Case No. 500050(2)
METHOD OF PREPARING A LUBRICANT COMPOSITION
This invention relates to a method of preparing a lubricant composition and in
particular to a method of preparing a lubricant composition comprising a mixture of at least
I one base oil component, at least one first additive component and at least one second
i 5 additive component.
Lubricant compositions comprising at least one base oil component and one or more
additive components are usually prepared in batch processes. Batch processes for the
1 preparation of lubricant compositions usually involve introducing at least one base oil
component and one or more additive components into a vessel and mixing the components
10 using an agitator, paddle stirrer or the like. Batch processes usually require the use of large
inventories of components in the vessel to achieve commercially acceptable production
rates. This may present problems associated with the energy consumption required for
mixing with stirrers, paddles or the like. Large inventories of components may also
present safety issues andlor cost implications. Large inventories of components may
15 require large feed lines from component storage to a mixing vessel. Large feed lines may
require flushing between production batches and this may contribute to potential waste.
Also, large feed lines may require heating. L
It is desirable that a prepared lubricant composition is clear and bright and does not
contain solids, gels or the like. It has been found that when preparing a lubricant
20 composition comprising a mixture of at least one base oil component, at least one first
additive and at least one second additive, incompatibility of some or all of the additive
components may result in the undesirable formation in the composition of solids, gels or
the like. Therefore, in batch processes, the sequence of introducing the components into a
mixing/reaction vessel and/or the duration of mixing between introductions of components
25 is usually controlled to provide adequate mixing of the components and in particular to
reduce or mitigate the risk of solids, gels or the like forming during the preparation of the
lubricant composition. This may require extended periods of mixing.
Static mixers (sometimes called static mixing devices or motionless mixing devices)
are known. For example, according to trade brochure
30 http://www.chernineer.comlimaaes/pdf/bulletin 800.pdf dated 201 1, ~enics@Sta tic
Mixers available from Chemineer Inc. Ohio, USA include helical mixing elements which
direct the flow of material radially towards the pipe walls and back to the centre.
Case No. 500050(2) 2
Ir
According to the brochure, typical applications in petrochemical and refining are blending
gaseous reactants, washing hydrocarbon streams, gas scrubbing, lube oil blending and
crude oil sampling.
US patent US3953002 relates to mixing devices for intermixing of a plurality of
5 fluids, and more specifically to motionless type mixing devices which do not employ
moving parts. US3953002 relates to a mixing device for intermixing a plurality of fluids
which comprises a housing having a cylindrical bore through which the fluids may flow
and a diffuser link supported centrally 'within the housing bore. The mixing device is said
to further comprise a right-hand helical baffle secured to one end of the diffusal link and a
10 left-hand helical baffle secured to the other end of the diffusal link.
In US3953002, one embodiment is said to include a means for introducing trace
additives into the device. The trace introductory means is said to include a tubular element
which transverses the tubular housing of the device and is plugged at one end by a cap. In
Figure 5 thereof only a single tubular element is shown. The tube is said to comprise two
15 or more substantially parallel slots located about opposite sides of the axis of the tubular
housing and the helical baffle. It is stated that with this configuration trace additives may
be introduced into the housing. The fluids are said to enter through the slots ahd are
caused to swirl in opposite directions and change directions of flow as they encounter the
adjacent baffle, which is said to result in excellent intermixing.
20 There remains a need for a method of preparing a lubricant composition which
overcomes, or at least mitigates at least some of these problems.
Thus, according to the present invention there is provided a method of preparing a
lubricant composition comprising at least one base oil component, at least one first additive
component and at least one second additive component which method comprises:
25 introducing into an elongate mixing vessel comprising at least one static mixer, at least one
base oil component, at least one first additive component and at least one second
additive component; the at least one first additive component being introduced into
the mixing vessel separately from the at least one second additive component; and
mixing the at least one second additive component with a mixture of the at least one first
3 0 additive component and the at least one base oil component in the elongate mixing
vessel using the at least one static mixer.
Case No. 500050(2) 3
The present invention reduces or at least mitigates at least some of the technical
problems identified above by providing a method of preparing a lubricant composition by
introducing at least one first additive component and at least one second additive
component separately from each other into a mixing vessel which is an elongate mixing
5 vessel comprising at least one static mixer. The first and second additive components are
not introduced into the mixing vessel together.
The at least one second additive component is mixed in the elongate mixing vessel
with a mixture of the at least one first additive component and the at least one base oil
component using the at least one static mixer. This reduces or mitigates the risk of solid,
10 gels or the like forming in the lubricant composition, for example due to incompatibility
between the first and second additive components, especially for example, when the first
additive component(s) and the second additive component(s) are mixed together at high
relative amounts and/or concentrations, and/or even in neat, undiluted form.
Furthermore, the use of an elongate mixing vessel comprising at least one static
15 mixer facilitates the use of smaller inventories of components which may reduce the
energy costs of the mixing process and/or reduce the costs of component inventories
compared to a batch process using for example, a mixing vessel comprising stmer, paddle
or the like.
The method may permit the use of mixing vessels which are smaller than mixing
20 vessels used in conventional batch mixing processes and this may provide an opportunity
to use mixing vessels each dedicated to the production of one or a few lubricant
compositions. This may reduce or obviate the need for feed line and/or mixing vessel
flushing, which may reduce potential waste when preparing several different lubricant
compositions.
25 The method may permit the use of feed lines with small inventories and this may (i)
reduce potential waste fiom flushing between production batches andlor (ii) reduce the cost
of heating the feed lines.
The use of static mixers in the mixing vessel may reduce or obviate any requirement
to heat the mixing vessel.
3 0 The extent of mixing of the at least one second additive component and the mixture
of at least one base oil component and the at least one first additive component may be
Case No. 500050(2)
controlled by adjusting the flow rate of components through the mixing vessel and/or the
configuration and/or type of static mixers in the mixing vessel.
In a first aspect, the at least one base oil component and the at least one first additive
component are introduced as a mixture of the at least one base oil component and the at
5 least one first additive component. This mixture is introduced into the mixing vessel
through the at least one first inlet.
Thus according to at least some embodiments, the mixing vessel is an elongate
mixing vessel comprising at least one first static mixer, at least one first inlet which is
upstream of the at least one first static mixer, at least one second inlet which is upstream of
10 the at least one first static mixer and at least one outlet which is downstream of the at least
one static mixer and the method comprises the steps of:
a) introducing a mixture of the at least one base oil component and the at least one first
additive component into the mixing vessel through the at least one first inlet;
b) introducing the at least one second additive component into the mixing vessel through
15 the at least one second inlet upstream of the at least one first static mixer;
c) flowing the at least one second additive component and the mixture of step a, through
the mixing vessel and past the at least one first static mixer to mix the at least bne second
additive component with the mixture of step a to produce a mixture of the at least one base
oil component, the at least one first additive component and the at least one second
20 additive component; and
d) removing the mixture produced in step c fiom the mixing vessel through the at least one
outlet downstream of the first static mixer.
The mixture of the at least one base oil component and the at least one first additive
component may be prepared by mixing the components in a mixing vessel before being
25 introduced as a mixture into the elongate mixing vessel through the at least one first inlet.
The mixture of the at least one base oil component and the at least one first additive
component may be prepared by circulating the at least one base oil component through a
mixing vessel, introducing into said mixing vessel the at least one first additive component
and mixing the components in said mixing vessel with or without the use of at least one
30 static mixer.
Case No. 500050(2)
In a second aspect, the at least one base oil component and one first additive
component are mixed together in the elongate mixing vessel before the resulting mixture is
mixed with the at least one second additive.
Thus, according to at least some embodiments, the mixing vessel is an elongate
5 mixing vessel comprising at least one first static mixer, at least one first inlet which is
upstream of the at least one first static mixer, at least one second inlet which is upstream of
the at least one first static mixer, at least one third inlet which is upstream of the at least
one first static mixer and is upstream of the at least one second inlet and at least one outlet
which is downstream of the at least one static mixer;
10 and in which the method comprises the steps of:
a') introducing the at least one base oil component into the mixing vessel through the at
least one first inlet, introducing the at least one first additive component into the mixing
vessel through the at least one third inlet and mixing together the at least one base oil
component and the at least one first additive component in the mixing vessel to produce a
15 mixture of the at least one base oil component and the at least one first additive
component;
b') introducing the at least one second additive component into the mixing vissel through
the at least one second inlet upstream of the at least one first static mixer;
i c') flowing the at least one second additive component and the mixture from step a',
20 through the mixing vessel and past the at least one first static mixer to mix the at least one
second additive component with the mixture from step a to produce a mixture of the at
U least one base oil component, the at least one first additive component and the at least one
second additive component; and
d') removing the mixture produced in step c' from the mixing vessel through the at least
25 one outlet downstream of the first static mixer.
According to at least some embodiments the at least one first inlet is upstream of the
at least one third inlet.
According to at least some embodiments the at least one third inlet is upstream of the
at least one first inlet.
3 0 According to at least some embodiments, mixing in step a', of the at least one base
oil component and the at least one first additive in the mixing vessel is undertaken using at
least one second static mixer in the mixing vessel. Thus, according to at least some
Case No. 500050(2) 6
embodiments, the elongate mixing vessel further comprises at least one second static mixer
which is upstream of the at least one first static mixer, is upstream of the at least one
second inlet, is downstream of the at least one first inlet and is downstream of the at least
one third inlet and in step a', the method comprises mixing together the at least one base
5 oil component and the at least one first additive component in the mixing vessel by flowing
them through the mixing vessel and past the at least one second static mixer to produce a
mixture of the at least one base oil component and the at least one first additive
component.
Mixing of the at least one base oil component and the at least one first additive
10 component by the at least one second static mixer disburses the at least one first additive
component in the at least one base oil component so that when the at least one second
additive component is introduced into the mixing vessel, the risk of forming solids, gels or
the like in the lubricating oil composition is reduced or mitigated. Thus, this embodiment
has an advantage that a static mixer can be used to achieve adequate mixing of the at least
15 one first additive component with the at least one base oil before mixing with the at least
one second additive component. This can reduce or mitigate the risk of forming solids,
gels or the like in the lubricating oil composition, for example, if the first and iecond
additive components have a tendency to form solids, gels or the like on mixing. The extent
of mixing of the at least one base oil component and the at least one first additive
20 component may be controlled by adjusting the flow rate of components through the mixing
vessel and/or the configuration and/or type of static mixers in the mixing vessel.
The mixing vessel may comprise more than one first inlet.
In at least some embodiments, the at least one first inlet is located at one end of the
mixing vessel. In at least some embodiments, the at least one first inlet is located at one
25 end of the mixing vessel and the at least one base oil component is introduced into the
mixing vessel through the at least one first inlet in the direction of the longitudinal axis of
the elongate mixing vessel.
The mixing vessel may comprise more than one second inlet.
In at least some embodiments, the at least one second additive component is
30 introduced into the mixing vessel through the at least one second inlet in a direction which
has a component perpendicular to the direction of longitudinal axis of the elongate mixing
vessel. In at least some embodiments, the at least one second additive component is
y*+: -
Case No. 500050(2) 7
introduced into the mixing vessel through the at least one second inlet in a direction which
is perpendicular to the direction of longitudinal axis of the elongate mixing vessel.
