CN103468357B - A kind of water-resisting type extreme pressure lithium base lubricating grease and preparation method thereof - Google Patents
A kind of water-resisting type extreme pressure lithium base lubricating grease and preparation method thereof Download PDFInfo
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- CN103468357B CN103468357B CN201310401449.4A CN201310401449A CN103468357B CN 103468357 B CN103468357 B CN 103468357B CN 201310401449 A CN201310401449 A CN 201310401449A CN 103468357 B CN103468357 B CN 103468357B
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Abstract
The present invention relates to a kind of lubricating grease and preparation method thereof, especially a kind of water-resisting type extreme pressure lithium base lubricating grease and preparation method thereof, belongs to chemical technology field.Percentage of the present invention, comprises following component: base oil 70-90%, lipid acid 9-15%, lithium hydroxide 1-2%, calcium hydroxide powder 0.3-0.7%, oxidation inhibitor 0.1-0.5%, rust-preventive agent 0.3-1.5%, extreme pressure agent 2-5%, tackifier 2-5%.Its beneficial effect is: ensure that product is under general operating mode, have higher dropping point and good shear stability; The water resisting property of product is excellent, guarantees to run off less when there being large water gaging to wash away, and works in the presence of water, not easily softening loss, good mechanical stability; Product has good rust-preventing characteristic and extreme pressure anti-wear, can improve good lubrication, and prevent lubricated surface corrosion for heavy loading equipment under moist operating mode.
Description
Technical field
The present invention relates to a kind of lubricating grease and preparation method thereof, especially a kind of water-resisting type extreme pressure lithium base lubricating grease and preparation method thereof, belongs to chemical technology field.
Background technology
Along with the fast development of China's economy, the use properties of lubricating grease is required increasingly strict, divide the work also more and more meticulousr.Equipment bearing as Steel Mill runs mostly under the environment of high temperature, heavy loading, Duo Shui, many dirt, common extreme pressure lithium base lubricating grease is subject to soap structure and additive limit, in use easily washed away by water or the phenomenon of thinning loss, and the extreme pressure property of fat in the presence of water also declines to a great extent, and can not meet lubricating requirement.Some constructional engineering machineries are also main to work under low speed, heavy loading and muddy environment, and lubrication node easily contacts with muddy water, requires that lubricating grease has good extreme pressure anti-wear, water resisting property and rust-preventing characteristic.
The character of lubricating grease is to a great extent by the impact of viscosifying agent, especially very large by the impact of metal species in viscosifying agent, common metal (calcium, sodium, barium, lithium, aluminium) for the preparation of lubricating grease respectively gives associated lubrication fat different features, and the feature as quicklime grease is water resisting property; The feature of lithium soap grease is the high and good mechanical stability of dropping point; The feature of aluminium soap grease is that oxidation stability is good etc.Therefore, exploitation hybrid metal soap base grease can have the feature of its single metallic soap base grease concurrently, and mutually learn from other's strong points to offset one's weaknesses, over-all properties is more superior.As lithium-calcium base grease, it not only has the good colloid stability of lithium soap grease, mechanical stability and higher dropping point, and has the excellent water resisting property of quicklime grease and resistance to abrasion.GB1376835 proposes a kind of preparation method of water-resistant oleosol, the two schemes proposed in that patent: one is add the additive improving Lubricating Greases water-based, the shortcoming of this scheme is that cost is higher, and additive also can lose efficacy in use for some time, and the life-span is short; Another kind of scheme is that the mixed grease preparing lithium base and calcium base makes it to possess excellent water resisting property, but water resisting property grease dropping point prepared by this technique is not high, and high thermal resistance is poor.Lithium-calcium base grease prepared by the step saponification method that US3891564 introduces is lower due to refining temperature, and the product prepared not only dropping point is low, and soap divides high, and water resistant scouring capability is not good.Domestic patent CN86103103 it is also proposed the technique that single stage method prepares lithium-calcium base grease, but the product dropping point prepared only has about 190 DEG C, and mechanical stability is poor.
Summary of the invention
The object of the invention is the defect existed for prior art, propose a kind of water-resisting type extreme pressure lithium base lubricating grease, there is high dropping point, good mechanical stability, colloid stability and extreme pressure property, water repelling property is excellent, can meet the lubricating requirement of mechanical means under humidity, heavy loading operating mode.
