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CN102604715A - Composite lithium based lubricating grease composition and its preparation method - Google Patents

Composite lithium based lubricating grease composition and its preparation method Download PDF

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Publication number
CN102604715A
CN102604715A CN2012100279839A CN201210027983A CN102604715A CN 102604715 A CN102604715 A CN 102604715A CN 2012100279839 A CN2012100279839 A CN 2012100279839A CN 201210027983 A CN201210027983 A CN 201210027983A CN 102604715 A CN102604715 A CN 102604715A
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China
Prior art keywords
grease
base oil
temperature
compound lithium
preparation
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Pending
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CN2012100279839A
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Chinese (zh)
Inventor
纪红兵
曾晖
李辉华
郑雄枫
梁伟灿
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Sun Yat Sen University
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Sun Yat Sen University
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Priority to CN2012100279839A priority Critical patent/CN102604715A/en
Publication of CN102604715A publication Critical patent/CN102604715A/en
Pending legal-status Critical Current

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Abstract

本发明公开了一种复合锂基润滑脂组合物及其制备方法,由如下重量百分数的组成:润滑脂基础油75%-85%,稠化剂12%-20%,添加剂0.1%-3%,所述润滑脂基础油为邻苯二甲酸二辛酯。本发明的复合锂基润滑脂组合物中采用邻苯二甲酸二辛酯作为润滑脂基础油,同时添加了抗氧化剂、极压抗磨剂、防锈剂等,产品具有良好的胶体安定性、机械安定性、高低温润滑性能等,能够适用于工程机械装置的低温润滑。The invention discloses a composite lithium-based lubricating grease composition and a preparation method thereof, which consist of the following components in weight percent: 75%-85% of lubricating grease base oil, 12%-20% of thickener, and 0.1%-3% of additives , the grease base oil is dioctyl phthalate. In the composite lithium-based grease composition of the present invention, dioctyl phthalate is used as the grease base oil, and antioxidants, extreme pressure antiwear agents, antirust agents, etc. are added at the same time, and the product has good colloidal stability, Mechanical stability, high and low temperature lubrication performance, etc., can be applied to low temperature lubrication of construction machinery devices.