In at least some embodiments, when introduced into the mixing vessel separately
fiom the at least one base oil component, the at least one first additive component is
5 introduced into the mixing vessel through the at least one third inlet in a direction which
has a component perpendicular to the direction of the longitudinal axis of the elongate
mixing vessel. In at least some embodiments, when introduced into the mixing vessel
separately fiom the at least one base oil component, the at least one first additive
component is introduced into the mixing vessel through the at least one third inlet in a
10 direction is perpendicular to the direction of the longitudinal axis of the elongate mixing
vessel.
By introducing the additive components into the mixing vessel in a direction which
has a component perpendicular to the direction of the longitudinal axis of the vessel or
which is perpendicular to the direction of the longitudinal axis of the elongate mixing
15 vessel, the additive components, which may have a viscosity greater than that of the
components andlor mixture flowing through the mixing vessel, may be efficiently mixed
therewith. L
In at least some embodiments, the at least one outlet is located at one end of the
elongate mixing vessel distal from the end of the elongate mixing vessel comprising the at
20 least one first inlet. The mixing vessel may comprise more than one outlet.
The mixing vessel may comprise more than one first static mixer. The mixing vessel
may comprise more than one second static mixer.
The mixing vessel may additionally comprise at least one fourth inlet and at least one
third static mixer downstream thereof. This combination of at least one fourth inlet and at
25 least one third static mixer may be located downstream of the at least one first static mixer.
Additionally or alternatively, a combination of at least one fourth inlet and at least one
third static mixer downstream thereof, may be located upstream of the at least one third
inlet. Additionally or alternatively, a combination of at least one fourth inlet and at least
one third static mixer downstream thereof may be located downstream of the at least one
30 second static mixer and upstream of the second inlet. In the method of the present
invention at least one additive component may be introduced into the mixing vessel
Case No. 500050(2) 8
through the at least one fourth inlet and passed by the at least one third static mixer thereby
to be mixed with the components and/or mixtures flowing through the mixing vessel.
In at least some embodiments, the at least one additive component is introduced into
the mixing vessel through the at least one third inlet in a direction which has a component
5 which is perpendicular to the longitudinal axis of the elongate mixing vessel, for example
in a direction which is perpendicular to the longitudinal axis of the elongate mixing vessel.
By introducing the additive components into the mixing vessel in a direction which has a
component which is perpendicular to, the direction of the longitudinal axis of the vessel,
the additive components, which may have a viscosity greater than that of the components
10 and/or mixture flowing through the mixing vessel, may be efficiently mixed therewith.
According to at least some embodiments, mixing of additive components which are
introduced into the elongate mixing chamber with components and/or mixture flowing
through the elongate mixing chamber may be facilitated by using at least one narrow bore
inlet. This may provide a velocity of the additive components which is greater than that
15 which is achieved using a broader bore inlet, which may enhance or facilitate mixing.
However, using a narrow bore inlet may increase the energy requirement and hence cost of
pumping the additive component(s) into the elongate mixing chamber. ~dditibnalolr~
alternatively, increasing longitudinal distance along the elongate mixing chamber between
two or more static mixers may enhance or facilitate mixing of components.
20 In at least some embodiments the at least third additive component is mixed in the
mixing vessel with the at least one base oil component, the at least one first additive
components and the at least one second additive component in the mixing vessel by
flowing the components through the mixing vessel and past the at least one third static
mixer at a temperature which is different to the temperature at which the components are
I 25 flowed past the at least one first static mixer which is different to the temperature the
I components are flowed past the at least one second static mixer, if present. This may be
L
beneficial in at least some embodiments for example, when the at least one third additive
which is introduced into the mixing vessel through the at least one fourth inlet comprises at
least one zinc dihydrocarbyl dithiophosphate (ZDDP). Generally, ZDDP's should be used
30 in processes for the preparation of lubricant compositions at temperatures less than 60°C.
At temperatures of 60°C or above ZDDP's may decompose to produce hydrogen sulphide.
Thus, in at least some embodiments when the at least one third additive which is
Case No. 500050(2) 9
introduced into the mixing vessel through the at least one fourth inlet comprises at least
one zinc dihydrocarbyl dithiophosphate the at least third additive component is mixed in
the mixing vessel with the at least one base oil component, the at least one first additive
components and the at least one second additive component in the mixing vessel by
5 flowing the components through the mixing vessel and past the at least one third static
mixer at a temperature which is less than 60°C, for example less than 55°C or less than
50°C. The temperature may be in the range of 20 to 55"C, for example in the range of 25
to 35 "C.
Additive components other than ZDDP's may be used in processes for the
10 preparation of lubricant compositions at temperatures up to 300°C for example, up to
200°C. Additive components other than ZDDP's may be used in processes for the
preparation of lubricant compositions at temperatures in the range of ambient temperature
to 300°C, for example in the range of ambient temperature to 200°C. Ambient temperature
may be about 10 to 40 "C, for example about 20 to 30 "C.
The components other than ZDDP's may be flowed through the elongate mixing
vessel at temperatures up to 300°C for example, up to 200°C. Additive components other
than ZDDP's may be flowed through the elongate mixing vessel at tempera&s in the
range of ambient temperature to 30O0C, for example in the range of ambient temperature to
200°C. Ambient temperature may be about 10 to 40 "C, for example about 20 to 30 "C.
Thus, in at least some embodiments zinc dihydrocarbyl thiophosphates (ZDDP's) is
mixed with the components of the lubricant composition at a temperature which is lower
than the temperature at which other components (for example dispersants andlor metalcontaining
detergents) are mixed with the components of the lubricant composition.
Thus, according to at least some embodiments the elongate mixing vessel comprises
at least one fourth inlet downstream of the at least one first static mixer and at least one
third static mixer which is downstream of the at least one first static mixer and which is
downstream of the at least one fourth inlet, and the method fkrther comprises introducing
at least one third additive component which comprises at least one zinc dihydrocarbyl
dithiophosphate, into the mixing vessel through the at least one fourth inlet; and mixing the
at least one third additive component in the mixing vessel with the at least one base oil
component, the at least one.first additive component and the at least one second additive
component in the mixing vessel by flowing them through the mixing vessel and past the at
Case No. 500050(2) 10
least one third static mixer at a temperature which is different to the temperature at which
the components are flowed past the at least one first static mixer and which is different to
the temperature at which the components are flowed past the at least one second static
mixer, if present, to produce a mixture of the at least one base oil component and the at
5 least one first additive component, the at least one second additive component and the at '
least one third additive component.
The mixing vessel may comprise more than one first static mixer. The mixing vessel
may comprise more than one second static mixer. The mixing vessel may comprise more
than one third static mixer.
10 The mixing vessel may comprise at least one additional static mixer. This at least
one additional static mixer may be located upstream of the at least one second inlet. In use
in the method of the present invention this further static mixer introduces turbulent flow
into the mixture of at least one base oil component and at least one first additive
component prior to mixing with the at least one second additive in the first static mixer.
15 This at least one additional static mixer may be located downstream of the at least one first
inlet and upstream of the at least one third inlet. In use in the method of the present
invention this further static mixer introduces turbulent flow into the at least oie base oil
component prior to mixing with the at least one first additive in the at least one second
static mixer.
20 The elongate mixing vessel may be cylindrical. The elongate mixing vessel may
have a circular transverse cross-section. The elongate mixing vessel may be cylindrical
with a circular transverse cross-section. The elongate mixing vessel may have a uniform
'4 transverse cross-section. The elongate mixing vessel may be cylindrical with a uniform,
circular transverse cross-section.
25 In at least some embodiments the elongate mixing vessel has a circular transverse
cross-section which has a diameter of at least lmm, for example at least 5mm or at least
1 Omm. In at least some embodiments the elongate mixing vessel has a circular transverse
cross-section which has a diameter of up to 100 mm. In at least some embodiments the
elongate mixing vessel has a circular transverse cross-section which has a diameter of
I
I 3 0 lmm to 1 OOrnm, for example 10 mm to 100mm.
The elongate mixing vessel may have a transverse cross-section which is other than
circular, for example an oval transverse cross section.
:*
*.Jt,??-; -
Case No. 500050(2)
The elongate mixing vessel may have a non-uniform cross-section. The non-uniform
cross-section may vary continuously along the axis of the elongate mixing vessel. The nonuniform
cross-section may vary discontinuously along the axis of the elongate mixing
vessel.
5 In at least some embodiments, the elongate mixing vessel is cylindrical with a
uniform, circular transverse cross-section.
In at least some embodiments, the elongate mixing vessel has a length of at least
lOmm, for example at least 100mm. 1; at least some embodiments, the elongate mixing
vessel has a length of up to 5000mrn, for example up to 1000mm. In at least some
10 embodiments, the elongate mixing vessel has a length of 10mm to 5000mm, for example
1 OOmm to 1000mm, typically 300mm.
In at least some embodiments, the elongate mixing vessel is cylindrical with a length
of 10mm to 5000mm, for example 100mm to lOOOmrn and having a uniform, circular
transverse cross-section with a diameter of lmm to 1 OOmrn, for example 10mm to 100mm.
15 In at least some embodiments more than one elongate mixing vessel is used. When
more than one elongate mixing vessel is used, the elongate mixing vessels may be used in
parallel and/or in series. 1
In at least some embodiments the components are recirculated through the elongate
mixing vessel.
20 The static mixers may each independently comprise a discontinuous, non-uniform
cross-section of the elongate mixing vessel. A discontinuous, non-uniform cross-section
may provide at least one shearing boundary to induce turbulent flow of mixtures andlor
components flowing through the mixing vessel to thereby mix them.
The static mixers may each independently comprise at least one passage for
25 components in the direction of the longitudinal axis of the elongate mixing chamber, each
passage having a discontinuous, non-uniform cross-section. A discontinuous, non-uniform
cross-section may provide at least one shearing boundary to induce turbulent flow of
mixtures andlor components flowing through the mixing vessel to thereby mix them.
Such passages may be provided by one or more plugs which are located along the
30 longitudinal axis of the elongate mixing vessel.
The static mixers may each independently comprise a plate having at least one orifice
and/or slot and being located transverse to the longitudinal axis of the elongate mixing
Case No. 500050(2) 12
vessel. The at least one orifice provides at least one shearing boundary surface to induce
turbulent flow of components andfor mixtures flowing through the mixing vessel to
thereby mix them.
The static mixers may each independently comprise one or more baffles. Suitable
5 baffles include motionless mixing devices for example as described in US3953002 in
particular a motionless mixing device comprising a diffusion link supported centrally
within a housing bore, and fbrther comprising a right-hand helical baffle secured to one
end of the difisal link a d a left-hand helical baffle secured to the other end of the diffusal
link. Suitable motionless mixing devices include ~enics@Sta tic Mixers which are
10 available from Chemineer Inc, Ohio USA. Suitable static mixers may comprise helical
static mixers.
The method may further comprise rotating the elongate mixing vessel about its
longitudinal axis. This may be beneficial in aiding mixing of components which have
i
I largely differing densities, which may facilitate higher throughputs.
