[0001] The present invention relates to a high dropping-point lithium-complex grease composition
having improved extreme pressure properties.
[0002] In the co-pending European patent application 83200077 high dropping-point lithium-complex
grease compositions are described, which contain (a) as gelling component e.g. a lithium
soap of a C
12 to C
24 hydroxy fatty acid and (b) as a complexing metal salt e.g. a lithium salt of a boric
acid.
[0003] Furthermore a high molecular weight viscosity-index improver, and/or succinimide
type dispersant and/or metal salt detergent is added in order to provide the grease
compositions with improved anti-noise properties.
[0004] Although the present grease compositions may also contain such anti-noise additives,
the purpose of the present invention is to render extreme pressure properties to high
dropping-point lithium-complex grease compositions of the above type.
[0005] It has been found that this purpose can surprisingly be met by combining the above-mentioned
components (a) and (b) with a component (c) which is a class of certain metal salts
of a boric acid.
[0006] This invention therefore relates to a high dropping-point lithium-complex grease
composition having improved extreme pressure properties, comprising a lubricating
oil and the following components:
(a) at least one lithium soap of a C12 to C24 hydroxy fatty acid,
(b) at least one lithium salt of a boric acid, and
(c) at least one metal salt selected from the group consisting of
1) a potassium salt of a boric acid,
2) a sodium salt of a boric acid,
3) an alkaline earth metal salt of a boric acid, and
4) a zinc salt of a boric acid.
Lubricating oil
[0007] Any conventional lubricating oil can be used. While a typical one is a mineral oil,
use can also be made, singly or in combination with the mineral oil, of a synthetic
oil including ester oils, such as a diester oil, e.g. dioctyl azelate, and a tetraester
oil, e.g. the pentaerythritol ester of an aliphatic monocarboxylic acid, or poly-alpha-olefin
oligcmers, such as octene-1/decene-1 copolymers, having a viscosity of 41.0 cSt at
37.8°C, a viscosity index (V.I.) of 130 and a flash point of 223°C.
[0008] The lubricating oil may have a viscosity ranging from about 2 to 500 cSt, preferably
from 20 to 200 cSt, at 40°C.
Component (a)
[0009] The C
12 to C
24 hydroxy fatty acids include saturated or unsaturated monocarboxylic fatty acids containing
a hydroxyl radical, especially those acids containing 18 carbon atoms and a hydroxyl
radical in the 9-, 10- or 12-position, such as 12-hydroxy stearic acid and ricinolic
acid.
[0010] The lithium salts of the above fatty acids and hydroxy fatty acids can be singly
used or combinedly with one or more of others. In addition, when said lithium salts
are prepared, said carboxylic acids can be reacted with lithium hydroxide not only
in the form of free acids but also as glycerides.
Component (b)
[0011] Suitable salts are lithium metaborate, lithium diborate, lithium tetraborate, lithium
pentaborate, lithium perborate and lithium ortho borate, such as the monolithium salt
of ortho boric acid (H
3BO
3).
Component (c)
[0012] Suitable salts are potassium, sodium, alkaline earth metal (e.g. Ca, Ba or Mg) and
zinc metaborate, diborate, tetraborate, pentaborate, perborate and ortho borate. Partial
as well as full salts are suitable.
[0013] The above components (a), (b) and (c) can be present as separate compounds or as
a mixed compound as explained hereinafter.
Preparation of these grease compositions
[0014] The grease composition according to the present invention can be prepared by uniformly
admixing and finely dispersing the three components (a), (b) and (c) in the base oil
mentioned above. While the amounts of these three components compounded in the base
oil above are not necessarily critical but can be variable for individual components,
it is generally advantageous to use them in the following proportions per 100 weight
parts (pbw) of the base oil;
Component (a): 2 to 40 weight parts, preferably 5 to 30 weight parts
Component (b): 0.05 to weight parts, preferably 0.1 to 10 weight parts
Component (c): 0.05 to 20 weight parts, preferably 0.1 to 10 weight parts
[0015] Also, it is particularly preferable to use the components (a) and (b) in the following
mol ratio within the above ranges of the proportions;
[0016] Component (a)/Component (b) mol ratio = 0.5 to 10, especially 1 to 5.
