CN101993769B - Complex lithium base grease and preparation method thereof - Google Patents
Complex lithium base grease and preparation method thereof Download PDFInfo
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Abstract
The invention relates to complex lithium base grease and a preparation method thereof. The preparation method comprises the following processes of: adding 1/4 of base oil and dibasic organic acid into a reaction kettle, heating and melting, and adding monobasic organic acid for reaction; adding 1/4 of base oil, cooling the base oil, and adding lithium hydroxide oil solution for saponification and warming; adding 1/4 of base oil, moving materials in the reaction kettle to an intermediate kettle, adding the rest 1/4 of base oil into the intermediate kettle, and circulating and cooling; adding an antioxidant, a corrosion inhibitor and an extreme pressure antiwear additive; and uniformly stirring, homogenizing and degassing to obtain the complex lithium base grease. The complex lithium base grease has a simple process, the time for producing the complex lithium base grease with a normal-pressure kettle is short, energy resources are saved, production cost is reduced, the utilization rate of equipment is improved, and the saponification reaction is quick and full.
Description
Technical field
The present invention relates to a kind of railway grease, especially a kind of complex lithium grease and preparation method thereof.
Background technology
Compositing lithio ester has good mechanical stability, colloid stability; Be in the high-performance railway grease consumption maximum with application surface type representative the most widely,, multiple-effect general with it, high temperature resistant and long-life characteristic are acknowledged as one of the most rising railway grease kind.Along with developing rapidly of industry such as China's automobile, iron and steel, weaving, papermaking, require maximum operation (service) temperature to reach more than 200 ℃ to railway grease, and can under a large amount of water surroundings, keep good structural stability and lubricity.Common complex lithium grease is difficult to satisfy harsh so lubricated requirement.
Composition and preparing method's patent at home and abroad about complex lithium grease have a lot, for example: U.S. Pat P3681242, USP4897210; Chinese patent CN1055384A, CN1052890A, CN1052891A; These complex lithium greases employing lithium hydroxide aqueous solution and two kinds and above organic acid or inorganic acid reaction generation complex lithium viscosifying agent without exception, the refining of multiviscosisty MO or synthetic oil forms again.This preparation method intensification dewatering time is longer, need consume a large amount of energy, and needs good mixing effect could guarantee the abundant, even of reaction, and therefore the production efficiency of complex lithium grease is still lower at present.
Summary of the invention
The objective of the invention is to overcome the deficiency that exists in the prior art, a kind of have favorable mechanical stability, colloid stability are provided, water resisting property and high extreme pressure property ladder nurse are agree the complex lithium grease of OK value.
Another object of the present invention provides the easy preparing complex lithium grease of a kind of technology, can save the energy, reduces production costs, and saponification reaction is more abundant.
According to technical scheme provided by the invention, a kind of complex lithium grease comprises following component, and its formula rate is counted by weight:
Said railway grease comprises following component: 0.05～5 part of 8～18 parts of monobasic organic acids, 3～7 parts of binary organic acids, 4.5～6.5 parts of Lithium Hydroxide MonoHydrate oil solutions, 73～85 parts of base oils, 0.05～0.5 part in oxidation inhibitor, 0.01～0.5 part of corrosion inhibitor and extreme pressure anti-wear additives; The mass percentage concentration of Lithium Hydroxide MonoHydrate is 30～40% in the said Lithium Hydroxide MonoHydrate oil solution.
1/4 and the binary organic acid that in reaction kettle, add the total amount base oil earlier, heating, fusing adds the monobasic organic acid again and reacts; Add 1/4 of total amount base oil then, cooling back adds the Lithium Hydroxide MonoHydrate oil solution and carries out saponification, intensification, adds 1/4 of total amount base oil again, still in the middle of the material in the reaction kettle is moved to, the residual content that in middle still, adds the total amount base oil cooling that circulates; Cooling back adds oxidation inhibitor, corrosion inhibitor and extreme pressure anti-wear additives, carries out homogeneous after stirring, the degassing obtains complex lithium grease.
Said monobasic organic acid is unary fatty acid or monohydroxylic lipid acid, and said monohydroxylic lipid acid is ten dihydroxyl lipid acid, and said unary fatty acid is a Triple Pressed Stearic Acid.
Said binary organic acid is C
6～C
14Binary lipid acid, said C
6～C
14Binary lipid acid is hexanodioic acid, nonane diacid, sebacic acid or bay diacid.
Said base oil is one or more the mixing oil in MO, synthetic hydrocarbon oil, ester class oil or the silicone oil.The viscosity of said base oil in the time of 100 ℃ is 15～40mm
2/ s.
