CN85108441B - Composition of compound lithium soap grease and its preparation - Google Patents
Composition of compound lithium soap grease and its preparation Download PDFInfo
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- CN85108441B CN85108441B CN85108441A CN85108441A CN85108441B CN 85108441 B CN85108441 B CN 85108441B CN 85108441 A CN85108441 A CN 85108441A CN 85108441 A CN85108441 A CN 85108441A CN 85108441 B CN85108441 B CN 85108441B
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- China
- Prior art keywords
- acid
- composition
- constituent
- lithium soap
- terephthalic acid
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Abstract
The present invention relates to a compound lithium soap grease composition for high-temperature bearing lubrication, and a preparation method thereof. The composition contains lubricating base oil and thickening agents, wherein the thickening agents are compound lithium soap of two kinds of acid (a) and (b), wherein the (a) is at least one kind of acid selected from hydroxy fatty acid of C12 to C 24 and fatty acid of C10 to C 34; (b) is terephthalic acid or the mixed acid of the terephthalic acid and the fatty dibasic acid of C2 to C12; the molar ratio of the two kinds of acid of the (b) to (a) is (b) /(a) =0.2 to 2.0. The preparation method comprises: firstly, all lithium alkali which saponifies the two kinds of acid is added to the mixture of the lubricating base oil and the acid (a) to saponify, and the acid (b) is added so as to further saponify and compound.
Description
The present invention is composition of compound lithium soap grease of the lubricated usefulness of relevant high-temperature bearing and preparation method thereof.
In recent years, high-temperature behavior, water repelling property and the bearing life etc. of the grease composition that fields such as automobile, iron and steel and printing and dyeing industry are used propose harsh day by day requirement, and are particularly stronger to the requirement of high-temperature behavior.The high-temperature behavior of grease composition can be estimated with the various performance tests under the high temperature, but usually also dropping point as one of index of weighing high-temperature behavior.
Generally, composition of compound lithium soap grease has higher dropping point, and at high temperature, has the long bearing lubrication life-span.Therefore, composition of compound lithium soap grease is the lubricant that a kind of high-temperature bearing that gets a good chance of is used.
The grease composition of the lubricated usefulness of high-temperature bearing, except should having high dropping point, in order to obtain the long high-temperature bearing life-span, enough denseness and as far as possible little branch oil also must at high temperature be arranged, in order to adapt to the development of concentrate giving the grease lubrication technology and to satisfy the requirement of low temperature environment use, also must have less low temperature similar viscosity.Grease composition is if there are enough high temperature denseness, and high temperature throws away from lubricated position with regard to being difficult for down.Grease composition when being pumped under the low temperature, just has good flowability if less low temperature similar viscosity is arranged, and lubricated machinery has good startability.
The Lithium soap grease constituent of known high dropping point is that the compound lithium soap with hydroxy fatty acid and binary acid prepares as viscosifying agent.Though also can obtain the composition of compound lithium soap grease of high dropping point according to known technique, also can't satisfy the requirement of above-mentioned each side comprehensively.Moreover, consider from angle economic and supply, also be necessary to seek the new raw material of the composition of compound lithium soap grease for preparing high dropping point.
The present invention adopts terephthalic acid or terephthalic acid and C
2～C
12The mixing acid of binary acid also can obtain the composition of compound lithium soap grease of high dropping point.Thereby, invented the composition of compound lithium soap grease that comprehensively satisfies above-mentioned various performance requriementss.
The United States Patent (USP) 3,791,973 of application on February 18th, 1972 once proposed a kind of preparation method of Lithium soap grease constituent of high dropping point.The feature of this known technology method is earlier binary acid to be added in the mixture of hydroxy fatty acid lithium soap and lubricating base oil, adds lithium hydroxide aqueous solution again.At this moment, exist two mutually reactions of competition simultaneously, first binary acid or its single lithium soap enter the lattice (complex reaction) of hydroxy fatty acid lithium soap, and it two is the two lithium soaps (saponification reaction) that binary acid or its single lithium soap changed into it.By the speed of the control reaction temperature and the hydro-oxidation lithium aqueous solution, complex reaction is taken place quickly than saponification reaction, thereby form compound.
But, since terephthalic acid with binary acid in structure with very big difference is arranged in nature, according to known technological method, the lithium soap of terephthalic acid and hydroxy fatty acid is difficult for compound.Therefore, be difficult to obtain the composition of compound lithium soap grease of high dropping point.
Make the lithium soap of terephthalic acid and hydroxy fatty acid compound, just must seek the new condition of the speed of relative movement (accelerate the former speed, speed or two effects of the attenuating latter have both at the same time) of change complex reaction and saponification reaction.