15 In at least some embodiments, the method is performed at a pressure in the range of
atmospheric to 10 bag. The operating temperature may be determined by the operating
pressure of the mixing vessel. 1
In at least some embodiments the pressure drop between the inlets and outlets of the
elongate mixing vessel is up to 5 bar, for example in the range of 1 to 3 bar.
20 In at least some embodiments the total flow rate of the components through one or
more mixing vessels is up to 1000 litres per minute.
In at least some embodiments the total flow rate of the components through the
mixing vessel is at least 10 litres per minute, for example at least 20 litres per minute, at
least 50 litres per minute or at least 100 litres per minute.
25 In at least some embodiments the total flow rate of the components through the
mixing vessel is in the range of 1 litre per minute to 150 litres per minute. In at least some
embodiments the total flow rate of the components through the mixing vessel is in the
range of 3 litres per minute to 40 litres per minute.
A conventional large batch method for preparing a lubricant composition might use a
30 26000 litre mixing vessel and a mixing time of 6 hours, which corresponds to only 72 litres
per minute. The elongate mixing vessel on the other hand, may have a volume of less than
about 1 litre, for example about 500ml. Thus, the use of an elongate mixing vessel
Case No. 500050(2) 13
comprising at least one static mixer facilitates the use of smaller inventories of components
which may reduce the energy costs of the mixing process and/or reduce the costs of
component inventories compared to a batch process using for example, a mixing vessel
comprising stirrer, paddle or the like.
5 In at least some embodiments the total residence time of all the components in the
elongate mixing vessel is less than about 1 minute, for example about 2 to 10 seconds. The
flow rate and residence time will depend upon the time required to mix the components to
the desired amount.
Usually the flow rate of components through the elongate mixing vessel is a uniform
10 flow rate, but other flow patterns may be used.
The ratio of cross section to length of the elongate mixing vessel is such that it may
facilitate heat exchange tolfiom the components, for example to heat or cool the
components andor mixtures thereof.
More than one mixing vessel may be used in the method of the present invention.
15 The multiple mixing vessels may be used in parallel or in sequence or in a combination
arrangement of both parallel and sequential mixing vessels.
The relatively small size of the elongate mixing vessel compared to con$entional
batch stirred mixing vessels means that several such elongate mixing vessels may be used
in a manufacturing site in an area equivalent to a large conventional stirred mixing vessel.
20 This may have an advantage of facilitating the use of dedicated mixing vessels to
preparation of particular lubricant compositions or classes of lubricant compositions,
thereby reducing equipment turnaround times and costs of cleaning and the like.
Suitable base oil components may be base stocks defined as Group I, 11,111, IV and V
base stocks according to API standard 1509, "ENGINE OIL LICENSING AND
25 CERTIFICATION SYSTEM", April 2007 version 16'~ed ition Appendix E.
Group I, Group I1 and Group 111 base stocks may be derived from mineral oils. Group
I base stocks are typically manufactured by known processes comprising solvent extraction
and solvent dewaxing, or solvent extraction and catalytic dewaxing. Group I1 and Group
I11 base stocks are typically manufactured by known processes comprising catalytic
30 hydrogenation andlor catalytic hydrocracking, and catalytic hydroisomerisation. Suitable
Group I and Group I1 base stocks are available from Indian Oil Corporation Limited
(IOCL), Hindustan Petroleum Corp. Ltd. (HPCL) or Exxon. Suitable group I11 base stocks
Case No. 500050(2) 14
include Yubase 4 and Yubase 6 available for example, from SK Lubricant. Suitable Group
V base stocks include for example ester base stocks. Suitable Group IV base stocks
include hydrogenated oligomers of alpha olefins. The oligomers may be made by free
radical processes, Zeigler catalysis or by cationic Friedel-Crafts catalysis. Polyalpha olefin
5 base stocks may be derived from C8, C 1 0, C 12, C 14 olefins and mixtures of one or more
thereof.
Suitable base oil components include natural oils, mineral oils (sometimes called
petroleum-derived oils or petroleum-derived mineral oils), non-mineral oils and mixtures
thereof. Natural oils include animal oils, fish oils, and vegetable oils. Mineral oils include
10 paraffinic oils, naphthenic oils and paraffinic-naphthenic oils. Mineral oils may also
include oils derived from coal or shale.
Suitable base oil components may be derived from processes such as chemical
combination of simpler or smaller molecules into larger or more complex molecules (for
example polymerisation, oligomerisation, condensation, alkylation, acylation).
15 Suitable base oil components may be derived from gas-to-liquids materials, coal-toliquids
materials, biomass-to-liquids materials and combinations thereof.
Gas-to-liquids materials (sometimes also referred to as GTL materials) may be
obtained by one or more process steps of synthesis, combination, transformation,
rearrangement, degradation and combinations of two or more thereof applied to gaseous
20 carbon-containing compounds. GTL derived base oil components may be obtained from
the Fischer-Tropsch synthesis process in which synthesis gas comprising a mixture of
hydrogen and carbon monoxide is catalytically converted to hydrocarbons, usually waxy
hydrocarbons that are generally converted to lower-boiling materials hydroisomerisation
and/or dewaxing (see for example, WO 200811 241 91).
2 5 Biomass-to-liquids materials (sometimes also referred to as BTL materials) may be
manufactured from compounds of plant origin for example by hydrogenation of carboxylic
acids or triglycerides to produce linear paraffins, followed by hydroisomerisation to
produced branched paraffins (see for example, WO-2007-068799-A).
Coal-to-liquids materials may be made by gasifying coal to make synthesis gas which
30 is then converted to hydrocarbons.
The at least one base oil component may have a kinematic viscosity at 100 O C in the
range of 2 to 100 cSt, for example in the range of 3 to 50 cSt or in the range 3.5 to 25 cSt.
Case No. 500050(2) 15
A further apect of the invention provides a method of preparing a lubricant
composition comprising at least one base oil component, the at least one base oil
component having a kinematic viscosity at 1 OO'C in the range of 2 to 100 cSt, the lubricant
composition comprising at least one first additive component and at least one second
5 additive component which method comprises:
introducing into an elongate mixing vessel comprising at least one static mixer, at least one
base oil component, at least one first additive component and at least one second
additive component; the at least one first additive component being introduced into
the mixing vessel separately from the at least one second additive component; and
10 mixing the at least one second additive component with a mixture of the at least one first
additive component and the at least one base oil component in the elongate mixing
vessel using the at least one static mixer.
Pour point depressants and dispersant viscositv modifiers.
It has been found that in some cases when a dispersant viscosity modifier comes
15 into contact with a pour point depressant, a highly viscous mixture may be formed. This
may block inlets to a mixing vessel used to prepare a lubricant composition. In some
cases, gelation may occur and this may result in an unacceptable increase in v;scosity. The
method of the present invention overcomes, or at least mitigates this problem. Thus, in at
least some embodiments the at least one first additive comprises at least one dispersant
20 viscosity modifier and the at least one second additive comprises at least one pour point
depressant.
Alternatively, the at least one first additive comprises at least one pour point
depressant and the at least one second additive comprises at least one dispersant viscosity
modifier.
25 Pour point depressants (also called pour point depressant additives, lube oil
improvers or lube oil flow improvers), lower the minimum temperature at which a
lubricant composition will flow and can be poured. Examples of suitable pour point
depressants include Cs to CIS dialkyl fumaratelvinyl acetate copolymers, methacrylates,
polyacrylates, polyarylamides, polymethacrylates, polyalkyl methacrylates, vinyl
30 fumarates, styrene esters, condensation products of haloparaffin waxes and aromatic
compounds, vinyl carboxylate polymers, terpolyrners of dialkyfumarates, vinyl esters of
fatty acids and ally1 vinyl ethers, wax naphthalene and the like.
Case No. 500050(2) 16
More than one pour point depressant may be used.
Dispersant viscosity modifiers (also called dispersant viscosity modifier additives)
may provide both viscosity index improving properties and dispersancy to a lubricant
composition. Such compounds are also known as dispersant viscosity improver additives
or multifunctional viscosity improvers. Examples of suitable dispersant viscosity modifiers
may be prepared by chemically attaching functional moieties (for example mines,
alcohols and amides) to polymers which tend to have number average molecular weights
of at least 15000, for example in the range 20000 to 600000 (for example as determined by
gel permeation chromatography or light scattering methods). Examples of suitable
dispersant viscosity modifiers and methods of making them are described in WO
9912 1902, WO20031099890, W020061099250, WO2006111663 and W02011/062914.
More than one dispersant viscosity modifier may be used.
The dispersant viscosity modifier may have a Kv100 of about 1000cSt.
The dispersant viscosity modifier may be HiTec5777 (Trade Mark). This is available
from Afton.
Dispersants and metal-containing detergents
It has been found that dispersant additives, for example those with low 6ase number
dispersants, may be difficult to mix with metal-containing detergent additives when
preparing lubricant compositions. This may be due to difficulty in forming the appropriate
sized micelles of detergent in the composition. Thus, in at least some embodiments the at
least one first additive component comprises at least one dispersant and the at least one
second additive component comprises at least one metal-containing detergent, or
alternatively, the at least one first additive component comprises at least one metalcontaining
detergent and the at least one second additive component comprises at least one
dispersant.
Dispersants (also called dispersant additives) help hold solid and liquid contaminants
for example resulting from oxidation of the lubricant composition during use, in
suspension and thus reduce sludge flocculation, precipitation and/or deposition for
example on lubricated surfaces. They generally comprise long-chain hydrocarbons, to
promote oil-solubility, and a polar head capable of associating with material to be
dispersed. Examples of suitable dispersant additive components include oil soluble
polymeric hydrocarbyl backbones each having one or more functional groups which are
Case No. 500050(2) 17
capable of associating with particles to be dispersed. The functional groups may be mine,
alcohol, mine-alcohol, a i d e or ester groups. The fimctional groups may be attached to
the hydrocarbyl backbone through bridging groups. More than one dispersant may be used.
Examples of suitable ashless dispersants include oil soluble salts, esters, aminoesters,
mides, imides and oxazolines of long chain hydrocarbon-substituted mono- and
polycarboxylic acids or anhydrides thereof; thiocarboxylate derivatives of long chain
hydrocarbons; long chain aliphatic hydrocarbons having polyarnine moieties attached
directly thereto; Mannich condensation products formed by condensing a long chain
substituted phenol with formaldehyde and polyalkylene polyamine; Koch reaction products
and the like. Examples of suitable dispersant additive components include derivatives of
long chain hydrocarbyl-substituted carboxylic acids, for example in which the hydrocarbyl
group has a number average molecular weight of up to 20000, for example 300 to 20000,
500 to 10000,700 to 5000 or less than 15000. Examples of suitable dispersant additive
components include hydrocarbyl-substituted succinic acid compounds, for example
succinimide, succinate esters or succinate ester amides and in particular, polyisobutenyl
succinimide dispersants. The dispersants may be borated or non-borated. Dispersant
additive components may be provided in DI (detergent inhibitor) additive packs. DI packs
typically comprise detergent(s), dispersant(s), antiwear additive(s), anti-oxidant(s) and
surfactant(s). Suitable DI packs include for example, Lubrizol890, Lubrizol6406 and
Infineum C9268 (trade marks).