Said oxidation inhibitor is N-phenyl αNai An or 2,6 toluene di-tert-butyl phenols.
Said corrosion inhibitor is benzotriazole or 1,2, the 3-benzotriazole.
Said extreme pressure anti-wear additives is dialkyl dithiocarbamate or dialkyl dithiophosphate.
A kind of preparing complex lithium grease comprises following process step: its component ratio is counted by weight,
(1) saponification: in reaction kettle, add 1/4 and 3～7 part binary organic acid of 18～23 parts of total amount base oils, be warming up to 130～140 ℃, be 5～10min heat-up time, and binary organic acid is melted fully; Add 8～18 parts of monobasic organic acids, reaction 3～5min; Add 1/4 of 18～23 parts of total amount base oils, make the material in the reaction kettle be cooled to 80～85 ℃, add 4.5～6.5 parts of Lithium Hydroxide MonoHydrate oil solutions and carry out saponification, saponification temperature is 100～105 ℃, and saponification time is 10～15min;
(2) after saponification is accomplished, reaction kettle is rapidly heated to 200～210 ℃, heat-up rate is: 1～2 ℃/min; Constant temperature keeps 10～15min; Add 18～23 parts of total amount base oils 1/4 after, still in the middle of the material in the reaction kettle moved to has been transferred afterwards the residual content of 18～23 parts of in middle still adding total amount base oils; The cooling that in middle still, circulates, be cooling time: 60～90min;
(3) treat in the middle of the temperature of still be cooled to 80～90 ℃; Add 0.5～0.05 part of oxidation inhibitor, 0.01～0.5 portion of corrosion inhibitor and 0.5～5 part of extreme pressure anti-wear additives; Under the stirring velocity of 30～50 commentaries on classics/min, stir 60～90min; In homogenizer, carry out homogeneous, homogenizing time 30～40min, homogenization pressure 15～25MPa after stirring; In degassing still, outgas behind the homogeneous and obtain complex lithium grease, the vacuum tightness in the said degassing still is 0.08～0.1MPa, and the degassing time is 10～15min.
Said monobasic organic acid: the mol ratio of binary organic acid is 1: 0.5～1: 0.4, said Lithium Hydroxide MonoHydrate: the mol ratio of the acid group summation of monobasic organic acid and binary organic acid is 1: 0.5～1.1: 1.0.
Complex lithium grease of the present invention adopts the novel Lithium Hydroxide MonoHydrate oil solution that does not contain crystal water, and technology is easy, and the time of producing complex lithium grease with the normal pressure still is short; Save the energy; Reduce production costs, improved usage ratio of equipment, saponification reaction is more fully fast.Made complex lithium grease has favorable mechanical stability, colloid stability, and water resisting property and high extreme pressure property ladder nurse are agree the OK value.
Embodiment
Below in conjunction with specific embodiment the present invention is described further.
The concentration that Lithium Hydroxide MonoHydrate oil solution used in the present invention adopts the extraordinary chemical industry of Lu Borun (Shanghai) Co., Ltd. to produce is 30～40% Lithium Hydroxide MonoHydrate oil solution.
Embodiment one: a kind of preparing complex lithium grease comprises following process step:
(1) saponification: the base oil that in reaction kettle, adds 118g: the binary organic acid of polyalphaolefin and 22g: sebacic acid, be warming up to 130 ℃, be 10min heat-up time, makes binary organic acid: sebacic acid melts fully; Add 55g monobasic organic acid: ten dihydroxystearic acids, reaction 3min; Add the 118g base oil: polyalphaolefin, make the material in the reaction kettle be cooled to 85 ℃, add 27.5g Lithium Hydroxide MonoHydrate oil solution and carry out saponification, saponification temperature is 100 ℃, behind the reaction 10min;
(2) reaction kettle is rapidly heated to 200 ℃; Heat-up rate is: 1 ℃/min, constant temperature keeps 10min, adds the 118g base oil: behind the polyalphaolefin; Material in the reaction kettle is moved to middle still; Transfer the back and in middle still, added the 118g base oil: polyalphaolefin, the cooling that in middle still, circulates, be cooling time: 60min;
(3) treat in the middle of the temperature of still be cooled to 80 ℃; Add 1.1g oxidation inhibitor: N-phenyl αNai An, 1.1g corrosion inhibitor: benzotriazole and 12g extreme pressure anti-wear additives: dialkyl dithiocarbamate; Under the stirring velocity of 30 commentaries on classics/min, stir 90min; In homogenizer, carry out homogeneous, homogenizing time 30min, homogenization pressure 15MPa after stirring; In degassing still, outgas behind the homogeneous and obtain complex lithium grease, the vacuum tightness in the said degassing still is 0.08MPa, and the degassing time is 10min.
