Lithium Complex Hybrid Grease

Abstract

A lithium complex hybrid grease is based on a lithium complex grease in combination with a PFPE grease. The lithium complex hybrid grease can be used at higher temperatures, does not form layers in the process, and exhibits a low hardening tendency. The lithium complex hybrid grease is usable in components in the automotive field and in the industrial field.

Claims

1. A lithium complex hybrid grease containing: (A) 70% to 7% by weight of an ester or an ester mixture selected from the group consisting of trimellitic acid esters containing linear and branched alkyl groups containing 6 to 18 carbon atoms, as alkoxy groups, wherein the alkoxy groups may be identical or different, pyromellitic acid esters, hydrogenated or unhydrogenated dimeric acids, estolides, (B) 0.5% to 20% by weight of unhydrogenated, hydrogenated or fully hydrogenated polyisobutylene or mixtures thereof, (C) 1% to 18% by weight of lithium complex soaps and (D) 5% to 70% by weight of perfluoropolyether (PFPE).

2. The lithium complex grease as claimed in claim 1, further containing: (E) 1% to 30% by weight of a further thickener.

3. The lithium complex hybrid grease as claimed in claim 1, further containing: (F) 0% to 20% by weight, preferably 2% to 20% by weight, of a further oil component.

4. The lithium complex hybrid grease as claimed in claim 1, further containing: (G) 0% to 10% by weight, preferably 0.1% to 10% by weight, of additives.

5. The lithium complex hybrid grease as claimed in claim 1, further containing (H) 0% to 10% by weight, preferably 2% to 5% by weight, of solid lubricant.

6. The lithium complex hybrid grease as claimed in claim 1, characterized in that the pyromellitic acid ester of component (A) is tetrakis(2-ethylhexyl)pyromellitate and the dimeric acid is bis(2-ethylhexyl)dimerate.

7. The lithium complex hybrid grease as claimed in claim 2, characterized in that the component (E) is selected from the group consisting of Al complex soaps, metal monosoaps of elements of the first and second main group of the periodic table without lithium, metal complex soaps of elements of the first and second main group of the periodic table without lithium, bentonites, sulfonates, silicates, aerosil, polyimides, PTFE and a mixture thereof.

8. The lithium complex hybrid grease as claimed in claim 3, characterized in that the component (F) is selected from the group consisting of mineral oil, alkylated benzenes, alkylated naphthalenes, aliphatic carboxylic acid and dicarboxylic acid esters, fatty acid triglycerides, alkylated diphenyl ethers, phloroglucinol esters and polyalphaolefins, alpha-olefin copolymers, metallocene-catalyzed polyalphaolefins.

9. The lithium complex hybrid grease as claimed in claim 4, characterized in that the component (G) is selected from the group consisting of anticorrosion additives, antioxidants, antiwear additives, and UV stabilizers.

10. The lithium complex hybrid grease as claimed in claim 5, characterized in that the component (H) is selected from the group consisting of BN, pyrophosphate, Zn oxide, Mg oxide, pyrophosphates, thiosulfates, Mg carbonate, Ca carbonate, Ca stearate, Zn sulfide, Mo sulfide, W sulfide, Sn sulfide, graphites, graphene, nanotubes, SiO.sub.2 modifications and a mixture thereof.

11. The use of the lithium complex hybrid grease as claimed in claim 1 for lubrication of components in the field of anti-friction bearings, plain bearings, transport and timing chains in vehicle technology, in rail vehicles, in conveying technology, in film orienting lines, in corrugated board lines, of track roller bearings, fan bearings, bearings of traction engines, for lubricating bevel gear and spur gear transmissions, springs, screws and compressors, pneumatic components, valves and of machine components and in plants where occasional unintentional contact with foodstuffs occurs.

12. A method for lubricating or greasing a component comprising: applying a lubricant composition to a surface of the component, the lubricant comprising: (A) 70% to 7% by weight of an ester or an ester mixture selected from the group consisting of trimellitic acid esters containing linear or branched alkyl groups containing 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, as alkoxy groups, wherein the alkoxy groups may be identical or different, pyromellitic acid esters, hydrogenated and unhydrogenated dimeric acids, estolides, (B) 0.5% to 20% by weight of unhydrogenated, hydrogenated or fully hydrogenated polyisobutylene or mixtures thereof, (C) 1% to 18% by weight of lithium complex soaps and (D) 5% to 70% by weight of perfluoropolyether (PFPE).

