# Patent

## Title
Lubricating grease based on perfluoropolyether

## Abstract

A lubricating grease is provided that comprises 90 to 99.45 percent by mass of perfluoropolyethers (PFPE) and 0.5 to 5 percent by mass of fumed silica.

## Background
The invention relates to an essentially thickener-free lubricating grease consisting of perfluoropolyethers (PFPE) and a small proportion of a fumed silica, and customary additives.
Perfluorinated polyethers (PFPE) are polymers having good lubrication properties, which are liquid at room temperature and have low surface energies. PFPE compounds are used in virtually all sectors of industry for lubrication, for example in the electronics industry, in aerospace and in the semiconductor industry. PFPE compounds are also used for lubrication of highly stressed ball bearings.
PFPE-based lubricating greases have been thickened using PTFE (Teflon powder), BN (boron nitride), graphite, MoS2, oxidic ceramic materials or organic thickeners, such as ureas and soaps, in concentrations of 20 to 40 percent by mass. Aerosils have likewise been used as individual thickeners or thickener components within the concentration range mentioned. PFPE-based lubricants thickened in this way typically have too high a solids content and their grains are too coarse to work with low noise.
In addition, PFPE lubricants are employed as antisqueak agents, especially on elastomer and textile surfaces, and leather. Here, however, there is unwanted penetration or diffusion of lubricant into the surface of the materials treated, and so regular relubrication becomes necessary.


In order to exploit the advantageous effects of the PFPE compounds as lubricating greases, it was therefore the aim of the present invention to provide an additive which has highly thickening properties in very low concentrations. It is thus possible to serve low-noise applications. The consistent state of the lubricant applied additionally reduces regularity of relubrication on porous material.
The addition of less than 4 percent by mass of fumed silica to PFPE compounds gives consistent lubricating greases. They have NLGI penetration values of 210 to 385 and thus belong to NLGI classes 0 to 3. The additives used may be either hydrophilic or hydrophobic fumed silicas, preference being given to the hydrophilic fumed silicas.
Compared to the known PFPE lubricating greases, the inventive PFPE greases having a very small proportion of fumed silica are superior to the known greases both in terms of their noise characteristics and in terms of their dynamic characteristics. Emphasis should also be given to the transparency of these lubricating greases, which appear visually neutral, for example, on black surfaces.
The surface protection achieved on the surfaces treated with the inventive PFPE lubricating grease is distinctly improved, since it has been shown that the inventive grease is immobilized and does not diffuse into the surface. For this purpose, studies have been conducted on corresponding elastomers and textile surfaces which are used in automobile interiors.
In the case of use of less than 2 percent by mass of fumed silica in the PFPE lubricating grease, the lubricating greases are substantially transparent. A thin lubricating film applied to black surfaces is therefore visually neutral and does not differ from pure PFPE, but has the advantage that the lubricating grease does not penetrate into the surface of the material; see table 1.
Especially in the form of an antisqueak agent in the sector of door seals and door profiles in the automotive sector, these advantages are of particular significance.







TABLE 1





Example formulation for an inventive PFPE 


lubricant compared to pure PFPE oil.



















Thickener
1.5% Aerosil
None



PFPE
100 cSt at 40° C.
100 cSt at 40° C.



Appearance
transparent
transparent



Characteristics
Thin lubricant
Thin oil layer



on EPDM material
layer applied by
applied by brush




brush is unchanged
has substantially




after 7 days.
diffused into





surface after 7





days.



Antisqueak
passed
passed



characteristics on





EPDM material, in-





house Kluber test










It is likewise possible to use the inventive lubricants, on the basis of the properties described above, in electrical contacts, slip rings and switches. PFPE lubricants here, because of their exceptional chemical stability, give very good protective action and prolonged lubricity. In the case of customary solids-based thickeners, the volume resistance in such components can vary impermissibly, since electrically insulating particles hinder current flow. With increasing thickener concentration, this problem increases. The inventive lubricant has two advantages here: the thickener concentration is significantly reduced; in addition, the thickener has a very low mean particle size of less than 1 micrometer. This ensures substantially unhindered current flow; see table 2.








TABLE 2





Properties of an inventive lubricant 


in electrical contact applications 


compared to a PTFE-thickened lubricant.



















Thickener
2.8% Aerosil
21% PTFE



PFPE
100 cSt at 40° C.
100 cSt at 40° C.



Characteristics in
No variations in
Variations in



electrical switch
passage
passage resistance



contacts (in-house 
resistance
after 100 electrical



test)

switching operations










The high-speed properties in roller bearings were confirmed in an SKF-ROF test run; see table 3.








TABLE 3





Properties of an inventive lubricant in roller bearing


applications compared to a PTFE-thickened lubricant.

















Thickener
3% Aerosil
24% PTFE


PFPE
300 cSt at 40° C.
300 cSt at 40° C.


Appearance
semitransparent
white


Consistency
NLGI 2
NLGI 2


Speed factor (ROF)
670000 (good)
330000 (poor)


Service life in
>500 h
>500 h


roller bearings at 200° C.




FAG MGG 11 noise tester
I (low noise)
IV (poor)









The inventive lubricating grease contains 90 to 99.45 percent by mass of perfluoropolyether (PFPE) and 0.5 to 5 percent by mass of fumed silica. The perfluoropolyether is a chemical compound of formula (I):

R1—(O—CF2)v—(O—C2F4)w—(O—C3F6)x—(O—CFCF3)y—(O—CF2CF(CF3))z—O—R2   (I)

where R1 and R2 are identical or different and are selected from —CF3, —C2F5 and —C3F7, v, w, x, y, z are integers from ≧0 to 500.

The fumed silica is preferably a hydrophilic silica.
In addition, the inventive lubricating grease may contain 0.05 to 5 percent by mass of anticorrosive.
The anticorrosive present in the lubricating grease is selected from the group consisting of functionalized PFPE derivatives; preference is given to carboxylic acids or metal salts thereof, and PFPE ethoxylates.
The inventive use of lubricating grease is used as an antisqueak agent in the automotive sector. It is likewise used for lubrication in the office and electronics sectors, especially in the case of plastic hinges of monitors/television mounts or clamshell cell-phones.

## Claims

1. A lubricating grease consisting of:
90 to 99.45 percent by mass of perfluoropolyethers (PFPE); and
0.5 to 5 percent by mass of fumed silica, in which the fumed silica is a hydrophilic silica,
wherein the perfluoropolyethers are a chemical compound of formula (I):


R1—(O—CF2)v—(O—C2F4)w—(O—C3F6)x—(O—CFCF3)y—(O—CF2CF(CF3))z—O—R2   (I)


where R1 and R2 are identical or different and are selected from —CF3, —C2F5 and —C3F7, v, w, x, z are integers from ≧0 to 500 and y is an integer from ≧1 to 500.

2. A lubricating grease consisting of:
90 to 99.45 percent by mass of perfluoropolyethers (PFPE);
0.5 to 5 percent by mass of fumed silica, in which the fumed silica is a hydrophilic silica; and
0.05 to 5 percent by mass of an anticorrosive additive,
wherein the perfluoropolyethers are a chemical compound of formula (I):


R1—(O—CF2)v—(O—C2F4)w—(O—C3F6)x—(O—CFCF3)y—(O—CF2CF(CF3))z—O—R2   (I)


where R1 and R2 are identical or different and are selected from —CF3, —C2F5 and —C3F7, v, w, x, z are integers from ≧0 to 500 and y is an integer from ≧0 to 500.

3. The lubricating grease as claimed in claim 2, wherein the anticorrosive is selected from the group consisting of functionalized PFPE derivatives, carboxylic acids or metal salts thereof, and PFPE ethoxylates.

4. The lubricating grease as claimed in claim 1 wherein the lubricating grease is suitable as an antisqueak agent to roller bearings in the automotive sector.

5. The lubricating grease as claimed in claim 1 wherein the lubricating grease is suitable as a lubricant to plastic hinges of monitors/television mounts or clamshell cell phones.