CN102250671A - Wide temperature range and high extreme pressure composite lithium lubricating grease composition - Google Patents

Wide temperature range and high extreme pressure composite lithium lubricating grease composition Download PDF

Info

Publication number
CN102250671A
CN102250671A CN2011101688157A CN201110168815A CN102250671A CN 102250671 A CN102250671 A CN 102250671A CN 2011101688157 A CN2011101688157 A CN 2011101688157A CN 201110168815 A CN201110168815 A CN 201110168815A CN 102250671 A CN102250671 A CN 102250671A
Authority
CN
China
Prior art keywords
feature
lubricating grease
complex lithium
acid
alkyl
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2011101688157A
Other languages
Chinese (zh)
Other versions
CN102250671B (en
Inventor
郭振俊
吴宝杰
刘庆廉
刘翠苹
高思嘉
李卓
刘洋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Original Assignee
China Petroleum and Chemical Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp filed Critical China Petroleum and Chemical Corp
Priority to CN 201110168815 priority Critical patent/CN102250671B/en
Publication of CN102250671A publication Critical patent/CN102250671A/en
Application granted granted Critical
Publication of CN102250671B publication Critical patent/CN102250671B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Lubricants (AREA)

Abstract

The invention relates to a wide temperature range and high extreme pressure composite lithium lubricating grease composition. The composite lithium-based lubricating grease composition provided by the invention is prepared from poly-alpha-olefin synthetic oil and ester oil as base oils and two-component composite lithium soap as a thickening agent, and an antioxidant, an anticorrosion and antirust agent and an extreme-pressure anti-wear additive are added. Due to the appropriate proportion of raw materials, the lubricating grease has excellent high and low temperature performance, the dropping point is greater than 260 DEG C, and the low-temperature (-40 DEG C) torque is not higher than 0.98 N.m during starting and is not higher than 0.50 N.m during running; the lubricating grease also has excellent extreme-pressure anti-wear properties, the sintering capacity is not lower than 3089 N, the Timken 0K value is up to 267 N, and the anti-wear performance (tested by a four-ball machine method) is not greater than 0.60 mm. Therefore, the lubricating grease provided by the invention can be used for lubricating high-load equipment within a wide temperature range.

