FIELD OF THE INVENTION
The present invention relates to a lubricant cum sealant formulation and in particular to a
lubricant cum sealant formulation in the form of solid grease stick/mass for simple and
effective application for lubrication of industrial valves and a process for manufacture of
such lubricant More particularly, the present invention is directed to a high performance
lubricant cum sealant adapted to suit a variety of applications including API Gate Valves,
Orbit Ball Valves and bottom discharge taper plug valves for tank wagons (BGOT, BTPN,
etc), used for carrying POL type hydrocarbon fuels and/or solvents Importantly, the
lubricant cum sealant formulation of the invention is directed for application /use in
various types of industrial valves The lubricant cum sealant stick can be obtained in
appropriate size/dimensions which can be inserted into the valve screw which is
subsequently tightened for achieving the desired lubrication and sealing properties
Advantageously also, the lubricant cum sealant stick/mass type solid lubricating grease is
capable of protecting the valve seating surface against corrosion and further preventing
leakage of the working fluid Importantly therefore the grease stick/mass type lubricant
cum sealant formulation according to the present invention is adapted to serve
satisfactorily the functions of lubrication, corrosion resistance and sealing even for
application in valve installation in pipelines having petroleum hydrocarbons as flowing
fluid The grease stick/mass type lubricant cum sealant formulation according to the
present invention is thus suitable for a wide range of industrial valves for various
applications with distinct advantage in user friendly and cost effective manner free of any
spillage or leakage, enhancing performance of valves, equipment and conduit/carriage
systems
BACKGROUND ART
It is known in the related art that plug valve lubricating greases are used in industrial
applications since long in the past Lubricating greases have stronger adhesion than oil
lubricants, facilitating simplifying design of machine parts/ subsystems such as simplifying
seal mechanisms Lubricating greases offer in general functional means of effectively
reducing friction in moving parts in operating a plug valve It also facilitates freeing the

plug in case it is stuck up during operation and also helps combating corrosion by giving
the seating surface a protective coating
It has also been observed that lubricating greases for such application require a number of
special properties which are not commonly available in regular commercial lubricating
greases Such special properties of lubricating greases that are prerequisite for application
in plug valves comprise the following
Insolubility It must remain insoluble and also must resist to a high degree to being washed away or solubilised by the contents carried through the pipeline or stored in the storage tanks/tank wagons It must also resist chemical attack from the line fluids and
not get washed away in service
Body It must have sufficient consistency and toughness to seal the valve against leakage
in closed position If the lubricant is of insufficient consistency, it will flow past the plug
instead of jacking it up
Temperature resistivity The lubricant must also be resistant to temperature in the
recommended limits for service and retain the desired properties throughout the
temperature range
Wetting effect It must adhere to the seating surfaces securely so that it is not washed
away by the flowing fluid in the pipeline
Lubrication It must be greasy with adequate lubrication properties so that the plug can be
easily rotated
Thixotropic behaviour It must not harden and choke the lubricant reservoir and
connecting system of grooves in the plug valve This property is essentially required to
enable fresh insertion of lubricant as and when needed
Corrosion protection Lubricant must protect seating surfaces against corrosion
The application of conventional lubricant formulation for plug valves or the like faces
limitation in specific cases where the reservoir/pipeline is used to store/transport different

