Abstract: The present invention relates to a fuel composition useful for jet engines. Particularly, the Invention provides a high density and thermally stable fuel composition useful for Ramjet propulsion system. The fuel has advantageous features in terms of having lesser aromatic content, a flash point greater than 60°C, lesser viscosity, higher density and high calorific value. The Invention also extends to provide a highly efficient process for the production of Penta Cyclo Tetra Decane (PCTD) which is further utilized in the production of Ramjet fuel composition of the present Invention.
FIELD OF THE INVENTION
The present invention relates to a fuel composition useful for jet engines. Particularly, the
Invention provides a high density and thermally stable fuel composition useful for Ramjet
propulsion system.
The Invention also extends to provide a highly efficient process for the production of Penta
Cyclo Tetra Decane (PCTD) which is further utilized in the production of Ramjet fuel
composition of the present Invention.
In the present embodiment, the invention has been described with reference to Ramjet
propulsion system, however such description should not be considered as restricting the
scope of the present invention. Further, it would be possible for a person skilled in the art to
practice the present Invention considering other jet engines as well without departing from
the scope of the present invention.
BACKGROUND OF THE INVENTION
Aerospace propulsion has achieved by different propulsive devices based on several
principles. The propulsive devices based on chemical energy can be classified as i) Air
breathing engines, ii) Non air breathing engines and iii) Hybrid engines. In the case of air
breathing engines-piston engines, gas turbine engines, ramjets and scramjets, the oxidizer is
atmospheric air. Flying for short duration at speeds of M= 2-3 has resulted in the
development of ramjets (for missiles). Ramjet does not produce any thrust at zero flight
speed. Therefore ramjets need an auxiliary system which propels to a speed (or Mach
number) range where they can work. In most missile systems, rocket engines boost the
vehicle to a range where ramjets can begin functioning. The data on ramjets are generally not
available because ramjets are mostly contemplated for use in military applications. Three of
the applications correspond to solid fuel ramjet (SFRJ), integral ram rockets (IRR) and liquid
fuel ramjet (LFRJ).
Presently, jet fuel plays two important roles in advanced flying machines. The first and most
obvious is to provide the propulsive energy for flight and second, the role fuel plays as the
2
coolant for airframe and engine subsystems. The need to cool hot parts in the engine had been
evident ever since the invention of the internal combustion engine. As engine performance
goals and flight speeds have increased, the need for 'thermal management' has become
apparent. Unfortunately, the thermal stability of present aviation turbine fuel is very limited.
Current and future vehicles will stress the fuel to higher temperatures. Fuel degradation
causes fouling/coking in engine main burner, fuel nozzles, fuel manifolds and injectors etc.
As technologies advance in the aerospace industry, a strong desire has emerged to design
more efficient, longer life, reusable liquid hydrocarbon fueled rocket engines. Hydrocarbon
fuel less in aromatics and high in density and calorific value are desirable for ramjet
propulsion system. To achieve this goal, a more complete understanding of the thermal
stability and chemical make up of the hydrocarbon propellant is needed. Liquid rocket
engines face extremely challenging thermal environments, and almost inevitably require
copper or copper alloys in construction due to their high thermal conductivity properties. It
has long been known that sulfur compounds and copper are incompatible, therefore a better
understanding of fuel's thermal stability and chemical interaction with copper chamber liners
is needed. Thermal stability describes the effect of temperature on hydrocarbon fuels. When a
fuel reaches the thermal decomposition temperature, its chemical structure begins to
breakdown and it deposits a hard film on engine parts as well as other plumbing within the
propulsion system in a process called coking. A thermally unstable fuel reaches this point at
relatively low temperatures and short time within the heated environment. Generally Jet
engine fuel begins to thermally decompose and forms "coke" inside the chamber. The
deposits formed contain a noticeable amount of copper sulfide. This phenomenon has been
attributed to sulfur compounds contained within the fuel reacting with the wetted copper
walls. The main concern over this reaction is that as the CU2S is formed, it leaves "pits" or
"craters" in some sections of the liner wall and flow obstructing particle "barnacles" in other
areas. Carbon deposits now have a rough surface finish to adhere to the chamber, which
contributes to increasing localized wall temperature and further coking. The total effect leads
to increased pressure drop in the system, decreased efficiency, and loss of structural integritypossibly
resulting in engine failure. In order to move forward, new improved fuels are
desired.