Description

The high extreme pressure compound lithium grease composition of a kind of wide temperature
Technical field
The present invention relates to a kind of compound lithium base grease composite of forming by base oil, viscosifying agent and additive with good extreme pressure anti-wear that can use at wide temperature range.
Background technology
Along with development of modern industry, especially the continuous upgrading and the update of industry technology such as metallurgy, automobile, mine and equipment, high warm nature to lubricating grease requires more and more higher, simultaneously, because China is vast in territory, industry such as automobile, mine needs also low temperature properties to be proposed high request at the equipment of outdoor application, and the minimum use temperature of the equipment requirements that has is-40 ℃ even lower.In order to enhance productivity and to reduce cost, in metallurgy, mine, automobile and other industries, equipment enlarging, automatization, heavy loading are development trends, and this just proposes higher requirement to the extreme pressure property of lubricating grease.Therefore, thus invention is a kind of to have that can use and the lubricating grease that have good extreme pressure and antiwear behavior of good high and low temperature and is necessary in wide temperature range.
Complex lithium grease has the good high-temperature performance, and dropping point generally can be greater than 260 ℃, close and, by the adjustment of technology and prescription, can make the brand-name grease of every balancing performance.Compound lithium soap divides by component, nearly three classes, one class is the complex lithium of binary acid (mainly being sebacic acid, nonane diacid, hexanodioic acid) with ten dihydroxystearic acids, second class is mineral acid such as boric acid, the phosphoric acid complex lithium with ten dihydroxystearic acids, and the 3rd class is to add aromatic acid such as Whitfield's ointment, phenylformic acid etc. again on above-mentioned two kinds of bases.
In the middle of existing invention, mainly be more at the prescription and the Study on manufacturing process of complex lithium viscosifying agent, and less to the high and low temperature and the extreme pressure property research of lubricating grease, thereby can not satisfy the requirements at the higher level that lubricating grease in use proposes well.Among the CN101705141 A, introduced a kind of preparing complex lithium grease, higher dropping point has been arranged; Among the CN101481637 A, introduced a kind of low temperature process and made preparing complex lithium grease; More than two patents all extreme pressure anti-wear, low temperature properties are not specifically noted.Among US4897210, the US5391309, also introduced different complex lithium grease preparation methods.
Summary of the invention
The purpose of this invention is to provide a kind of grease composition that has good high and low temperature and have good extreme pressure and antiwear behavior.It is base oil that compound lithium base grease composite provided by the invention adopts poly-alpha-olefin synthetic oil, ester class oil, and two component compound lithium soaps are viscosifying agent, and has added oxidation inhibitor, corrosion prevention rust preventer, extreme-pressure anti-friction additive and made.This lubricating grease has good high and low temperature and extreme pressure and antiwear behavior, and minimum use temperature can reach-40 ℃, and terraced nurse is agree the 0K value can reach 267N.
Technology of the present invention is as follows:
Viscosifying agent is two component compound soaps of ten dihydroxystearic acids and diprotic acid, and base oil is a synthetic base oil, adds one group of additive such as compound extreme-pressure anti-wear, and its composition and weight percentage are as follows:
Two component compound soaps of ten dihydroxystearic acids and diprotic acid: 9~15%,
Base oil: 85~91%;
With base oil and viscosifying agent total amount is 100% calculating, adds additive (additives ratio of adding is a radix with base oil and viscosifying agent total amount):
The dialkyl dithio amido formate: 0.5~5%,
Zinc dialkyl dithiophosphate: 0~3%,
Boric acid ester: 0~3%,
Thiophosphatephosphorothioate: 0.5~3%.
Oxidation inhibitor: 0.5~2%;
Corrosion prevention rust preventer: 0.05~1.5%;
The used multiviscosisty viscosifying agent of the present invention is the complex thickener of 12-oxystearic acid lithium soap and diprotic acid lithium, and diprotic acid is nonane diacid, sebacic acid, SL-AH preferably; The mol ratio of 12-oxystearic acid and diprotic acid is 1: 0.2~1: 2, and preferably at 1: 0.4~1: 0.8, the monohydrate lithium hydroxide consumption is 2%~3%.
The used base oil of the present invention is ester class oil or poly alpha olefine synthetic oil, and mixing range of viscosities (40 ℃) is 100~500mm 2/ s.
Oxidation inhibitor: amine, phenolic antioxidant, alkylating amine, phenolic antioxidant;
