;
Described multi-functional dose of mixture that refers to zinc dialkyl dithiocarbamate and methylene radical-two (Keywords dibutyl dithiocarbamates), the part by weight of zinc dialkyl dithiocarbamate and methylene radical-two (Keywords dibutyl dithiocarbamates) is (2-4): 7; Described oxidation inhibitor refers to the phenyl αnaphthylamine; Described metal passivator refers to thiadiazoles derivative T561;
The production technique of described complex lithium grease comprises the steps:
1) base oil of the described weight of adding in the saponification still is opened and is stirred, and rotating speed 30-60 rev/min, add whole 12 oxystearic acids, be warmed up to 90-100 ℃, 12 oxystearic acids are all dissolved;
2) 1/2 part of lithium hydroxide getting described weight is dissolved in 6-10 times of 95-100 ℃ of hot water, slowly adds and carries out saponification reaction, and the joining day is no less than 30 minutes, and saponification time is no less than 1 hour; Slowly be warming up to 120-150 ℃;
3) add sebacic acid, stirred 20 minutes, 1/2 of weight part of lithium hydroxide is dissolved in 6-10 times of 95-100 ℃ of hot water under the remainder, slowly adds and reacts, and the joining day is no less than 30 minutes, then is incubated;
4) heat up dehydration to 150 ℃ of 1/2 oxidation inhibitor that add described weight, continue to be warming up to 200-220 ℃, be incubated 10-30 minute;
5) with material pumping to blending kettle, be cooled to 120-100 ℃ of 1/2 oxidation inhibitor that adds remaining weight, adds multi-functional dose and metal passivator, usefulness circulation shear and dispersed with stirring 20 minutes;
6) above-mentioned material is uniformly dispersed with high pressure homogenizer, is pumped to blending kettle, add tackifier, stirred 20 minutes, for subsequent use;
7) composite calcium sulfonate grease lubricant is added in the above-mentioned material, be uniformly dispersed by stirring and circulation shear, namely obtain complex lithium grease.
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|---|---|---|---|---|
| WO2017120000A1 (en) * | 2016-01-07 | 2017-07-13 | Nch Corporation | Manufacturing calcium sulfonate greases using alkali metal hydroxide and delayed addition of non-aqueous converting agents |
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| CN105602659A (en) * | 2016-01-25 | 2016-05-25 | 龙笑琼 | Complex lithium grease and preparing method thereof |
| US10087387B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
| US10087391B2 (en) | 2016-05-18 | 2018-10-02 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases without a conventional non-aqueous converting agent |
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