[0001] This invention relates to a process for the continuous manufacture of a lubricating
grease and in particular of a base grease which serves as a basis for the manufacture
of a wide variety of lubricating grease formulations containing one or more additives.
By first making a base grease a great flexibility is obtained in making a great variety
of grease formulations using the same grease manufacturing basic unit.
[0002] From European patent application 0072184 a process for the continuous manufacture
of a lubricating grease, which process shows a great flexibility, is already known.
According to this process a rotating screw process unit is used.
[0003] It has now been found that such processes, which enable the manufacture of a great
variety of greases, such as the greases described in said European patent application,
can be carried out in a smpler way without the use of moving parts, namely by using
motionless mixers, which are readily commercially available.
[0004] Therefore the present invention relates to a process for the continuous manufacture
of a lubricating grease comprising blending feed materials and lubricating oil and
pumping the resulting blend through at least one motionless mixer which is heated
to such a temperature that soap formation takes place and a resultant grease is formed.
[0005] Suitable feed materials are the usual thickening or gelling agents which in the case
of soaps are often made in situ in at least part of the lubricating oil from saponifiable
material, saponification agents and optionally canplexing agents.
[0006] Suitable saponifiable materials are long chain fatty esters, especially glycerides,
in particular where the fatty group contains a hydroxy radical, such as ricinoleyl
(castor oil) or hydrogenated ricinoleyl (hydrogenated castor oil).
[0007] Another method of soap formation is to neutralize fatty acids or hydroxy fatty acids
in mineral oil with alkali metal or alkaline earth metal hydroxides (or mixtures of
both) or hydrates thereof - in particular lithium hydroxide monohydrate (LiOH.H
2O). Alternatively hydrogenated fatty acids or hydrogenated hydroxy fatty acids are
commonly used in the neutralization.
[0008] Suitable saponification agents are alkali metal or alkaline earth metal hydroxides
(or mixtures of both), in particular lithium hydroxide, or hydrates thereof. Therefore,
the feed materials preferably comprise
a) hydrogenated castor oil (HCO) and lithium hydroxide or lithium hydroxide monohydrate;
b) HCO and lithium hydroxide (or monohydrate) or calcium hydroxide;
c) Hydrogenated castor oil fatty acid (HCOFA) and lithium hydroxide or lithium hydroxide
monohydrate; and/or
d) . HCOFA and lithium hydroxide (or monohydrate) or calcium hydroxide.
[0009] Suitable complexing agents are short chain fatty acids, such as acetic acid, dicarboxylic
acids, such as azelaic acid, hydroxy aromatic acids such as salicylic acid, boric
acid, aluminium compounds, etc. If such complexing agents are used the proportion
of saponification agents is usually increased with about the stoichiometric quantity
of the complexing agent.
[0010] Other suitable thickening agents are clays, including coated clays, silica gels,
polymers, polyureas, carbon black, dyes, etc.
[0011] Suitable lubricating oils are mineral oils, including hydrogenated mineral oils,
synthetic oils, such as ester oils, polyolefin oils, silicon oils, phosphate esters,
polyphenyl ethers, etc. Suitable mineral lubricating oils include HVI, paraffinic
MVI, naphthenic MVI and LVI oils.
[0012] To the base greases may be added additional lubricating oil and additives, such as
antioxidants, anti-rust, anti-wear and extreme pressure agents, pour point depressants,
metal deactivators etc.
[0013] Suitable laboratory-type motionless or static mixers have the form of a cylinder
or tube having a length of 65.5 to 66.5 cm and a diameter of 3.3 to 3.6 cm. They are
provided with an insulated heating jacket, using e.g. electric tape having a heating
capacity of e.g. 400 watt per mixer, or a heating medium as the heating source. The
inside of the cylinder is provided with e.g. vanes, corrugated plates, perforated
plates, intermeshing and intersecting bars and similar fixed mechanical obstacles
causing mixing and heat exchange. A suitable motionless mixer containing perforated
plates is described in e.g. British patent specification 2086249, but other types
may be used as well.
[0014] Suitable mixers are: the Sulzer motionless mixer SMX type which is 655 mm long x
36 mm internal diameter and the Sulzer motionless heat exchanger SMXL type which is
665 mm long x 32.8 mn internal diameter.
[0015] For commercial production the sizes of the mixers require scaling up.
[0016] According to the present process the base grease-making ingredients are preferably
blended at room temperature in a container from which they are pumped through at least
one motionless mixer, preferably several motionless mixers, preferably longitudinally
connected. They may also be, or additionally be, connected in a parallel manner.
