CN1052891A - Composite lithium-base grease - Google Patents
Composite lithium-base grease Download PDFInfo
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- CN1052891A CN1052891A CN 89109442 CN89109442A CN1052891A CN 1052891 A CN1052891 A CN 1052891A CN 89109442 CN89109442 CN 89109442 CN 89109442 A CN89109442 A CN 89109442A CN 1052891 A CN1052891 A CN 1052891A
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Abstract
A kind of complex lithium grease of high temperature resistant, anti-heavy loading.Its viscosifying agent is the compound soap of 12-oxystearic acid lithium soap, Whitfield's ointment lithium salts and boric acid lithium salts three components.Base oil can be selected Dormant oils, synthetic hydrocarbon oil, ester class oil, silicone oil or its mixing oil.Additive is one group and contains dialkyl group curing carboxylamine metal-salt, compound extreme-pressure anti-friction additives such as nitrogen heterocyclic ring amine salt and tackifier.The dropping point of this lubricating grease is more than 260 ℃, and integrated abrasion value is greater than 588.4N (60kgf), has good high temperature resistant, extreme-pressure anti-wear and adhesion property, can satisfy in-20～200 ℃ of temperature ranges and heavy load conditions under the power lubrication requirement.
Description
The present invention relates to a kind of extreme pressure compound lithium base grease that is applied under high temperature, the heavy load conditions, the product that it is made up of base oil, complex thickener and extreme-pressure anti-friction additive.
In diversified lubricant, though the ratio of lubricating grease output is little, occupies very consequence in industrial application, it plays the normal operation of safeguarding various mechanical means, the crucial effects such as wearing and tearing, prolonged mechanical service life of equipment of reducing friction.In various lubricating grease, lithium soap grease has multiple function and long work-ing lifes such as good mechanical stability, colloid stability, oxidation stability and anti-water, protection.Lithium saponify has replaced calcium grease and sodium-base grease commonly used within the specific limits as general multiple-effect fat, and its output shared ratio in the lubricating grease ultimate production day by day increases.But, because the dropping point scope of lithium saponify between 170～200 ℃, is unsuitable for using at the high temperature position that is higher than 120 ℃.And the compositing lithio ester lithium soap grease of new generation faster that is development in recent years, it is that the compound soap that forms with two or more acid and lithium hydroxide reaction is the lithium soap grease of viscosifying agent with the base oil multiviscosisty, is attracted attention by the user with its outstanding high temperature resistance.The dropping point of compositing lithio ester is more than 260 ℃, and it has improved the use properties under the high temperature again widely except that the premium properties that has kept common lithium saponify in mesophilic range.It maintains the denseness of fat sample under 250 ℃ temperature, in that it has bearing life more than 400 hours under 177 ℃ the temperature, compound lithium soap all has thickening ability preferably to various types of base oils, and is good to the susceptibility of multiple additives, is the high temperature grease of developing at present.U.S.P.3,758,407 and U.S.P.3,988,248 patent documentations all once disclosed relevant complex lithium grease and preparation method.But disclosed content only limits to basic lubricating grease, there is no extreme-pressure additive prescription and performance evaluation.
In recent years, along with the development that the modernization of industry is built, industrial sectors such as iron and steel, mine, automobile, railway, chemical fibre, printing and dyeing, aerospace all propose harsh day by day requirement to many-sided performances such as high temperature resistant, the extreme-pressure anti-wear of lubricating grease, anti-water, protection, bearing lives.For example some equipment of Iron And Steel Industry often be in process of production high temperature, water drench, at a high speed, the bad working environments condition of heavy duty, many dirt.The charging roller table bearing stands the baking that the smelting furnace high temperature width of cloth is penetrated for a long time, also will stand heavy duty and powerful impact load simultaneously.Under this exacting terms as use common lithium saponify can very fast loss to lose efficacy and cause the heavy wear of equipment, card to sting even sintering.Though the high-temperature behavior of compositing lithio ester is good, do not possess good extreme pressure and antiwear behavior during not doping yet.