types of hydrocarbon fuels/solvents The requirements of certain individual products could
be met to some extent by the conventional lubricants used but meeting the requirement of
the whole range of hydrocarbon fuels/solvents has been a practical difficulty for
conventional lubricant compositions
Again from the conventional considerations of grease/lubricant injection in plug valves or
like application installed on pipeline, the same is forced into the plug valve by regular
periodic feeding through conventional fittings provided on such valves or by means of a
lubrication gun specially designed to handle the full bodied lubricants used in these valves
There have been, therefore, been a persistent need in the art of lubrication of plug valve
or the like devices, to provide for a lubricant cum sealant formulation and simple means
for its administration in the various valve configurations like API gate valve stems, plug
valves, orbit ball valves and also valves for tank wagons carrying hydrocarbon fuels and
solvents In particular, it is desired that said lubricant formulation be obtained in solid
stick/mass form adapted for ease of application without leakage and serve the functions of
lubrication, corrosion prevention and also as sealant by providing a secure layer of said
lubricant on the total valve seating area in closed condition, such as to favor easy
insertion of stick of proper dimension into the valve screw and feeding said lubricant
simply by tightening the screw whereby also the lubricant is applied to fill voids inside the
valve or to all friction surfaces needed to be protected, sealed or made free of leakage
Also it is desired that the lubricant composition be adapted for favored use as sticks/solid
mass in plug or other type valves which would not wash away in service and would be
capable of meeting the requirements of different individual /mixed compositions of various
types of hydrocarbon fluids
OBJECTS OF THE INVENTION
It is thus the basic object of the present invention to provide a lubricant cum sealant
formulation and a process for its manufacture preferably in the form of solid grease stick
or mass for easy and simple application in plug valves and other types of valves including
the valves for tank wagons carrying hydrocarbon fuels and/or solvents

A further object of the present invention is directed to a lubricant cum sealant formulation
wherein said lubricant cum sealant could be obtained in the form of solid grease stick or
mass capable of adhering to the valve seating area and providing a seal between the plug
and the valve body to thereby achieve complete leak proofing of the valve in closed
condition
A still further object of the present invention is directed to a lubricant cum sealant
formulation wherein said lubricant cum sealant could be obtained in the form of solid
grease sticks or mass for application in plug valve or the like, that would be greasy and
would provide adequate lubrication between the mating surfaces so that the plug can be
easily rotated
A still further object of the present invention is directed to a lubricant cum sealant
formulation wherein said lubricant cum sealant could be obtained in the form of solid
grease sticks or mass for application in plug valve or the like, wherein the lubricant would
not pass around the plug and satisfactorily jack up the plug
A still further object of the present invention is directed to a lubricant cum sealant
formulation wherein said lubricant cum sealant could be obtained in the form of solid
grease sticks or mass for application in plug valve or the like, wherein said lubricant would
prevent corrosion and chemical action by the contents of the reservoir/ pipe line
A still further object of the present invention is directed to a lubricant cum sealant
formulation wherein said lubricant cum sealant could be obtained in the form of solid
grease sticks or mass for application in plug valve or the like, wherein said lubricant cum
sealant would be adapted to provide satisfactory lubrication cum sealing performance
even when the contents of the reservoir/pipeline are having combined characteristics
because it is suitable for the entire range of petroleum hydrocarbon fuels/solvents
A still further object of the present invention is directed to a lubricant cum sealant
formulation wherein said lubricant cum sealant could be obtained in the form of solid
grease sticks or mass for application in plug valve or the like, wherein said lubricant cum
sealant composition would not harden and choke the lubricant reservoir and connecting
system of grooves in plug valve facilitating easy insertion of fresh lubricant when needed

A still further object of the present invention is directed to a lubricant cum sealant
formulation wherein said lubricant cum sealant could be obtained in the form of solid
grease sticks or mass for application in plug valve or the like, wherein said lubricant cum
sealant composition would be resistant to temperature in the recommended limits for
service and retain the desired properties throughout the service temperature range and
also be resistant to chemical attack by the contents of the reservoir/pipeline
SUMMARY OF THE INVENTION ,
Thus according to the basic aspect of the present invention, it is directed to a lubricant
cum sealant formulation comprising as major components the following
gellant in an amount of upto 25 % by wt comprising
Silica Amorphous,
amino functional Silane coupling agent,
Solvent for coupling agent like diethyl ether,
Corrosion inhibitor, and
a polymeric (amido) resin in amounts of 70 to 80 % by wt
A further aspect of the present invention is directed to said lubricant cum sealant
formulation developed in stick/mass form for plug valve and the like adapted for
handling/servicing petroleum hydrocarbon solvents/fuels, comprising
Polyamide (amido) resin 70 to 80 preferably 75 parts by weight,
Silica Amorphous 15 to 25 preferably 20 parts by weight,
amino functional silane coupling agent 2 to 5 preferably 3 parts by weight,
Solvent for coupling agent like diethyl ether 1 to 3 preferably 1 5 parts by weight,
Corrosion inhibitor 0 2 to 1 preferably 0 5 part by weight
A further aspect of the present invention is directed to said lubricant cum sealant
formulation adapted for sealing and completely adhering to the seating surface avoiding
washing/pin holes even at a high air pressure upto 6 5 kg/cm2 and thereby favouring
complete sealing
A still further aspect of the present invention is directed to a lubricant cum sealant
formulation, wherein said lubricant cum sealant composition is non-reactive to different