Corrosion prevention rust preventer: 124 Triazole derivative and thiadiazoles derivative, mahogany acid salt corrosion prevention rust preventer;
Extreme pressure anti-wear additives:
Dialkyl dithio amido formate, alkyl are preferably butyl, octyl group or the combination of the two.
Zinc dialkyl dithiophosphate, alkyl be one or both in butyl, octyl group, the primary/secondary alkyl preferably;
Boric acid ester, the carboxylate of nitrogenous compound and boric acid preferably, alkyl can be normal-butyl, octyl group or ethyl;
Thiophosphatephosphorothioate, alkylthio phosphoric acid ester preferably, alkyl can be normal-butyl, octyl group or two kinds of alkyl combinations.
Complex lithium grease manufacture method of the present invention is as follows:
(1) 12-oxystearic acid and diprotic acid and lithium hydroxide are joined in the part base oil, heat up 100~115 ℃, reacted 2~3 hours.
(2) intensification dehydration, constant temperature is 30~60 minutes when rising to 125~140 ℃.
(3) continue to heat up, add oxidation inhibitor, top temperature is 200~220 ℃.
(4) add a part of cooling oil, then cooling.
(5) add the surplus base oil, when being cooled to 90 ℃, add additive.
(6) three beaming rollers grind.
Lubricating grease result of performance test of the present invention shows to have following advantage: owing to selected proper raw material proportioning for use, make this lubricating grease have good high temperature performance, dropping point is greater than 260 ℃, low temperature torque (40 ℃) startup is not higher than 0.98N.m, running is not higher than 0.50N.m, and has good extreme pressure and antiwear behavior, and sintering load is not less than 3089N, the ladder nurse is agree the 0K value can reach 267N, and abrasion resistance (four-ball tester method) is not more than 0.60mm.Therefore lubricating grease of the present invention can be used for the lubricated of the interior high loading equipment of wide temperature range.
Embodiment
Example 1:
The 300g base oil is joined in the lab scale still, be warming up to 85 ℃, add 60g ten dihydroxystearic acids and 16g sebacic acid, add lithium hydroxide then, be warming up to 105~115 ℃ of reaction 2h by the water-soluble 16g of 80g.Heat up then and dewater, be warming up to 130~140 constant temperature 0.5h, continue to heat up, add the 4.2g di-iso-octyldiphenylamine, top temperature is 208 ℃.Add the cooling of 160g base oil, temperature adds remaining 304g base oil when reducing to below 150 ℃, add the 8.4g barium mahogany sulfonate when temperature is lower than 90 ℃ respectively, 4.2g thiadiazoles derivative, 42g dialkyl dithio amido formate, 25.2g thiophosphatephosphorothioate, 4.2g zinc dialkyl dithiophosphate.Grind homogenizing at three beaming rollers at last, and survey PERFORMANCE OF GREASES.
The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 1
Table 1
Figure BDA0000070210160000031
Example 2:
The 450g base oil is joined in the lab scale still, be warming up to 85 ℃, add 80g ten dihydroxystearic acids and 40g nonane diacid, add lithium hydroxide then, be warming up to 100~110 ℃ of reaction 2.5h by the water-soluble 30g of 110g.Heat up then and dewater, be warming up to 125~135 constant temperature 45 minutes, continue to heat up, add 8g di-iso-octyldiphenylamine and 8g tert-butyl phenol derivative, top temperature is 200 ℃.Add the cooling of 150g base oil, temperature adds remaining 80g base oil and 0.4g benzotriazole when reducing to below 150 ℃, add 4g dialkyl dithio amido formate when temperature is lower than 90 ℃ respectively, the 9.6g thiophosphatephosphorothioate, the 24g zinc dialkyl dithiophosphate, the 8g boric acid ester.Grind homogenizing at three beaming rollers at last, and survey PERFORMANCE OF GREASES.
The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 2
Table 2
Figure BDA0000070210160000032
Figure BDA0000070210160000041
Example 3:
The 300g poly alpha olefine synthetic oil is joined in the lab scale still, be warming up to 85 ℃, add 60g ten dihydroxystearic acids and 35g SL-AH, add lithium hydroxide then, be warming up to 105~115 ℃ of reaction 3h by the water-soluble 21g of 120g.Heat up then and dewater, be warming up to 130~140 constant temperature 1h, continue to heat up, add the 6g di-iso-octyldiphenylamine, top temperature is 220 ℃.Add the cooling of 235g base oil, temperature adds remaining 220g base oil and 0.8g benzotriazole when reducing to below 150 ℃, add 17g dialkyl dithio amido formate when temperature is lower than 90 ℃ respectively, 4.25g thiophosphatephosphorothioate, 25.5g boric acid ester.Grind homogenizing at three beaming rollers at last, and survey PERFORMANCE OF GREASES.
The PERFORMANCE OF GREASES that technical recipe of the present invention makes is listed in table 3
Table 3
Figure BDA0000070210160000042
A kind of novel lubricating oil/fat composition that the present invention proposes, be described by preferred embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to component as herein described and method is changed or suitably change reorganization close, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.