Now a days fuel technology and material development remain two of the main challenges to
the realization of the high speed flight vision. Though hydrogen is a good fuel in terms of its
heat of combustion and cooling capacity but two major disadvantages are there, first, its
3
handling is not safe and second, it has very low density. Greater ease of use and higher
density make hydrocarbon fuels an attractive option for Ramjet engines.
Therefore, there is a need to develop new set of hydrocarbon fuels to meet the requirements
of Ramjet Engines.
The exo-isomer of hydrogenated dicyclopentadiene known as JP-10, perhydro di
norbornadiene known as RJ-5, are being used as the high energy liquid fuel for rockets as
well as jet engines such as turbo-jet, ram-jet, pulse jet and the like. However, the former fuel
i.e. JP-10 has disadvantages such as insufficient net heat of combustion, insufficient density
and the like, whilst RJ-5 has a disadvantage of having extremely high cost, because synthesis
of the fuel is difficult, besides a raw material of norbornadiene is insufficiently supplied.
US 5320692 A discloses a solid fuel ramjet composition. The composition comprises
Hydroxyl terminated polybutadiene aluminum, magnesium, and boron carbide. The solid fuel
has inherent property of having lower specific impulse or the lower exhaust velocity as
compared to the liquid fuel composition. Therefore, a liquid jet fuel composition is always
preferred over the solid fuel composition.
WO2005/019393 (Fuel For Jet, Gas Turbine, Rocket, And Diesel Engines) discloses fuel for
jet engine (applicable for ramjet engine also).The fuel composition essentially comprises
i
A
m . wherein A moiety is selected from benzene, toluene, xylene, cyclohexane, L moiety
is a linear acyclic aliphatic hydrocarbyl such that the sum of carbons in the L moiety, R', and
R" is from 5 to 25 carbons, fuel additives and from conventional jet/ gas turbine/ rocket
blendstocks like ultra low sulfur refined petroleum blendstocks or Fischer Tropsch
blendstocks. This fuel has density of atleast about 0.700g/ml, preferably about 0.700g/ml to
about 0.900g/ml. However, the technology disclosed in this patent application is not specific
for Ramjet engine and also the density of the fuel is too low for ramjet application.
US4087257 (High density-high volumetric heating value liquid ramjet) discloses a
combination of about 80 weight percent hydrogenated norbornadiene dimer and about 20
weight percent iso-butyl benzene which meet the volumetric heat of combustion, viscosity
and flash point requirements of the Modern Ramjet Engine. The combination exhibits density
of 1.02 g/ml (at 20 DEG C) and a freezing point below -40 DEG C. However, the viscosity of
4
this fuel at -40 DEG C is 162Cp, which is too high for pumping and therefore this fuel is not
suitable for ramjet application.
However, there is still need to explore about the high density and thermally stable aviation
fuel which could be used in jet engines like Ramjet Engine.
OBJECT OF THE INVENTION
A main object of the invention is to overcome the drawbacks / disadvantages of the prior art.
Yet another object of the invention is to provide a high density and thermally stable fuel
composition for Ramjet propulsion engine.
Yet another object of the invention is to provide a jet fuel composition which has a density
ranging from 0.840 to 0.845 gm/cc (at 20°C) measured by the method D-1298.
Yet another object of the invention is to provide a jet fuel composition which has higher
thermo-oxidizing stability as the composition qualifies Jet Fuel Thermal Oxidation Tester
(JFTOT) (D-3241).
Yet another object of the invention is to provide a jet fuel composition which has aromatic
content of less than 10%.
Yet another object of the invention is to provide a jet fuel composition which has differential
pressure drop of about 15mm Hg.
Yet another object of the invention is to provide a jet fuel composition which does not
degrade/decompose at a temperature ranging to about 240 degree Celsius.
Yet another object of the invention is to provide an aviation turbine fuel having boiling
temperature ranging from 200 to 260 degree celsius.