The present invention is technical solution problem by the following technical programs, and a kind of water-resisting type extreme pressure lithium base lubricating grease, comprises the component of following percentage:
Wherein, described base oil is at least one in paraffin base oil and naphthenic base oils, and the kinematic viscosity of 40 DEG C is 90-400mm
2/ s;
Described lipid acid is at least one in 12-oxystearic acid and stearic acid;
Described oxidation inhibitor is pentanoic or N-phenyl-a-naphthylamine;
Described rust-preventive agent is the one in benzotriazole, barium mahogany sulfonate or dinonyl naphthalene sulfonate barium;
Described extreme pressure agent is at least one in sulfide isobutene, aminothio fat, antimony dialkyl-dithiocarbamate or three potassium borates;
Described tackifier are at least one in polyisobutene and ethylene-propylene copolymer.
The present invention further provides the preparation method of water-resisting type extreme pressure lithium base lubricating grease, comprise said components in described ratio, carry out with following step:
Step one, the 1/3-1/2 base oil of lubricating grease total amount will be accounted for, lipid acid drops into saponification still, be heated with stirring to 75-85 DEG C, treat that described lipid acid all dissolves;
Step 2, to add with 3-5 doubly water-soluble lithium hydroxide solution, and be warming up to 105-115 DEG C, saponification reaction 45-75min;
Step 3, continue to be warming up to 160-170 DEG C, add calcium hydroxide powder, and stirring reaction 30-45min, be then warming up to 205-215 and carry out high temperature refining, insulation 3-5min;
Step 4, add remaining base oil, be chilled to 165-175 DEG C, turn still, circulating filtration, be cooled to 110-120 DEG C, after homogenizing, add additive successively, stir, after degassed finished product.
The present invention draws following advantage by testing and carrying out evaluation to product performance:
1, in preparation technology, calcium hydroxide is added in the form of a powder, not only substantially reduce saponification dewatering time, solve calcium hydroxide adds the fashionable still that easily overflows, dehydration difficulty problem in aqueous solution mode, and calcium soap and lithium soap cool in the molten state and form mixed crystal fiber, ensure that product has higher dropping point and good shear stability, meet working temperature the equipment lubrication demand of-20 to 120 DEG C.
2, the water resisting property of product is excellent, guarantees to run off less when there being large water gaging to wash away, and works in the presence of water, not easily softening loss, good mechanical stability.
3, product has good rust-preventing characteristic and extreme pressure anti-wear, can improve good lubrication, and prevent lubricated surface corrosion for heavy loading equipment under moist operating mode.
4, with add compared with complex lithium-calcium base grease prepared by diprotic acid compound, not only preparation cost is low for the products scheme that this technology proposes, and avoid because adding diprotic acid compound tense temperature and adding alkali speed control improper and occur the problem of the not high and mechanical stability difference of dropping point, for moist operating mode and maximum operating temperature provides another kind of solution lower than the equipment lubrication of 120 DEG C.
Embodiment
Set forth the present invention further below in conjunction with embodiment, if raw material involved in embodiment is without specified otherwise, is market and sells.
Embodiment one
Raw material is prepared water-resisting type extreme pressure lithium base lubricating grease by the present embodiment by the following method:
Step one: by the kinematic viscosity 92mm of the base oil 500SN(40 of 1500kg DEG C
2/ s), the 12-oxystearic acid of 375kg and the stearic acid of 93kg drop into saponification still successively, open and stir and be warming up to 80 DEG C, lipid acid is all dissolved;
Step 2: add the solution with the water-soluble 54kg lithium hydroxide of 250kg, and be warming up to 105 DEG C, saponification reaction 60min;
Step 3: continue to be warming up to 165 DEG C, adds 11.2kg calcium hydroxide powder, and stirring reaction 35min, be then warming up to 210 DEG C and carry out high temperature refining, insulation 3min;
Step 4: the base oil 500SN adding 1200kg in saponification still, material is chilled to 170 DEG C, then mediation still is proceeded to, circulating filtration, add remaining base oil 500SN500kg and temperature of charge is down to 115 DEG C, add 12kg pentanoic, 48kg barium mahogany sulfonate, 100kg tri-potassium borate and 80kg polyisobutene after homogenizing successively, stir, after degassed, obtain finished product.
After testing, end properties index is in table 1.