[0017] The present grease composition can also be prepared as follows. The base oil is admixed
with a hydroxy fatty acid for forming a component (a), followed by an e.g., equivalent,
amount of LiOH to form a soap. Then, a boric acid for a component (b) is admixed,
followed successively by an, e.g equivalent, amount of LiOH, another portion of a
boric acid and an e.g., equivalent, amount of a metal compound of a metal of component
(c), e.g. an oxide or hydroxide of K, Na, an alkaline earth metal or Zn. Alternatively,
the total of the two portions above of boric acid may be admixed simultaneously in
the first mixture, followed by LiOH and said metal compound.
[0018] These procedures, which result into socalled mixed compounds, may be carried out
at 70 to 90°C. Subsequently, the reaction mixture is dehydrated gradually at e.g.
140 to 225°C to complete the preparation.
[0019] It is also possible to add an aqueous slurry of LiOH.H
2O, the metal compound of a metal of components (c) and boric acid to e.g. an autoclave
containing lubricating oil and hydroxy fatty acid.
[0020] In the grease composition according to the present invention, use can be made, in
addition to the three components (a), (b) and (c) above, of other metal borates or
other lubricant-additives, such as neutral or basic metallic detergents, such as basic
Ca salicylate, or ashless dispersants, rust inhibitors (e.g., paraffin oxide, amino
imidazoline or barium dinonylnaphthalene-sulphonate), oxidation inhibitors (e.g. 2,6-ditertiary
butyl-4-methylphenol), N-phenyl-a-naphthylamine or diphenylamine octylate) and conventional
extreme-pressure additives (e.g. zinc naphthenate or other zinc compounds such as
zinc dithiophosphates or zinc-oxide, lead naphthenate, sulphurized oils and fats,
or tricresyl phosphate), in the proportions ordinarily employed.
[0021] The present grease compositions can be used, for example, for the lubrication of
the bearings of electric motors as well as of the wheel bearings in automotive bearing/axle
integrated structures.
[0022] In the following, the present greases are further illustrated by means of examples
(the boric acid used was ortho boric acid).
Example 1
[0023] Component (a) was lithium 12-hydroxy stearate, component (b) lithium borate and component
(c) potassium borate.
[0024] This grease was prepared in situ by mixing and heating 9.00 %w of 12-hydroxy stearic
acid, 2.96 %w boric acid, 2.33 %w lithium hydroxide, 0.45 %w potassium hydroxide and
85.26 %w mineral lubricating oil.
Example 2
[0025] As Example 1 except for (c) which was sodium borate.
Example 3
[0026] As Example 1 except for (c) which was calcium borate.
Example 4
[0027] As Example 1 except for (c) which was zinc borate.
[0028] Test results of these greases are shown in the following Table.

1. High dropping-point lithium-ccnplex grease composition having improved extreme
properties, comprising a lubricating oil and the following components:
(a) at least one lithium soap of a C12 to C24 hydroxy fatty acid,
(b) at least one lithium salt of a boric acid, and
(c) at least one metal salt selected from the group consisting of
1) a potassium salt of a boric acid,
2) a sodium salt of a boric acid,
3) an alkaline earth metal salt of a boric acid, and
4) a zinc salt of a boric acid.
2. Composition as claimed in claim 1, wherein the boric acid is ortho boric acid.
3. Composition as claimed in claim 1 or 2, wherein the alkaline earth metal salt is
a calcium, barium or magnesium salt.
4. Composition as claimed in any one of claims 1-3, wherein the proportions per 100
pbw of base oil are:
Component (a) : 2-40 pbw
Component (b): 0.05-20 pbw
Component (c) : 0.05-20 pbw
5. Process for the preparation of a composition according to any one of claims 1-4
comprising mixing and heating together in a lubricating oil a C12 to C24 hydroxy fatty acid, a boric acid, lithium hydroxide and an oxide or a hydroxide from
a metal selected from the group consisting of potassium, sodium, an alkaline earth
metal and zinc.