Yet another object of the invention is to provide an aviation turbine fuel which can stand upto
the temperature of about or more than 275 degree celsius.
Yet another object of the invention is to provide a process for the production of aviation
turbine fuel having boiling temperature ranging from 200 to 260 degree celsius.
Yet another object of the invention is to provide a process for the production of high density
and thermally stable fuel composition useful for Ramjet propulsion engine.
Yet another object of the invention is to provide a process for the production of jet fuel
composition which could be upscaled to about 10 litres batch level.
5
Yet another object of the invention is to provide an efficient process for the production of
Synthetic Penta Cyclo Tetra Decane which could be completed in approximately 0.5 to 2
hours.
These and other advantages of the present invention will be more apparent from the foregoing
description in conjunction with the accompanying drawings.
SUMMARY OF THE INVENTION
The following presents a simplified summary of the invention in order to provide a basic
understanding of some aspects of the invention. This summary is not an extensive overview
of the present invention. It is not intended to identify the key/critical elements of the
invention or to delineate the scope of the invention. Its sole purpose is to present some
concept of the invention in a simplified form as a prelude to a more detailed description of
the invention presented later.
In an aspect of the present Invention, there is provided a jet fuel composition comprising an
aviation turbine fuel having boiling temperature ranging from 200 to 260 degree Celsius, a
synthetic hydrocarbon i.e. Pentacyclotetradecane (PCTD), Decahydronapthalene and an
auxiliary component.
In another embodiment of the Invention, there is provided a jet fuel composition comprising
an aviation turbine fuel having boiling temperature ranging from 200 to 260 degree Celsius,
which is present in an amount ranging from 70 to 80 % (v/v), synthetic hydrocarbon i.e. penta
cyclo tetradecane present in an amount ranging from 15 to 20% (v/v), decahydronapthalene
present in an amount ranging from 5 to 15%(v/v) and an auxiliary component present in an
amount of about 0.02 (w/w)%.
In another embodiment of the Invention, there is provided a process for the production of a
synthetic pentacyclotetradecane, said process comprising steps:
a) selective dimerization of bicycloheptadiene to obtain hepta cyclotetradecane, said
dimerization occurs in the presence of a catalyst which is selected from a group comprising of
cobalt bromide, Triphenylphosphine complex, Boron Trifluoride complex etherate or
6
combination(s) thereof and a toluene based solvent, wherein said Triphenylphosphine
complex, Boron Trifluoride complex etherate and Bicycloheptadiene is present in a molar
ratio of 1:4: 200 to 400.
b) hydrogenation of Hepta cyclotetradecane obtained from step (a) to obtain
pentacyclotetradecane wherein said hydrogenation is performed in the presence of 5%
Rh/C catalyst present in a methyl cyclohexane solvent in a ratio of about 1:2.
BRIEF DESCRIPTION OF THE DRAWINGS
The following drawings are illustrative of particular examples for enabling methods of the
present invention, are descriptive of some of the methods, and are not intended to limit the
scope of the invention. The drawings are not to scale (unless so stated) and are intended for
use in conjunction with the explanations in the following detailed description.
Figure 1: Reaction scheme for synthesis of PCTD
DETAILED DESCRIPTION OF THE INVENTION
Accordingly, the present Invention provides a hydrocarbon based high density and thermally
stable fuel composition. The fuel composition essentially comprises a special cut (edge) of
Aviation Turbine Fuel (ATF), a synthetic hydrocarbon (i.e. pentacyclotetradecane),
decahydronaptlialene and an additive/ auxiliary component. The composition is well suited for
application in Liquid Fuel Ramjet (LFRJ).
The hydrocarbon based fuel has surprising features in the terms of having lesser aromatic
content, a flash point greater than 60 C, a viscosity less than 60cSt (at -40 C), high in density
(.842 gm/cm3) and high calorific value (43000 KJ / kg), which are the desirable
characteristics for ramjet propulsion system.
Specifically, the fuel composition comprises about 70 to 80%(v/v) of special cut of Aviation
Turbine fuel (ATF), which has boiling point ranging from 200 to 260 degree Celsius, Penta
cyclo tetra decane (PCTD) present in an amount ranging from 15 to 20%(v/v),
Decahydronaphthalene present in an amount ranging from 5 to 15%(v/v), and auxiliary
component like 2,6-Di-tert-butyl-4-methyl phenol (DBPC) in an amount of about 0.02 wt%.