Embodiment two: a kind of preparing complex lithium grease comprises following process step:
(1) saponification: the base oil that in reaction kettle, adds 117g: the binary organic acid of 150BS and 30g: sebacic acid, be warming up to 135 ℃, be 5min heat-up time, makes binary organic acid: sebacic acid melts fully; Add 72g monobasic organic acid: ten dihydroxystearic acids, reaction 5min; Add 117g base oil: 150BS, make the material in the reaction kettle be cooled to 82 ℃, add 35.8g Lithium Hydroxide MonoHydrate oil solution and carry out saponification, saponification temperature is 102 ℃, behind the reaction 12min;
(2) reaction kettle is rapidly heated to 205 ℃; Heat-up rate is: 2 ℃/min, constant temperature keeps 12min, adds 117g base oil: 150BS; Material in the reaction kettle is moved to middle still; Transfer the back and in middle still, added 117g base oil: 150BS, the cooling that in middle still, circulates, be cooling time: 90min;
(3) treat in the middle of the temperature of still be cooled to 85 ℃; Add 1.8g oxidation inhibitor: N-phenyl αNai An, 1.8g corrosion inhibitor: benzotriazole and 18g extreme pressure anti-wear additives: dialkyl dithiophosphate; Under the stirring velocity of 50 commentaries on classics/min, stir 90min; In homogenizer, carry out homogeneous, homogenizing time 40min, homogenization pressure 25MPa after stirring; In degassing still, outgas behind the homogeneous and obtain complex lithium grease, the vacuum tightness in the said degassing still is 0.1MPa, and the degassing time is 15min.
Embodiment three: a kind of preparing complex lithium grease comprises following process step:
(1) saponification: the base oil that in reaction kettle, adds 110g: the binary organic acid of polyalphaolefin and 36g: sebacic acid, be warming up to 140 ℃, be 8min heat-up time, makes binary organic acid: sebacic acid melts fully; Add 84g monobasic organic acid: Triple Pressed Stearic Acid, reaction 4min; Add the 110g base oil: polyalphaolefin, make the material in the reaction kettle be cooled to 85 ℃, add 38g Lithium Hydroxide MonoHydrate oil solution and carry out saponification, saponification temperature is 105 ℃, behind the reaction 15min; The mass percentage concentration of said Lithium Hydroxide MonoHydrate oil solution is 35%;
(2) reaction kettle is rapidly heated to 210 ℃; Heat-up rate is: 2 ℃/min, constant temperature keeps 15min, adds the 110g base oil: behind the polyalphaolefin; Material in the reaction kettle is moved to middle still; Transfer the back and in middle still, added the 110g base oil: polyalphaolefin, the cooling that in middle still, circulates, be cooling time: 80min;
(3) treat in the middle of the temperature of still be cooled to 90 ℃; Add 2.4g oxidation inhibitor: 2; 6 toluene di-tert-butyl phenols, 2.4g corrosion inhibitor: benzotriazole and 24g extreme pressure anti-wear additives: dialkyl dithiocarbamate, under the stirring velocity of 40 commentaries on classics/min, stir 80min, homogeneous is carried out in the back that stirs in homogenizer; Homogenizing time 35min, homogenization pressure 20MPa; In degassing still, outgas behind the homogeneous and obtain complex lithium grease, the vacuum tightness in the said degassing still is 0.09MPa, and the degassing time is 12min.
The physicochemical property of the complex lithium grease that the present invention obtains is as shown in table 1.