13. A method for lubricating or greasing track roller bearings in continuous casting lines, transport roller bearings in conveyor furnaces, of open ring gears in rotary furnaces, tube mills, drums and mixers, bearings in corrugated board lines or film orienting lines or bearings in lines for production and transport of foodstuffs, the method comprising: applying a lubricant composition to the surface of the component, the lubricant comprising: (A) 70% to 7% by weight of an ester or an ester mixture selected from the group consisting of trimellitic acid esters containing linear or branched alkyl groups containing 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, as alkoxy groups, wherein the alkoxy groups may be identical or different, pyromellitic acid esters, hydrogenated and unhydrogenated dimeric acids, estolides, (B) 0.5% to 20% by weight of unhydrogenated, hydrogenated or fully hydrogenated polyisobutylene or mixtures thereof, (C) 1% to 18% by weight of lithium complex soaps and (D) 5% to 70% by weight of perfluoropolyether (PFPE).

14. A method for reducing the hardening of lubricating greases at 200° C. and/or for reducing the oil separation of lubricating greases on track roller bearings in continuous casting lines, transport roller bearings in conveyor furnaces, of open ring gears in rotary furnaces, tube mills, drums and mixers, bearings in corrugated board lines or film orienting lines or bearings in lines for production and transport of foodstuffs, the method comprising: applying a lubricant composition to the surface of the component, the lubricant comprising: (A) 70% to 7% by weight of an ester or an ester mixture selected from the group consisting of trimellitic acid esters containing linear or branched alkyl groups containing 6 to 18 carbon atoms, preferably 8 to 14 carbon atoms, as alkoxy groups, wherein the alkoxy groups may be identical or different, pyromellitic acid esters, hydrogenated and unhydrogenated dimeric acids, estolides, (B) 0.5% to 20% by weight of unhydrogenated, hydrogenated or fully hydrogenated polyisobutylene or mixtures thereof, (C) 1% to 18% by weight of lithium complex soaps and (D) 5% to 70% by weight of perfluoropolyether (PFPE).

15. The lithium complex hybrid grease as claimed in claim 1, wherein the branched alkyl groups of component (A) contains 8 to 14 carbon atoms.

Description

[0074] FIG. 1 shows the worked penetration 60 dT,

[0075] FIG. 2 shows the oil separation, i.e. the loss of oil from the lubricating grease.

[0076] The invention will now be more particularly elucidated with reference to the following examples.

[0077] Production of the Inventive Lubricant Compositions

[0078] Production of the lubricant compositions according to the invention is not restricted and may be performed by any suitable methods.

[0079] Production of the lubricant composition according to the invention may be carried out for example by producing a base oil mixture with the components (A) and/or (B) and/or (F). The acids required for the lithium complex thickener (C) are melted into this base oil mixture which is entirely or only partly initially charged in a suitable reaction vessel containing heating, cooling and stirring means, and an aqueous lithium hydroxide solution is added. This forms a liquor containing the lithium soaps of the carboxylic acids. The acids may be added and neutralized individually or else the monocarboxylic acid is added and neutralized first and the higher-functional carboxylic acid is added and neutralized in a second step. The liquor is heated to 130° C. to expel water. The swelling of the thickener (lithium complex soap) is performed by thermal treatment at 150° C. to 210° C. The thermally treated liquor is then cooled and a portion of the base oil mixture may also be used. The components (D), (E), (G), (H) and the components (A), (B) and (F) which are optionally not used for the base oil mixture are added at a suitable temperature and pre-homogenized by stirring.

[0080] Solid lubricant additives soluble in the base oil mixture are for example added at temperatures above their melting point. Liquid additives or non-melting additives/solid lubricants/thickener components are added at temperatures below 80° C. The resulting lithium complex hybrid grease may be homogenized by suitable apparatuses such as three-roll mills, colloid mills or a Gaulin homogenizer.

[0081] The above-described method produces the inventive lubricant composition in one process. Alternatively, the addition of the PFPE oil (D) and the optional thickener component (E) may be omitted in the above-described method to form a lithium complex grease. The components (D) and (E) may be combined to afford a PFPE grease by stirring, homogenizing as described above. The lithium complex grease and the PFPE grease may be combined in a second method step to produce the inventive lubricant composition therefrom by stirring and homogenizing.

[0082] Production may also be effected by continuous methods, wherein ready-made Li complex soap in powder form may also be used.