[0017] The average velocity of the mixture in the mixers may be 3 kg to 50 kg/h, preferably
7 to 30 kg/h, the flow preferably being laminar.
[0018] The pressure at the entrance of the first mixer may be between 1 and 30 bar, preferably
between 1 and 15 bar.
[0019] The mixers are heated to a suitable high temperature, e.g. at least 120 °C, preferably
between 120 and 250 °C, preferably up to a maximum temperature between 180 and 230
°C, so that a grease structure is formed on cooling. Preferably the temperature of
each of the heated mixers is higher than that of the preceding mixer and so on.
[0020] Thermocouples may be placed between the mixers for temperature control.
[0021] If desired part of the finished grease may be recycled. Also the pump at the entrance
of the first mixer may be provided with a recycling circuit.
[0022] The subsequent removal of water can be accomplished by simply dumping the resulting
grease in an open vessel, whereafter any further lubricating oil and any desired additives
can be added.
[0023] Due to condensation some water may be present in the open vessel. If required complete
dehydration may be accomplished using conventional flash vacuum equipment.
[0024] Preferably the base grease together with additional lubricating oil and additives
is pumped through a heat exchanger tube for mixing and cooling to obtain the desired
consistency.
[0025] Homogenisation of the grease, if necessary, is carried out using e.g. a Manton Gaulin
hcnogeniser at 3000 psig (20.7 MPa), a mill or a rolling device etc.
[0026] The invention is illustrated by the following Examples.
EXAMPLE 1
1.3 kg feed containing:
12 %w hydrogenated castor oil
1.7 %w LiOH.H2O
[0027] 86.3 %w mineral lubricating oil (HVI, viscosity 10.7-11.8 cSt at 100 °C, VI =
96 (min), and 3 %w (= 39 g) water is mixed at room temperature for at least 10 minutes
in a container and then pumped at a flow rate of 8.3 kg/h once through a series of
4 Sulzer motionless mixers (each unit containing 2 mixing elements) which are beforehand
adjusted to temperatures of 130, 170, 190 and 230 °C, respectively, by 4 200 watt
electric heaters per mixer.
[0028] The finished grease is obtained at the outlet and cooled in a jacketed SULZER MONOTUBE
HEAT EXCHANGER which consists of 2 units each 1540 mm long x 32.8 mm internal diameter.
Each unit contains 1 SMXL type heat exchanger. The unworked/worked penetration at
25 °C was 262/273 dmm (ASTM D217-82) (1 dmm corresponds with 0.1 mm) and the dropping
point was 197 °C. (Worked penetration is the penetration at 25 °C after 60 double
strokes in a standard grease worker).
[0029] The first two Sulzer mixers were of the type SMX DN32, having a length of 655 mm
and an internal diameter of 36 mm and the last two were of the type SMXL DN32 (heat
exchanger type for boosting the heat transfer during warming up of the viscous mixture),
having a length of 665 mm and an internal diameter of 32.8 mm.
[0030] Subsequently the water present in the grease was flashed off.
[0031] Examples 2-6 are carried out in the arrangement of Example 1, but the flow rate is
changed, resulting in different outlet temperatures, penetrations and dropping points
(see Table A).

1. A process for the continuous manufacture of a lubricating grease comprising blending
feed materials and lubricating oil and pumping the resulting blend through at least
one motionless mixer which is heated to such a temperature that soap formation takes
place and a resultant grease is formed.
2. A process according to claim 1, wherein the blending of feed materials and lubricating
oil is carried out at room temperature.
3. A process according to claim 1 or 2, wherein the feed materials comprise
a) hydrogenated castor oil (HCO) and lithium hydroxide or lithium hydroxide monohydrate;
b) HCO and lithium hydroxide (or monohydrate) or calcium hydroxide;
c) Hydrogenated castor oil fatty acid (HCOFA) and lithium hydroxide or lithium hydroxide
monohydrate; and/or
d) HCOFA and lithium hydroxide (or monohydrate) or calcium hydroxide.
4. A process according to any one of claims 1-3, wherein a series of heated motionless
mixers is used, each mixer having a higher temperature than the preceding one.
5. A process according to any one of claims 1-4, wherein the motionless mixers have
vanes.
6. A process according to any one of claims 1-5, wherein the mixers are heated to
a temperature between 120 and 250 °C.
7. A process according to any one of claims 1-6, wherein the resulting grease is cooled
in a heat exchanger tube.
8. A process according to any one of claims 1-7, wherein to the resulting grease additional
lubricating oil and additives are added.
9. A process according to claim 1, substantially as hereinbefore described.
10. A lubricating grease whenever prepared, according to a process as claimed in any
one of claims 1-9.