CN101935573B - Complex calcium lubricating grease and production technology thereof - Google Patents
Complex calcium lubricating grease and production technology thereof Download PDFInfo
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- CN101935573B CN101935573B CN2010105022738A CN201010502273A CN101935573B CN 101935573 B CN101935573 B CN 101935573B CN 2010105022738 A CN2010105022738 A CN 2010105022738A CN 201010502273 A CN201010502273 A CN 201010502273A CN 101935573 B CN101935573 B CN 101935573B
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Abstract
The invention discloses complex calcium lubricating grease and a production technology thereof. The complex calcium lubricating grease comprises base oil and a complex calcium thickener, wherein the base oil accounts for 70-88% of the total weight of the lubricating grease and the complex calcium thickener accounts for12-30% of the total weight of the lubricating grease; the complex calcium thickener is generated by the reaction of acid and calcium hydroxide, and the acid is an acid mixture of high molecular acid, middle molecular acid and low molecular acid, wherein the added amount of the calcium hydroxide occupies 3.80-9.50% of the lubricating grease by weight, and the added amounts of the high molecular acid, the middle molecular acid and the low molecular acid respectively accounts for 1.80-4.50%, 2.10-5.20% and 4.30-10.80% of the total weight of the lubricating grease The production technology comprises the steps of: adding 49-61-6 wt% of base oil and 2.66-6.65 wt% of calcium hydroxide in a reaction kettle and mixing evenly; and then, adding the high molecular acid, the middle molecular acid and the low molecular acid in sequence, adding 0.76-1.90 wt% of calcium hydroxide, adding 0.38-0.95 wt% of calcium hydroxide, refining and grinding. Compared with the prior art, the invention has the biggest advantage of improvement to the hardening phenomenon.
Description
Technical field
The present invention relates to a kind of complex calcium lubricating grease and production technique thereof.
Background technology
Complex calcium lubricating grease is the high dropping point grease of developing the earliest, because it has good temperature resistance, extreme pressure property, water resisting property, mechanical stability, therefore paid close attention to widely, but the sclerosis problem is its widely used lethal factor of restriction always.Because there is case-hardened defective in quicklime grease, use and storage aspect make troubles.In recent years; For improving the performance of composite calcium-base fat; Have on prescription and ME to make improvements, like CN1888036, through to small molecules acid and the selection of long chain organic acid kind and the adjustment of ratio; And select for use some small molecules acid (boric acid) and other shops to help thing (titanium oxide) to improve the sclerosis problem of complex calcium lubricating grease, but the PT is oversize and the improvement degree of hardening is limited; Also have through introducing polyurea grease to carry out improved to its performance; Like CN1493673 and CN1493673, complex calcium lubricating grease is mixed with polyurea grease, both are had complementary advantages; But this series products needs two kinds of fat of compound calcium and polyureas to mix, and raw materials for production and technology are all comparatively complicated.Some solutions of present stage can not reach good effect in a word, and the method that has more complicated also, even need change equipment.
Summary of the invention
The object of the present invention is to provide that a kind of surface hardening value is little, period of storage is long, simple relatively complex calcium lubricating grease of technology and production technique thereof.
Comprise base oil and composite calcium-base viscosifying agent in the complex calcium lubricating grease of the present invention, wherein base oil accounts for 70～88% of railway grease gross weight, and the composite calcium-base viscosifying agent accounts for 12～30% of railway grease gross weight; The composite calcium-base viscosifying agent is generated by acid and calcium hydroxide complex reaction; Said acid is the mixing acid of polymer acid, middle molecule acid and low molecular acid; Wherein the add-on of calcium hydroxide accounts for 3.80～9.50% of railway grease gross weight, and the add-on of polymer acid, middle molecule acid and low molecular acid accounts for 1.80～4.50%, 2.10～5.20%, 4.30～10.80% of railway grease gross weight respectively; Said low molecular acid is one or more in acetate, boric acid, propionic acid, the oxalic acid; In molecule acid be in Whitfield's ointment, phenylformic acid, hexanodioic acid, sad, isocaprylic acid, the sebacic acid one or more; Polymer acid is one or more in LAURIC ACID 99 MIN, Triple Pressed Stearic Acid, ten dihydroxystearic acids, the palmitic acid.
Produce the production technique of above-mentioned complex calcium lubricating grease, comprise the steps:
(1), preparation work: in reaction kettle, add the base oil of 49～61.60 heavy % and the calcium hydroxide of 2.66～6.65 heavy %, mix;
(2), acid-base reaction: after mixing, add basic, normal, high molecule acid successively;
(3), complex reaction: after step (2) is accomplished, add the calcium hydroxide of 0.76～1.90 heavy %;
(4), dehydration reaction: after step (3) is accomplished, add the calcium hydroxide of 0.38～0.95 heavy %;
(5), refining reaction: after step (4) is accomplished, add the base oil of 7～8.80 heavy %, be warmed up to refining temperature again, the reaction certain hour;
(6), mill: after step (5) is accomplished, add the base oil of 14～17.60 heavy %, cool to assigned temperature, mill through three-roller.
Preferred implementation of the present invention is: the temperature of acid-base reaction is 20～120 ℃ in the step (2), and the complex reaction in the step (3) is carried out under 90～150 ℃, and the dehydration reaction in the step (4) is carried out under 130～180 ℃.A kind of acid of every adding all requires to react 10～60 minutes time.Refining in the step (5) is reflected under 180～240 ℃ to be carried out, and requires 5～20 minutes time of reaction.Milling in the step (6) carried out under 80～110 ℃, requires to mill 2～4 times.
The present invention compared with prior art, biggest advantage is exactly the improvement to hardening phenomenon.Complex calcium lubricating grease surface hardening value of the present invention can be controlled in 5 units; And shear hardening also improves simultaneously, is controlled in 15 units through cone penetration changing value behind 100,000 tasks; And whole hardenability deposits through experiment showed, that the cone penetration changing value is controlled in 10 units after 1 year.Through the suitable selection of basic, normal, high molecule acid and the optimization of molar ratio thereof are confirmed finally to have reached the case-hardened purpose of reduction complex calcium lubricating grease with the innovation of production technique.The innovation of production technique of the present invention can reduce the content of soap in the railway grease in the production process of complex calcium lubricating grease, thereby has also helped the improvement of its hardening phenomenon.Production technique of the present invention is fairly simple, easy to operate simultaneously, and production unit is not had particular requirement, and general opening normal pressure still can be produced.
Description of drawings
Fig. 1 is technological process of production figure of the present invention.
Embodiment
Embodiment 1:
Getting 40 ℃ of viscosity is that the MO of 46sCt and the mixing oil of poly & Alpha ,-olefin oil: 539g add in the system fat still, adds calcium hydroxide 73.20g simultaneously, stirs.Below 60 ℃, add Glacial acetic acid min. 99.5 118.80g, stirring reaction 40min; Add hexanodioic acid 24g and sebacic acid 33.20g again, need stirring reaction 20min equally; When being warmed up to 90 ℃ again, add ten dihydroxystearic acid 49.50g, stirring reaction 10min reheat heats up.Complex reaction 120min between 90～150 ℃, when compound carry out 60min after, add calcium hydroxide 20.90g, the compound continued that finishes heats up.When temperature to 160～180 ℃, add calcium hydroxide 10.40g and 77g thickened oil again.When temperature continues to rise to 220～240 ℃, behind insulation refining 5～15min, add the 154g cooling oil, wait to be cooled to below 80 ℃, mill twice, be finished product with three-roller.Each component concentration is a viscosifying agent content 30% in the railway grease, base oil content 70%.Product performance are as shown in table 1.
Embodiment 2:
Getting 40 ℃ of viscosity is that the MO of 1000sCt and the mixing oil of poly & Alpha ,-olefin oil: 539g add in the system fat still, adds calcium hydroxide 73.20g simultaneously, stirs.Below 60 ℃, add Glacial acetic acid min. 99.5 118.80g, stirring reaction 40min; Add hexanodioic acid 24g and sebacic acid 33.20g again, need stirring reaction 20min equally; When being warmed up to 90 ℃ again, add ten dihydroxystearic acid 49.50g, stirring reaction 10min reheat heats up.Complex reaction 120min between 90～150 ℃, when compound carry out 60min after, add calcium hydroxide 20.90g, the compound continued that finishes heats up.When temperature to 160～180 ℃, add calcium hydroxide 10.40g and 77g thickened oil again.When temperature continues to rise to 220～240 ℃, behind insulation refining 5～15min, add the 154g cooling oil, wait to be cooled to below 80 ℃, mill twice, be finished product with three-roller.Each component concentration is a viscosifying agent content 30% in the railway grease, base oil content 70%.Product performance are as shown in table 1.
Embodiment 3:
Getting 40 ℃ of viscosity is that the MO of 46sCt and the mixing oil of poly & Alpha ,-olefin oil: 492.80g add in the system fat still, adds calcium hydroxide 21.30g simultaneously, stirs.Below 60 ℃, add Glacial acetic acid min. 99.5 34.40g, stirring reaction 40min; Add hexanodioic acid 7g and sebacic acid 9.80g again, need stirring reaction 20min equally; When being warmed up to 90 ℃ again, add ten dihydroxystearic acid 14.40g, stirring reaction 10min reheat heats up.Complex reaction 120min between 90～150 ℃, when compound carry out 60min after, add calcium hydroxide 6.10g, the compound continued that finishes heats up.When temperature to 160～180 ℃, add calcium hydroxide 3g and 70.40g thickened oil again.When temperature continues to rise to 220～240 ℃, behind insulation refining 5～15min, add the 140.80g cooling oil, wait to be cooled to below 80 ℃, mill twice, be finished product with three-roller.Each component concentration is a viscosifying agent content 12% in the railway grease, base oil content 88%.Product performance are as shown in table 1.
Embodiment 4:
Getting 40 ℃ of viscosity is that the MO of 1000sCt and the mixing oil of poly & Alpha ,-olefin oil: 492.80g add in the system fat still, adds calcium hydroxide 21.30g simultaneously, stirs.Below 60 ℃, add Glacial acetic acid min. 99.5 71.70g, stirring reaction 40min; Add hexanodioic acid 7g and sebacic acid 9.80g again, need stirring reaction 20min equally; When being warmed up to 90 ℃ again, add ten dihydroxystearic acid 14.40g, stirring reaction 10min reheat heats up.Complex reaction 120min between 90～150 ℃, when compound carry out 60min after, add calcium hydroxide 6.10g, the compound continued that finishes heats up.When temperature to 160～180 ℃, add calcium hydroxide 3g and 70.40g thickened oil again.When temperature continues to rise to 220～240 ℃, behind insulation refining 5～15min, add the 140.80g cooling oil, wait to be cooled to below 80 ℃, mill twice, be finished product with three-roller.Each component concentration is a viscosifying agent content 12% in the railway grease, base oil content 88%.Product performance are as shown in table 1.
Embodiment 5:
Getting 40 ℃ of viscosity is that the MO of 500sCt and the mixing oil of poly & Alpha ,-olefin oil: 560g add in the system fat still, adds calcium hydroxide 44.30g simultaneously, stirs.Below 60 ℃, add Glacial acetic acid min. 99.5 34.4g, stirring reaction 40min; Add hexanodioic acid 14.60g and sebacic acid 20.40g again, need stirring reaction 20min equally; When being warmed up to 90 ℃ again, add ten dihydroxystearic acid 30g, stirring reaction 10min reheat heats up.Complex reaction 120min between 90～150 ℃, when compound carry out 60min after, add calcium hydroxide 12.70g, the compound continued that finishes heats up.When temperature to 160～180 ℃, add calcium hydroxide 6.30g and 80g thickened oil again.When temperature continues to rise to 220～240 ℃, behind insulation refining 5～15min, add the 160g cooling oil, wait to be cooled to below 80 ℃, mill twice, be finished product with three-roller.Each component concentration is a viscosifying agent content 20% in the railway grease, base oil content 80%.Product performance are as shown in table 1.
The performance of table 1 NEW TYPE OF COMPOSITE quicklime grease
Can find out from last table; Adopt the formula for raw stock of NEW TYPE OF COMPOSITE quicklime grease among the present invention; And new production technique, adopt the ratio of multiple base oil and viscosifying agent all can obtain having good mechanical stability, good extreme pressure property and the NEW TYPE OF COMPOSITE quicklime grease of minimum surface hardening value.
Claims (9)
1. a complex calcium lubricating grease is characterized in that comprising base oil and composite calcium-base viscosifying agent in this railway grease, and wherein base oil accounts for 70～88% of railway grease gross weight, and the composite calcium-base viscosifying agent accounts for 12～30% of railway grease gross weight; The composite calcium-base viscosifying agent is generated by acid and calcium hydroxide complex reaction; Said acid is the mixing acid of polymer acid, middle molecule acid and low molecular acid; Wherein the add-on of calcium hydroxide accounts for 3.80～9.50% of railway grease gross weight, and the add-on of polymer acid, middle molecule acid and low molecular acid accounts for 1.80～4.50%, 2.10～5.20%, 4.30～10.80% of railway grease gross weight respectively; Said low molecular acid is one or more in acetate, boric acid, propionic acid, the oxalic acid; In molecule acid be in Whitfield's ointment, phenylformic acid, hexanodioic acid, sad, isocaprylic acid, the sebacic acid one or more; Polymer acid is one or more in LAURIC ACID 99 MIN, Triple Pressed Stearic Acid, ten dihydroxystearic acids, the palmitic acid.
2. complex calcium lubricating grease according to claim 1 is characterized in that said base oil is that 40 ℃ of kinematic viscosity are 46～1000mm
2The mixture of one or more in the MO of/s, vegetables oil, the synthetic oil.
3. complex calcium lubricating grease according to claim 2 is characterized in that said synthetic oil is disclosed other synthetic oils on ester class oil, polyethers, alkylnaphthalene, poly-a-olefin oil or the market.
4. the complex calcium lubricating grease production technique like one of claim 1 to 3 comprises the steps:
(1), preparation work: in reaction kettle, add the base oil of 49～61.60 heavy % and the calcium hydroxide of 2.66～6.65 heavy %, mix;
(2), acid-base reaction: after mixing, add the low molecular acid of 4.30～10.80 heavy %, the middle molecule acid of 2.10～5.20 heavy %, the polymer acid of 1.80～4.50 heavy % successively;
(3), complex reaction: after step (2) is accomplished, add the calcium hydroxide of 0.76～1.90 heavy %;
(4), dehydration reaction: after step (3) is accomplished, add the calcium hydroxide of 0.38～0.95 heavy %;
(5), refining reaction: after step (4) is accomplished, add the base oil of 7～8.80 heavy %, be warmed up to refining temperature again, the reaction certain hour;
(6), mill: after step (5) is accomplished, add the base oil of 14～17.60 heavy %, cool to assigned temperature, mill through three-roller.
5. complex calcium lubricating grease production technique according to claim 4 is characterized in that the temperature of acid-base reaction in the step (2) is 20～120 ℃; Complex reaction in the step (3) is carried out under 90～150 ℃; Dehydration reaction in the step (4) is carried out under 130～180 ℃.
6. complex calcium lubricating grease production technique according to claim 4 is characterized in that: the refining temperature in step (5) is 180～240 ℃, and the reaction times is 5～20 minutes.
7. complex calcium lubricating grease production technique according to claim 4 is characterized in that a kind of acid of every adding all requires to react 10～60 minutes time.
8. complex calcium lubricating grease production technique according to claim 4 is characterized in that the assigned temperature in step (6) is 80～110 ℃, and requiring grinding times is 2～4 times.
9. complex calcium lubricating grease production technique according to claim 5 is characterized in that a kind of acid of every adding all requires to react 10～60 minutes time.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105022738A CN101935573B (en) | 2010-10-11 | 2010-10-11 | Complex calcium lubricating grease and production technology thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105022738A CN101935573B (en) | 2010-10-11 | 2010-10-11 | Complex calcium lubricating grease and production technology thereof |
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| Publication Number | Publication Date |
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| CN101935573A CN101935573A (en) | 2011-01-05 |
| CN101935573B true CN101935573B (en) | 2012-11-14 |
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| CN2010105022738A Expired - Fee Related CN101935573B (en) | 2010-10-11 | 2010-10-11 | Complex calcium lubricating grease and production technology thereof |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031181B (en) * | 2011-09-29 | 2016-01-13 | 中国石油化工股份有限公司 | A kind of complex calcium lubricating grease and preparation method thereof |
| EP2785821B1 (en) * | 2011-11-28 | 2021-03-03 | Shell International Research Maatschappij B.V. | Grease composition |
| JP6072532B2 (en) * | 2012-12-21 | 2017-02-01 | 昭和シェル石油株式会社 | Grease composition |
| CN104263457B (en) * | 2014-09-19 | 2016-06-29 | 黄山学院 | 12-tricaprylate stearic acid magnesium salt detersive and preparation method thereof |
| CN106753697B (en) * | 2016-11-25 | 2020-09-01 | 中石化江钻石油机械有限公司 | Ultrahigh-temperature-resistant composite multi-soap-based self-repairing bearing lubricating grease and preparation method thereof |
| CN108611159B (en) * | 2016-12-12 | 2021-06-01 | 中国石油天然气股份有限公司 | Boron-containing composite calcium sulfonate-based lubricating grease composition and preparation method thereof |
| JP6895863B2 (en) | 2017-10-02 | 2021-06-30 | シェルルブリカンツジャパン株式会社 | Grease composition |
| CN109694766B (en) * | 2017-10-23 | 2022-06-28 | 中国石油化工股份有限公司 | Lubricating grease composition and preparation method thereof |
| CN108165356B (en) * | 2017-11-01 | 2021-05-25 | 新疆现代特油科技股份有限公司 | Cotton picker spindle lubricating grease and preparation method thereof |
| CN108546584B (en) * | 2017-12-22 | 2021-03-16 | 新乡市恒星科技有限责任公司 | Sodium-calcium-based lubricating grease with water resistance and preparation method thereof |
| CN109797032A (en) * | 2019-02-25 | 2019-05-24 | 深圳市山立欣业科技有限公司 | A kind of novel anhydrous calcium-base grease and preparation method |
| CN113122354B (en) * | 2021-04-20 | 2023-08-15 | 中国石油化工股份有限公司 | Composite calcium-based lubricating grease and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1122592A (en) * | 1993-03-23 | 1996-05-15 | 埃克森化学专利公司 | Basic calcium carboxylates |
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- 2010-10-11 CN CN2010105022738A patent/CN101935573B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1122592A (en) * | 1993-03-23 | 1996-05-15 | 埃克森化学专利公司 | Basic calcium carboxylates |
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