Example 1

[0083] Production of several inventive lubricant compositions, comparison with the lithium complex grease and PFPE/PTFE grease used for production, comparison with urea hybrid greases

[0084] Production

[0085] Lithium complex soap grease (grease A) and a PFPE/PTFE grease (grease B) are produced separately and the two greases A and B are mixed in different ratios, stirred and homogenized by rollers.

[0086] Grease A

[0087] A lithium complex grease consisting of 77% of a mixture of an alkyl diphenyl ether (100 mm.sup.2/sec/40° C.) and trimellitic acid ester and fully hydrogenated polyisobutylene (fully hydrogenated, Mn about 1300 g/mol) is produced as a base oil, wherein a viscosity at 40° C. of 100 mm.sup.2/sec is established, before 15% of a lithium complex of azelaic acid and 12-hydroxystearic acid and 8% of an additive package consisting of aminic antioxidants, phosphates, thiadiazoles, triazoles and amine phosphates are added. The worked penetration is 270 1/10 mm (see table 1).

[0088] Grease B

[0089] A PFPE/PTFE grease containing 70% of a mixture of linear and branched PFPE, kinematic viscosity 200 mm.sup.2/sec at 40° C., 26% PTFE micropowder, average particle size d50 (laser diffraction, DIN ISO 9277) about 5 μm, specific surface area (DIN ISO 9277) about 5 m.sup.2/g, and 4% disodium sebacate as anticorrosion additive is produced. The worked penetration is 286 1/10 mm (see table 1).

Example 1 (B1)

[0090] Mixture of grease A and grease B in the ratio 10% by weight to 90% by weight.

Example 2 (B2)

[0091] Mixture of grease A and grease B in the ratio 30% by weight to 70% by weight.

Example 3 (B3)

[0092] Mixture of grease A and grease B in the ratio 50% by weight to 50% by weight.

Example 4 (B4)

[0093] Mixture of grease A and grease B in the ratio 70% by weight to 30% by weight.

Example 5 (B5)

[0094] Mixture of grease A and grease B in the ratio 90% by weight to 10% by weight.

Comparative Example 1 (VG1)

[0095] A urea hybrid grease consisting of 50% by weight of grease B and 50% by weight of a urea grease is produced. The urea grease consists of a mixture of trimellitic acid ester and a reaction product of octylamine and oleylamine with an MDI/TDI mixture as the urea thickener and additives. The base oil viscosity is about 80 mm.sup.2/sec. The worked penetration is 265 mm.sup.2/sec (see table 2).

Comparative Example 2 (VG2)

[0096] A urea hybrid grease consisting of a complex ester based on a dimeric acid, V 40 about 400 mm.sup.2/sec at 40° C., and branched PFPE oil having a kinematic viscosity of about 400 mm.sup.2/sec in a mass ratio of 2:1 is produced. The urea thickener is present in a proportion of 10% and is a reaction product of octylamine and oleylamine with an MDI/TDI mixture. Also present are 8% by weight of PTFE powder (as in grease B) and 5% by weight of soluble additives (antioxidants, amine phosphates). The worked penetration is 290 mm.sup.2/sec (see table 2).

[0097] Table 1 shows the general characteristics of the inventive lithium complex hydrogen greases of examples B1 to B5 and of greases A and B.

TABLE-US-00001 TABLE 1 Grease Grease Parameter/grease (B) B1 B2 B3 B4 B5 (A) Worked penetration 286 279 254 253 262 273 270 60 dT [1/10 mm] (DIN ISO 2137) Delta worked 15 28 31 45 44 39 45 penetration after 100 000 dT [1/10 mm] (DIN ISO 2137) Dripping point [° C.] >300 >300 >300 >300 >300 294 >300 (DIN ISO 2176) Flow pressure [mbar] 200 375 575 850 875 875 925 (−40° C.) (DIN 51805) Flow pressure [mbar] 325 575 1025 >1400 >1400 >1400 >1400 (−50° C.) (DIN 51805) Shear viscosity at 6095 7557 7253 7210 6849 6106 5966 25° C., shear rate 300 1/s (DIN 53019-1, -3) Evaporation loss, 0.12 0.19 0.24 0.36 0.36 0.45 0.46 22 h/100° C. [% by wt.] (DIN 58397) Oil separation, 6.93 7.42 2.05 0.57 1.49 3.95 5.18 24 h/150° C. [% by wt.] (ASTM D 6184) Oil separation, 7.24 7.75 2.81 0.73 3.01 7.12 7.84 72 h/150° C. [% by wt.] (ASTM D 6184) Oil separation, 2.88 2.89 1.28 0.22 0.76 1.29 1.41 168 h/40° C. [% by wt.] (DIN 51817) Water resistance, 0 0 1 1 1 1 1 static, 3 h/90° C. (DIN 51807) Copper corrosion, 2 1-2 1 1 1 1 1 24 h/120° C. (DIN 51811)

[0098] Table 2 shows the data for comparative examples VG1 to 2.