Description

A kind of compound lithium base grease composite and preparation method thereof
Technical field
The present invention relates to a kind of compound lithium base grease composite and preparation method thereof.
Background technology
Railway grease is one of staple product of industrial lubricants; It is a kind ofly to have plastic solid to semi-solid lubricant by what viscosifying agent and base oil were formed; For satisfying harsh application conditions, often add various functional additives and improve its performance and be widely used in iron and steel, automobile, aerospace and war industry.Complex lithium grease is one type of high-performance grease product being processed as viscosifying agent by the compound lithium soap of 12-oxystearic acid and diprotic acid; Because of it has good mechanical stability; The bearing wastage is few; Outstanding water-resistant antirust and oxidation stability have application widely in industries such as Iron And Steel Industry, automotive industrys.
DOP (DOP) has good mixing property, and plasticizing efficiency is high, and volatility is lower; Advantages such as low-temperature pliability is better, and electric property is high, and thermotolerance and weathering resistance are good; In industry, be used widely, be mainly used in the auxiliary agent or the raw material of industries such as coating, film, cable.
The low-temperature performance of compositing lithio ester that with MO is base oil is relatively poor, and because it contains organic acids and base usually, so easily lubricating component is caused corrosion.With the viscous silicone fluid be the compositing lithio ester of base oil because its lubricity is relatively poor, thereby can not be used for the lubricated of precision instrument.
It is the high-performance composite grease sulphonate lubricating grease and preparation method thereof of raw material with the Octyl adipate that CN101824357A discloses a kind of, and this patent is to utilize Octyl adipate to be used for high-performance composite grease sulphonate lubricating grease as base oil.
In the research of above lithium soap grease and since the relatively poor decisions in aspect such as high temperature performance, oxidative stability, lubricity its can not be in the use in high-end lubricated fields such as precision meter, aviation.
DOP uses in high-end lubricated field as a kind of synthetic oil, like lubricating of fields such as precision meter, aviation.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of compsn of new complex lithium grease is provided.
Another object of the present invention provides the preparation of compositions method of above-mentioned complex lithium grease.
A kind of compound lithium base grease composite, be made up of the material of following weight percentage: grease base oil 75%-85%, viscosifying agent 12%-20%, additive 0.1%-3%, said grease base oil are DOP (DOP).
In the above-mentioned compound lithium base grease composite, said viscosifying agent is the mixture of 12-oxystearic acid lithium salts and sebacic acid lithium salts, and the mass ratio of described 12-oxystearic acid lithium salts and sebacic acid lithium salts is 1:2 ~ 2:1.
In the above-mentioned compound lithium base grease composite; Said additive is the mixture of two kinds of inhibitor, extreme pressure anti-wear additives, sanitas, rust-preventive agent etc. or three kinds; Wherein the mass percent of inhibitor is 0.01%-3%; The ratio of extreme pressure anti-wear additives is 0.01%-0.1%, and the ratio of sanitas is 0.01%-0.1%, and the mass percent of rust-preventive agent is 0.01%-1%.
In the above-mentioned compound lithium base grease composite, described inhibitor is one or more in pentanoic, di-iso-octyldiphenylamine, phenolic ester type oxidation inhibitor, the oxidation inhibitor 618.
In the above-mentioned compound lithium base grease composite, described extreme pressure anti-wear additives is one or more in clorafin, titanium oxide, dibutyl dithiocaarbamate oxygen molybdenum, the molybdenumdisulphide.
In the above-mentioned compound lithium base grease composite, described rust-preventive agent is one or more in barium mahogany sulfonate, synthetic sodium sulfonate, the zinc naphthenate.
The preparation method of above-mentioned compound lithium base grease composite is characterized in that comprising the steps:
(1) with in the middle of 12-oxystearic acid, sebacic acid, the grease base oil adding reactor drum, be adjusted to temperature A, heated and stirred dissolving back adds the hot strong solution of Lithium Hydroxide MonoHydrate and carries out saponification;
(2) intensification is dewatered, and carries out high temperature puffing afterwards;
(3) add to remain under certain temperature behind the additive and stir, the system of treating naturally cools to room temperature and obtains product.
Among the above-mentioned preparation method, step (1) saponification temperature is 90 ℃-120 ℃; The described dehydration temperaturre of step (2) is 130 ℃-150 ℃, and swelling temperature is 170 ℃-190 ℃; The said temperature of step (3) is 110 ℃-130 ℃.
Compared with prior art, the present invention has following beneficial effect: complex lithium grease of the present invention is a grease base oil with the DOP, makes full use of characteristics such as the ester oil high temperature performance is good, oxidative stability is good, lubricity excellence; Adopt compound lithium base metal soap base to carry out the single stage method multiviscosisty, method is simply practiced thrift production energy consumption; Product possesses good colloid stability and mechanical stability; Contain the performance that inhibitor possesses work under certain high temperature; And the adding through extreme pressure anti-wear additives makes compound lithium base grease composite possess excellent extreme pressure anti-wear, can extensively in engineering machinery field, use.
Embodiment
Below in conjunction with embodiment the present invention is done further explanation, but protection scope of the present invention is not limited to the scope that embodiment representes.
Embodiment 1:
In the middle of 10 kilograms of 12-oxystearic acids and 80 kilograms of DOP of 5 kilograms of sebacic acid addings; 100 ℃ of following heated and stirred; Treat that two kinds of lipid acid dissolving backs add the hot strong solution of Lithium Hydroxide MonoHydrate and carry out saponification, will be warming up to 140 ℃ then and dewater, under 200 ℃, carry out expanded after dehydration is accomplished; Treat will be dissolved with the base oil adding of 618,0.25 kilogram of titanium oxide of 0.5 kilogram of oxidation inhibitor and 0.25 kilogram of barium mahogany sulfonate and keep stirring after the expanded end, system naturally cools to room temperature and obtains product.
 
Embodiment 2:
In the middle of 10 kilograms of 12-oxystearic acids and 80 kilograms of DOP of 5 kilograms of sebacic acid addings; 100 ℃ of following heated and stirred; Treat that two kinds of lipid acid dissolving backs add the hot strong solution of Lithium Hydroxide MonoHydrate and carry out saponification; To be warming up to 140 ℃ then dewaters; Dehydration is accomplished the back and under 200 ℃, is carried out expandedly, and the base oil of treating will to be dissolved with after the expanded end 0.5 kilogram of pentanoic, 0.25 kilogram of dibutyl dithiocaarbamate oxygen molybdenum and 0.25 kilogram of barium mahogany sulfonate adds and keeps stirring, and system naturally cools to room temperature and obtains product.
 
Embodiment 3:
In the middle of 10 kilograms of 12-oxystearic acids and 80 kilograms of DOP of 5 kilograms of sebacic acid addings; 100 ℃ of following heated and stirred; Treat that two kinds of lipid acid dissolving backs add the hot strong solution of Lithium Hydroxide MonoHydrate and carry out saponification, will be warming up to 140 ℃ then and dewater, under 200 ℃, carry out expanded after dehydration is accomplished; Treat will be dissolved with the base oil adding of 0.5 kilogram of di-iso-octyldiphenylamine, 0.25 kilogram of clorafin and 0.25 kilogram of barium mahogany sulfonate and keep stirring after the expanded end, system naturally cools to room temperature and obtains product.
 