Embodiment two
Water-resisting type extreme pressure lithium base lubricating grease prepared by raw material by the present embodiment by the following method, and (base oil selected in the present embodiment is 500SN and L-AN100, and mixing rear 40 DEG C of kinematic viscosity is 110mm
2/ s):
Step one: the 12-oxystearic acid resin acid of the above-mentioned mixed base oil of 1600kg and 450kg is dropped into saponification still successively, opens and stirs and be warming up to 85 DEG C, lipid acid is all dissolved;
Step 2: add the solution with the water-soluble 53kg lithium hydroxide of 300kg, and be warming up to 110 DEG C, saponification reaction 45min;
Step 3: continue to be warming up to 170 DEG C, adds 14kg calcium hydroxide powder, and stirring reaction 45min, be then warming up to 215 DEG C and carry out high temperature refining, insulation 5min;
Step 4: the above-mentioned mixed base oil adding 1200kg in saponification still, material is chilled to 175 DEG C, then mediation still is proceeded to, circulating filtration, add remaining above-mentioned mixed base oil 400kg and temperature of charge is down to 120 DEG C, add 16kgN-phenyl-a-naphthylamine, 40kg dinonyl naphthalene sulfonate barium, 80kg tri-potassium borate, 40kg sulfide isobutene and 60kg ethylene-propylene copolymer after homogenizing successively, stir, after degassed, obtain finished product.
After testing, end properties index is in table 1.
Embodiment three
Water-resisting type extreme pressure lithium base lubricating grease prepared by raw material by the present embodiment by the following method, and (base oil selected in the present embodiment is 400SN and 150BS, and mixing rear 40 DEG C of kinematic viscosity is 160mm
2/ s):
Step one: the 12-oxystearic acid resin acid of the above-mentioned mixed base oil of 1500kg and 445kg is dropped into saponification still successively, opens and stirs and be warming up to 82 DEG C, lipid acid is all dissolved;
Step 2: add the solution with the water-soluble 55kg lithium hydroxide of 300kg, and be warming up to 105 DEG C, saponification reaction 60min;
Step 3: continue to be warming up to 165 DEG C, adds 12.4kg calcium hydroxide powder, and stirring reaction 30min, be then warming up to 210 DEG C and carry out high temperature refining, insulation 3min;
Step 4: the above-mentioned mixed base oil adding 1200kg in saponification still, material is chilled to 175 DEG C, then mediation still is proceeded to, circulating filtration, add remaining above-mentioned mixed base oil 600kg and temperature of charge is down to 115 DEG C, add 12kg pentanoic, 12kg benzotriazole, 40kg tri-potassium borate, 80kg aminothio fat, 30kg ethylene-propylene copolymer and 30kg polyisobutene after homogenizing successively, stir, after degassed, obtain finished product.
Comparative example
Point out different from embodiment one of the raw material of this comparative example is not add calcium hydroxide powder, and other are consistent with embodiment.
After testing, the performance index of finished product and comparative example are in table 1.
The physicochemical property check data of each embodiment lubricating grease of table 1
As shown in Table 1, not only dropping point is high for water-resisting type extreme pressure lithium base lubricating grease product prepared by the present invention, and water-tolerant, in the presence of water good mechanical stability, has excellent water resistant erosion.Soap divides identical, and the extreme pressure lithium base lubricating grease prepared under the also identical condition of preparation technology, detect find its water drench number of dropouts, add water 20% Drawing cone in-degree and add water 10% drum functions 1h after cone penetration changing value all obviously not as water-resisting type Lithium-base grease prepared by the present invention.In addition, the extreme-pressure additive contained in product is guaranteed to provide good lubrication for equipment lubrication position under heavy load conditions.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (7)
1. the preparation method of water-resisting type extreme pressure lithium base lubricating grease, comprises the following steps:
Step one, the 1/3-1/2 base oil of lubricating grease total amount will be accounted for, lipid acid drops into saponification still, be heated with stirring to 75-85 DEG C, treat that described lipid acid all dissolves;
Step 2, add 3-5 doubly water-soluble lithium hydroxide solution by mass, and be warming up to 105-115 DEG C, saponification reaction 45-75min;
Step 3, continue to be warming up to 160-170 DEG C, add calcium hydroxide powder, and stirring reaction 30-45min, be then warming up to 205-215 DEG C and carry out high temperature refining, insulation 3-5min;
Step 4: add remaining base oil, be chilled to 165-175 DEG C, turn still, circulating filtration, be cooled to 110-120 DEG C, add additive successively after homogenizing, stir, obtains finished product after degassed;
Described water-resisting type extreme pressure lithium base lubricating grease, percentage, comprises following component,
Base oil 70-90%
Lipid acid 9-15%
Lithium hydroxide 1-2%
Calcium hydroxide powder 0.3-0.7%
Oxidation inhibitor 0.1-0.5%
Rust-preventive agent 0.3-1.5%
Extreme pressure agent 2-5%
Tackifier 2-5%, each component concentration sum is 100%.