Claims (10)

1. high extreme pressure compound lithium base grease of wide temperature, its viscosifying agent is two component compound soaps of ten dihydroxystearic acids and diprotic acid, base oil is a synthetic base oil; It is characterized in that being to add one group of compound extreme-pressure anti-friction additive, its composition and weight percentage are as follows:
Two component compound soaps of ten dihydroxystearic acids and diprotic acid: 9~15%,
Base oil: 85~91%;
With base oil and viscosifying agent total amount is 100% calculating, adds additive;
The dialkyl dithio amido formate: 0.5~5%,
Zinc dialkyl dithiophosphate: 0~3%,
Boric acid ester: 0~3%,
Thiophosphatephosphorothioate: 0.5~3%.
Oxidation inhibitor: 0.5~2%;
Sanitas: 0.05~1.5%.
2. according to the said complex lithium grease of claim 1, the said diprotic acid of its feature is nonane diacid, sebacic acid or SL-AH.
3. according to the said complex lithium grease of claim 1, the mol ratio of said 12-oxystearic acid of its feature and diprotic acid is 1: 0.2~1: 2.
4. according to the said complex lithium grease of claim 1, the said base oil of its feature is ester class oil or poly alpha olefine synthetic oil, is 100~500mm when mixing range of viscosities and be 40 ℃ of temperature 2/ s.
5. according to the said complex lithium grease of claim 1, the said dialkyl dithio amido formate of its feature, alkyl are butyl, octyl group or the combination of the two.
6. according to the said complex lithium grease of claim 1, the said zinc dialkyl dithiophosphate of its feature, alkyl are one or both in butyl, octyl group, uncle or the secondary alkyl.
7. according to the said complex lithium grease of claim 1, the said boric acid ester of its feature is the carboxylate of nitrogenous compound and boric acid, and alkyl is normal-butyl, octyl group or ethyl.
8. according to the said complex lithium grease of claim 1, the said thiophosphatephosphorothioate of its feature is the alkylthio phosphoric acid ester, and alkyl can be normal-butyl, octyl group or two kinds of alkyl combinations.
9. according to the said complex lithium grease of claim 1, the said oxidation inhibitor of its feature is amine or phenolic antioxidant; The amine of preferred alkylization, phenolic antioxidant.
10. according to the said complex lithium grease of claim 1, the said sanitas of its feature is: 124 Triazole derivative, thiadiazoles derivative or mahogany acid salt corrosion prevention rust preventer.
CN 201110168815 2011-06-22 2011-06-22 Wide temperature range and high extreme pressure composite lithium lubricating grease composition Active CN102250671B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201110168815 CN102250671B (en) 2011-06-22 2011-06-22 Wide temperature range and high extreme pressure composite lithium lubricating grease composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201110168815 CN102250671B (en) 2011-06-22 2011-06-22 Wide temperature range and high extreme pressure composite lithium lubricating grease composition

Publications (2)

Publication Number Publication Date
CN102250671A true CN102250671A (en) 2011-11-23
CN102250671B CN102250671B (en) 2013-06-05

Family

ID=44978244

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201110168815 Active CN102250671B (en) 2011-06-22 2011-06-22 Wide temperature range and high extreme pressure composite lithium lubricating grease composition

Country Status (1)

Country Link
CN (1) CN102250671B (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102899127A (en) * 2012-09-13 2013-01-30 太平洋联合(北京)石油化工有限公司 Thiadiazole dimer lubricating grease additive, and preparation and application thereof
CN102899128A (en) * 2012-09-13 2013-01-30 太平洋联合(北京)石油化工有限公司 Borate lubricating grease additive, and preparation and application 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
CN105368413A (en) * 2015-11-25 2016-03-02 四川西南油大石油工程有限公司 Anti-wear anti-seize lubricant for drilling fluid
CN107033993A (en) * 2017-04-25 2017-08-11 南宁市钱隆汽车租赁有限公司 Automobile soft shaft lubricating grease
CN112195057A (en) * 2020-07-28 2021-01-08 重庆安美新材料有限公司 Robot harmonic reducer lubricating grease
CN114806682A (en) * 2022-03-28 2022-07-29 深圳市优宝新材料科技有限公司 Lubricating grease composition and preparation method thereof, thiazole compound, intermediate and preparation method thereof
CN116024026A (en) * 2021-10-25 2023-04-28 中国石油化工股份有限公司 Grease composition, preparation method thereof and application of dibasic fatty acid