The new composition of compound lithium soap grease that high-temperature behavior is better in order to seek, raw material cheap and the source is abundant, we have studied (a) from C
12～C
24Hydroxy fatty acid and C
10～C
34Hydroxy fatty acid at least one acid and (b) terephthalic acid or terephthalic acid and C of selecting
2～C
12The lithium soap generation compound condition of mixing acid of binary acid.
The object of the present invention is to provide (a) from C
12～C
24Hydroxy fatty acid and C
10At least one acid and (b) terephthalic acid or terephthalic acid and C of selecting in the lipid acid of～Cv
2～C
12The composition of compound lithium soap grease of mixing acid of binary acid.Constituent of the present invention has high dropping point and excellent high-temperature performance etc.
Another purpose of the present invention is to provide the method that is exclusively used in preparation grease composition of the present invention.Preparation method of the present invention has the simple and easy to operate advantage of technology.
Grease composition of the present invention contains lubricating base oil and viscosifying agent.Viscosifying agent of the present invention is (a) and (b) compound lithium soap of two kinds of acid, is from C (a)
12The hydroxy fatty acid of～Cv and C
10～C
34Lipid acid at least one acid of selecting, (b) be terephthalic acid or terephthalic acid and C
2～C
12The mixing acid of binary acid.Wherein, (a) and (b) mol ratio of two kinds of acid (b)/(a)=0.2～2.0 preferably equals 0.5～1.2.
(a) and (b) during the mol ratio of two kinds of acid (b)/(a) less than 0.2, can not form the grease composition of high dropping point, greater than 2.0 o'clock, consistency of grease was not enough or need too much viscosifying agent consumption.
Select C
12～C
24Hydroxy fatty acid the time, preferably from C
16～C
20Hydroxy fatty acid in select, for example, 12-oxystearic acid, 13-oxystearic acid, 12-hydroxy-palmitic acid and the acid of 12-hydroxy-20 carbon can be selected the 12-oxystearic acid for use especially for selecting for use.
Select C
10～C
34Lipid acid the time, preferably from C
16～C
22Lipid acid in select, can select stearic acid for use especially.
Can from above-mentioned hydroxy fatty acid and lipid acid, select an acid or a plurality of acid to prepare constituent of the present invention.When the preparation lithium soap,, had better use the reaction of free acid and lithium alkali though also can use the glyceryl ester of above-mentioned acid.
When the acid of selecting for use terephthalic acid to make (b) prepares lithium soap, not only free acid can be used, and two lower alkyl esters, particularly dimethyl ester and the reaction of lithium alkali of terephthalic acid can be used.
Select terephthalic acid and C for use
2～C
12The mixing acid of fat diacid when doing (b) sour, preferably use terephthalic acid and C
6～C
10Binary acid, can use the mixing acid of terephthalic acid and sebacic acid, terephthalic acid and nonane diacid or terephthalic acid and hexanodioic acid especially.The mol ratio of terephthalic acid and binary acid though there is no particular limitation, is preferably selected from 0.1～10.0 scope.
In the grease composition of the present invention, the viscosifying agent consumption can be 3～40 weight %, can be 10～30 weight % especially, when viscosifying agent is used quantity not sufficient 3 weight %, and the denseness deficiency of grease composition, when surpassing 40 weight %, grease composition is really up to the mark, should not use.
The lubricating base oil that the present invention uses can be selected from various Dormant oils commonly used and ucon oil.Usually can select oil petroleum refined by naphthenic, polysiloxane (as PSI and poly-ethylsiloxane), synthetic hydrocarbon (as alkylbenzene and poly-a-olefin oil), ester class oil and polyglycol ether etc. for use.Can select oil petroleum refined by naphthenic, polysiloxane and synthetic hydrocarbon especially for use.Lubricating base oil can have 50 ℃ of kinematic viscosity of 3～400 centistokes down, preferably has 8～200 centistokes.
Grease composition of the present invention to various additives commonly used, has excellent adaptability as oxidation inhibitor (pentanoic and phenyl αNai An etc.), extreme pressure agent and corrosion inhibitor etc.Therefore, as required, grease composition of the present invention can also contain various types of additives.
Preparation method of the present invention comprises the following steps: that handle is from C
12～C
24Hydroxy fatty acid and C
10～C
34Lipid acid at least one acid of selecting add in lubricating base oil and heating for dissolving.At first, add the necessary whole lithium alkali of two step saponification, carry out the first step saponification, be warmed up to 120 ℃～150 ℃ rapidly, lithium alkali is uniformly dispersed and sloughs water basically as lithium hydroxide aqueous solution or single hydronium(ion) oxidation lithium.Secondly, add terephthalic acid or terephthalic acid and C down at about 120 ℃～140 ℃
2～C
12Binary acid carry out the second step saponification and compound.
Though above-mentioned preparation method's most convenient also can adopt ready-formed, at least one sour lithium soap of selecting from hydroxy fatty acid and lipid acid prepares grease composition of the present invention.