Additionally or alternatively, dispersancy may be provided by polymeric compounds
capable of providing viscosity index improving properties and dispersancy. Such
compounds are generally known as dispersant viscosity improver additives or
multifunctional viscosity improvers. Examples of suitable dispersant viscosity modifiers
are described herein.
More than one dispersant may be used.
The at least one additive component comprising at least one dispersant may have a
viscosity of about 1000 cSt or more. The at least one additive component comprising at
least one dispersant may have a Kv100 of less than 1000cSt, for example of about 5OOcSt.
Detergents (also called detergent additives) may help reduce high temperature
deposit formation for example on pistons in internal combustion engines, including for
example high-temperature varnish and lacquer deposits, by helping to keep finely divided
Case No. 500050(2)
solids in suspension in the lubricating composition. Detergents may also have acidneutralising
properties. Metal-containing detergent comprises at least one metal salt of at
least one organic acid, which is called soap or surfactant. Detergents may be overbased in
which the detergent comprises an excess of metal in relation to the stoichiometric amount
5 required to neutralise the organic acid. The excess metal is usually in the form of a
colloidal dispersion of metal carbonate andlor hydroxide. Examples of suitable metals
include Group I and Group 2 metals, more suitably calcium, magnesium and combinations
thereof, especially calcium. More than one metal may be present.
Examples of suitable organic acids include sulphonic acids, phenols (sulphurised or
10 preferably sulphurised and including for example, phenols with more than one hydroxyl
group, phenols with fused aromatic rings, phenols which have been modified for example
alkylene bridged phenols, and Mannich base-condensed phenols and saligenin-type
phenols, produced for example by reaction of phenol and an aldehyde under basic
conditions) and sulphurised derivatives thereof, and carboxylic acids including for
15 example, aromatic carboxylic acids (for example hydrocarbyl-substituted salicylic acids
and sulphurised derivatives thereof, for example hydrocarbyl substituted salicylic acid and
derivatives thereof). More than one type of organic acid may be present. 1
Examples of suitable metal-containing detergents include 400 BN calcium sulphonate
(e.g. Lubrizol6446, trade mark), 300 BN calcium sulphonate (e.g. Lubrizol6446C, trade
20 mark), 250 BN calcium phenate (e.g. Lubrizol6499, trade mark), 400 TBN magnesium
sulphonate (e.g. Lubrizol6465A, trade mark), 400 BN magnesium sulphonate (e.g.
Infineum C9340, trade mark), 300TBN calcium sulphonate (e.g. Infineum C9330, trade
mark), 300 BN calcium sulphonate (e.g. HiTec 61 1, trade mark) and 400 BN magnesium
sulphonate (e.g. HiTec 7637, trade mark
25 Additionally, non-metallic detergents may be used to prepare the lubricant
composition. Suitable non-metallic detergents are described for example in US762243 1.
More than one detergent may be used.
The at least one additive component comprising at least one metal-containing
detergent may have a viscosity of about 1000 cSt or more. The at least one additive
30 component comprising at least one metal-containing detergent may have a KvlOO of less
than 1000cSt, for example of about 5OOcSt.
Case No. 500050(2) 19
In at least some embodiments, the at least one base oil and the at least one first
component and the at least one second additive component are mixed in the absence of any
zinc dihydrocarbyl dithiophosphate when the at least one first additive component
comprises at least one dispersant and the at least one second additive component comprises
5 at least one metal-containing detergent or when the at least one first additive component
comprises at least one metal-containing detergent and the at least one second additive
component comprises at least one dispersant. In this aspect, mixing of the at least one first
I additive component and the at least one second additive component in the absence of any
I
zinc dialkyl thiophosphate is performed at a temperature different (for example higher)
10 than the temperature at which any zinc dialkyl thiophosphate is subsequently mixed with
the components. The at least one dispersant and the at least one metal-containing detergent
1 may be mixed at a temperature in the range of ambient temperature to 300°C, for example
in the range of ambient temperature to 200°C. Ambient temperature may be about 10 to 40
"C, for example about 20 to 30 "C.
15 In at least some embodiments, the at least one dihydrocarbyl dithiophosphate is
mixed with the other components at a temperature which is not greater than 60°C, for
example less than 55°C or less than 50°C. The at least one dihydrocarbyl dit~ophosphate
may be mixed with the other components at a temperature in the range of 20 to 55"C, for
example in the range of 25 to 35 "C.
20 Thus according to this aspect, the elongate mixing vessel may comprise at least one
fourth inlet downstream of the at least one first static mixer and at least one third static
mixer which is downstream of the at least one first static mixer and is downstream of the at
least one fourth inlet and the method further comprises:
introducing the at least one third additive component into the mixing vessel through
25 the at least one fourth inlet; and
mixing the at least one third additive component in the mixing vessel with the at least
one base oil component, the at least one first additive component and the at least one
second additive component in the mixing vessel by flowing them through the mixing
vessel and past the at least one third static mixer to produce a mixture of the at least
3 0 one base oil component and the at least one first additive component, the at least one
I second additive component and the at least one third additive component.
Case No. 500050(2) 20
In this embodiment, the at least one third additive component may be mixed in the
mixing vessel with the at least one base oil component, the at least one first additive
component and the at least one second additive component in the mixing vessel by flowing
them through the mixing vessel and past the at least one third static mixer at a temperature
5 which is different to the temperature at which the components are flowed past the at least
one first static mixer and which is different to the temperature at which the components are
flowed past the at least one second static mixer, if present.
Thus, the components that are mixed by the at least one third static mixer may be
mixed at a temperature which is not greater than 60°C, for example less than 55°C or less
10 than 50°C. This temperature may be in the range of 20 to 55"C, for example in the range
of 25 to 35 "C.
The components that are mixed by the at least one first static mixer may be mixed at
a temperature in the range of ambient temperature to 300°C, for example in the range of
ambient temperature to 200°C. Ambient temperature may be about 10 to 40 "C, for
15 example about 20 to 30 "C.
The components that are mixed by the at least one second static mixer if present, may
be mixed at a temperature in the range of ambient temperature to 30OoC, for eiample in the
range of ambient temperature to 200°C. Ambient temperature may be about 10 to 40 "C,
for example about 20 to 30 "C.
20 The use of different temperatures for mixing the components by the third static mixer
and the first (and second, if present) mixers has a benefit, for example when the at least
one third additive component comprises at least one zinc dialkyl thiophosphate, of being -
able to operate the first and second static mixers (for example to mix together at least one
dispersant and at least one metal-containing detergent) at a higher temperature than the
25 temperature of operation of the third static mixer, which may be used to mix in at least one
dialkyl thiophosphate. In this way, at least one zinc dialkyl thiophosphate may be mixed
with the other components for example after the dispersant and the metal-containing
detergent have been mixed together, suitably at a higher temperature.
The temperatures of the components may be maintained by the use of one or more
30 heat exchangers which may be external to the elongate mixing vessel. The heat
exchangers may introduce heat into the components as they are mixed by the respective
static mixers and/or may remove heat from the components if the mixing is exothermic.
Case No. 500050(2) * Zinc dihydrocarbyl dithiophosphates are often referred to as ZDDP's. The ZDDP's
may comprise hydrocarbyl groups independently having 1 to 18 carbon atoms, suitably 2
to 13 carbon atoms or 3 to 18 carbon atoms, more suitably 2 to 12 carbon atoms or 3 to 13
carbon atoms, for example 3 to 8 carbon atoms. Examples of suitable hydrocarbyl groups
5 include alkyl, cycloalkyl and alkaryl groups which may contain ether or ester linkages and
also which may contain substituent groups for example, halogen or nitro groups. The
hydrocarbyl groups may be alkyl groups which are linear andor branched and suitably
may have from 3 to 8 carbon atoms. Particularly suitable ZDDP's have hydrocarbyl
groups which are a mixture of secondary alkyl groups and primary alkyl groups for
10 example, 90 mol. % secondary alkyl groups and 10 mol. % primary alkyl groups.
Detergents and Detergent Boosters
When preparing a lubricant composition by mixing at least one base oil component
with at least one additive component comprising at least one detergent (for example metalcontaining
detergent) and at least one additive component comprising at least one detergent
15 booster haziness of the mixture might result if the first and second additive components are
not introduced into the mixture in a correct sequence.
Thus, in at least some embodiments, the at least one first additive comp&ent
comprises at least one detergent and the at least one second additive component comprises
at least one detergent booster, or alternatively, the at least one first additive component
20 comprises at least one detergent booster and the at least one second additive component
comprises at least one detergent.
Examples of suitable-detergents are described herein.
Detergent boosters are over based metal salts which may increase the total base
number (TBN) of the lubricant composition. They may be provided as components in one
25 or more DI (detergent inhibitor) additive packs. DI packs typically comprise detergent(s),
dispersant(s), antiwear additive(s), anti-oxidant(s) and surfactant(s). Examples of
detergent boosters include calcium andlor magnesium salts or sulphonates, phenates,
salicylates and/or phosphates.
More than one detergent booster may be used.
30 Anti-foam Additives and additives other than anti-foam additives.
Anti-foam additives (sometimes called anti-foams or anti-foaming agents) retard the
formation of stable foams. Examples of suitable anti-foam agents include silicones,
Case No. 500050(2) 22 +
organic polymers, siloxanes (including poly siloxanes and (poly) dimethyl siloxanes,
phenyl methyl siloxanes), acrylates and the like. Anti-foams may be provided as
components in DI (detergent inhibitor) additive packs. More than one anti-foam may be
used.
5 When preparing a lubricant composition comprising at least one base oil component,
at least one additive component comprising at least one anti-foam additive and at least one
additive component comprising at least one lubricant additive other than an anti-foam
additive haziness may result. Anti-foam additives in general may be difficult to mix with
other components of a lubricant composition. It is generally beneficial to introduce the
10 additive components comprising at least one anti-foam additive after other additive
components have been mixed with the at least one base oil component. The present
invention may help mitigate the difficulties of mixing anti-foam additive components with
other components of lubricant compositions.
Thus, in at least some embodiments, the at least one second additive component
15 comprises at least one anti-foam additive and the at least one first additive component is at
least one lubricant additive which is other than an anti-foam additive.
Friction Modifier Additives and additives other than friction modifiers. 1
Friction modifiers and additives other than friction modifiers may be mixed together
in at least some embodiments.
20 Thus in some embodiments at least, the at least one second additive component
comprises at least one friction modifier additive and the at least one first additive
component is at least one lubricant additive which is other than a friction modifier additive.
Suitable friction modifiers may be ash-producing additives or ashless additives.
Examples of such friction modifiers include fatty acid derivatives including for example,
25 other fatty acid esters, amides, amines, and ethoxylated amines. Examples of suitable
ester friction modifiers include esters of glycerol for example, mono-, di-, and tri-oleates,
mono-palmitates and mono-myristates. A particularly suitable fatty acid ester friction
modifier is glycerol monooleate. Examples of fiiction modifiers also include molybdenum
compounds for example, organo molybdenum compounds, molybdenum
30 dialkyldithiocarbamates, molybdenum dialkylthiophosphates, molybdenum disulphide, trimolybdenum
cluster dialkyldithiocarbamates, non-sulphur molybdenum compounds and
the like. Suitable molybdenum-containing compounds are described for example, in EPCase
No. 500050(2) * 1533362-A1 for example in paragraphs [0101] to [0117].