TABLE-US-00002 TABLE 2 Parameter/grease VG1 VG2 Worked penetration 60 dT [1/10 262 290 mm] (DIN ISO 2137) Delta worked penetration after 47 43 100 000 dT [1/10 mm] (DIN ISO 2137) Dripping point [° C.] (DIN ISO 285 285 2176) Flow pressure [mbar] (−40° C.) 725 625 (DIN 51805) Flow pressure [mbar] (−50° C.) 1200 1375 (DIN 51805) Shear viscosity at 25° C., shear 5913 11880 rate 300 1/s (DIN 53019-1, -3) Evaporation loss, 22 h/100° C. [% 0.37 0.42 by wt.] (DIN 58397) Oil separation, 24 h/150° C. [% by 0.42 0.11 wt.] (ASTM D 6184) Oil separation, 72 h/150° C. [% by 0.52 0.21 wt.] (ASTM D 6184) Oil separation, 168 h/40° C. [% by 0.82 0.39 wt.] (DIN 51817) Water resistance, static, 0 0 3 h/90° C. (DIN 51807) Copper corrosion,24 h/120° C. 1 1 (DIN 51811)

[0099] As is apparent in FIG. 1 (worked penetration of the inventive compositions) especially the compositions B2, B3 and B4 show a lower worked penetration than the two employed greases A and B. This shows an unexpected synergistic effect brought about by the combination of the two grease types to afford the inventive compositions.

[0100] As is apparent in FIG. 2 (comparison of the oil separation of the inventive compositions) the inventive compositions for a lower oil separation and the greases A and B from which they were produced. This behavior shows the unexpected synergistic effect brought about by the inventive composition. The oil separation virtually achieves the low values of the two comparative products VG1 and VG2. The reduction of the oil separation and comparative grease B demonstrates the advantage over the pure PFPE/PTFE greases.

[0101] The data also show that a desired oil separation behavior can be established through selection of the amount of greases A and B.

[0102] Determination of Evaporation Loss

[0103] The inventive lubricant compositions were tested for their thermal stability and the results compared especially with those of the urea hybrid greases. To this end investigations in respect of evaporation and viscosity under thermal stress of a 5 g initial weight of grease weighed into a stainless steel dish at 200° C. were performed. The results are shown in tables 3 and 4.

[0104] Evaporation loss is determined according to DIN standard 58397. For each grease sample three evaporation loss dishes made of stainless steel were required. The geometry of the dishes is described in the standard for determining evaporation loss (DIN 58397). Initially the respective empty weight of the dishes was determined. Subsequently the three evaporation loss dishes were filled with the grease sample. It must be ensured that the grease is applied so as to avoid air bubbles. A scraper is used to smooth the surface and excess grease that has entered the edge depression of the dish is removed. The dishes are subsequently stored in a customary laboratory drying cabinet with convection with the door closed at the appropriate test temperature (here 200° C.). After the duration specified in each case (48 h, 96 h, 144 h and 168 h) the dishes are removed from the drying cabinet and allowed to cool. The dishes are then weighed. The evaporation loss is determined from the difference between the initial weight and the measured weight. Three individual values are used to determine an average value (V.sub.M). Together with the average value of the three initial weights (A.sub.M) the evaporation loss may be calculated. V=(V.sub.M/A.sub.M)*100 [%]. After weighing, the dishes are replaced in the drying cabinet until the next time point. This is repeated until 168 h have elapsed.

TABLE-US-00003 TABLE 3 Evaporation loss test 200° C. B1 B2 B3 B4 B5 Evaporation loss DIN % by 3.97 6.60 11.28 14.51 16.44 test 48 h/200° C. 58397 wt. Evaporation loss DIN % by 5.27 8.75 15.22 19.69 22.17 test 96 h/200° C. 58397 wt. Evaporation loss DIN % by 6.33 10.63 18.42 24.71 27.91 test 144 h/200° C. 58397 wt. Evaporation loss DIN % by 7.15 12.35 21.15 28.98 33.11 test 168 h/200° C. 58397 wt.