In addition, also can in the presence of solvent, prepare grease composition of the present invention.At first, terephthalic acid or terephthalic acid and C
2～C
12The hot ethanol solution of binary acid add lubricating base oil and from C
12～C
24Hydroxy fatty acid and C
10～C
34Lipid acid in the mixture of at least one sour lithium soap of selecting.Then, add lithium alkali down at about 90 ℃～110 ℃ and carry out saponification and compound.But solvent-free preparation method has the simple and easy to operate advantage of technology, is more suitable in industrial application.
Preparation method of the present invention except adopting above-mentioned characterization step, as required, also can adopt other post-processing step commonly used.After saponification is finished, append a certain amount of lubricating base oil, be warmed up to 190 ℃～210 ℃, cooling adds an amount of additive, carries out the suitable homogenizing and the degassing, obtains all even slick grease composition.
Composition of compound lithium soap grease of the present invention, have general high-temperature bearing lubricant prerequisite excellent high-temperature performance, water repelling property and long bearing life, compare with known composition of compound lithium soap grease, not only has littler high temperature Stencil oil-dividing and better thick (degree) temperature (degree) characteristic (promptly, penetration degree is littler with the variation of temperature value), therefore enough high temperature denseness are arranged, and also have littler similar viscosity under the low temperature.
General high-temperature bearing lubricant often has relatively poor low temperature properties, and grease composition of the present invention has both high temperature and cryogenic good characteristic preferably.Therefore, grease composition of the present invention can use in wide temperature range.
For the present invention is described better, enumerate following embodiment.But scope of the present invention is not limited only to this.
Embodiment 1
The 12-oxystearic acids of 100 grams (0.33 mole) are added in the oil petroleum refined by naphthenic (100 ℃ of following 20 centistokes of kinematic viscosity) of 500 grams, be heated to 80 ℃～95 ℃ and make its dissolving.At first, in the adding and the aqueous solution of whole lithium hydroxide (0.72 mole) of 12-oxystearic acid and terephthalic acid, heating up dewaters to 120 ℃～150 ℃.Secondly, temperature is remained under 130 ℃～140 ℃, add the terephthalic acid of 30 grams (0.18 mole).Stirring reaction is about 10 minutes under this temperature.Then, be warming up to about 160 ℃, append same a kind of Dormant oils of 455 grams, be warmed up to 210 ℃, be cooled to again about 120 ℃, add 5 gram pentanoic, stir, continue cooling.At last, grinding homogenizing on three disc sharpeners, obtain dropping point＞300 ℃, is 67 lubricating grease 25 ℃ of following micropenetrations.
Embodiment 2
Except replacing the Dormant oils among the embodiment 1 with the PSI of equivalent and do not add the pentanoic, remaining various raw material, consumption and treatment process be fully with embodiment 1, obtains dropping point＞300 ℃, is 63 lubricating grease 25 ℃ of following micropenetrations.
Embodiment 3
Except 12-oxystearic acid with 9.7 grams (0.032 mole), 10.6 gram (0.064 mole) benzene two is arrived, 0.168 the lithium hydroxide aqueous solution of mole, 50 grams and the oil petroleum refined by naphthenic (kinematic viscosity: 20 centistokes under 100 ℃) replace the corresponding composition of embodiment 1 and do not add beyond the pentanoic of appending 29 grams, all the other treatment processs are fully with embodiment 1, obtaining dropping point＞300 ℃, is 78 lubricating grease 25 ℃ of following micropenetrations.
Embodiment 4
Except replace the 12-oxystearic acid among the embodiment 1 with 10 stearic acid that restrain (0.033 mole), terephthalic acid with 3 grams (0.018 mole), 0.072 the lithium hydroxide aqueous solution of mole, 50 grams and the oil petroleum refined by naphthenic (kinematic viscosity: 100 ℃ of following 20 centistokes) replace the corresponding composition among the embodiment 1 and do not add beyond the pentanoic of appending 37 grams, all the other treatment processs are fully with embodiment 1, obtaining 241 ℃ of dropping points, is 72 lubricating grease 25 ℃ of following micropenetrations.
Embodiment 5
Except 12-oxystearic acid with 9 grams (0.030 mole), 0.075 the lithium hydroxide aqueous solution of mole, 50 grams and the oil petroleum refined by naphthenic (kinematic viscosity: the corresponding composition among the replacement embodiment 1 20 centistokes under 100 ℃) of appending 37 grams, with the terephthalic acid among the mixing acid replacement embodiment 1 of the sebacic acid of 2 grams (0.01 mole) and the terephthalic acid of 1.7 grams (0.01 mole) and do not add beyond the pentanoic, all the other treatment processs are fully with embodiment 1, obtaining 260 ℃ of dropping points, is 77 lubricating grease 25 ℃ of following micropenetrations.