f
types of petroleum hydrocarbon fuels/solvents including commercial petrol, naphtha,
diesel, kerosene, MTO, LDO, furnace oil, pentane, hexane, heptane and also petroleum
based lubricating oils
An important aspect of the present invention is directed to said lubricant cum sealant
formulation that is adapted for use in bottom discharge valves of POL tank wagons, having
desired high dropping point above 200°C and low evaporation loss of max 1 percent at 105
±1 °C for 2 hrs
Another aspect of the present invention is directed to said lubricant cum sealant
formulation comprising a thickener of amorphous silica type having the following
properties
Type Hydrophobic amorphous fluffy white powder
BET surface area 105 to 130 sq mpergm,
Bulk density 3 3 to 3 5 lb/ cu ft ,
Loss on heating 0 80% max,
Average particle (aggregate) length 0 2 to 0 3 micron,
Another aspect of the present invention is directed to said lubricant cum sealant
formulation comprising an amino functional silane coupling agent having the following
properties
Appearance Clear and colourless liquid ,
Sp Gravity at 25°C 0 945 to 0 955,
Boiling Point (760 mm of Hg ) 220 to 222°C,
Refractive Index at 25°C 1 40 to 1 45,
Flash Point (Pensky-Martms closed Cup °C) 95 to 100,
A further aspect of the present invention is directed to said lubricant cum sealant
formulation wherein said polymeric (amido) resin has the following properties
Appearance Reddish yellow viscous clear liquid,
Specific gravity at 20 deg C 0 965-0 975
Acid Value (mg KOH/g) of 3 0 max,

Amine Value (mgKOH/g) in the range of 290 to 320,
Viscosity at 25 deg C in the range of 400 to 600 Poise,
% N V M 120°C/1 hr of 98 mm
The said lubricant cum sealant formulation of the present invention further comprises said
ashless corrosion inhibitor having the following properties
Sp Gravity at 15 6 °C of 0 945 to 0 955 ,
Viscosity , kinematic at 100°C (cSt) of 10 tol2,
Flash Point (COC) of 125 to 135°C,
Acid Number (mg KOH / g) of 70 to 78
Yet another important aspect of the present invention is directed to a process for
manufacture of a lubricant cum sealant formulation according to the invention, comprising
(i) adding the Polymeric (amido) resin fluid into a mixer preferably steam
jacketed Sigma Mixer,
(n) adding Silica powder in small increments to the fluid under stirring action to
obtain a good dispersion,
(in) providing the Amino functional Silane coupling agent solubilised in diethyl ether
into the sigma mixer preferably in spray mode such that it covers the
maximum surface area to facilitate homogeneous reaction,
(iv) heating the sigma mixer with steam to a temperature of 100-105°C, with the lid
covered for 1 hour,
(v) opening the lid after 1 hour and maintaining the temperature at 100 - 105 deg
C for another 1 hour,
(vi) Stopping the heating and when the temperature reaches below 60 °C
preferably about 50°C adding the corrosion inhibitor thereafter and after about
15 minutes time, stopping the stirring to thereby obtain the said lubricant cum
sealant product
Yet another aspect of the present invention is directed to a process for manufacture of a
lubricant cum sealant formulation wherein the finished product /mass is subjected to stick
formation of defined dimensions e g 40 mm length and 16 mm diameter and weight of
approximately 10 grams