[0105] Determination of Shear Viscosity

[0106] Shear viscosity is determined according to DIN standard 53019 part 1 and 3. The grease samples are in each case transferred into three evaporation loss dishes made of stainless steel. The geometry of the dishes is described in the standard for determining evaporation loss (DIN 58397). The dishes are subsequently dried in a customary laboratory drying cabinet with convection recirculation at the appropriate test temperature (here 200° C.). After the duration specified in each case (48 h, 96 h, 144 h and 168 h) the dishes are removed from the drying cabinet and allowed to cool. The starting value for the shear viscosity is determined for each grease before subjection to thermal stress.

[0107] Measurement of shear viscosity is carried out with a standard instrument for determining rheological parameters of lubricating greases (for example Anton Paar MCR 302 rheometer).

[0108] A cone and plate system is employed (DIN EN ISO 3219 and DIN 53019), preferably with a measuring cone having a diameter of 25 mm. The required amount of grease sample is based on typical amounts required for rheological measurements. The measurement duration is 120 seconds, of which 60 seconds are heating/holding time. Measurement is performed at a constant shear rate of 300 1/s and a temperature of 25° C. The value that may be read off after 90 seconds represents the shear viscosity for the respective grease sample. The three individual values determined are used to form an average value and finally reported.

TABLE-US-00004 TABLE 4 B1 B2 B3 B4 B5 Shear viscosity DIN 53019- mPas 7557 7253 7210 6849 6106 starting value 1, -3 Shear viscosity DIN 53019- mPas 6848 9857 9210 8651 5091 48 h/200° C. 1, -3 Shear viscosity DIN 53019- mPas 7671 10479 10292 9624 6587 96 h/200° C. 1, -3 Shear viscosity DIN 53019- mPas 6800 11764 11112 9986 8917 144 h/200° C. 1, -3 Shear viscosity DIN 53019- mPas 7494 10994 15452 9340 13623 168 h/200° C. 1, -3

[0109] The greases of examples 1 to 5 were then compared with the greases of comparative examples 1 and 2 and the two individual greases (A) and (B) in respect of their thermal stability. The results are shown in tables 5 and 6.

TABLE-US-00005 TABLE 5 Evaporation loss test 200° C. VG1 VG2 Grease A Grease B Evaporation loss test DIN % by 10.43 11.98 17.87 0.88 48 h/200° C. 58397 wt. Evaporation loss test DIN % by 13.47 14.17 24.75 1.11 96 h/200° C. 58397 wt. Evaporation loss test DIN % by 17.03 16.70 31.39 1.30 144 h/200° C. 58397 wt. Evaporation loss test DIN % by 20.67 19.18 37.66 1.45 168 h/200° C. 58397 wt.

TABLE-US-00006 TABLE 6 VG1 VG2 Grease A Grease B Shear viscosity DIN mPas 5913 11880 6095 5966 starting value 53019-1, -3 Shear viscosity DIN mPas 9400 45976 7801 5800 48 h/200° C. 53019-1, -3 Shear viscosity DIN mPas 12844 100000 8317 7104 96 h/200° C. 53019-1, -3 Shear viscosity DIN mPas 18286 100000 7737 12093 144 h/200° C. 53019-1, -3 Shear viscosity DIN mPas 35172 100000 8365 16025 168 h/200° C. 53019-1, -3

[0110] The above results show that for the inventive lithium complex hybrid greases the increase in shear viscosity is markedly lower than for the comparative products VG1 and VG2. VG2 shows a shear viscosity of 100 000 mPas and is no longer capable of lubrication after only 96 h. After a test time of 168 h VG1 shows a shear viscosity which is twice as high as all inventive compositions B1 to B5, see table 4.

[0111] The PFPE/PTFE grease (grease B) shows the lowest evaporation losses in the test as expected. Surprisingly, the shear viscosity of the inventive examples B1, B2 and B4 is lower than for grease B after a test time of 168 h and therefore exhibits hardening behavior that is more advantageous.

[0112] It is altogether apparent that the hardening behavior of the inventive greases at high temperatures is more advantageous than for urea hybrid greases. It has surprisingly even been found that some of the inventive compositions even exhibit a lower hardening than a PFPE/PTFE grease. It has surprisingly also been found that the oil separation behavior of the inventive lubricants can be adjusted and thus adapted to different requirements through selection of particular mixing ratios of the greases A (lithium complex grease) and B (PTFE/PFPE grease).