Reference example 1 and example 2
For grease composition of the present invention was compared with former grease composition, the compound lithium soap that has prepared with hydroxy fatty acid and binary acid by the known technology method is the reference example 1 of viscosifying agent and the grease composition of example 2.
The composition of the lubricating grease of embodiments of the invention 1～5 and reference example 1 relatively and example 2 is listed in the table 1:
Embodiment 6
Estimated the present invention (embodiment 1～2) and the performance of the constituent of the lubricating grease of (reference example 1～2) relatively, test-results is given in table 2.
# is the Stencil oil-dividing under 180 ℃
## is-50 ℃, 10 seconds
-1Under similar viscosity
Annotate (1): get three fat cups, fill lubricating grease, wipe off on the surface, places baking oven, constant temperature is 30 minutes under the temperature of regulation, takes out the fat cup and scrapes plane surface rapidly, measures (not working) micropenetration immediately, each fat cup is only surveyed once, then, asks the mean value of the measured value of three fat cups.
By the result of table 2 as can be seen, compare with grease composition relatively, grease composition of the present invention not only has good thick (degree) temperature (degree) characteristic, little branch oil and high temperature Stencil oil-dividing, but also have less low temperature similar viscosity and long bearing life.
Claims (13)
1, composition of compound lithium soap grease and preparation method thereof
2, a kind of composition of compound lithium soap grease contains lubricating base oil and viscosifying agent, the invention is characterized in that this viscosifying agent is (a) and (b) compound lithium soap of two kinds of acid, is from C (a)
12～C
24Hydroxy fatty acid and C
10～C
34Lipid acid at least one acid of selecting, (b) be terephthalic acid or terephthalic acid and C
2～C
12The mixing acid of binary acid, wherein, (a) and (b) mol ratio of two kinds of acid (b)/(a)=0.2～2.0.
3,, it is characterized in that (a) and (b) mol ratio of two kinds of acid (b)/(a)=0.5～1.2 according to the described constituent of claim 1.
4,, it is characterized in that (a) can be the 12-oxystearic acid according to the described constituent of claim 1.
5,, it is characterized in that (a) can be the 12-oxystearic acid according to the described constituent of claim 2.
6,, it is characterized in that (a) can be stearic acid according to the described constituent of claim 1.
7,, it is characterized in that (a) can be stearic acid according to the described constituent of claim 2.
8,, it is characterized in that (b) can be terephthalic acid according to any one constituent described in the claim 1 to 6.
9,, it is characterized in that (b) can be terephthalic acid and C according to any one constituent described in the claim 1 to 6
6～C
10The mixing acid of binary acid.
10,, it is characterized in that (b) can be the mixing acid of terephthalic acid and sebacic acid according to any one constituent described in the claim 1 to 6.
11,, it is characterized in that (b) can be the mixing acid of terephthalic acid and nonane diacid according to any one constituent described in the claim 1 to 6.
12,, it is characterized in that (b) can be the mixing acid of terephthalic acid and hexanodioic acid according to any one constituent described in the claim 1 to 6.
13, a kind of preparation method of composition of compound lithium soap grease the invention is characterized in that this method comprises the following steps: that handle is from C
12～C
24Hydroxy fatty acid and C
10～C
34Lipid acid at least one acid of selecting add in lubricating base oil, and heating for dissolving, add the necessary whole lithium alkali of two step saponification and carry out the first step saponification, be warmed up to 120 ℃～150 ℃ rapidly, lithium alkali is uniformly dispersed and sloughs water substantially, secondly, under about 120 ℃～140 ℃, add terephthalic acid or terephthalic acid and C
2～C
12Binary acid carry out the second step saponification and compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85108441A CN85108441B (en) | 1985-11-22 | 1985-11-22 | Composition of compound lithium soap grease and its preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85108441A CN85108441B (en) | 1985-11-22 | 1985-11-22 | Composition of compound lithium soap grease and its preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85108441A CN85108441A (en) | 1987-06-03 |
| CN85108441B true CN85108441B (en) | 1988-07-20 |
Family
ID=4796015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85108441A Expired CN85108441B (en) | 1985-11-22 | 1985-11-22 | Composition of compound lithium soap grease and its preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85108441B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100404655C (en) * | 2003-11-13 | 2008-07-23 | 中国石油化工股份有限公司 | Composite lithium base lubricant and its preparing method |
| EP2027242B1 (en) * | 2006-05-31 | 2016-07-06 | Shell Internationale Research Maatschappij B.V. | Process for preparing a soap concentrate |
| CN101481637B (en) * | 2008-01-09 | 2012-09-05 | 中国石油化工股份有限公司 | Process for preparing composite lithium base grease |
-
1985
- 1985-11-22 CN CN85108441A patent/CN85108441B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85108441A (en) | 1987-06-03 |
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