Further the said method of plug valve lubrication involving the lubricant cum sealant
formulation comprises (i) feeding desired amount of said lubricant sticks/mass into the
screw of the valve and (n) tightening the valve screw to apply said lubricant uniformly on
the friction surfaces and the valve seating area under desired pressure enabling achieving
leak free operation of the valve
The present invention and its objects and advantages are described in greater details with
reference to the accompanying non -limiting illustrative example
DETAILED DESCRIPTION OF THE INVENTION WITH REFERENCE TO THE
ACCOMPANYING EXAMPLE
The present invention is directed to a lubricant cum sealant formulation that is obtained in
the form of grease sticks or mass and its process of manufacture, adapted for application
as lubricant cum sealant in API Gate Valve stems, Plug valves, Orbit ball valves and also
valves for tank wagons for carrying hydrocarbon fuels and solvents Advantageously, the
lubricant grease sticks produced in preferred sizes/dimensions or mass facilitate easy
application without requiring any conventional fittings on valves or any external device like
lubricant gun, by simply inserting the grease stick of appropriate size into the valve screw
itself and then tightening the screw to fill/apply to all friction surfaces/seat to be lubricated
or protected, at a preferred pressure of the lubricant
The amount of lubricant or the number of sticks to be used depends on the frequency of
operation of a particular type of valve If a valve is operated/opened and closed at
frequent intervals, it requires quite frequent lubrication Again, if a valve is totally empty
of lubricant at any instant, the lubricant fitting turns on easily and as the lubricant system
gets filled up, the fitting turns with increased difficulty until filled to the fullest extent It is
an acceptable practice to keep the lubricant fitting turned down, and thus maintaining
constant pressure on the lubricant system inside the valve Application of lubricant at
regular frequency makes the valve operate easily, preserves the seating surfaces and
prevents leakage of contents

The lubricant formulation and the grease stick/mass type lubricant as end product are
suitable for application in API Gate Valve stems, Plug valves, Orbit ball valves and also
valves for tank wagons for carrying hydrocarbon fuels and solvents, including commercial
petrol, lubricating oils, naphtha, hydrocarbon solvents like hexane, etc
The present invention thus directed to a simple/non-destructive energy saving process for
production of a lubricant composition, that is obtained in the form of grease sticks/mass
for end application in various types of valves on pipelines or tank wagons is described in
details with reference to the following example 1
Example 1:
An exemplary form of the lubricant cum sealant formulation of the invention was obtained
involving the following input ingredients having specified properties used in the following
weight proportions
Ingredients Parts by wt proportion
f|0 l Polymenc(amido) resin_ 75 parts by weight, (
Silica Amorphous 20 parts by weight,
amino functional Silane coupling agent 3 parts by weight,
Corrosion inhibitor 0 5 part by weight The selective characteristics/ properties of the input materials desired are as hereunder
a amino functional Silane coupling agent meets the following specification
Appearance clear and colourless liquid
Sp Gravity at 25°C 0 945 to 0 955,
Boiling Point (760 mm of Hg) 220-222°C,
Refractive Index at 25°C 1 40 to 1 45,
Flash Pomt( Pensky-Martms closed Cup °C) 95-100

b Amorphous Silica meets the following specification
Type Hydrophobic amorphous fluffy white powder
BET surface area 105 to 130 sq m per gm
Bulk density 3 3 to 3 5 lb/ cu ft
Loss on heating 0 80% max
Average particle(aggregate) length 0 2 to 0 3 micron
c The polymeric (amido) resin, has the following specifications
Appearance Reddish yellow viscous clear liquid,
Specific gravity at 20 deg C 0 965-0 975
Acid Value (mg KOH/g) of 3 0 max,
Amine Value (mg KOH/g) in the range of 290 to 320,
Viscosity at 25 deg C in the range of 400 to 600 Poise,
% N V M 120°C/1 hr of 98 mm
d Ashless corrosion inhibitor is a proprietary blend of ester/amide/carboxylate
with dodecyldimethyl amine having following specification
Sp Gravity at 15 6 °C of 0 945 to 0 955 ,
Viscosity , kinematic at 100°C (cSt) of 10 tol2,
Flash Point (COC) of 125 to 135°C,
Acid Number (mg KOH / g) of 70 to 78
The process for manufacture of the lubricant cum sealant composition involving tne
above input materials was carried out following the sequence of steps as discussed
hereunder
i)addmg the Polymeric (amido) resin fluid into a mixer preferably steam jacketed
Sigma Mixer,
n)addmg Silica powder in small increments to the fluid under stirring action to obtain a
good dispersion,