Friction modifiers may also include a combination of an alkoxylated hydrocarbyl
mine and a polyol partial ester of a saturated or unsaturated fatty acid or a mixture of such
esters, for example as described in WO 93/21288.
5 Friction modifiers which are fatty acid derivative friction modifiers may be
introduced into the mixing vessel to produce a lubricant composition in which the friction
modifiers are present at a concentration of 0.01 to 5 % by weight actives, for example in
the range of 0.01 to 1.5 % by weight actives.
Molybdenum containing friction modifiers may be introduced into the mixing vessel
10 to produce a lubricant composition in which the friction modifiers are present at a
concentration of 10 to 1000 ppm by weight molybdenum, for example in the range of 400
to 600 ppm by weight.
Other additive components
The method of the present invention may be used to prepare lubricant compositions
15 comprising additive components which may suitably include: dispersant viscosity
modifiers, pour point depressants, dispersants, metal-containing detergents, detergent
boosters, anti-foam additives, friction modifiers, anti-wear additives, viscosity'index
L improvers, viscosity modifiers, rust inhibitors, corrosion inhibitors, anti-oxidants
(sometimes also called oxidation inhibitors), seal swell agents (sometimes also called
20 compatibility agents), extreme pressure additives (metallic, non-metallic, phosphorus
containing, non-phosphorus containing, sulphur containing and non-sulphur containing),
surfactants, demulsifiers, anti-seizure agents, wax modifiers, lubricity agents, anti-staining
agents, chromophoric agents and metal deactivators. Such additive components may be
first additive components, second additive components or third additive components as
25 herein described or may be other additive components. Some additive components may
exhibit more than one function. The method of the present invention may be used to
prepare a lubricant composition which comprises at least two additive components. The
method of the present invention may be used to prepare a lubricant composition which
comprises up to 18 additive components, for example up to 6 additive components. The
30 method of the present invention may be used to prepare a lubricant composition which
comprises typically up to about 20% by weight in total of additive components, for
example up to about 10% by weight in total of additive components. The method of the
Case No. 500050(2) 24
present invention may be used to prepare a lubricant composition which comprises
typically at least about 80% by weight in total of base oil components, for example, at
least about 90% by weight in total of base oil components.
The method of the present invention may be used to prepare a lubricant composition
5 in which the additive components have a viscosity which is typically in the range of 10 to
15 times more than that of the base oil components. The method of the present invention
may be used to prepare a lubricant composition in which the additive components have a
Kv100 of 1000 cSt or more. The limitation may be determined by the limit of the pump(s)
available for introducing the component into the mixing vessel.
10 The method of the present invention may be used to prepare a lubricant composition
in which during the preparation one or more of the additive components react with each
other. The use of an elongate mixing vessel in the method of the present invention may
facilitate temperature control by heat removal or heat addition to the components in the
mixing vessel.
15 Suitable anti-wear additives may be ash-producing additives or ashless additives.
Examples of such anti-wear additives include non-phosphorus containing additives for
example, sulphurised olefins. Examples of such anti-wear additives also include
phosphorus-containing antiwear additives. Examples of suitable ashless phosphoruscontaining
anti-wear additives include trilauryl phosphite and triphenylphosphorothionate
20 and those disclosed in paragraph [0036] of US2005l0198894. Examples of suitable ashforming,
phosphorus-containing anti-wear additives include dihydrocarbyl dithiophosphate
metal salts. Examples of suitable metals of the dihydrocarbyl dithiophosphate metal salts
include alkali and alkaline earth metals, aluminium, lead, tin, molybdenum, manganese,
nickel, copper and zinc. Particularly suitable dihydrocarbyl dithiophosphate metal salts are
25 zinc dihydrocarbyl dithiophosphates (ZDDP). The ZDDPYsm ay have hydrocarbyl groups
independently having 1 to 18 carbon atoms, suitably 2 to 13 carbon atoms or 3 to 18
carbon atoms, more suitably 2 to 12 carbon atoms or 3 to 13 carbon atoms, for example 3
to 8 carbon atoms. Examples of suitable hydrocarbyl groups include alkyl, cycloalkyl and
alkaryl groups which may contain ether or ester linkages and also which may contain
30 substituent groups for example, halogen or nitro groups. The hydrocarbyl groups may be
alkyl groups which are linear and/or branched and suitably may have fiom 3 to 8 carbon
atoms. Particularly suitable ZDDP's have hydrocarbyl groups which are a mixture of
Case No. 500050(2) 2 5
4
secondary alky groups and primary alkyl groups for example, 90 mol. % secondary alkyl
groups and 10 mol. % primary alkyl groups.
Phosphorus-containing anti-wear additives may be introduced into the mixing vessel
to produce a lubricant composition in which the phosphorus-containing anti-wear additives
5 are present at a total concentration of 10 to 6000 ppm by weight of phosphorus, suitably 10
to 1000 ppm by weight of phosphorus, for example 200 to 1400 ppm by weight of
phosphorus, or 200 to 800 ppm by weight of phosphorus or 200 to 600 ppm by weight of
phosphorus.
Viscosity index improvers (also called viscosity modifiers, viscosity improvers or VI
10 improvers) impart high and low temperature operability to a lubricant composition and
facilitate it remaining shear stable at elevated temperatures whilst also exhibiting
acceptable viscosity and fluidity at low temperatures.
Examples of suitable viscosity modifiers include high molecular weight hydrocarbon
polymers (for example polyisobutylene, copolymers of ethylene and propylene and higher
1 5 alpha-olefins); polyesters (for example polymethacrylates); hydrogenated poly(styrene-cobutadiene
or isoprene) polymers and modifications (for example star polymers); and
esterified poly(styrene-co-maleic anhydride) polymers. Oil-soluble viscosity modifying
polymers generally have number average molecular weights of at least 15000 to 1000000,
preferably 20000 to 600000 as determined by gel permeation chromatography or light
20 scattering methods.
Viscosity modifiers may have additional functions as multifunction viscosity
modifiers. More than one viscosity index improver may be used.
Rust inhibitors generally protect lubricated metal surfaces against chemical attack by
water or other contaminants. Examples of suitable rust inhibitors include non-ionic
25 polyoxyalkylene polyols and esters thereof, polyoxyalkylene phenols, polyoxyalkylene
polyols, anionic alky sulphonic acids, zinc dithiophosphates, metal phenolates, basic metal
sulphonates, fatty acids and amines.
More than one rust inhibitor may be present.
Corrosion inhibitors (also called anti-corrosive agents) reduce the degradation of
30 metallic parts contacted with the lubricating composition. Examples of corrosion
inhibitors include phosphosulphurised hydrocarbons and the products obtained by the
reaction of phosphosulphurised hydrocarbon with an alkaline earth metal oxide or
Case No. 500050(2) 26
18
hydroxide, non-ionic polyoxyalkylene polyols and esters thereof, polyoxyalkylene phenols,
thiadiazoles, triazoles and anionic alkyl sulphonic acids. Examples of suitable epoxidised
ester corrosion inhibitors are described in US200610090393.
More than one corrosion inhibitor may be used.
5 Antioxidants (sometimes also called oxidation inhibitors) reduce the tendency of oils
to deteriorate in use. Evidence of such deterioration might include for example the
production of varnish-like deposits on metal surfaces, the formation of sludge and viscosity
increase. ZDDP's exhibit some antioxidant properties.
Examples of suitable antioxidants other than ZDDP's include alkylated
1 0 diphenylarnines, N-alkylated phenylenediamines, phenyl-a-naphthylamine, alkylated
phenyl-a-naphthylarnines, dimethylquinolines, trimethyldihydroquinolines and oligomeric
compositions derived therefrom, hindered phenolics (including ashless (metal-free)
phenolic compounds and neutral and basic metal salts of certain phenolic compounds),
aromatic amines (including alkylated and non-alkylated aromatic amines), sulphurised
15 alkyl phenols and alkali and alkaline earth metal salts thereof, alkylated hydroquinones,
hydroxylated thiodiphenyl ethers, alkylidenebisphenols, thiopropionates, metallic
dithiocarbamates, 1,3,4-dimercaptothiadiazole and derivatives, oil soluble copber
compounds (for example, copper dihydrocarbyl thio- or thio-phosphate, copper salts of a
synthetic or natural carboxylic acids, for example a C8 to CIS fatty acid, an unsaturated acid
20 or a branched carboxylic acid, for example basic, neutral or acidic CU' and/or ~u%alts
derived from alkenyl succinic acids or anhydrides), alkaline earth metal salts of
alkylphenolthioesters, suitably having Cg to C12 alkyl side chains, calcium nonylphenol -
sulphide, barium t-octylphenyl sulphide, dioctylphenylamine, phosphosulphised or
sulphurised hydrocarbons, oil soluble phenates, oil soluble sulphurised phenates, calcium
25 dodecylphenol sulphide, phosphosulphurised hydrocarbons, sulphurised hydrocarbons,
phosphorus esters, low sulphur peroxide decomposers and the like.
More than one anti-oxidant may be used. More than one type of anti-oxidant may be
used.
Seal swell agents (sometimes also called seal compatibility agents or elastomer
30 compatibility aids) help to swell elastomeric seals for example by causing a reaction in the
fluid or a physical change in the elastomer. Examples of suitable seal swell agents include
Case No. 500050(2)
long chain organic acids, organic phosphates, aromatic esters, aromatic hydrocarbons,
esters (for example butylbenzyl phthalate) and polybutenyl succinic anhydride.
More than one seal swell agent may be used.
The additive components (first, second, third or other) may comprise solvent.
5 Examples of suitable solvents include highly aromatic, low viscosity base stocks, for
example 1 OON, 60 N and 100SP base stocks. The additive components (first, second,
third or other) may comprise Group I base stock as solvent.
The representative suitable and more suitable independent amounts of additives (if
present) in the lubricant composition produce by the method of the invention are given in
10 Table 1, although any effective amounts may be used. The concentrations expressed in
Table 1 are by weight of active additive compounds that is, independent of any solvent or
diluent.
More than one of each type of additive may be present. Within each type of additive,
more than one class of that type of additive may be present. More than one additive of
15 each class of additive may be present. Additives may suitably be supplied by
manufacturers and suppliers in solvent or diluents.