Example 2

[0113] Production of an Inventive Grease with Different Production Methods

[0114] As previously described the inventive greases may be produced in different ways. In the “vessel-mixed” variant a lithium complex grease (grease C) and a PFPE/PTFE grease (grease D) are produced separately and then mixed by stirring in a vessel in a ratio of 40% to 60% by weight. The resulting lithium complex hybrid grease B6 is subsequently homogenized using a three-roll mill.

[0115] In the “in situ” production the lithium complex grease is produced identically to grease C but, in a departure, the constituents of grease D are then also added, thus producing the inventive lubricant composition in one operation. The inventive grease composition B6 is also subsequently rolled.

[0116] Grease C

[0117] A lithium complex grease consisting of 80% by weight of a mixture of an alkyl diphenyl ether (100 mm.sup.2/sec at 40° C.) and a trimellitic acid ester and fully hydrogenated polyisobutylene (fully hydrogenated, Mn about 1300 g/mol) is produced as a base oil, resulting in a viscosity at 40° C. of 100 mm.sup.2/sec. 15% by weight of a lithium complex of azelaic acid and 12-hydroxystearic acid and 5% by weight of an additive package consisting of aminic antioxidants and phosphates are provided. The worked penetration is 327 1/10 mm.

[0118] Grease D

[0119] A PFPE/PTFE grease containing 65% by weight of a mixture of linear and branched PFPE having a kinematic viscosity of 145 mm.sup.2/sec at 40° C., 33% by weight of PTFE micropowder, average particle size d50 (laser diffraction, DIN ISO 9277) about 5 μm, specific surface area (DIN ISO 9277) about 5 m.sup.2/g, and 2% by weight of disodium sebacate as anticorrosion additive is produced. The worked penetration is 286 1/10 mm.

TABLE-US-00007 TABLE 7 Data for inventive example B6 according to example 2 Parameter/grease Vessel-mixed Cooked in situ Worked penetration 60 dT [1/10 mm] 298 265 (DIN ISO 2137) Dripping point [° C.] (DIN ISO 2176) >300 277 Delta worked penetration after 100 000 25 36 dT [1/10 mm] (DIN ISO 2137) Flow pressure −40° C. [mbar] (DIN 51805) 550 725 Flow pressure −50° C. [mbar] (DIN 51805) 1025 1250 Shear viscosity at 25° C., shear rate 4392 5378 300 1/s [mPa * s] (DIN 53019-1, -3) Evaporation loss, 24 h/150° C. [% by wt. ] 0.46 0.50 (DIN 58397) Oil separation, 30 h/150° C. [% by wt.] 0.44 1.47 (ASTM D 6184) Oil separation, 72 h/150° C. [% by wt. ] 0.53 2.11 (ASTM D 6184) Oil separation, 168 h/40° C. [% by wt. ] 1.15 0.84 (DIN 51817) Water resistance, static, 3 h/90° C. (DIN 0 0 51807) Copper corrosion, 24 h/120° C. (DIN 1 1 51811)

TABLE-US-00008 TABLE 8 Evaporation loss test Cooked 220° C. Vessel-mixed in situ Evaporation loss, DIN 58397 % by 11.37 10.67 48 h/220° C. wt. Evaporation loss, DIN 58397 % by 15.84 15.15 96 h/220° C. wt. Evaporation loss, DIN 58397 % by 20.65 19.48 144 h/220° C. wt. Evaporation loss, DIN 58397 % by 23.02 21.65 168 h/220° C. wt.

TABLE-US-00009 TABLE 9 Vessel- Cooked mixed in situ Shear viscosity, (DIN 53019-1, -3) mPas 4392 5378 starting value Shear viscosity, (DIN 53019-1, -3) mPas 6848 5823 48 h/220° C. Shear viscosity, (DIN 53019-1, -3) mPas 6449 7732 96 h/220° C. Shear viscosity, (DIN 53019-1, -3) mPas 10892 9342 144 h/220° C. Shear viscosity, (DIN 53019-1, -3) mPas 10927 11753 168 h/220° C.

[0120] Both production variants provide identical values within the experiment error.

[0121] The present data show that B6 according to production example 1 and production example 2 may be employed as a lubricant with both production variants.

[0122] It has therefore been demonstrated that the inventive lubricant compositions may be produced by different methods.