111) providing the amino functional Silane coupling agent solubilised in diethyl ether into
the sigma mixer preferably in spray mode such that it covers the maximum surface
area to facilitate homogeneous reaction,
iv)heating the sigma mixer with steam to a temperature of 100-105°C, with the lid
covered for 1 hour,
v) opening the lid after 1 hour and maintaining the temperature at 100 - 105 deg C for
another 1 hour,
vi) Stopping the heating and when the temperature reaches below 60 °C preferably
about 50°C adding the corrosion inhibitor thereafter and after about 15 minutes time,
stopping the stirring to thereby obtain the said lubricant cum sealant product
vn) Unloading the finished product at ambient temperature and subjecting it to
formation of sticks of definite dimension eg 40 mm length X 16 mm dia
The prepared stick/mass is next subjected to a number of tests to evaluate the conformity
to expected performance as enumerated in accompanying Table 1



Performance test
Performance test for effectiveness of the lubricant cum sealant formulation has been
performed on bottom discharge (BD) plug valves of tank wagons The observed data
/results are as follows
Type of valve tested 100mm B D Valve
Number of sticks (40mm length, 16mm dia , weight 10 grams) used on
(i) taper plug surface 4 nos and
(n) in screw hole of valve 4 nos
Observation No leakage found even after two rotations (at air pressure of 6 5 kg/cm2)
It is thus possible by way of the present invention to provide a lubricant cum sealant
formulation for plug valves and/or other valves for a wide range of applications including
the bottom discharge valves on tank wagons for carrying petroleum hydrocarbon fuels and
c — _
solvents, wherein said lubricant cum sealant formulation could be obtained
advantageously in the form of solid grease sticks of desired dimensions or in mass form
The grease stick/mass lubricant of the present invention, on one hand is easy to apply

without the requirement for any device like grease gun or any mounting on the valve, by
just inserting required number of sticks or mass into the valve and then tightening the
screw for proper fixation of the lubricant around the taper plug facilitating desired jacking
of the plug and on the other hand ensuring firm adhesion on the entire valve seating
without being washed away by the contents of the pipeline/ tank carriage, avoiding
leakage or any separation for longer duration and at reasonably high service pressure The
lubricant cum sealant formulation in its solid grease stick/mass form reduces waste or
spillage economising consumption of such lubricant depending on actual frequency of
operation of a particular type of valve device and thus favoring wide industrial application
with substantial economic advantage

WE CLAIM:

1 A lubricant cum sealant formulation majorly comprising
i) gellant in an amount of upto 25% by wt comprising
Silica Amorphous,
amino functional Silane coupling agent,
Solvent for coupling agent like diethyl ether,
Corrosion inhibitor, and
n) a polymeric (amido) resin in amounts of 70 to 80 % by wt
2 A lubricant cum sealant formulation as claimed in claim 1 developed in stick/mass form
for plug valve and the like adapted for handling/servicing petroleum hydrocarbon
solvents/fuels comprising
Polymeric (amido) resin 70 to 80 preferably 75 parts by weight,
Silica Amorphous 15 to 25 preferably 20 parts by weight,
amino functional Silane coupling agent 2 to 5 preferably 3 parts by weight,
Solvent for coupling agent like diethyl ether 1 to 3 preferably 1 5 parts by weight,
Corrosion inhibitor 0 2 to 1 0 preferably 0 5 part by weight
3 A lubricant cum sealant formulation as claimed in anyone of claims 1 or 2 adapted for
sealing and completely adhering to the seating surface avoiding washing/pin holes even at a
high air pressure upto 6 5 kg/cm2 and thereby favouring complete sealing
4 A lubricant cum sealant formulation as claimed in anyone of claims 1 to 3, wherein said
lubricant composition is non-reactive to different types of petroleum hydrocarbon fuels/
solvents including commercial petrol, naphtha, diesel, kerosene, MTO, LDO, furnace oil,
pentane, hexane, heptane and also petroleum based lubricating oils
5 A lubricant cum sealant formulation as claimed in anyone of claims 1 to 4 adapted for use
in bottom discharge valves of POL tank wagons, having desired high dropping point above
200°C and low evaporation of max 1% at 105 ±1 °C for 2 hrs