1
Case No. 500050(2)
Table 1
According to a further aspect of the present invention there is provided a lubricant
5 composition obtainable by the method as herein described. According to a further aspect
of the present invention there is provided a lubricant composition prepared by the method
as herein described. . -
The method of the present invention may be used to prepare lubricant compositions
which may be used for a range of applications including:
10 - as a metalworking fluid which may be used to lubricate metals during machining,
rolling and the like;
- as a power transmission fluid for example useful as an automatic transmission fluid, a
fluid in a clutch (for example a dual clutch), a gear lubricating composition, or in
other automotive applications and the like;
- as an aviation lubricant composition;
- as a lubricant composition suitable for lubricating a turbine;
ADDITIVE TYPE
Friction modifiers
Phosphorus-containing anti-wear additives
Molybdenum-containing anti-wear additives
Boron-containing anti-wear additives
Molybdenum-containing friction modifiers
Dispersants
Detergents
Viscosity index improvers
Pour point depressants
Corrosion andlor rust inhibitors
Anti-oxidants
Antifoams containing silicon
Lubricating composition
Suitable amount
(actives), if present
(by weight)
0.01 to 5%
corresponding to 10
to 6000 ppm P
corresponding to 10
to 1000 pprn Mo
corresponding to 10
to 250 ppm B
corresponding to 10
to 1000 pm Mo
0.1 to 20 %
0.01 to 6 %
0.01 to 20%
0.01 to 5 %
0.01 to 5 %
0.1 to 10 %
corresponding to 1
to 20 ppm Si
More suitable amount
(actives), if present
(by weight)
0.01 to 1%
corresponding to 1 0
to 1000 ppm P
corresponding to 40
to 600 pprn Mo
corresponding to 50
to 100 ppm B
corresponding to 400
to 600 pprn Mo
0.1 to 8 %
0.01 to 4 %
0.01 to 15%
0.01 to 1.5 %
0.01 to 1.5%
0.5 to 5 %
corresponding to 1 to
10 ppm'~i
Case No. 500050(2) 29
0
- as a lubricant composition for lubricating a solid surface, including for example
metallic surfaces and non-metallic surfaces;
- as a lubricant for an internal combustion engine, for example a compression ignition
engine or a spark-ignition engine; or
5 - as a lubricant for a marine or power engine, for example as trunk piston oil lubricant
composition;
The invention will now be described with respect to the following examples in which
Figures 1 to 8 represent in simplified schematic form apparatus in use in the method of the
present invention. Figure 9 represents in elevated schematic form, a static mixer which
10 may be used in an elongate mixing vessel. Figure 10 represents in schematic form a set of
static mixers in the form of plugs which may be located in a cylindrical mixing vessel,
each plug defining at least one passage for components in the direction of the longitudinal
axis of the elongate mixing chamber, each passage having a discontinuous, non-uniform
cross-section. In particular:-
15 Figure 1 represents in schematic form, apparatus comprising an elongate mixing vessel
comprising a first inlet, a second inlet a static mixer and an outlet;
Figure 2 represents in schematic form, apparatus comprising an elongate mixibg vessel
comprising a first inlet, a second inlet, a third inlet, a first static mixer, a second static
mixer and an outlet;
20 Figure 3 represents in schematic form, apparatus comprising an elongate mixing vessel
! comprising a first inlet, a second inlet, a third inlet, a first static mixer, a second static
mixer, an outlet and downstream of the first static mixer, a fourth inlet and downstream
thereof a third static mixer;
Figure 4 represents in schematic form, apparatus comprising an elongate mixing vessel
25 comprising a first inlet, a second inlet, a third inlet, a first static mixer, a second static
mixer, an outlet and upstream of the third inlet, a fourth inlet and downstream thereof a
third static mixer;
Figure 5 represents in schematic form, apparatus comprising an elongate mixing vessel
comprising a first inlet, a second inlet, a third inlet, a first static mixer, a second static
30 mixer, an outlet and downstream of the second static mixer and upstream of the second
inlet, a fourth inlet and downstream thereof a third static mixer;
Case No. 500050(2)
v
Figure 6 represents in schematic form, the apparatus of Figure 1 with an additional static
mixer upstream of the second inlet.
Figure 7 represents in schematic form, the apparatus of Figure 2 with an additional static
mixer downstream of the first inlet and upstream of the third inlet.
5 Figure 8 represents in schematic form, the apparatus of Figure 3 with an additional static
mixer downstream of the first inlet and upstream of the third inlet.
Figure 9 represents in elevated schematic form, a static mixer which may be used in the
elongate mixing vessel.
Figure 10 represents in schematic form a set of static mixers in the form of plugs which
10 may be located in a cylindrical mixing vessel, each plug defining at least one passage for
components in the direction of the longitudinal axis of the elongate mixing chamber, each
passage having a discontinuous, non-uniform cross-section in which Figure 10a is an
isometric view of the set of plugs, Figure lob is a longitudinal, cross section of the set of
plugs, Figure 10c is a transverse end view of the set of plugs and Figure 10d is a detailed
15 longitudinal cross-section of one of the plugs.
Key to common features of the drawings are identified by common reference numerals as
follows: t
1. mixing vessel;
2. first static mixer;
20 3. first inlet;
4. second inlet;
5. outlet;
6. second static mixer;
7. third inlet;
2 5 8. mixture of the at least one base oil component and the at least one first additive
component;
9. mixture of the at least one base oil component and the at least one first additive
component and the at least one second additive component;
10. fourth inlet;
3 0 1 1. third static mixer;
12. further optional static mixer;
13. longitudinal axis of elongate mixing vessel;
Case No. 500050(2) 3 1
14. circular orifice in plate of static mixer;
15. slot in plate of static mixer and
16. plate of static mixer.
Figure 1 - represents in schematic form, an apparatus which may be used in a method
5 of preparing a lubricant composition according to the present invention, which method
comprises introducing into an elongate mixing vessel comprising at one static mixer:
at least one base oil component,
at least one first additive component, and
at least one second additive component;
10 in which method:
the at least one first additive component is introduced into the mixing vessel separately
from the at least one second additive component and
the at least one second additive component is mixed in the elongate mixing vessel with a
mixture of the at least one first additive component and the at least one base oil component
15 using the at least one static mixer
in which the elongate mixing vessel (1) comprises:
at least one first static mixer (2), L
at least one first inlet (3) which is upstream of the at least one first static mixer (2),
at least one second inlet (4) which is upstream of the at least one first static mixer (2),
20 and
at least one outlet (5) which is downstream of the at least one first static mixer;
and in which the method comprises the steps of:
a) introducing a mixture of the at least one base oil component and the at least one first
additive component into the mixing vessel (1) through the at least one first inlet (3);
25 b) introducing the at least one second additive component into the mixing vessel (1)
through the at least one second inlet (4) upstream of the at least one static mixer (2);
c) flowing the at least one second additive component and the mixture from step a,
through the mixing vessel and past the at least one static mixer (2) to produce a mixture (9)
of the at least one base oil component, the at least one first additive component and the at
30 least one second additive component; and
d) removing the mixture (9) produced in step c from the mixing vessel (I) through the at
least one outlet (5) downstream of the static mixer (2).
Case No. 500050(2) 3 2 *
Figure 2 represents in schematic form, an apparatus which may be used in a method
of preparing a lubricant composition according to the present invention, which method
comprises introducing into an elongate mixing vessel comprising at least one static mixer:
at least one base oil component,
5 at least one first additive component, and
at least one second additive component;
in which method:
the at least one first additive component is introduced into the mixing vessel separately
from the at least one second additive component; and
10 the at least one second additive component is mixed in the elongate mixing vessel with a
mixture of the at least one first additive component and the at least one base oil component
using the at least one static mixer
in which the mixing vessel is an elongate mixing vessel (1) comprising:
at least one first static mixer (2),
15 at least one first inlet (3) which is upstream of the at least one first static mixer (2),
at least one second inlet (4) which is upstream of the at least one first static mixer (2),
at least one third inlet (7) which is upstream of the at least one first static mixer (2) and
is upstream of the at least one second inlet (4),
at least one outlet (5) which is downstream of the at least one first static mixer (2),
20 at least one second static mixer (6) which is upstream of the at least one first static
mixer (2), is upstream of the at least one second inlet (4), is downstream of the at least
one first inlet (3) and is downstream of the at least one third inlet (7); -
which method comprises the steps of:
a) introducing at least one base oil component into the mixing vessel (1) through the at
25 least one first inlet (3), introducing the at least one first additive component into the mixing
vessel (1) through the at least one third inlet (7), and mixing together the at least one base
oil component and the at least one first additive component in the mixing vessel by flowing
them through the mixing vessel and past the at least one second static mixer (6) to produce
a mixture (8) of the at least one base oil component and the at least one first additive
30 component;
b) introducing the at least one second additive component into the mixing vessel (1)
through the at least one second inlet (4) upstream of the at least one static mixer (2);
Case No. 500050(2)
c) flowing the at least one second additive component and the mixture (8) from step a,
through the mixing vessel and past the at least one first static mixer (2) to produce a
mixture (9) of the at least one base oil component, the at least one first additive component
and the at least one second additive component; and
5 d) removing the mixture (9) produced in step c from the mixing vessel (1) through the at
least one outlet (5) downstream of the static mixer (2).
Figures 3,4 and 5 represent in schematic form apparatus as in Figure 2 except that
the mixing vessel (1) additionally comprises at least one fourth inlet 10 (for additional
additives) and downstream thereof at least one third static mixer (1 1). This combination of
10 at least one fourth inlet (10) and at least one third static mixer (1 1) may be located
downstream of the at least one first static mixer (2) as shown schematically in Figure 3.
This combination of at least one fourth inlet (1 0) and at least one third static mixer (1 1)
may be located upstream of the at least one third inlet (7) as shown schematically in Figure
4. This combination of at least one fourth inlet (1 0) and at least one third static mixer (1 1)
15 may be located downstream of the at least one second static mixer (6) and upstream of the
second inlet (4) as shown schematically in Figure 5. In use in the method of the present
invention the additional additive is introduced into the mixing vessel (1) through the at
least one further inlet (1 0).
Figure 6 represents in schematic form apparatus as in Figure 1 with an additional
20 static mixer (12) upstream of the at least one second inlet (4). In use in the method of the
present invention this further static mixer introduces turbulent flow into the mixture of at
least one base oil component and at least one first additive component prior to mixing with
the at least one second additive in the first static mixer (2).
Figures 7 and 8 represent in schematic form apparatus as in Figures 2 and 3 with an
25 additional static mixer (12) downstream of the at least one first inlet and upstream of the at
least one third inlet (7). In use in the method of the present invention this further static
mixer introduces turbulent flow into the at least one base oil component prior to mixing
with the at least one first additive in the at least one second static mixer (6).
In Figures 1 to 8 the elongate mixing vessel has a longitudinal axis (13). The
30 additive components may be introduced into the mixing vessel in a direction which has a
component which is perpelidicular to the direction of the longitudinal axis (13). The
additive components may be introduced into the mixing vessel in a direction which is
Case No. 500050(2)
perpendicular to the direction of the longitudinal axis (1 3). The first inlet is used to
introduce the at least one base oil component (optionally as a mixture with at least one first
additive component) into the mixing vessel in the direction of the longitudinal axis (13) of
the elongate mixing vessel (1).
5 Figure 9 shows in elevated schematic form, a static mixer which may be used in an
elongate mixing vessel, for example as shown schematically in Figures 1 to 8. The static
mixer (2) comprises a plate (16) which comprises four circular orifices (14) and four slots
(15), the slots interconnecting with the orifices. This plate may be located in an elongate
mixing vessel transverse to the longitudinal axis of the elongate mixing vessel. In use, the
10 orifices and slots provides shearing boundary surfaces to induce turbulent flow of
components andlor mixtures flowing through the mixing vessel to thereby mix them.