Purpose of the present invention just is in order to overcome above-mentioned weak point of the prior art, provide a kind of can be high temperature resistant, again ability extreme pressure, wear-resistant, anti-water, have the complex lithium grease of use propertieies such as adhesivity, long lifetime concurrently,, heavy industry light to satisfy in development to the actual needs of lubricating grease.
The invention is characterized in and use compositing lithio ester as basic fat, add the binder component of one group of extreme-pressure anti-wear tackify, include extreme pressure agent dialkyldithiocarbamacompositions antimony (D), extreme pressure anti-wear additives dialkyldithiocarbamacompositions oxygen moly-sulfide (E), oiliness improver benzotriazole amine salt (F), tackifier ethylene/propene copolymer (G) composition.
Base oil in the lubricating grease is the principal element of a characteristic such as oxidation-resistance, vaporization losses, low-temperature fluidity and lubricity of decision lubricating grease, because lubricating grease of the present invention is used under hot conditions, so can select higher middle matter of viscosity or the neutral basic mineral oil of heavy for use.Also can require to select for use synthetic hydrocarbon oil, ester class oil, the mixing oil of silicone oil or above-mentioned oils according to property to product.The base oil consumption accounts for 70～95% of lubricating grease weight.
The effect of the viscosifying agent in the lubricating grease is lubricating grease to be become the base oil multiviscosisty stable colloid of plasticity, adhesivity and stopping property is arranged.Grease thickener system of the present invention by (A), (B) and (C) compound lithium soap of three components form.
(A) be C
16～C
20Hydroxy fatty acid or its lower alkyl esters (as methyl) are preferably the 12-oxystearic acid, and its consumption accounts for 5～20% of lubricating grease weight.
(B) be C
3～C
14Hydroxycarboxylic acid or its lower alkyl esters (as methyl, ethyl, propyl group etc.), the carbon atom that wherein connects hydroxyl is leaving on the molecular chain that carboxylic acid is no more than 6 carbon atoms, and commonly used is Whitfield's ointment, lactic acid etc.Consumption accounts for 0.1～5% of lubricating grease weight.
(C) be boronic acid compounds, boric acid list lithium salts commonly used, its consumption accounts for 0.1～5% of lubricating grease weight.
(A), the consumption of (B), (C) is with (A) 5～20%, (B) 0.5～3%, (C) 0.2～2% is better.The amount of viscosifying agent accounts for 5～30% of lubricating grease weight, and less than 5% o'clock, the denseness of finished product fat was not enough, and greater than 30% o'clock, the denseness of product was really up to the mark, all is not suitable for.
The effect of additive is a use properties of improving lubricating grease, as the extreme pressure and antiwear behavior of lubricating grease of the present invention, delays lubricating grease deterioration by oxidation process in use, prolongs its durable life-span.One group of composite additive that lubricating grease of the present invention adds comprises two kinds of extreme pressure anti-wear additives, oiliness improver and tackifier.
Have report (A.T.Polishuk with the dialkyldithiocarbamacompositions metal-salt in the past as extreme-pressure anti-wear, antioxidant addn, NLGI Spokesman, 43, No, 6,200-205[1979]), in this report, once joined in the lithium soap grease and can significantly improve its extreme pressure and antiwear behavior with zinc dialkyl dithiocarbamate, lead, antimony and the molybdenum salt of 1-3%.But, there is not satisfied requirement to the high temperature use properties though improved extreme pressure and antiwear behavior because used fat is common lithium saponify.In addition, use plumbiferous additive also can cause pollution, in grease product, also should avoid using as far as possible environment.It is extreme pressure agent that the present invention has adopted dialkyldithiocarbamacompositions antimony (D), and its structural formula is:
Its add-on is with respect to 0.5～5% of basic lubricating grease weight.Second kind of extreme pressure anti-wear additives that the present invention adopts is dialkyldithiocarbamacompositions oxygen moly-sulfide (E), and its structural formula is:
Its add-on is with respect to 0.1～3% of basic lubricating grease weight.These two kinds of extreme pressure agents all have oxidation resistant performance concurrently.