7
The jet fuel composition has advantageous characteristic of having the desired volumetric
heat of combustion, viscosity, aromatic content and flash point requirements for running of
the Ramjet Engine.
The ATF is a mixture of paraffinic (straight chain), naphthenic and aromatic (ring structured)
compounds produced from the distillation of petroleum crude. The mixture has a minimum
of freezing point and a certain boiling range,as required for the propulsion of Ramjet Engines.
This ATF is further used for the production of high density Ramjet fuel.
Process for the production of fuel composition:
The fuel composition is prepared by blending special cut of ATF (aviation turbine fuel) and
synthetic liquid hydrocarbon fuel i.e. 'Pentacyclo tetradecane'. The process is up-scaled at
semi pilot plant level to yield 10 litre of the fuel.
The process is divided into following three phases:
(A) Synthesis of PCTD;
(B) Preparation of special cut of ATF K-50;
(C) Major blending, formulation with additive and physical properties evaluation (ASTM).
These steps are detailed below:
(A) Synthesis of Pentacyclo Tetradecane (PCTD):
Bi cyclo heptadiene (BCH) is selectively dimerised to heptacyclo tetradecane (HCTD) using
Cobalt (II) bromide, Tri phenyl phosphine (PPI13) complex and Boron tri fluoride etherate as
catalyst(s) in Toluene. A suitable solvent toluene is used in the dimerization reaction. Since
the dimerization reaction is exothermic the solvent can serve as heat sink. It can also
solubilize the reaction components and thereby obtain good mixing. The excessive amount of
solvent can decrease the reaction rate and that can adversely affect the economics for a
commercial operation. The selective dimerization of NBD occurs in a liquid phase and
therefore it is not desirable to have the reaction temperature largely exceed the boiling point
8
of the BCH. Conversely if the temperature is much below the optimal temperature for the
dimerization, the rate would be too low. Therefore, the specific customization has been done
for reaction temperature and time. Number of experiments are further carried out to optimize
the various reaction parameters, viz. (i) Reaction temperature (ii) Reaction time (iii) Molar
ratio of catalyst (iv) Solvent and (v) Effect of pressure on the reaction. The optimized
parameters are mentioned below in Table 1:
Optimum Parameters:
1.
2
3.
4.
5.
Molar Ratio
Reaction Temperature
Reaction Time
Initial N2 Pressure
Solvent
•
•
•
Complex : BF3. OEt2 : BCH
1 : 4 : 400
80° C
0.5 Hrs.
7.5 Kg./cm2
dry toluene: BCH (1:1.5)
Table 1
The above mentioned parameters provided about 84% Heptacyclo Tetradecane (HCTD)
conversion with 85% selectivity.
The solid Heptacyclo Tetradecane is hydrogenated to PCTD using 5% Rh/C catalyst in
methyl cyclohexane (Solvent) in the ratio of about 1:2 at temperature ranging from 200 to
220 C and hydrogen pressure 600 psi in parr reactor. After hydrogenation liquid PCTD is
obtained in quantitative yield 98%. The material is characterized by IR and NMR has been
and is evaluated for its physical properties. The reaction scheme for synthesis of PCTD is
shown in Fig 1.
(B) Preparation of Special cut of ATF:
9
A particular grade of aviation turbine fuel ATF K-50 obtained from IOCL is used as raw
material. This has been further customized by subjecting it to a process of acid treatment
where aromatic content of the fuel is brought down to be low 10% by volume. Fuel is washed
with distilled water several times to remove its extra acidic nature and brought to neutral
value of pH. After this treatment total acidity and chemical composition is determined in the
laboratory. In the next step, this acid treated ATF is subjected to distillation to remove its
lower cut boiling below 200°C. Distillation is done in a round bottom flask using heating
mantle. Reliable parameters are generated to collect desirable boiling range of ATF. This
higher cut is evaluated for its physical properties.