Figure 10 represents in schematic form a set of static mixers in the form of plugs (1 7)
which may be located in a cylindrical mixing vessel (not shown). Each plug (1 7) may be
a first second or third static mixer depending upon the location of inlets to the mixing
15 vessel in which it is located. Each plug (1 7) defines at least one passage (1 8) for
components in the direction of the longitudinal axis (13) of the elongate mixing chamber,
each passage having a discontinuous, non-uniform cross-section. The plugs (20)(207) at
each end of the set have passages with cross-sections which increase or decrease along the
longitudinal axis. The other plugs (2 1)(2 1 ') have passages with cross-sections which
20 increase along the longitudinal axis towards the centre of the plug (22) and decrease
towards the ends of each plug (23). The plugs are spaced longitudinally apart by four
retaining rods (1 9). Figure 10a is an isometric view of the set of plugs, Figure lob is a
longitudinal, cross section of the set of plugs, Figure 10c is a transverse end view of the set
of plugs and Figure 10d is a detailed longitudinal cross-section of one of the plugs.
25 Example 1
A lubricating composition for lubricating the crankcase of an automotive internal
combustion engine comprising base oil, a first additive component comprising pour point
depressant and a second additive component comprising dispersant viscosity modifier was
prepared using apparatus as shown schematically in Figure 6 but with a set of nine static
30 mixers in the form of plugs each plug defining a passage having a discontinuous, nonuniform
cross-section as shown in Figure 10. The set of plugs was 298 mm long
corresponding to the length of the elongate mixing vessel, with the two end plugs (20)(20')
Case No. 500050(2) 35
having a length of 7 mm and the seven other plugs (21)(21') a length of 14 mm. The plugs
(20)(20') and (21)(2 1 ') had a diameter of 1 Ornrn to fit within a cylindrical elongate mixing
vessel (not shown). The passages (1 8) varied in cross-section diameter from 2 mm to 6mm
giving a conical angle (24) of 32". For end plug (20)(20') adjacent the first inlet (3) the
5 cross section varied fi-om 6mm down to 2 mrn in the direction of flow of components
through the vessel. For each of the seven other plugs (2 1)(2 1 ') which were not at the ends,
the cross-section of the passage varied linearly fi-om 2 mm up to 6 mm at the middle of the
plug and then back down to 2 rnm in the direction of flow of components through the
mixing vessel. The plugs were spaced apart along the mixing vessel typically by 21 mm
10 with the first end plug (20) counting in the general direction of component flow through
the vessel being 18 mm from the first inlet end of the elongate mixing chamber.
In the method a mixture of a base oil and a first additive component comprising pour
point depressant was introduced into the elongate mixing vessel through first inlet (3) at a
flow rate of 28 litres per minute using a pump operating at a temperature of less than 75°C
15 in the direction (shown as X in Figure 10a) of the longitudinal axis (1 3) of the elongate
mixing vessel at the end, upstream of the first (counting in the general direction of flow of
components) end plug (20) along the mixing vessel. The composition of this mixture is
given in Table 2.
Table 2
* may be used in part in second additive component mixture
A second additive component comprising dispersant viscosity modifier was
introduced into the elongate mixing vessel through second inlet (4) in a direction which
25 was perpendicular to the longitudinal axis (13) of the elongate mixing vessel using a pump
Composition of mixture of base oil and first
additive component
Mobil Jurong 500 SN Base oil
Detergent Inhibitor pack
Antioxidant Irganox-L-67
Antiwear additive LZ 1396
Pour point depressant Kusa kp -30
Amount corresponding to % by 1
weight in final lubricant composition
66.7"
5.2
0.15
0.25
0.1
-
Case No. 500050(2) * (not shown) operating at a temperature of less than 55°C at a location between the second
and third plugs (counting in the direction of general fluid component flow along the mixing
vessel) and downstream of the first end plug (20) shown as location Z in Figure 10. This
component was introduced at a flow rate of 12 litres per minute. The second additive
5 component could be introduced into the mixing vessel at a location between the first end
plug (20) and the first middle plug (2 1 ') plug (counting in the direction of general fluid
component flow along the mixing vessel) shown as location Y in Figure 10.
Table 3
10
The method was performed at a temperature of 30°C without any temperature
control. The pressure drop across the mixing vessel was 2.39 bar
In the method, the mixture (8) comprising the base oil components and the first
Composition of second additive component
comprising dispersant viscosity modifier
Mobil Jurong 150 SN Base oil
Yubase 6 base oil
Polymer concentrate 7% LZ 7067C
Dye OS Red Dye
Hitech 5777 dispersant viscosity modifier
additive component (pour point depressant) was passed through the mixing vessel (1) and
15 past the first (counting in the direction of general fluid component flow) end plug (20) and
the first (counting in the direction of general fluid component flow) middle plug (2 1 ')
which provides the at least one further static mixer (12) shown in Figure 6. These and the
change in geometry between the inlet and the vessel introduced turbulent flow into the
mixture (8) of base oil components and first additive component prior to mixing with the
20 second additive component comprising dispersant viscosity modifier in the at least one first
static mixer (2) in the form of one or more of the middle plugs (2 1) and the other end plug
(20').
The flow rate of the mixture (8) of base oil components and the first additive
component introduced into the mixing vessel through the first inlet (3) was 28 litres per
25 minute. The flow rate of the second additive component mixture introduced into the
Amount corresponding to % by
weight in final lubricant composition
10
10
5.5
0.01 925
2.1
i
Case No. 500050(2)
mixing vessel (1) through the second inlet (4) was 12 litres per minute. Therefore, the rate
of removal of the mixture from the mixing vessel through outlet (5) was 40 litres per
minute.
The formulated crankcase lubricant composition product removed through outlet (5)
5 was clear and bright.
The presence of dye in the composition comprising the dispersant viscosity modifier
provided a visual indicator of the mixing which was seen to be uniform. The pressure drop
across the mixing vessel became constant as the method progressed. The method produced
product at 40 litres per minute using small inventories (the volume of the mixing vessel
10 was estimated to be merely 500 ml). This demonstrates for exaniple that the method of the
present invention may permit production of lubricating compositions using apparatus
which has a very small size.
This example demonstrates the method of the present invention using a first additive
component which comprises a pour point depressant and a second additive component
15 which comprises a dispersant viscosity modifier (DVM) to prepare a lubricant composition
suitable for lubricating the crankcase of an internal combustion engine.
Example 2 1
Example 1 was repeated except that the flow rate of the mixture (8) of the base oil
components and the first additive component comprising pour point depressant was
20 introduced into the mixing vessel(1) through the first inlet (3) was 22.4 litres per minute.
The second additive component comprising dispersant viscosity modifier was into the
mixing vessel (1) through the second inlet (4) at 9.6 litres per minute. Therefore, the rate
of removal of the mixture fiom the mixing vessel through outlet (5) was 32 litres per
minute and the ratio of the flow rates through the first and second inlets was the same as in
25 Example 1. The pressure drop across the mixing vessel was 2.21 bar and the temperature
was the same as in Example 1. This example demonstrated the same results as Example 1.
Example 3
Example 1 was repeated except that the flow rate of the mixture (8) of the base oil
components and the first additive component comprising pour point depressant was 7.2
30 litres per minute, the flow rate of the second additive component mixture comprising
dispersant viscosity modifier was 7.2 litres per minute, the rate of removal of the mixture
Case No. 500050(2)
fiom the mixing vessel through outlet (5) was 24 litres per minute and the pressure drop
across the mixing vessel was 2.02 bar.
This example demonstrated the same results as Example 1.
Example 4
5 Apparatus as described for Examples 1 to 3 was used except that the second inlet was
positioned with respect to the static mixers as shown in Figure 6, upstream of the first
static mixer, but between the first end plug (20) and the first middle plug (21') shown at
location Y in Figure 10a.
The flow rate of the mixture (8) of the base oil components and the first additive
10 component comprising pour point depressant was 19.6 litres per minute, the flow rate of
the second additive component mixture comprising dispersant viscosity modifier was 8.4
litres per minute, the rate of removal of the mixture fiom the mixing vessel through outlet
(5) was 28 litres per minute and the pressure drop across the mixing vessel was 2.13 bar.
This example demonstrated the same results as Example 1.
15 Example 5
Apparatus as used in Examples 1 to 3 and shown in Figure 10 and represented by
configuration as shown in Figure 6 with additional static mixers downstream i f static
mixer (2) was used to prepare a trunk piston oil lubricant composition.
Referring to Figures 6 and 10, a mixture of at least one base oil component (BO-I)
20 and least one first additive component comprising at least one additive other than an antifoam
additive (that is, a pour point depressant) was into the mixing vessel through first
inlet (3) in the direction (shown as X in Figure 10a) of the longitudinal axis (1 3) of the
elongate mixing vessel at the end, upstream of the first (counting in the general direction of
flow of components) end plug (20) along the mixing vessel.
2 5 The first end plug (20) representing a further static mixer (12), introduced turbulent
flow into the mixture of BO-I and pour point depressant prior to mixing with a second
additive component. The flow rate of base oil (BO-I) and first additive component (pour
point depressant) was 35 litres per minute.
A mixture comprising a base oil (BO), detergent inhibitor package (DI) and anti-
30 foam second additive component was introduced into the mixing vessel through the second
inlet (4) upstream of the first static mixer (2) in a direction perpendicular to the
longitudinal axis (13) of the elongate mixing vessel (1) as shown in Figure 7, at allocation
Case No. 500050(2)
t
between the first middle plug (2 1 ')(second static mixer (6)) and the next middle plug (2 1)
(first static mixer (2), shown as location Z in Figure 10a. The mixture comprising a base oil
(BO), detergent inhibitor package (DI) and anti-foam and was introduced at a feed rate of
15 litres per minute.
5 In the method, turbulent flow was introduced into the mixture (8) of base oil
component (BO-I) and pour point depressant by the first end plug (20) (being a further
static mixer (12)). The mixture (8) and the second additive component (introduced through
second inlet (4) at location Z) was passed through the mixing vessel (1) and past the at
least one first static mixer (2) (middle plugs (2 1) and the second end lug (20')) to produce
10 a mixture (9) of the base oil component, the first additive component and the second
additive component before being removed from the mixing vessel (1) through the outlet
(5) downstream of the at least one first static mixer (2).
The rate of removal of the mixture from the mixing vessel through outlet (5) was 50
litres per minute. The mixing vessel was operated at 30 OC without temperature control.
15 The pressure drop across the mixing vessel between first inlet (3) and the outlet (5) was
2.16 bar.
No compatibility problems were observed with the components. This e;ample
demonstrates the preparation of a lubricating composition comprising at least one base oil
component, at least one first additive component comprising at least on lubricant additive
20 other an anti-foam additive and at least one second additive comprising at least one antifoam
additive.
This also shows benefit of introducing each additive component downstream of at
least one static mixer.
Example 6
25 Example 5 was repeated except that the flow rate of the mixture (8) of the base oil
component (BO-I) and the first additive component comprising at least one additive other
than an anti-foam additive (that is, a pour point depressant),through the mixing vessel was
22.4 litres per minute. The flow rate of the second additive component mixture (base oil
(BO), DI pack and anti-foam) introduced into the mixing vessel (1) through the second
30 inlet (4) was 9.6 litres per minute. The rate of removal of the mixture from the mixing
vessel through outlet (5) was 32 litres per minute. The mixing vessel was operated at 30
Case No. 500050(2)
"C without temperature control. The pressure drop across the mixing vessel between first
inlet (3) and the outlet (5) was 2.13 bar.