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1852969A (en) * 2002-10-04 2006-10-25 R·T·范德比尔特公司 Synergistic organoborate compositions and lubricating compositions containing same
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1852969A (en) * 2002-10-04 2006-10-25 R·T·范德比尔特公司 Synergistic organoborate compositions and lubricating compositions containing same
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

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102899127A (en) * 2012-09-13 2013-01-30 太平洋联合(北京)石油化工有限公司 Thiadiazole dimer lubricating grease additive, and preparation and application thereof
CN102899128A (en) * 2012-09-13 2013-01-30 太平洋联合(北京)石油化工有限公司 Borate lubricating grease additive, and preparation and application thereof
CN102899127B (en) * 2012-09-13 2015-09-16 太平洋联合(北京)石油化工有限公司 A kind of thiadiazoles dimer grease additive and Synthesis and applications 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
CN105368413A (en) * 2015-11-25 2016-03-02 四川西南油大石油工程有限公司 Anti-wear anti-seize lubricant for drilling fluid
CN105368413B (en) * 2015-11-25 2017-12-26 四川西南油大石油工程有限公司 A kind of wear-resistant anti-seize lubricant of drilling fluid
CN107033993A (en) * 2017-04-25 2017-08-11 南宁市钱隆汽车租赁有限公司 Automobile soft shaft lubricating grease
CN112195057A (en) * 2020-07-28 2021-01-08 重庆安美新材料有限公司 Robot harmonic reducer lubricating grease
WO2022021921A1 (en) * 2020-07-28 2022-02-03 安美科技股份有限公司 Lubricating grease for robot harmonic reducer
CN116024026A (en) * 2021-10-25 2023-04-28 中国石油化工股份有限公司 Grease composition, preparation method thereof and application of dibasic fatty acid
CN114806682A (en) * 2022-03-28 2022-07-29 深圳市优宝新材料科技有限公司 Lubricating grease composition and preparation method thereof, thiazole compound, intermediate and preparation method thereof
CN114806682B (en) * 2022-03-28 2023-08-25 深圳市优宝新材料科技有限公司 Grease composition and preparation method thereof, thiazole compound, intermediate and preparation method thereof

Also Published As

Publication number Publication date
CN102250671B (en) 2013-06-05

Similar Documents

Publication Publication Date Title
CN102250671B (en) Wide temperature range and high extreme pressure composite lithium lubricating grease composition
CN102757847B (en) Anhydrous albany grease and preparation method thereof
CN104371796A (en) Low-temperature lubricating grease composition and preparation method thereof
US9725672B2 (en) Method for lubricating a continuously variable transmission, and a continuously variable transmission
CN102433195B (en) Open gear lubricating grease composition
KR102127029B1 (en) Grease composition
CN103981004B (en) Extreme pressure Al Matrix Grease composition and preparation method
CN105238519A (en) Lubricant composition and application thereof
JP5638256B2 (en) Lubricating oil composition
CN109161431A (en) A kind of robot planetary reducer lubricant composition and preparation method
CN102604729A (en) Lubricant composition used for gear of wind turbine
CN103415603B (en) Grease composition
CN103013628A (en) Complex aluminum-based grease composition and preparation method thereof
CA2838171C (en) Lubricating grease composition for extreme pressure applications
CN104342252A (en) Antirust oil composition, and preparation method and application thereof
CN101974362A (en) Grease for low speed and heavy duty
CN106635325A (en) Open gear oil and preparation method thereof
CN104450117A (en) Lubricating grease composition for water pump bearing of automobile and preparation method thereof
CN105623797A (en) Weak-smell low-corrosion gear lubricant additive composition and preparation method thereof
JP6051097B2 (en) Grease manufacturing method
CN105482869B (en) A kind of anti-friction agent of nitrogenous sulphur molybdenum phosphate and preparation method thereof
CN103773580B (en) A kind of preparation method of complex lithium grease
CN104357182A (en) Hydraulic oil combination and preparing method thereof
CN103805324A (en) Heavy loading-resistant lubricating grease
CN105441164B (en) Chain lubricating oil and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant