CN102417854B - 8-uril grease lubricant and its preparation method - Google Patents
8-uril grease lubricant and its preparation method Download PDFInfo
- Publication number
- CN102417854B CN102417854B CN 201010292926 CN201010292926A CN102417854B CN 102417854 B CN102417854 B CN 102417854B CN 201010292926 CN201010292926 CN 201010292926 CN 201010292926 A CN201010292926 A CN 201010292926A CN 102417854 B CN102417854 B CN 102417854B
- Authority
- CN
- China
- Prior art keywords
- preparation
- diamines
- vulcabond
- reaction
- monoamine
- 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.)
- Active
Links
Images
Landscapes
- Lubricants (AREA)
Abstract
An 8-uril grease lubricant contains, by weight, 70-90% of lubricating base oil and 10-30% of an 8-uril densifier calculated according to the total weight of the grease lubricant being 100%. The preparation method of the 8-uril grease lubricant provided by the invention comprises a step of respectively performing reactions between diisocyanate and diamines and between diisocyanate and monoamines to obtain the 8-uril grease lubricant. In comparison with a 2-uril grease lubricant, the 8-uril grease lubricant has higher dropping point, better extreme pressure performance, colloid stability and shearing stability.
Description
Technical field
The present invention relates to a kind of eight urea greases and preparation method thereof
Background technology
Lubricating grease is comprised of lubricating grease, viscosifying agent and additive, and viscosifying agent is indispensable composition in lubricating grease, and its character is one of principal element directly affected PERFORMANCE OF GREASES.Polyurea thickening agent and polyurea grease are that the fast-developing and then more harsh requirement that lubricant is proposed for meeting modern industrial technology and equipment grows up.
Develop rapidly along with modern industry, requirement to lubricant is day by day harsh, the mechanical means of continuous operation under high loading, high speed and high temperature, the lubricating grease high-temperature use range is reached to 175～235 ℃ or higher, and require to have long lubricated work-ing life, change the fat cycle with prolongation, enhance productivity, reduce production costs.Polyurea grease is exactly a class high-quality high temperature grease of developing in order to adapt to above-mentioned needs.
Polyurea grease (be called for short polyurea grease or areidofat) is that to contain the organic compound multiviscosisty base oil of urea groups in molecule prepared.Because polyurea thickening agent is different from metal soap base viscosifying agent, metal ion not, avoided the catalysed oxidn of metal ion to grease base oil in the soap base viscosifying agent, therefore polyurea grease has good oxidation stability and thermostability, and there are a series of good use propertieies, as good pumping, antioxygen, mechanical stability, colloid stability and anti-water drenching, be specially adapted to high temperature, high loading, wide velocity range and the lubricated occasion contacted with impedance dielectric, widespread use now and electrical industry, metallurgical industry, foodstuffs industry, paper industry, automotive industry, airplane industry etc.
At present, the report of prior art mainly concentrates on preparation and the synthetic aspect of two urea greases, and for the report of eight urea greases seldom., with excessive isocyanic ester, with organic amine, react in base oil as CN1087025C, then in water and unreacted isocyanic ester, continue to be warming up to 130～200 ℃, obtained two urea greases of high dropping point.CN1230500C, by organic amine and isocyanate reaction, after temperature of charge is elevated to 100～150 ℃, adds utmost point cold oil to make material cooling rapidly, grinds two urea greases that obtained low noise.
Summary of the invention
The invention provides a kind of eight urea greases and preparation method thereof.
A kind of eight urea greases, comprise lubricant base and six urea viscosifying agents.
Eight urea greases provided by the invention, take the lubricating grease gross weight as 100%, comprises following component: the lube base weight of oil is 70%～90%, preferably 80%～90%; Eight urea viscosifying agent weight are 10%～30%, preferably 10%～20%.
Can also contain various additives in lubricating grease of the present invention.
Said lubricant base can be mineral oil, vegetables oil, synthetic oil or wherein two or more mixture, preferably mineral oil.Synthetic oil wherein can be ester class oil, polyolefin oil, ethers oil, Fischer-Tropsch synthesis oil etc.
Said eight urea viscosifying agents have following structure:
R wherein
1can be alkyl, cycloalkyl or aryl, the carbon number of alkyl or cycloalkyl can be 8～24, preferably 10～18, and aryl can be the phenyl of phenyl or replacement, the phenyl that preferably phenyl or C1～C3 alkyl or halogen replace.
R wherein
2can be alkylidene group or arylidene, the carbon number of alkylidene group can be 2～12, preferably 2～8, and arylidene can be phenylene or biphenylene.
R wherein
3can be that carbon number is 6～30, preferably 6～20 arylidene, alkylidene group or cycloalkylidene, preferably at least one in tolyl, methyldiphenyl base, dicyclohexyl methyl, an xylylene and hexylidene.
The preparation method of eight urea greases provided by the invention comprises:
(1) slowly add diamines in the vulcabond be dissolved in the part base oil, be warming up to 60 ℃～100 ℃ and reacted;
(2) again slowly add diamines in the product of step (1), reacted at 60 ℃～100 ℃;
(3) add monoamine in the product of step (2), reacted at 60 ℃～100 ℃;
(4) continue to be warming up to 180 ℃～220 ℃, then add the surplus base oil, cooling, grind.
Said vulcabond structure is OCN-R
3-NCO, R
3can be that carbon number is 6～30, preferably 6～20 arylidene, alkylidene group or cycloalkylidene, preferred tolyl, methyldiphenyl base, dicyclohexyl methyl, an xylylene, hexylidene etc.For example described vulcabond can be tolylene diisocyanate (TDI), methyldiphenyl group diisocyanate (MDI), 1,6-hexylidene diisocyanate (HDI), dicyclohexyl methyl vulcabond (HMDI), or at least one in an xylylene vulcabond (XDI) etc.
Said monoamine can be aliphatic amide, aliphatic cyclic amine or arylamine, and structural formula is R
1-NH
2, R wherein
1can be alkyl, cycloalkyl or aryl, the carbon number of alkyl or cycloalkyl can be 8～24, preferably 10～18, and aryl can be the phenyl of phenyl or replacement, the phenyl that preferably phenyl or C1～C3 alkyl or halogen replace.Preferred monoamine can be the arylamine that is selected from aniline, m-chloro aniline, p-Chlorobenzoic acid amide, para-totuidine, and/or is selected from the aliphatic amide of amino dodecane, tetradecy lamine, cetylamine, stearylamine.
Said diamines can be aliphatic amide or arylamine, and structural formula is NH
2-R
2-NH
2, R wherein
2can be alkylidene group or arylidene, the carbon number of alkylidene group can be 2～12, preferably 2～8, and arylidene can be phenylene or biphenylene.Preferred diamines can be to be selected from Ursol D, O-Phenylene Diamine, 4,4, the aromatic amine of-benzidine and/or be selected from quadrol, propylene diamine, 1, the straight-chain fatty amine of 6-hexanediamine.
Said lubricant base can be mineral oil, vegetables oil, synthetic oil or its mixture, preferably mineral oil.Synthetic oil wherein can be ester class oil, polyolefin oil, ethers oil, Fischer-Tropsch synthesis oil etc.
According to the inventive method, the temperature of reaction of step (1) is 60 ℃～100 ℃, and preferably 70～85 ℃, the reaction times is 3-30 minute.The temperature of reaction of step (2) is 60 ℃～100 ℃, and preferably 70～85 ℃, the reaction times is 3-30 minute.The temperature of reaction of step (3) is 60 ℃～100 ℃, and preferably 70～85 ℃, the reaction times is 3-30 minute.Step (4) continues to be warming up to 180 ℃～220 ℃, and preferably 200 ℃～210 ℃, then add the surplus base oil, and be cooled to 60 ℃～100 ℃, grind and get final product.
In step (1), the mol ratio of vulcabond and diamines is 2: 1.
The mol ratio of the diamines added in the diamines added in step (2) and step (1) is 1: 2.
The mol ratio of the diamines in the monoamine added in step (3) and step (1) is 1: 1.
In step (1) and (2), the speed that adds of diamines is that per second is 0.05ml～0.2ml, preferably 0.05ml～0.1ml.
In the prepared lubricating grease of the inventive method, the lube base weight of oil is 70%～90%, preferably 80%～90%; The weight of the eight urea viscosifying agents that monoamine and diamines and di-isocyanate reaction generate is 10%～30%, preferably 10%～20%.
According to the inventive method, being solid-state monoamine and diamines for normal temperature can first be dissolved in base oil, to react fully.
Front three-step reaction of the present invention carries out very soon, usually can within 3min minute, complete, and is controlled at the 30min left and right and can makes reaction thoroughly complete.
Eight urea greases that the present invention synthesizes, outside the performance of possessing two urea greases, also there is higher dropping point, better extreme pressure property, colloid stability and shear stability energy, can be for fields such as electrical equipment industry, metallurgical industry, foodstuffs industry, paper industry, automotive industry, airplane industries mechanically.
The accompanying drawing explanation
The infrared analysis spectrogram of eight urea viscosifying agents in the lubricating grease that Fig. 1 is embodiment 1 preparation.As can be seen from the figure, 3310～3323cm
-1the peak at place is in eight urea molecules-the stretching vibration absorption peak of NH-, and 1630cm
-1the peak at place is in eight urea molecules-vibration absorption peak of CO-.
The nuclear magnetic resonance spectroscopy spectrogram of eight urea viscosifying agents in the lubricating grease that Fig. 2 is embodiment 1 preparation.As can be seen from the figure, the peak of δ=155HZ left and right is in eight urea molecules-chemical shift of CO-.
The Electrospray Ionization Mass Spectrometry spectrogram of eight urea viscosifying agents in the lubricating grease that Fig. 3 is embodiment 1 preparation.As can be seen from the figure, the mass-to-charge ratio of sample is 1721.4m/z.The relative molecular mass of this and eight urea viscosifying agents matches.
Get the sherwood oil (cut 90～120) of 150ml left and right, be placed in the beaker of 200ml, then get 10g left and right product and add in beaker, magnetic agitation 2h, then be placed in vibrator 1～2 day, then takes out.Filter with funnel, use petroleum ether during filtration, until sample is pure white, then takes out sample and be placed in baking oven, 100 ℃, place the 1h left and right, take out and obtain the Powdered material of solid white, be viscosifying agent, characterized, Fig. 1,2,3 is characterization result.
Embodiment
First by the 500SN (40 ℃ of kinematic viscosity are 92-98cSt) and 37.8 gram MDI Hybrid Heating to 50 ℃ of 145 gram left and right, slowly add 9.08 gram quadrols, be warming up to 80 ℃, reaction 30min, slowly add 4.54 gram quadrols, 80 ℃ of constant temperature, reaction 30min, base oil and the 20.37 gram stearylamine Hybrid Heating to 60 ℃ of 145 gram left and right join in said mixture, 80 ℃ of constant temperature, reaction 30min, continue to be warming up to 210 ℃, then add the base oil of 145 about grams to be cooled to about 100 ℃ grindings to get final product.
Embodiment 2
First by the 150BS (100 ℃ of kinematic viscosity are 29cSt) and 23.77 gram TDI Hybrid Heating to 40 ℃ of 146.67 gram left and right, slowly add 5.57 gram propylene diamine, be warming up to 70 ℃, reaction 30min, slowly add 2.79 gram propylene diamine, 70 ℃ of constant temperature, reaction 30min, 146.67 base oil and the 27.88 gram amino dodecane Hybrid Heating to 50 ℃ of gram left and right join in said mixture, 70 ℃ of constant temperature, reaction 30min, continue to be warming up to 200 ℃, then add the base oil of 146.67 about grams to be cooled to about 80 ℃ grindings to get final product.
Embodiment 3
First by the PAO10 synthetic oil (100 ℃ of kinematic viscosity are 9.8-10.2cSt) and 31.27 gram HDI Hybrid Heating to 45 ℃ of 148.33 gram left and right, slowly add 10.05 gram Ursol D, be warming up to 75 ℃, reaction 30min, slowly add 5.03 gram Ursol D, 75 ℃ of constant temperature, reaction 30min, 148.33 base oil and the 8.66 gram aniline Hybrid Heating to 55 ℃ of gram left and right join in said mixture, 75 ℃ of constant temperature, reaction 30min, continue to be warming up to 205 ℃, then add the base oil of 148.33 about grams to be cooled to about 90 ℃ grindings to get final product.
Embodiment 4
First by the rapeseed oil (100 ℃ of kinematic viscosity are 52.5cSt) and 48.35 gram XDI Hybrid Heating to 45 ℃ of 141.67 gram left and right, slowly add 10.7 gram O-Phenylene Diamines, be warming up to 75 ℃, reaction 30min, slowly add 5.35 gram O-Phenylene Diamines, 75 ℃ of constant temperature, reaction 30min, 141.67 base oil and the 10.60 gram para-totuidine Hybrid Heating to 55 ℃ of gram left and right join in said mixture, 75 ℃ of constant temperature, reaction 30min, continue to be warming up to 205 ℃, then add the base oil of 141.67 about grams to be cooled to about 90 ℃ grindings to get final product.
Comparative Examples 1
500SN (40 ℃ of kinematic viscosity are 92-98cSt) and 20.61 gram MDI Hybrid Heating to 50 ℃ by 145 gram left and right, base oil and the 44.39 gram stearylamine Hybrid Heating to 60 ℃ of 145 gram left and right, join in said mixture, be warming up to 80 ℃, reaction 30min, continue to be warming up to 210 ℃, then add the base oil of 145 about grams to be cooled to about 100 ℃ grindings to get final product.
Table 1 analytical results
Claims (14)
1. the preparation method of a urea grease comprises:
(1) slowly add diamines in the vulcabond be dissolved in the part base oil, be warming up to 60 ℃～100 ℃ and reacted;
(2) again slowly add diamines in the product of step (1), reacted at 60 ℃～100 ℃;
(3) add monoamine in the product of step (2), reacted at 60 ℃～100 ℃;
(4) continue to be warming up to 180 ℃～220 ℃, then add the surplus base oil, cooling, grind.
2. according to preparation method claimed in claim 1, wherein, said monoamine structural formula is R
1-NH
2, R wherein
1be alkyl, cycloalkyl or aryl, the carbon number of alkyl or cycloalkyl is 8～24, and aryl is the phenyl of phenyl or replacement.
3. according to preparation method claimed in claim 2, R wherein
1the phenyl that phenyl or C1～C3 alkyl or halogen replace, or the carbon number alkyl or cycloalkyl that is 10～18.
4. according to preparation method claimed in claim 1, wherein, said monoamine is the arylamine that is selected from aniline, m-chloro aniline, p-Chlorobenzoic acid amide and/or para-totuidine, and/or is selected from the aliphatic amide of amino dodecane, tetradecy lamine, cetylamine and/or stearylamine.
5. according to preparation method claimed in claim 1, wherein, said diamines structural formula is NH
2-R
2-NH
2, R wherein
2be alkylidene group or arylidene, the carbon number of alkylidene group is 2～12, and arylidene is phenylene or biphenylene.
6. according to preparation method claimed in claim 1, wherein, said diamines is selected from Ursol D, O-Phenylene Diamine, 4,4, the aromatic amine of-benzidine, and/or be selected from quadrol, propylene diamine, 1, the straight-chain fatty amine of 6-hexanediamine.
7. according to preparation method claimed in claim 1, wherein, said vulcabond structure is OCN-R
3-NCO, R
3arylidene, alkylidene group or the cycloalkylidene that carbon number is 6～30.
8. according to preparation method claimed in claim 7, wherein, R
3arylidene, alkylidene group or the cycloalkylidene that carbon number is 6～20.
9. according to preparation method claimed in claim 7, wherein, described vulcabond is selected from tolylene diisocyanate, the methyldiphenyl group diisocyanate, the hexamethylene vulcabond, dicyclohexyl methyl vulcabond, or at least one in an xylylene vulcabond.
10. according to preparation method claimed in claim 1, wherein, the temperature of reaction of step (1) is 70～85 ℃, and the reaction times is 3-30 minute; The temperature of reaction of step (2) is 70～85 ℃, and the reaction times is 3-30 minute; The temperature of reaction of step (3) is 70～85 ℃, and the reaction times is 3-30 minute; Step (4) continues to be warming up to 200 ℃～210 ℃, then adds the surplus base oil, is cooled to 60 ℃～100 ℃, grinds and gets final product.
11., according to preparation method claimed in claim 1, wherein, in step (1), the mol ratio of vulcabond and diamines is 2:1; The mol ratio of the diamines added in the diamines added in step (2) and step (1) is 1:2; The mol ratio of the diamines in the monoamine added in step (3) and step (1) is 1:1.
12., according to preparation method claimed in claim 1, in step (1) and (2), the speed that adds of diamines is that per second is 0.05ml～0.2ml.
13., according to preparation method claimed in claim 1, in resulting lubricating grease, the lube base weight of oil is 70%～90%, the weight of the eight urea viscosifying agents that monoamine and diamines and di-isocyanate reaction generate is 10%～30%.
14. eight urea greases that the described method of one of claim 1-13 obtains.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010292926 CN102417854B (en) | 2010-09-27 | 2010-09-27 | 8-uril grease lubricant and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010292926 CN102417854B (en) | 2010-09-27 | 2010-09-27 | 8-uril grease lubricant and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102417854A CN102417854A (en) | 2012-04-18 |
| CN102417854B true CN102417854B (en) | 2013-12-25 |
Family
ID=45942498
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010292926 Active CN102417854B (en) | 2010-09-27 | 2010-09-27 | 8-uril grease lubricant and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102417854B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6026971B2 (en) * | 2013-08-06 | 2016-11-16 | 出光興産株式会社 | Grease manufacturing method |
| CN109777563A (en) * | 2019-03-26 | 2019-05-21 | 常熟理工学院 | A kind of octa-polyurea lubricating grease and preparation method thereof |
| CN116891771A (en) * | 2023-06-05 | 2023-10-17 | 武汉理工大学 | Polyurea grease and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3243372A (en) * | 1961-01-24 | 1966-03-29 | Chevron Res | Greases thickened with polyurea |
| CN1493670A (en) * | 2002-10-30 | 2004-05-05 | 中国石油化工股份有限公司 | Ureido lubricating grease and its preparation method |
| CN101153238A (en) * | 2006-09-29 | 2008-04-02 | 中国石油化工股份有限公司 | Preparation of high dropping point carbamido grease lubricant and obtained product |
-
2010
- 2010-09-27 CN CN 201010292926 patent/CN102417854B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3243372A (en) * | 1961-01-24 | 1966-03-29 | Chevron Res | Greases thickened with polyurea |
| CN1493670A (en) * | 2002-10-30 | 2004-05-05 | 中国石油化工股份有限公司 | Ureido lubricating grease and its preparation method |
| CN101153238A (en) * | 2006-09-29 | 2008-04-02 | 中国石油化工股份有限公司 | Preparation of high dropping point carbamido grease lubricant and obtained product |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102417854A (en) | 2012-04-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102417855B (en) | Calcium sulfonate tetra-polyurea lubricating grease and preparation method thereof | |
| CN102453599B (en) | Composite calcium-sulfonate-based tetrapolyurea lubricating grease and preparation method thereof | |
| CN103328488B (en) | Imide compound and manufacture method, lubricating grease thickening material and grease composition | |
| CN102453600B (en) | Composite calcium sulfonate-based hexaurea grease | |
| CN103740434A (en) | Thickener, grease, method for producing thickener, method for producing grease, and greased bearing | |
| CN103060067B (en) | Lubricating grease and preparation method thereof | |
| CN102382707B (en) | Tetra-urea lubricating grease and preparation method thereof | |
| CN101153238A (en) | Preparation of high dropping point carbamido grease lubricant and obtained product | |
| CN102417854B (en) | 8-uril grease lubricant and its preparation method | |
| CN104560265B (en) | A kind of polyurea grease and preparation method thereof | |
| CN102417853B (en) | Calcium sulfonate octaurea lubricating grease and preparation method thereof | |
| CN102417856B (en) | Calcium-sulfonate-based hexapolyurea lubricating grease and preparation method thereof | |
| CN103275785A (en) | Polyurea grease composition and preparation method thereof | |
| CN102417843B (en) | Hexaurea lubricating grease and preparation method thereof | |
| CN106147941B (en) | A kind of composite polyurea lubricating grease and preparation method thereof | |
| CN103031184B (en) | Composite zirconium-based tetraurea lubrication grease and its preparation method | |
| CN102952607B (en) | Composite zirconium-based urea hexamer grease and preparation method thereof | |
| CN109825358A (en) | A kind of four polyurea grease of compound lithium base and preparation method thereof | |
| CN106147926B (en) | A kind of composite polyurea lubricating grease and preparation method thereof | |
| CN106147940B (en) | A kind of environment-friendly type composite polyurea lubricating grease and preparation method thereof | |
| CN102952605A (en) | Composite zirconium-based urea tetramer grease and preparation method thereof | |
| CN109777563A (en) | A kind of octa-polyurea lubricating grease and preparation method thereof | |
| CN103031183A (en) | Composite zirconium-based hexaurea lubrication grease and its preparation method | |
| CN103571571A (en) | Calcium naphthenate-based hexapolyurea lubricating grease and preparation method thereof | |
| CN107986992B (en) | Compound with thickening effect, lubricating grease 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 |