For prevent lubricating grease for a long time with contingent corrosion during mechanical part contacts, should add a spot of anticorrosive agent.Existing being reported in adds the benzotriazole aliphatic amide to increase protection against corrosion and oxidation resistant performance (refining of petroleum, 1982, No, 8,6) in the lubricating oil.The structural formula of this additive is:
Its advantage is to have oiliness, wear-resistant, anti-oxidant, protection against corrosion, multiple function such as antirust concurrently.In addition, especially when with the compound use of various sulfur-containing extreme-pressure additives, extreme pressure property there is the synergic effect.The amount that adds benzotriazole aliphatic amide (F) in the lubricating grease of the present invention is with respect to 0.05～1% of basic lubricating grease weight.
For the lubricating grease that is applied in lubricant housings such as bigger bearing of vibration and gear, require to have the good adhesive force performance.Generally select for use the polymer organic polymer as tackifier.According to nearest report (refining of petroleum, 1986, No, 12,34), ethylene/propene copolymer is all superior than polyisobutene and polymethacrylate commonly used aspect tackifying ability, shear stability and heat-resistant quality.Therefore to have selected ethylene/propene copolymer (G) for use be tackifier to lubricating grease of the present invention, and its molecular weight ranges is 3 * 10
4～10
5Between.Its consumption is with respect to 0.5～5% of basic lubricating grease weight.
The extreme pressure anti-wear additives (D) of four kinds of above-mentioned excellent performances, (E), oiliness improver (F) and tackifier (G), the present invention has further produced the synergism of pulling together with its compound adapted, and is applied in the complex lithium grease with hot properties, these four kinds of additives cooperation ratio preferably is (D) 1～4%, (E) 0.5～2%, (F) 0.1～0.5%, (G) 1～3%, total amount is 3～10%, is the weight percentage with respect to basic lubricating grease.These four kinds of additives all have Industrial products at home.
The advantage of lubricating grease of the present invention is that the efficient extreme pressure and antiwear behavior with the high-temperature behavior of compositing lithio ester and composite additive combines, and makes a kind of lubricating grease that can the high temperature resistant heavy loading of ability again.The dropping point of this lubricating grease is more than 260 ℃, and integrated abrasion value can be up to 588N(60kgf).And the dropping point of at present commercially available industrial extreme pressure lithium base lubricating grease is only about 180 ℃, and the temperature range of use if when using under surpassing 150 ℃ condition, will run off only in-20～130 ℃, therefore can not satisfy industrial high temperature service requirements.Lubricating grease of the present invention can use in-20～200 ℃ wide temperature range, long service life, this be existing extreme pressure lithium base fat can not with its analogy.
Below in conjunction with embodiment, lubricating grease of the present invention further is described in detail.
Embodiment 1:
Present embodiment is the step of preparation lubricating grease
Component weight, gram
500SN Dormant oils 255
12-oxystearic acid 42.0
Wintergreen oil 2.13
Boric acid 0.86
One hydronium(ion) oxidation lithium 7.1
42.0 gram 12-oxystearic acids, 2.13 gram wintergreen oils are joined in the 500SN Dormant oils of 127.5 grams, be heated to 82-88 ℃, after treating the fusing of 12-oxystearic acid, add a hydronium(ion) oxidation lithium of 7.1 grams and the mixed aqueous solution of 0.86 gram boric acid, after the saponification dehydration, be warming up to 200 ℃, the 127.5 gram Dormant oils that add surplus are made quenching oil, leave standstill after stirring and be cooled to room temperature, grind evenly.Grease dropping point＞260 ℃, 1/4 cone penetration 69.
Embodiment 2:
The system fat step of present embodiment is identical with embodiment 1, but the proportion scale difference.