This example demonstrates the same results as Example 5.
Example 7
5 Example 5 was repeated but using apparatus as shown in Figure 10 and represented
by configuration as shown in Figure 1 where static mixer (2) is shown in Figure 1 a as plug
20, inlet 3 is in direction X and inlet 4 is at location Y', perpendicular to the longitudinal
axis 13 of the mixing vessel. Additional static mixing plugs 2 1 ' and 2 1 being located
downstream of the first static mixer (20,2).
10 The flow rate of flow rate of a mixture (8) of the base oil component and the first
additive component comprising at least one additive other than an anti-foam additive (that
is, a pour point depressant), introduced into the mixing vessel in direction (shown as X in
Figure 10a) of the longitudinal axis (13) of the elongate mixing vessel through the first
inlet (3) was 29.4 litres per minute. The flow rate of the second additive component
15 mixture (base oil (BO), DI pack and anti-foam) introduced into the mixing vessel (1)
through the second inlet (4) was 12.6 litres per minute perpendicular to the longitudinal
axis (13) upstream of the first static mixer (2'20). The rate of removal of the hxture from
the mixing vessel through outlet (5) was 42 litres per minute. The mixing vessel was
operated at 30 "C without temperature control. The pressure drop across the mixing vessel
20 between first inlet (3) and the outlet (5) was 2.13 bar.
This example demonstrated the same results as Example 5.
Example 8
A firther lubricating composition was prepared using the apparatus and configuration
as in Examples 1 to 3. The base oillfirst additive component and the second additive
25 component compositions are given in Tables 4 and 5 below.
No issues of compatibility were observed.
Case No. 500050(2)
Table 4
Table 5
Mixture of base oil component and first
additive component comprising pour point
depressant
Mobil Jurong 150 SN Base oil
Yubase 6 base oil
Detergent Inhibitor pack
Anti-oxidant Irganox-L-67
Anti-wear LZ 1396
Pour Point depressant Kusa kp -30
Amount corresponding to % by
weight in final lubricant composition
10
10
5.2
0.15
0.25
0.1
5 In the examples, further additive components may be introduced into the elongate
mixing vessel (1) in a direction transverse to the longitudinnl axis (13). Depending upon
the solubility of each additive component each may be introduced further downstream of
the elongate mixing vessel - at locations shown as W in Figure 10a upstream of further
middle plugs (21) and the second end plug (20'). The more soluble the additive
10 component, the further downstream it may be introduced.
This example demonstrated the same results as Example 5.
Example 9
Example 5 was repeated but with the additive components other than anti-foam
introduced separately. Thus, referring to the locations of inlets shown in Figure 10a, a
15 mixture of base oil (BO) and DI pack was introduced at location X through inlet (3) at a
flow rate of 14.7 llmin, a mixture of base oil (BO-I) and pour point depressant was
Second additive component comprising
dispersant viscosity modifier
Mobil Jurong 500 SN Base oil
Polymer concentrate 7% LZ 7067C
Dye OS red
Dispersant viscosity modifier HiTec 5777
Amount corresponding to % by
weight in final lubricant composition
66.7
5.5
L
0.01925
2.1
Case No. 500050(2) 42
R
introduced at location Y at a flow rate of 14.7 llmin and a mixture of base oil (BO) and
anti-foam was introduced at a flow rate of 12.6 Ymin at location Z.
No additive incompatibilities were observed.
Example 10
5 Example 9 was repeated with flow rates of 17.5 Wmin, 17.5 Ymin and 15 llmin at
locations X, Y and Z respectively. The same results as in Example 9 were observed.

Case No. 500050(2)
Claims:
1. A method of preparing a lubricant composition comprising at least one base oil
component, the at least one base oil component having a kinematic viscosity at 1 0 0in~ ~
the range of 2 to 100 cSt, the lubricant composition comprising at least one first additive
5 component and at least one second additive component which method comprises:
introducing into an elongate mixing vessel comprising at least one static mixer, at least one
base oil component, at least one first additive component and at least one second
additive component; the at least one first additive component being introduced into
the mixing vessel separately from the at least one second additive component; and
10 mixing the at least one second additive component with a mixture of the at least one first
additive component and the at least one base oil component in the elongate mixing
vessel using the at least one static mixer.
2. A method as claimed in claim 1 in which the mixing vessel is an elongate mixing vessel
comprising at least one first static mixer, at least one first inlet which is upstream of the at
15 least one first static mixer, at least one second inlet which is upstream of the at least one
first static mixer and at least one outlet which is downstream of the at least one static mixer
and in which the method comprises the steps of: L
a) introducing a mixture of the at least one base oil component and the at least one first
additive component into the mixing vessel through the at least one first inlet;
20 b) introducing the at least one second additive component into the mixing vessel through
the at least one second inlet upstream of the at least one first static mixer;
c) flowing the at least one second additive component and the mixture of step a, through
the mixing vessel and past the at least one first static mixer to mix the at least one
second additive component with the mixture of step a to produce a mixture of the at
2 5 least one base oil component, the at least one first additive component and the at least
one second additive component; and
d) removing the mixture produced in step c from the mixing vessel through the at least one
outlet downstream of the first static mixer.
3. A method as claimed in claim 1 in which,the mixing vessel is an elongate mixing vessel
30 comprising at least one first static mixer, at least one first inlet which is upstream of the at
least one first static mixer, at least one second inlet which is upstream of the at least one
first static mixer, at least one third inlet which is upstream of the at least one first static
. . - . f
;, " & L&-e't*ie
Case No. 500050(2) 44 p-3
% L> /
mixer and is upstream of the at least one second inlet and at least one outlet which is
downstream of the at least one static mixer;
and in which the method comprises the steps of:
a') introducing the at least one base oil component into the mixing vessel through the at
5 least one first inlet, introducing the at least one first additive component into the
mixing vessel through the at least one third inlet and mixing together the at least one
base oil component and the at least one first additive component in the mixing vessel
to produce a mixture of the at least one base oil component and the at least one first
additive component;
10 b') introducing the at least one second additive component into the mixing vessel through
the at least one second inlet upstream of the at least one first static mixer;
c') flowing the at least one second additive component and the mixture from step a',
through the mixing vessel and past the at least one first static mixer to mix the at least
one second additive component with the mixture from step a to produce a mixture of
15 the at least one base oil component, the at least one first additive component and the at
least one second additive component; and
d') removing the mixture produced in step c' from the mixing vessel throughihe at least
one outlet downstream of the first static mixer.
. 4. A method as claimed in claim 3 in which the elongate mixing vessel further comprises
20 at least one second static mixer which is upstream of the at least one first static mixer, is
upstream of the at least one second inlet, is downstream of the at least one first inlet and is
downstream of the at least one third inlet and in which in step a', the method comprises
mixing together the at least one base oil component and the at least one first additive
component in the mixing vessel by flowing them through the mixing vessel and past the at
25 least one second static mixer to produce a mixture of the at least one base oil component
and the at least one first additive component.
5. A method as claimed in any one of claims 1 to 4 in which the at least one first additive
component comprises at least one dispersant viscosity modifier and the at least one second
additive component comprises at least one pour point depressant.
30 6. A method as claimed in any one of claims 1 to 4 in which the at least one first additive
component comprises at least one pour point depressant and the at least one second
additive component comprises at least one dispersant viscosity modifier.
- .,
Case No. 500050(2)
7. A method as claimed in any one of claims 1 to 4 in which the at least one first additive
component comprises at least one dispersant and the at least one second additive
component comprises at least one metal-containing detergent.
8. A method as claimed in any one of claims 1 to 4 in which the at least one first additive
5 component comprises at least one metal-containing detergent and the at least one second
additive component comprises at least one dispersant.
9. A method as claimed in claim 7 or claim 8 in which the dispersant is a dispersant
viscosity modifier.
10. A method as claimed in claim 7, claim 8 or claim 9 in which the at least one base oil
10 and the at least one first additive component and the at least one second additive
component are mixed in the absence of any zinc dihydrocarbyl dithiophosphate.
11. A method as claimed in any one of claims 1 to 4 in which the at least one first additive
component comprises at least one detergent and the at least one second additive component
comprises at least one detergent booster.
15 12. A method as claimed in any one of claims 1 to 4 in which the at least one first additive
component comprises at least one detergent booster and the at least one second additive
component comprises at least one detergent. L
13. A method as claimed in any one of claims 1 to 4 in which the at least one second
additive component comprises at least one anti-foam additive and the at least one first
20 additive component is at least one lubricant additive which is other than an anti-foam
additive.
14. A method as claimed in any one of claims 1 to 4 in which the at least one second
additive component comprises at least one friction modifier additive and the at least one
first additive component is at least one lubricant additive which is other than a friction
25 modifier additive.
15. A method as claimed in any one of claims 1 to 14 in which the elongate mixing vessel
further comprises:
at least one fourth inlet downstream of the at least one first static mixer and
at least one third static mixer which is downstream of the at least one first static
30 mixer and which is downstream of the at least one fourth inlet
and in which the method further comprises:
. -- n , _ ; f L * U ~ A ? - * .
r? p, ;\Ti r 7 '
Case No. 500050(2) 46 . . . ,Ab
--" -- "d
2 ?801 zDt3
introducing at least one third additive component into the mixing vessel through the
at least one fourth inlet; and
mixing the at least one third additive component in the mixing vessel with the at least
one base oil component, the at least one first additive component and the at least one
second additive component in the mixing vessel by flowing them through the mixing
vessel and past the at least one third static mixer to produce a mixture of the at least
one base oil component and the at least one first additive component, the at least one
second additive colnponent and the at least one third additive component.
16. A method as claimed in claim 15 in which the at least one third additive component is
mixed in the mixing vessel with the at least one base oil component, the at least one first
additive component and the at least one second additive component in the mixing vessel by
flowing them through the mixing vessel and past the at least one third static mixer at a
temperature which is different to the temperature at which the components are flowed past
the at least one first static mixer and which is different to the temperature at which the
components are flowed past the at least one second static mixer, if present.
17. A method as claimed in claim 15 or claim 16 in which the at least one third additive
component which is introduced into the mixing vessel through the at least one' fourth inlet
comprises at least one zinc dihydrocarbyl dithiophosphate.
18. A method as claimed in any one of the preceding claims in which the elongate mixing
vessel has a volume of less than about 1 litre.
19. A method as claimed in any one of the preceding claims in which the total residence
time of all the components in the elongate mixing vessel is less than about 1 minute.
20. A method as claimed in any one of the preceding claims in which the lubricant
composition is substantially non-aqueous.
2 1. A method of preparing a substantially non-aqueous lubricant composition comprising
at least one base oil component, at least one first additive component and at least one
second additive component which method comprises:
introducing into an elongate mixing vessel comprising at least one static mixer, at least one
base oil component, at least one first additive component and at least one second
additive component; the at least one first additive component being introduced into
the mixing vessel separately from the at least one second additive component; and
Case No. 500050(2)
I b
mixing the at least one second additive component with a mixture of the at least one firs
additive component and the at least one base oil component in the elongate mixing
vessel using the at least one static mixer.
Dated this 2211 112013
(NEHA S ~ A S T A V A )
OF REMFRY & SAGAR I
ATTORNEY FOR THE APPLICANTS