CN1052890A - Antifrictional lithium-base composite grease - Google Patents
Antifrictional lithium-base composite grease Download PDFInfo
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- CN1052890A CN1052890A CN 89109441 CN89109441A CN1052890A CN 1052890 A CN1052890 A CN 1052890A CN 89109441 CN89109441 CN 89109441 CN 89109441 A CN89109441 A CN 89109441A CN 1052890 A CN1052890 A CN 1052890A
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Abstract
A kind of have low-friction coefficient, a high temperature resistant and long-life Antifrictional lithium-base composite grease, and its viscosifying agent system is the compound soap of 12-oxystearic acid lithium soap, Decane dioic, dilithium salts and Whitfield's ointment lithium salts three components.Base oil can be Dormant oils, synthetic hydrocarbon oil, ester class oil, silicone oil or its mixing oil.Feature of the present invention is to have added one group of wear-resistant, anti-oxidant, antirust and oiliness composite additive.The dropping point of this lubricating grease is more than 260 ℃, has performances such as good high-temperature, antirust, anti-water, is applicable to the lubricated of the rolling bearing of-30～200 ℃ of temperature ranges and sliding friction position.
Description
The present invention relates to a kind of composition and preparation method with low-friction coefficient, high temperature resistant and long-life complex lithium grease.
Along with developing rapidly of China's modernization of industry, harsh day by day requirement has been proposed for the quality of lubricating grease.As the sealed Idler bearing that on endless belt conveyor, uses, be the disposable fat that fills, not restock or replacing in operational process.Therefore the lubricating grease that uses on this bearing is required the long especially life-span, general requirement reached more than 6 years, promptly with the same life-span of bearing.This lubricating grease also requires to have good abrasion resistance reducing the rotational resistance of carrying roller, thereby reduces the driving power of equipment, reduces energy consumption and cuts operating costs.To being in the bearing of high temperature position work, as in the smeltery, the charging roller table of sintering plant, the bearing in the equipment such as the dryer of ceramics factory and printing and dyeing mill, uptake ventilator, its working temperature can be up to 200 ℃ about.These above-mentioned working conditions all require lubricating grease to have wear-resistant, high temperature resistant and long-life use properties.But the anti-attrition lubricating grease of commodity mostly is calcium grease at present, can only use under general temperature, in case surpass the 80 ℃ of dry grinding damages that promptly can run off and cause the equipment parts.Even the multi-usage of being described as, long-life lithium soap grease, its use temperature scope also can only be at-20～120 ℃.When use temperature surpassed 120 ℃, will shorten dramatically the work-ing life of lubricating grease.When temperature surpassed 150 ℃, common lithium soap grease just grossed incompetence.
Compositing lithio ester is the complex thickener that generates with two or more organic acid or mineral acid and lithium hydroxide reaction, the lubricating grease that Dormant oils or synthetic oil multiviscosisty are made.The characteristics of this lubricating grease be dropping point more than 260 ℃, its high-temperature behavior, antioxidant property and durable life-span all are better than common lithium saponify.Therefore, compositing lithio ester is within the specific limits as the industrial general fat of multiple-effect.U.S.3, patents such as 929,651 and U.S.3,711,407 have been introduced the composition and the preparation method of relevant complex lithium grease, but the content of patent disclosure only limits to the composition of basic fat and does not relate to the finished product lubricating grease that adds additive.Its preparation method is the two-step approach saponification process, will have repeatedly to be warming up to cooling in saponification reaction, and step is more loaded down with trivial details, and the production cycle is longer, and this is its weak point.
The object of the present invention is to provide a kind ofly to have good abrasion resistance, high temperature resistant and long-life Antifrictional lithium-base composite grease, and propose a kind of technology of making compositing lithio ester than the simple saponification of prior art.
In order to achieve this end, the present invention with compositing lithio ester as basic fat, added one group of wear-resistant, anti-oxidant, antirust, butyrous composite additive, and the grease making process that step alkaline saponification, a circulation shear becomes fat is proposed, make and have well wear-resistant, high-temperature behavior and long-life Antifrictional lithium-base composite grease.
The base oil of Antifrictional lithium-base composite grease of the present invention is that 100 ℃ viscosity is 3～40mm
2The Dormant oils of/s also can select for use the weight of synthetic hydrocarbon oil, ester class oil, silicone oil or its mixing oil, base oil to account for 70～95% of lubricating grease weight.
Its viscosifying agent system of Antifrictional lithium-base composite grease of the present invention is made of the compound lithium soap of (A), (B), (C) three kinds of acid.(A) be C
16～C
20Hydroxy fatty acid or its lower alkyl esters, 12-oxystearic acid preferably, consumption accounts for 5～20% of lubricating grease weight; (B) be C
4～C
12Di-carboxylic acid or its lower alkyl esters, as nonane diacid or sebacic acid, consumption accounts for 1～5% of lubricating grease weight; (C) be C
3～C
14Hydroxycarboxylic acid or its lower alkyl esters, as lactic acid, Whitfield's ointment and P-hydroxybenzoic acid, consumption accounts for 0.1～5% of lubricating grease weight.The total amount of viscosifying agent accounts for 5～30% of lubricating grease weight.
The use properties of lubricating grease is decided by the composition of its selection, i.e. base oil, viscosifying agent and additive.Three's effect is complementary, even good basis oil and good viscosifying agent are arranged, but during the additive that adds at particular requirement, does not still have good use properties.As previously mentioned, one of feature of complex lithium grease of the present invention is exactly to have added one group of anti-attrition, anti-oxidant, antirust and oiliness improver.This composite additive is made up of (D), (E), (F) three components, that is:
Amine type oxidation inhibitor (D) 0.1～2%, with 0.3～1% for well, (phase
For basic fat is for 100%, down together)
Benzotriazole amine salt rust-preventive agent (E) 0.05～1%, with 0.1～0.5% for well;
Aromatic dicarboxylic acids's ester oiliness improver (F) 0.1～2%, with 0.5～2% for well;
(D), the total amount of (E), (F) three kinds of additives is 0.3～5%, with 1～4% for well.
In order to prevent the deterioration by oxidation of lubricating grease in long storage and use, should add oxidation inhibitor to prolong the work-ing life of product.Oxidation inhibitor commonly used has phenols and aminated compounds.The present invention adopts pentanoic (D) or di-iso-octyldiphenylamine as oxidation inhibitor, and its structural formula is:
Benzotriazole amine salt (E) is a kind of have oiliness, wear-resistant, anti-oxidant, protection against corrosion, multi-functional additive (refining of petroleum, 1982, No.8,6) such as antirust, during the compound use of it and sulfur-bearing abrasion resistant extreme-pressure additive, also has obvious synergistic effect.As one of component of composite additive, its structural formula is with the benzotriazole octadecylamine in the present invention:
Oiliness improver is the additive that improves the lubricated abrasion resistance of lubricant, and it can be adsorbed on the firm oil film of formation on the metallic surface more securely to reach lubricated purpose.It is wear-resistant oiliness improver that the present invention uses aromatic dicarboxylic acids's ester of low-carbon alcohol (F), and as dibutyl phthalate, its antifriction effect in lithium saponify is better than other oiliness improvers commonly used, and its structural formula is:
Three kinds of above binder components all have the commercial goods.The present invention produces synergy with its compound use, and the effect of each component is able to further synergy performance.
Antifrictional lithium-base composite grease of the present invention is through multinomial performance test, show have good anti-attrition, performance and favorable mechanical stability, colloid stability and oxidation stability such as high temperature, antirust, protection against corrosion, anti-water, frictional coefficient is little, long service life has reached its intended purposes.Can be used for rolling bearing and sliding friction position in-30～200 ℃ of temperature ranges.
Antifrictional lithium-base composite grease of the present invention prepares with the single stage method method for saponification, and Fig. 1 is the schema of this method.For the ease of relatively, Fig. 2 is U.S.3, used schema in the patents such as 929,651 and U.S.3,711,407.Method of the present invention is with the dehydration of twice saponification in the art methods, twice intensification heating, and twice cooling is simplified to a saponification of three kinds of acid, once intensification heating, once cooling, the technology of passing through circulation shear again.This method is tangible in the advantage aspect shortening production cycle, the save energy.
The present invention is described in further detail by following embodiment.
Embodiment 1 present embodiment explanation is a base oil with silicone oil and ester class oil
The composition of compositing lithio ester and preparation method
Component weight, g
Tolyl silicone oil 82.0
Trihydroxymethylpropanyl ester 82.0
12-oxystearic acid 30.4
Sebacic acid 4.09
Wintergreen oil 1.54
One hydronium(ion) oxidation lithium 6.38
12-oxystearic acid, sebacic acid and wintergreen oil are added in the tolyl silicone oil, be heated to 86 ℃, after treating the lipid acid fusing, add lithium hydroxide aqueous solution, the saponification dehydration is warming up to 195 ℃～200 ℃, add trihydroxymethylpropanyl ester and make quenching oil, stir, be cooled to room temperature, grind homogenizing.268 ℃ of grease dropping points, 1/4 cone penetration 56.
Embodiment 2
The present embodiment difference from Example 1 is variant on the raw material composition proportioning, and preparation process is identical.
Component weight, g
Toluene base oil 80.0
Trihydroxymethylpropanyl ester 80.0
12-oxystearic acid 23.65
Sebacic acid 7.96
Wintergreen oil 8.39
One hydronium(ion) oxidation lithium 8.93
Grease dropping point＞300 ℃, 1/4 cone penetration 76
Embodiment 3
The oil base stock of present embodiment is a synthetic hydrocarbon oil.The preparation method is identical with embodiment 1, adds additive down at 100 ℃ behind the one-tenth fat and grinds evenly.
Component weight, g
Synthetic hydrocarbon oil 1275
12-oxystearic acid 142.5
Sebacic acid 48
Wintergreen oil 36
One hydronium(ion) oxidation lithium 28.4
Pentanoic 7.5
Benzotriazole octadecylamine 3.0
Dibutyl phthalate 15
Grease dropping point＞282 ℃, cone penetration 280
Embodiment 4
Present embodiment is the scale-up of 15kg of feeding intake on middle-scale device, and base oil is a Dormant oils.
Component weight, umber
500SN Dormant oils 85
12-oxystearic acid 9.5
Sebacic acid 3.2
Wintergreen oil 2.3
One hydronium(ion) oxidation lithium 3.3
Pentanoic 0.5
Benzotriazole amine salt 0.1
Dibutyl phthalate 1.0
Dormant oils, 12-oxystearic acid, sebacic acid, the wintergreen oil input of part are had in the system fat still of stirring, circulation shear device, material is heated to 86 ℃, after treating the lipid acid fusing, the aqueous solution that adds lithium hydroxide, material saponification dehydration, be warming up to 196 ℃～200 ℃, the Dormant oils that adds surplus is made quenching oil, and circulation is cooled to 130 ℃.About 78.4 * 10
4Pa(8kgf)/cm
2Circulation shear became fat in 30 minutes under the gauge pressure.Circulating after adding pentanoic, benzotriazole amine salt and dibutyl phthalate under 100 ℃ of temperature stirs, through getting product after the degassing, the filtration.Its performance is listed in table 2 and the table 3.
The physicochemical property of table 2 pilot product
| Test subject | Test-results | Test method |
| Dropping point, ℃ Drawing cone in-degree, 1/10mm prolongs the Drawing cone in-degree, 100,000 Stencil oil-dividing amounts, (100 ℃, 3h), % corrodes (T3 copper sheet, 100 ℃, 24h) volatile grade is (99 ℃, 22h), % water drenches (38 ℃ of numbers of dropouts, 1h), the % similar viscosity,-20 ℃, (100 ℃ of Pa.S oxidation stabilities, 100h) pressure falls, (52 ℃ of Pa non-corrosibilities, 48h), (104 ℃ of level wheel bearing wastages, 6h), g | ＞282 268 292 2.08 qualified 0.5 1.64 1,160 4.9 * 103One-level 0.8 | GB3498 GB269 GB269 SY2729 GB7326 first method ASTM D972 SY 2718 SY 2720 SY 2715 GB 5018 ASTM D1263 |
The anti-attrition performance of table 3 pilot product
| Test subject | Basis fat | Finished product fat behind the adding additive |
| Tetra-ball machine test, (GB 3142) rupture of oil film load P BN (kgf)/mm 15 frictional coefficient, f (d) 40 ＇ 15 grinding defect diameters, d, mm 40 ＇ 20 d, mm 30 ＇ | 490(50) /0.30 0.167 0.59 0.64 | 490(50)/ 0.37 0.12 0.41 0.58 |
The data declaration of table 2, be higher than 260 ℃ from the dropping point of lubricating grease of the present invention, vaporization losses 0.5%, the cone penetration difference is in 30 units after 100,000 shearing tests, the antirust one-level that reaches is corroded test-results such as qualified and is shown that lubricating grease of the present invention has excellent high-temperature performance, antirust, protection against corrosion, water repelling property and favorable mechanical stability, colloid stability and oxidation stability.From the tetra-ball machine test result of table 3 as can be seen, with not additivated basic fat relatively, after adding additive, though rupture of oil film load P
BValue is suitable, but frictional coefficient and grinding defect diameter all have reduction largely, have reached intended purposes high temperature resistant, anti-attrition.
Claims (5)
1, a kind of have low-friction coefficient, a resistant to elevated temperatures complex lithium grease, its viscosifying agent system is made of the compound lithium soap of hydroxy fatty acid (A), di-carboxylic acid (B) and three kinds of acid of hydroxycarboxylic acid (C), the invention is characterized in and contain one group of anti-oxidant, antirust and oiliness composite additive, it consists of:
(with respect to basic fat is 100% to amine type oxidation inhibitor (D) 0.1～2%
, down together)
Benzotriazole amine salt rust-preventive agent (E) 0.05～1%
Ester class oiliness improver (F) 0.1～2%
The total amount of three kinds of additives (D), (E), (F) is 0.3～5%.
2, a kind of have low-friction coefficient, resistant to elevated temperatures complex lithium grease, its viscosifying agent system and be made of the compound lithium soap of hydroxy fatty acid (A), di-carboxylic acid (B) and three kinds of acid of hydroxycarboxylic acid (C), the invention is characterized in above three kinds of acid with a step alkaline saponification react, circulation shear technology makes complex lithium grease.
3, according to the said complex lithium grease of claim 1, it is characterized in that the amine type oxidation inhibitor (D) in the composite additive is pentanoic or di-iso-octyldiphenylamine, benzotriazole amine salt rust-preventive agent (E) is the benzotriazole octadecylamine, and ester class oiliness improver (F) is a dibutyl phthalate.
4,, it is characterized in that used base oil is that 100 ℃ viscosity is 3～40mm according to the said complex lithium grease of claim 1
2The Dormant oils of/s, synthetic hydrocarbon oil, ester class oil, silicone oil or its mixing oil, the content of base oil accounts for 70～95% of lubricating grease weight.
5,, it is characterized in that forming hydroxy fatty acid (A) C of viscosifying agent system according to the said complex lithium grease of claim 1
16～C
20Hydroxy fatty acid or its lower alkyl esters, as the 12-oxystearic acid, its content is that fat weighs 5～20%; Di-carboxylic acid (B) is C
4～C
12Di-carboxylic acid or its lower alkyl esters, as sebacic acid, nonane diacid, its content is that fat weighs 1～5%; Hydroxycarboxylic acid (C) is C
3～C
14Hydroxycarboxylic acid or its lower alkyl esters, as wintergreen oil, its content be fat heavy 0.1～5%, the total amount of viscosifying agent accounts for 5～30% of lubricating grease weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89109441 CN1017344B (en) | 1989-12-23 | 1989-12-23 | Antifrictional lithium-base composite grease |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89109441 CN1017344B (en) | 1989-12-23 | 1989-12-23 | Antifrictional lithium-base composite grease |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1052890A true CN1052890A (en) | 1991-07-10 |
| CN1017344B CN1017344B (en) | 1992-07-08 |
Family
ID=4858009
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89109441 Expired CN1017344B (en) | 1989-12-23 | 1989-12-23 | Antifrictional lithium-base composite grease |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1017344B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6214778B1 (en) | 1995-08-24 | 2001-04-10 | The Lubrizol Corporation | Polyurea-thickened grease composition |
| CN1302094C (en) * | 2004-01-18 | 2007-02-28 | 许晓华 | Lubricating grease composition for motor gearbox |
| CN101270315B (en) * | 2008-05-12 | 2010-12-22 | 中国人民解放军总装备部军械技术研究所 | Work liquid special for breechblock bumper absorber of antiaircraft gun |
| CN101177645B (en) * | 2006-11-10 | 2011-07-20 | 协同油脂株式会社 | Lubricating grease as well as bearing and gear using the same |
| CN101619260B (en) * | 2009-08-07 | 2013-01-09 | 安庆市中天石油化工有限公司 | Preparation method of high shear stability lithium grease |
| CN103627476A (en) * | 2013-12-12 | 2014-03-12 | 新乡市恒星化工有限责任公司 | Low-noise lubricating grease and preparation method and application thereof |
| CN104327906A (en) * | 2014-10-25 | 2015-02-04 | 中国石油化工股份有限公司 | Composition of compound calcium sulfonate-based lubricating grease for improving high-temperature performance and preparation method thereof |
| CN104629887A (en) * | 2013-11-08 | 2015-05-20 | 中国石油天然气股份有限公司 | Composite lithium-based lubricating grease and preparation method thereof |
-
1989
- 1989-12-23 CN CN 89109441 patent/CN1017344B/en not_active Expired
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6214778B1 (en) | 1995-08-24 | 2001-04-10 | The Lubrizol Corporation | Polyurea-thickened grease composition |
| CN1302094C (en) * | 2004-01-18 | 2007-02-28 | 许晓华 | Lubricating grease composition for motor gearbox |
| CN101177645B (en) * | 2006-11-10 | 2011-07-20 | 协同油脂株式会社 | Lubricating grease as well as bearing and gear using the same |
| CN101270315B (en) * | 2008-05-12 | 2010-12-22 | 中国人民解放军总装备部军械技术研究所 | Work liquid special for breechblock bumper absorber of antiaircraft gun |
| CN101619260B (en) * | 2009-08-07 | 2013-01-09 | 安庆市中天石油化工有限公司 | Preparation method of high shear stability lithium grease |
| CN104629887A (en) * | 2013-11-08 | 2015-05-20 | 中国石油天然气股份有限公司 | Composite lithium-based lubricating grease and preparation method thereof |
| CN103627476A (en) * | 2013-12-12 | 2014-03-12 | 新乡市恒星化工有限责任公司 | Low-noise lubricating grease and preparation method and application thereof |
| CN104327906A (en) * | 2014-10-25 | 2015-02-04 | 中国石油化工股份有限公司 | Composition of compound calcium sulfonate-based lubricating grease for improving high-temperature performance and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1017344B (en) | 1992-07-08 |
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