6 A lubricant cum sealant formulation as claimed in anyone of claims 1 to 5 comprising a
thickener of amorphous silica type having the following properties
Type Hydrophobic amorphous fluffy white powder
B E T surface area 105 to 130 sq m per gm
Bulk density 3 3 to 3 5 lb/ cu ft
Loss on heating 0 80% max
Average particle (aggregate) length 0 2 to 0 3 micron
7 A lubricant cum sealant formulation as claimed in anyone of claims 1 to 6 comprising an
amino functional silane coupling agent having the following properties
Appearance clear and colourless liquid,
Sp Gravity at 25°C 0 945 to 0 955,
Boiling Point (760 mm of Hg) 220-222°C,
Refractive Index at 25°C 1 40 to 1 45,
Flash Pomt( Pensky-Martms closed Cup °C) 95-100
8 A lubricant cum sealant formulation as claimed in anyone of claims 1 to 7 comprising said
polymeric (amido) resin having the following properties
Appearance Reddish yellow viscous clear liquid,
Specific gravity at 20 deg C 0 965-0 975
Acid Value (mg KOH/g) of 3 0 max,
Amine Value(mg KOH/g) in the range of 290 to 320,
Viscosity at 25 deg C in the range of 400 to 600 Poise,
% N V M 120°C/1 hr of 98 mm
9 A lubricant cum sealant formulation as claimed in anyone of claims 1 to 8 comprising
ashless corrosion inhibitor having the following properties
Sp Gravity at 15 6 °C of 0 945 to 0 955,
Viscosity , kinematic at 100°C (cSt) of 10 tol2,
Flash Point (COC) of 125 to 135°C,
Acid Number (mg KOH / g) of 70 to 78,

10 A process for manufacture of a lubricant cum sealant formulation as claimed in anyone
of claims 1 to 9 comprising
i) adding the Polymeric (amido) resin fluid into a mixer preferably steam jacketed
Sigma Mixer,
n) adding Silica powder in small increments to the fluid under stirring action to
obtain a good dispersion,
in) providing the Amino functional Silane coupling agent solubilised in diethyl ether
into the sigma mixer
preferably in spray mode such that it covers the maximum surface area to
facilitate homogeneous reaction,
iv) heating the sigma mixer with steam to a temperature of 100-105°C, with the lid
covered for 1 hour,
v) opening the lid after 1 hour and maintaining the temperature at 100 - 105 deg C
for another 1 hour,
vi) Stopping the heating and when the temperature reaches below 60 °C preferably
about 50°C adding the corrosion inhibitor thereafter and after about 15 minutes
time, stopping the stirring to thereby obtain the said lubricant cum sealant
product
11 A process for manufacture of a lubricant cum sealant formulation as claimed in anyone
of claims 1 to 10 wherein the finished product /mass is subjected to stick formation of
defined dimensions involving about 40 mm length and about 16 mm diameter and weight of
about 10 grams

ABSTRACT

TITLE LUBRICANT CUM SEALANT FORMULATION IN STICK/MASS FORM AND ITS
PRODUCTION PROCESS AND METHOD OF APPLICATION IN INDUSTRIAL VALVES
The invention relates to a lubricant cum sealant formulation in the form of solid grease
stick/mass and a process for production of such lubricant More particularly, the lubricant
cum sealant formulation of the invention is adapted for a number of applications
comprising API Gate Valve Stems, Orbit Ball Valves, taper plug valves of tank wagons
carrying hydrocarbon fuels/solvents Importantly, the lubricant cum sealant formulation
for various types of industrial valves comprises optimum levels of an inorganic gellant and
a polymeric (amido) resin with an amino functional Silane coupling agent The lubricant
sticks of the invention could be inserted into the valve screw and the screw tightened to
apply a securely adhering layer on desired friction/seating surfaces, so as to prevent
leakage of working fluid, and serving functions of lubrication, corrosion resistance and
sealing, even for applications having combined characteristics of hydrocarbon type fluid ,
at a air pressure of upto 6 5kg/cm2, making such lubricant cum sealant capable of
application in a wide range of industrial valves with distinct advantage in user friendly and
cost effective manner