Component weight, gram
500SN Dormant oils 255
12-oxystearic acid 33.2
Wintergreen oil 8.40
Boric acid 3.42
One hydronium(ion) oxidation lithium 9.3
Grease dropping point＞260 ℃, 1/4 cone penetration 78
From the data of table 1 as can be seen, in the lubricating grease of embodiment 3 to embodiment 6, be added with compound extreme-pressure anti-friction additive of the present invention, when comparing with not additivated compound lithium base basis fat, both dropping points are all more than 260 ℃, after in basic fat, adding additive, the mechanical stability of its denseness and tumbler test is almost constant, and the branch oil mass has improvement slightly, reduces to about 1% by 4%.Therefore, add composite additive of the present invention after, the structure of lubricating grease is not had destruction.The tetra-ball machine test data of evaluation lubricant extreme pressure and antiwear behavior show, at rupture of oil film load (P
B), sintering load (P
D) and integrated abrasion value (ZMZ) numerical value on all be greatly improved with the contrast of basic fat.At embodiment 3,4, in 5, consumption (is 100% with basic fat amount) when dibutyl dithiocaarbamate oxygen moly-sulfide (E), adding additive capacity is 1% o'clock, along with the consumption of dibutyl dithiocaarbamate antimony (D) drops to 1% by 3%, the integrated abrasion value of lubricating grease (ZMZ) also drops to 482 by 635 gradually.In embodiment 6, the add-on of dibutyl dithiocaarbamate oxygen moly-sulfide (E) is increased to 2%, but with embodiment 3 relatively, its extreme pressure property substantially quite and not further improves.Therefore the add-on of dibutyl dithiocaarbamate oxygen moly-sulfide (E) needn't increase again.Multinomial performance data in the table 1 illustrate that all the extreme pressure and antiwear behavior of embodiment 3 is best.
Embodiment 7:
Present embodiment is scale-up result on middle-scale device, and products obtained therefrom is carried out more comprehensive performance evaluation.
Component weight, (kilogram)
650SN Dormant oils 15.8
12-oxystearic acid 2.8
Wintergreen oil 0.142
Boric acid 0.058
One hydronium(ion) oxidation lithium 0.47
Dibutyl dithiocaarbamate antimony 0.56
Dibutyl dithiocaarbamate oxygen moly-sulfide 0.20
Benzotriazole amine salt 0.40
Ethylene/propene copolymer (dried agent content 25%) 1.60
In system fat still with agitator and circulation shear device, add part 650SN oil petroleum refined by naphthenic, the 12-oxystearic acid, wintergreen oil, mixture is stirred and be heated to 86 ℃, treat that lipid acid fusing back adds the mixed aqueous solution of a hydronium(ion) oxidation lithium and boric acid (earlier a hydronium(ion) oxidation lithium being mixed with the aqueous solution of 8% concentration), treats the material saponification, be warming up to 200 ℃ after the dehydration, add remaining oil petroleum refined by naphthenic and make quenching oil.The material circulation is cooled to 130 ℃ then, and 78.4 * 10
4Circulation shear became fat in 30 minutes under the pressure of Pa.Right dibutyl dithiocaarbamate antimony (D), dibutyl dithiocaarbamate oxygen moly-sulfide (E), benzotriazole ammonium salts (F) and the ethylene/propene copolymer additives such as (G) of under 108 ℃ temperature, adding, circulation mixes, and promptly obtains extreme pressure compound lithium base grease of the present invention through the degassing and after filtering.Its performance is listed in table 2.
Table 2
| Test subject | The result | Test method |
| Dropping point, ℃ Drawing cone in-degree, 1/10mm prolongs worker's cone penetration, 100,000 times, 1/10mm adds water 10%, 100,000 times, (100 ℃ of 1/10nn Stencil oil-dividing amounts, 22h), (180 ℃ of % steam output, 22h), (104 ℃ of % wastages, 6h), g water drenches (38 ℃ of numbers of dropouts, 1h), % tetra-ball machine test rupture of oil film load, P B, N sintering load, P D, N integrated abrasion value ZMZ, N | ＞260 267 328 341 1.19 4.40 0.60 4.60 657 4903 746 | GB3498 GB269 GB269 SY2729 GB7325 ASTMD1263 SY2718 GB3142 |
Data from table 2 find out that extreme pressure compound lithium base grease denseness of the present invention is 2 grades of NLGI, and dropping point is greater than 260 ℃, and less than 5%, sintering load reaches 4903N at the evaporation losses of 180 ℃ of following long periods of high temperature, and integrated abrasion value is up to 746N.These data show lubricating grease of the present invention except that having common lithium saponify favorable mechanical stability, colloid stability, water repelling property, also have excellent especially high-temperature behavior and extreme pressure and antiwear behavior, reach its intended purposes of the present invention, can satisfy the lubricating requirement that in-20～200 ℃ of temperature ranges, reaches machinery under the heavy load conditions.
Claims (4)
1, a kind of extreme pressure compound lithium base grease of high temperature resistant, anti-high loading, its viscosifying agent is three component compound soaps of 12-oxystearic acid lithium soap, Whitfield's ointment lithium salts and boric acid lithium salts, the invention is characterized in to add one group of compound extreme-pressure anti-wear, tackify multipurpose additive, its composition and weight percentage (with respect to not additivated basic fat) are respectively:
Dialkyl dithiocarbamate 0.5～5%
Dialkyldithiocarbamacompositions oxysulfide 0.1～3%
Benzotriazole amine salt 0.05～1%
Tackifier 0.5～5%
2, according to the said complex lithium grease of claim 1, it is characterized in that the dialkyl dithiocarbamate in the said additive component is a dialkyldithiocarbamacompositions antimony, the dialkyldithiocarbamacompositions oxysulfide is a dialkyldithiocarbamacompositions oxygen moly-sulfide, and tackifier are ethylene/propene copolymer.
3, according to the said complex lithium grease of claim 1, the content of 12-oxystearic acid lithium soap accounts for 5～20% of lubricating grease weight in its viscosifying agent, the Whitfield's ointment lithium salts accounts for 0.1～5% of lubricating grease weight, the total amount that the boric acid lithium salts accounts for 0.1～5%, three kinds of compound lithium soap thickening agents of lubricating grease weight accounts for 5～30% of lubricating grease weight.
4, according to the said complex lithium grease of claim 1, its base oil can be the mixing oil of the neutral basic mineral oil of middle matter or heavy, synthetic hydrocarbon oil, ester class oil, silicone oil or above-mentioned oils, and base oil accounts for 70～95% of lubricating grease weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89109442 CN1016514B (en) | 1989-12-23 | 1989-12-23 | Extreme pressure type composite lithium-based lubricating grease |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89109442 CN1016514B (en) | 1989-12-23 | 1989-12-23 | Extreme pressure type composite lithium-based lubricating grease |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1052891A true CN1052891A (en) | 1991-07-10 |
| CN1016514B CN1016514B (en) | 1992-05-06 |
Family
ID=4858010
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89109442 Expired CN1016514B (en) | 1989-12-23 | 1989-12-23 | Extreme pressure type composite lithium-based lubricating grease |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1016514B (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046758C (en) * | 1996-08-29 | 1999-11-24 | 赵亦军 | Lubricant tackifier and production method thereof |
| US6214778B1 (en) | 1995-08-24 | 2001-04-10 | The Lubrizol Corporation | Polyurea-thickened grease composition |
| CN1078240C (en) * | 1997-09-25 | 2002-01-23 | 中国科学院兰州化学物理研究所 | High-low-temp. extreme-pressure resisting special lubricant |
| CN1311062C (en) * | 2003-03-04 | 2007-04-18 | 夏位松 | Protective oil and grease |
| CN101200670B (en) * | 2006-12-12 | 2010-05-19 | 中国石油天然气集团公司 | Composite lithium-base grease and method for making same |
| CN101990570A (en) * | 2008-04-11 | 2011-03-23 | 出光兴产株式会社 | Grease composition and linear motion device using same |
| CN101037636B (en) * | 2006-03-14 | 2011-05-25 | 上海帕卡兴产化工有限公司 | Antirust composition and preparation method thereof |
| CN102959064A (en) * | 2010-06-30 | 2013-03-06 | 雪佛龙美国公司 | Lithium complex grease with improved thickener yield |
| CN105219489A (en) * | 2015-10-29 | 2016-01-06 | 山东万友工业油脂有限公司 | A kind of lithium soap grease and preparation method thereof |
| CN106497629A (en) * | 2016-10-05 | 2017-03-15 | 中国石油化工股份有限公司 | A kind of compositionss of three component lithium complex greases and preparation method |
| CN108699479A (en) * | 2016-03-11 | 2018-10-23 | 株式会社电装 | Lubricant composition, mechanical component and starter freewheel clutch |
| CN114106907A (en) * | 2021-12-13 | 2022-03-01 | 广州诺拜因化工有限公司 | Composite lithium-based grease type damping high-temperature bearing lubricant |
| US11390826B2 (en) | 2016-03-11 | 2022-07-19 | Denso Corporation | Grease composition, machine component, and starter overrunning clutch |
| CN117821142A (en) * | 2023-12-27 | 2024-04-05 | 广州友乐润滑材料有限公司 | Compound additive, preparation method thereof and lubricating ester |
-
1989
- 1989-12-23 CN CN 89109442 patent/CN1016514B/en not_active Expired
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6214778B1 (en) | 1995-08-24 | 2001-04-10 | The Lubrizol Corporation | Polyurea-thickened grease composition |
| CN1046758C (en) * | 1996-08-29 | 1999-11-24 | 赵亦军 | Lubricant tackifier and production method thereof |
| CN1078240C (en) * | 1997-09-25 | 2002-01-23 | 中国科学院兰州化学物理研究所 | High-low-temp. extreme-pressure resisting special lubricant |
| CN1311062C (en) * | 2003-03-04 | 2007-04-18 | 夏位松 | Protective oil and grease |
| CN101037636B (en) * | 2006-03-14 | 2011-05-25 | 上海帕卡兴产化工有限公司 | Antirust composition and preparation method thereof |
| CN101200670B (en) * | 2006-12-12 | 2010-05-19 | 中国石油天然气集团公司 | Composite lithium-base grease and method for making same |
| US8673830B2 (en) | 2008-04-11 | 2014-03-18 | Idemitsu Kosan Co., Ltd. | Grease composition and direct-acting devices with the grease composition |
| CN101990570A (en) * | 2008-04-11 | 2011-03-23 | 出光兴产株式会社 | Grease composition and linear motion device using same |
| CN102959064A (en) * | 2010-06-30 | 2013-03-06 | 雪佛龙美国公司 | Lithium complex grease with improved thickener yield |
| CN102959064B (en) * | 2010-06-30 | 2015-08-19 | 雪佛龙美国公司 | There is the lithium double composition grease of the thickening efficiency of improvement |
| CN105219489A (en) * | 2015-10-29 | 2016-01-06 | 山东万友工业油脂有限公司 | A kind of lithium soap grease and preparation method thereof |
| CN105219489B (en) * | 2015-10-29 | 2018-07-24 | 山东万友工业油脂有限公司 | A kind of lithium base grease and preparation method thereof |
| CN108699479A (en) * | 2016-03-11 | 2018-10-23 | 株式会社电装 | Lubricant composition, mechanical component and starter freewheel clutch |
| US11390826B2 (en) | 2016-03-11 | 2022-07-19 | Denso Corporation | Grease composition, machine component, and starter overrunning clutch |
| US11713430B2 (en) | 2016-03-11 | 2023-08-01 | Denso Corporation | Grease composition, machine component, and starter overrunning clutch |
| CN106497629A (en) * | 2016-10-05 | 2017-03-15 | 中国石油化工股份有限公司 | A kind of compositionss of three component lithium complex greases and preparation method |
| CN114106907A (en) * | 2021-12-13 | 2022-03-01 | 广州诺拜因化工有限公司 | Composite lithium-based grease type damping high-temperature bearing lubricant |
| CN117821142A (en) * | 2023-12-27 | 2024-04-05 | 广州友乐润滑材料有限公司 | Compound additive, preparation method thereof and lubricating ester |
| CN117821142B (en) * | 2023-12-27 | 2024-05-31 | 广州友乐润滑材料有限公司 | Compound additive, preparation method thereof and lubricating ester |
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|---|---|
| CN1016514B (en) | 1992-05-06 |
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