Embodiment 4:
In the middle of 10 kilograms of 12-oxystearic acids and 80 kilograms of DOP of 5 kilograms of sebacic acid addings; 100 ℃ of following heated and stirred; Treat that two kinds of lipid acid dissolving backs add the hot strong solution of Lithium Hydroxide MonoHydrate and carry out saponification, will be warming up to 140 ℃ then and dewater, under 200 ℃, carry out expanded after dehydration is accomplished; Treat will be dissolved with the base oil adding of 0.5 kilogram of phenolic ester type oxidation inhibitor, 0.25 kilogram of titanium oxide and 0.25 kilogram of synthetic sodium sulfonate and keep stirring after the expanded end, system naturally cools to room temperature and obtains product.
 
Embodiment 5:
In the middle of 10 kilograms of 12-oxystearic acids and 80 kilograms of DOP of 5 kilograms of sebacic acid addings; 100 ℃ of following heated and stirred; Treat that two kinds of lipid acid dissolving backs add the hot strong solution of Lithium Hydroxide MonoHydrate and carry out saponification, will be warming up to 140 ℃ then and dewater, under 200 ℃, carry out expanded after dehydration is accomplished; Treat will be dissolved with the base oil adding of 618,0.25 kilogram of molybdenumdisulphide of 0.5 kilogram of oxidation inhibitor and 0.25 kilogram of synthetic sodium sulfonate and keep stirring after the expanded end, system naturally cools to room temperature and obtains product.
 
Embodiment 6:
In the middle of 10 kilograms of 12-oxystearic acids and 80 kilograms of DOP of 5 kilograms of sebacic acid addings; 100 ℃ of following heated and stirred; Treat that two kinds of lipid acid dissolving backs add the hot strong solution of Lithium Hydroxide MonoHydrate and carry out saponification; To be warming up to 140 ℃ then dewaters; Dehydration is accomplished the back and under 200 ℃, is carried out expandedly, and the base oil of treating will to be dissolved with after the expanded end 0.5 kilogram of phenolic ester type oxidation inhibitor, 0.25 kilogram of dibutyl dithiocaarbamate oxygen molybdenum and 0.25 kilogram of zinc naphthenate adds and keeps stirring, and system naturally cools to room temperature and obtains product.
The product performance contrast of each embodiment is as shown in table 1
Table 1:
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Characterizing method
Cone penetration/0.1mm 256 263 260 265 258 255 GB/T 269-91
Dropping point/℃ 295 >300 296 290 >300 297 GB/T 4929-85(91)
Stencil oil-dividing/% 0.72 0.85 0.79 0.88 0.75 0.90 SH/T 0324-92
Moisture/% Trace Trace Trace Trace Trace Trace GB/T 512-65(90)

Claims (8)