2. the preparation method of water-resisting type extreme pressure lithium base lubricating grease according to claim 1, is characterized in that: described base oil is at least one in paraffin base oil and naphthenic base oils, and the kinematic viscosity of 40 DEG C is 90-400mm
2/ s.
3. the preparation method of water-resisting type extreme pressure lithium base lubricating grease according to claim 1, is characterized in that: described lipid acid is at least one in 12-oxystearic acid and stearic acid.
4. the preparation method of water-resisting type extreme pressure lithium base lubricating grease according to claim 1, is characterized in that: described oxidation inhibitor is pentanoic or N-phenyl-a-naphthylamine.
5. the preparation method of water-resisting type extreme pressure lithium base lubricating grease according to claim 1, is characterized in that: described rust-preventive agent is the one in benzotriazole, barium mahogany sulfonate or dinonyl naphthalene sulfonate barium.
6. the preparation method of water-resisting type extreme pressure lithium base lubricating grease according to claim 1, is characterized in that: described extreme pressure agent is at least one in sulfide isobutene, aminothio fat, antimony dialkyl-dithiocarbamate or three potassium borates.
7. the preparation method of water-resisting type extreme pressure lithium base lubricating grease according to claim 1, is characterized in that: described tackifier are at least one in polyisobutene and ethylene-propylene copolymer.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105331426A (en) * | 2015-10-23 | 2016-02-17 | 中国石油化工股份有限公司 | Anti-rust extreme pressure lithium lubricating grease composition and preparation method |
| CN105670741A (en) * | 2015-12-24 | 2016-06-15 | 东莞市安美润滑科技有限公司 | Gearbox lubricant grease |
| CN105695066A (en) * | 2016-01-19 | 2016-06-22 | 张志强 | Novel lubricating grease and preparing method thereof |
| CN111205917A (en) * | 2018-11-22 | 2020-05-29 | 北京盛鑫和谐润滑油脂有限公司 | Water-resistant extreme pressure lithium-based lubricating grease and preparation method thereof |
| CN109913286B (en) * | 2019-04-28 | 2022-04-19 | 南通润博润滑油有限公司 | Preparation method of special long-life lubricating grease for joints and bearings of intelligent robot |
| CN111849590B (en) * | 2020-06-19 | 2022-07-19 | 中国石油化工股份有限公司 | Low-noise mixed soap-based lubricating grease composition and preparation method thereof |
| CN112646639A (en) * | 2020-12-23 | 2021-04-13 | 北京市政建设集团有限责任公司 | Low-odor lubricating grease and preparation method thereof |
| CN113621423B (en) * | 2021-08-05 | 2022-10-21 | 陈春华 | Water-resistant lubricating grease and preparation method thereof |
| CN115558537A (en) * | 2022-09-29 | 2023-01-03 | 东莞市唯纳孚润滑科技有限公司 | Rotating shaft lubricating grease and preparation method thereof |
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| CN102433189A (en) * | 2011-10-24 | 2012-05-02 | 中国石油化工股份有限公司 | Composite calcium-sulfonate-based lubricating grease composition and preparation method thereof |
| CN102977979A (en) * | 2012-12-17 | 2013-03-20 | 江苏龙蟠石化有限公司 | Composite lithium-calcium base lubricating grease and preparation method thereof |
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|---|---|---|---|---|
| EP2075314A1 (en) * | 2007-12-11 | 2009-07-01 | Shell Internationale Research Maatschappij B.V. | Grease formulations |
| CN102433189A (en) * | 2011-10-24 | 2012-05-02 | 中国石油化工股份有限公司 | Composite calcium-sulfonate-based lubricating grease composition and preparation method thereof |
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Address after: 210038 No. 6 Hengtong Road, Nanjing economic and Technological Development Zone, Jiangsu Applicant after: JIANGSU LOPAL TECH. CO., LTD. Address before: 210038 No. 6 Hengtong Road, Nanjing economic and Technological Development Zone, Jiangsu Applicant before: Jiangsu Lopal Petrochemical Co., Ltd. |
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