Table 1
Claims (1)
1. preparing complex lithium grease, it is characterized in that: its component ratio is counted by weight, comprises following process step:
(1) saponification: in reaction kettle, add 1/4 and 3～7 part binary organic acid of 73～85 parts of total amount base oils, be warming up to 130～140 ℃, be 5～10min heat-up time, and binary organic acid is melted fully; Add 8～18 parts of monobasic organic acids, reaction 3～5min; Add 1/4 of 73～85 parts of total amount base oils
, make the material in the reaction kettle be cooled to 80～85 ℃, add 4.5～6.5 parts of Lithium Hydroxide MonoHydrate oil solutions and carry out saponification, saponification temperature is 100～105 ℃, saponification time is 10～15min;
(2) after saponification is accomplished, reaction kettle is rapidly heated to 200～210 ℃, heat-up rate is: 1～2 ℃/min; Constant temperature keeps 10～15min; Add 73～85 parts of total amount base oils 1/4 after, still in the middle of the material in the reaction kettle moved to has been transferred afterwards the residual content of 73～85 parts of in middle still adding total amount base oils; The cooling that in middle still, circulates, be cooling time: 60～90min;
(3) treat in the middle of the temperature of still be cooled to 80～90 ℃; Add 0.05～0.5 part of oxidation inhibitor, 0.01～0.5 portion of corrosion inhibitor and 0.05～5 part of extreme pressure anti-wear additives; Under the stirring velocity of 30～50 commentaries on classics/min, stir 60～90min; In homogenizer, carry out homogeneous, homogenizing time 30～40min, homogenization pressure 15～25MPa after stirring; In degassing still, outgas behind the homogeneous and obtain complex lithium grease, the vacuum tightness in the said degassing still is 0.08～0.1MPa, and the degassing time is 10～15min;
The mass percentage concentration of Lithium Hydroxide MonoHydrate is 30～40% in the said Lithium Hydroxide MonoHydrate oil solution;
Said monobasic organic acid is unary fatty acid or monohydroxylic lipid acid, and said monohydroxylic lipid acid is ten dihydroxyl lipid acid, and said unary fatty acid is a Triple Pressed Stearic Acid;
Said binary organic acid is C
6～C
14Binary lipid acid, said C
6～C
14Binary lipid acid is hexanodioic acid, nonane diacid, sebacic acid or bay diacid;
Said base oil is one or more in MO, synthetic hydrocarbon oil, ester class oil or the silicone oil, and the viscosity of said base oil in the time of 100 ℃ is 15～40mm
2/ s;
Said oxidation inhibitor is N-PA or 2, the 6-toluene di-tert-butyl phenol;
Said corrosion inhibitor is a benzotriazole;
Said extreme pressure anti-wear additives is dialkyl dithiocarbamate or dialkyl dithiophosphate.
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| CN102796603B (en) * | 2011-05-27 | 2014-07-02 | 中国石油化工股份有限公司 | Method for preparing lithium lubricating grease |
| CN102433206B (en) * | 2011-10-27 | 2014-08-20 | 无锡惠源高级润滑油有限公司 | Composite lithium-calcium lubricating grease and preparation method thereof |
| CN102604715A (en) * | 2012-02-09 | 2012-07-25 | 中山大学 | Composite lithium based lubricating grease composition and its preparation method |
| CN103450978A (en) * | 2013-09-05 | 2013-12-18 | 江苏龙蟠石化有限公司 | Lubricating grease for hub bearing of heavy load truck 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 |
| CN105482885A (en) * | 2015-07-17 | 2016-04-13 | 路伯润滑油（苏州）有限公司 | Robot-arm grease and preparation method thereof |
| CN105154195B (en) * | 2015-08-27 | 2018-07-10 | 中国科学院兰州化学物理研究所 | A kind of extreme pressure compound lithium base grease composition |
| CN105132105A (en) * | 2015-09-06 | 2015-12-09 | 新乡市恒星化工有限责任公司 | Preparation method for special lubricating grease for dragging chain |
| CN106520273A (en) * | 2016-10-08 | 2017-03-22 | 江苏大学 | Preparation method of silicone-oil-containing lithium complex lubricating grease |
| CN108300543A (en) * | 2018-01-23 | 2018-07-20 | 合肥欧仕嘉机电设备有限公司 | A kind of lubricating grease and preparation method thereof for speed reducer |
| CN111334364A (en) * | 2020-04-14 | 2020-06-26 | 无锡中石油润滑脂有限责任公司 | Engineering machinery lubricating grease and preparation method thereof |
| CN113549492A (en) * | 2021-06-18 | 2021-10-26 | 安美科技股份有限公司 | Lithium-based lubricating grease and saponification method thereof |
| 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 |
| CN115651734A (en) * | 2022-10-24 | 2023-01-31 | 东莞市欧迪斯润滑剂科技有限公司 | Wear-resistant silicon oil composite lithium-based lubricating grease and preparation process thereof |
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| US2844537A (en) * | 1956-01-19 | 1958-07-22 | Gulf Research Development Co | Homogeneous lithium base lubricating grease compositions |
| CN101705141A (en) * | 2009-11-18 | 2010-05-12 | 南通山浦润滑油科技有限公司 | Composite lithium grease and preparation method thereof |
| CN101792689B (en) * | 2010-02-03 | 2013-01-16 | 上海禾泰特种润滑技术有限公司 | High-performance complex lithium-calcium base grease composition and method for preparing same |
| CN101880581A (en) * | 2010-06-29 | 2010-11-10 | 濮阳市航天化工有限公司 | Universal lithium base grease and preparation method thereof |
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