1. compound lithium base grease composite is characterized in that being made up of the material of following weight percentage: grease base oil 75%-85%, and viscosifying agent 12%-20%, additive 0.1%-3%, said grease base oil are DOP.
2. compound lithium base grease composite according to claim 1 is characterized in that: said viscosifying agent is the mixture of 12-oxystearic acid lithium salts and sebacic acid lithium salts, and wherein the mass ratio of 12-oxystearic acid lithium salts and sebacic acid lithium salts is 1:2 ~ 2:1.
3. compound lithium base grease composite according to claim 1 is characterized in that: said additive is two kinds or three kinds a mixture in inhibitor, extreme pressure anti-wear additives, sanitas, the rust-preventive agent.
4. compound lithium base grease composite according to claim 3 is characterized in that: said inhibitor is one or more in pentanoic, di-iso-octyldiphenylamine, phenolic ester type oxidation inhibitor, the oxidation inhibitor 618.
5. compound lithium base grease composite according to claim 3 is characterized in that: said extreme pressure anti-wear additives is one or more in clorafin, titanium oxide, dibutyl dithiocaarbamate oxygen molybdenum, the molybdenumdisulphide.
6. compound lithium base grease composite according to claim 3 is characterized in that: said rust-preventive agent is one or more in barium mahogany sulfonate, synthetic sodium sulfonate, the zinc naphthenate.
7. the preparation method of the said compound lithium base grease composite of claim 2 is characterized in that comprising the steps:
In the middle of 12-oxystearic acid, sebacic acid, grease base oil adding reactor drum, heated and stirred dissolving back adds the hot strong solution of Lithium Hydroxide MonoHydrate and carries out saponification;
Intensification is dewatered, and carries out high temperature puffing afterwards;
Remain under certain temperature behind the adding additive and stir, the system of treating naturally cools to room temperature and obtains product.
8. preparation method according to claim 7 is characterized in that: the said saponification temperature of step (1) is 90 ℃-120 ℃; The described dehydration temperaturre of step (2) is 130 ℃-150 ℃, and swelling temperature is 170 ℃-190 ℃; The described temperature of step (3) is 110 ℃-130 ℃.
CN2012100279839A 2012-02-09 2012-02-09 Composite lithium based lubricating grease composition and its preparation method Pending CN102604715A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102839041A (en) * 2012-08-23 2012-12-26 中国石油化工股份有限公司 Composition of composite lithium grease and preparation method
CN103146466A (en) * 2013-03-17 2013-06-12 中山大学惠州研究院 Composite lithium-based lubricating grease composition and preparation method thereof
CN103160369A (en) * 2013-03-29 2013-06-19 哈尔滨工业大学 Self-repairing compound titanium-based grease and preparation method thereof
CN106190508A (en) * 2016-06-29 2016-12-07 安徽中天石化股份有限公司 A kind of Hmp grease and preparation method thereof
CN104419506B (en) * 2013-08-29 2017-02-08 中国石油化工股份有限公司 Ester oil lubricating grease and preparation method thereof
CN106479608A (en) * 2015-08-25 2017-03-08 石海旺 A kind of heat resistant type lubricant grease
CN106675734A (en) * 2016-11-18 2017-05-17 郑州人造金刚石及制品工程技术研究中心有限公司 Lithium-based lubricating grease containing nano diamond ene and preparation method thereof
CN111979029A (en) * 2020-09-09 2020-11-24 中国科学院兰州化学物理研究所 Composite lithium-based thickening agent, lubricating grease prepared from composite lithium-based thickening agent and preparation method of lubricating grease
CN114395438A (en) * 2022-01-14 2022-04-26 中海油气(泰州)石化有限公司 High-temperature-resistant long-life composite lithium-based lubricating grease and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1295119A (en) * 1999-11-04 2001-05-16 中国石油化工集团公司 Lubricant grease for electric contact
US20080280791A1 (en) * 2007-05-01 2008-11-13 Chip Hewette Lubricating Oil Composition for Marine Applications
CN101481637A (en) * 2008-01-09 2009-07-15 中国石油化工股份有限公司 Process for preparing composite lithium base grease
CN101993769A (en) * 2010-11-25 2011-03-30 无锡中石油润滑脂有限责任公司 Complex lithium base grease and preparation method thereof
CN102051257A (en) * 2010-12-31 2011-05-11 鞍山海华油脂化学有限公司 Complex lithium-base lubricating grease and production technique thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1295119A (en) * 1999-11-04 2001-05-16 中国石油化工集团公司 Lubricant grease for electric contact
US20080280791A1 (en) * 2007-05-01 2008-11-13 Chip Hewette Lubricating Oil Composition for Marine Applications
CN101481637A (en) * 2008-01-09 2009-07-15 中国石油化工股份有限公司 Process for preparing composite lithium base grease
CN101993769A (en) * 2010-11-25 2011-03-30 无锡中石油润滑脂有限责任公司 Complex lithium base grease and preparation method thereof
CN102051257A (en) * 2010-12-31 2011-05-11 鞍山海华油脂化学有限公司 Complex lithium-base lubricating grease and production technique thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102839041A (en) * 2012-08-23 2012-12-26 中国石油化工股份有限公司 Composition of composite lithium grease and preparation method
CN103146466A (en) * 2013-03-17 2013-06-12 中山大学惠州研究院 Composite lithium-based lubricating grease composition and preparation method thereof
CN103160369A (en) * 2013-03-29 2013-06-19 哈尔滨工业大学 Self-repairing compound titanium-based grease and preparation method thereof
CN103160369B (en) * 2013-03-29 2014-06-04 哈尔滨工业大学 Self-repairing compound titanium-based grease and preparation method thereof
CN104419506B (en) * 2013-08-29 2017-02-08 中国石油化工股份有限公司 Ester oil lubricating grease and preparation method thereof
CN106479608A (en) * 2015-08-25 2017-03-08 石海旺 A kind of heat resistant type lubricant grease
CN106190508A (en) * 2016-06-29 2016-12-07 安徽中天石化股份有限公司 A kind of Hmp grease and preparation method thereof
CN106675734A (en) * 2016-11-18 2017-05-17 郑州人造金刚石及制品工程技术研究中心有限公司 Lithium-based lubricating grease containing nano diamond ene and preparation method thereof
CN111979029A (en) * 2020-09-09 2020-11-24 中国科学院兰州化学物理研究所 Composite lithium-based thickening agent, lubricating grease prepared from composite lithium-based thickening agent and preparation method of lubricating grease
CN114395438A (en) * 2022-01-14 2022-04-26 中海油气(泰州)石化有限公司 High-temperature-resistant long-life composite lithium-based lubricating grease and preparation method thereof

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Application publication date: 20120725