(C) Blending & formulation of fuel samples:
A high energy high density hydrocarbon fuel for Ramjet was prepared through the specific
blending of synthesized PCTD, low aromatic ATF and commercially available
decahydronaphthalene. The fuel has been analyzed for its physical properties. Depending on
the requirement of ramjet fuel, various blends were prepared and their resulting properties
were determined. Volumetric ratio of 15% PCTD, 80% low aromatic ATF and 5%
decahydronaphthalene has excellent properties to meet requirement of ramjet fuel.
Decahydronaphthalene has several potential benefits such as enhanced fuel density and a
lowered fuel freeze point leading to better high altitude operability. This naphthenic
component is commercially available but it has a drawback of having low flash point (57°C).
Therefore in the present invention only 5% decahydronaphthalene is used to formulate the
required fuel composition. Finally 0.02 wt% of 2, 6-Di-tert-butyl-4-methyl phenol (DBPC) is
added to improve oxidation stability. The resulting fuel is then tested for its physico-chemical
characteristics to explore its suitable applicability as Ramjet fuel.
(D) Evaluation:
The formulated fuel was evaluated for the following properties in comparison with Russian
fuel T-6
SI. No. PROPERTIES
METHODS
10
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
Appearance
Density of 20°C, (gm/cc )
Kinematic viscosity, (mm /sec):
At 20°C
At-40°C,Max
Low combustion heat, (kcal/kg)
Height of soot less flames (mm)
Acidity, mg of KOH for 100 cm3 of fuel:
Flash point in closed crucible, °C not below
Temperature of beginning of crystallization, °C
Thermo oxidizing stability.
(JFTOT Test)
Fraction of total aromatic hydrocarbons, (vol %)
Colour test with standing on copper plate
Visual
D-1298
D-448
D-3338
D-1322
D-3242
D-56
D-2386
D-3241
D-1319
D-130
Table 2
Laboratory Evaluation Report of Developed fuel, special cut of ATF, PCTD, and
T-6 fuel:
The developed fuel has also been compared with other existing fuels and the differentiating
characteristics are mentioned below in the table:
SI.
No.
Properties Special cut of ATF
PCTD
Developed
Fuel
T-6 Fuel
11
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
Appearance
Density at 20°C,
(gm/cc)
Kinematic viscosity,
(mm /sec):
At 20°C
At-40°C,Max
Low combustion heat,
(kcal/kg)
Height of soot less
flames (mm)
Acidity, mg of KOH
for 100 cm3 of fuel:
Flash point in closed
crucible, °C not below
Temperature of
beginning of
crystallization, °C
Thermo oxidizing
stability.
(JFTOT Test)
Fraction of total
aromatic
hydrocarbons, (vol %)
Colour test with
standing on copper
plate
colourless
0.794
2.2
13.82
10208
23
0.068
68
<-50
pass
8.5
withstand
Colourless
1.05
15
Viscous
10754
24
0.047
115
<-50
—
Nil
Withstand
colourless
0.843
2.8
17.29
10316
24
0.06
65
<-50
pass
8.2
withstand
colourless
0.842
2.66
18.9
10235
24
0.037
73
<-50
pass
7.9
withstand
12
Table 3
The following description is of exemplary embodiments only and is not intended to limit the
scope, applicability or configuration of the invention in any way. Rather, the following
description provides a convenient illustration for implementing exemplary embodiments of
the invention. Various changes to the described embodiments may be made in the function
and arrangement of the elements described without departing from the scope of the invention.
In an embodiment of the present Invention, there is provided a jet fuel composition
comprising components selected from a group comprising an aviation turbine fuel having
boiling edge of more than 200 degree Celsius, a synthetic hydrocarbon i.e. penta
cyclotetradecane, decahydronapthalene, an auxiliary component or any combination thereof.
In another embodiment of the present Invention, there is provided an aviation turbine fuel
having boiling edge of more than 200 degree Celsius present in an amount of about 80 v/v%,
a synthetic hydrocarbon i.e. penta cyclo tetra decane present in an amount of about 15 wt%,
decahydronapthalene present in an amount of about 5 wt% and an auxiliary component
present in an amount of about 0.02 wt%.
In another embodiment of the present Invention, the aviation turbine fuel is ATF K-50.
In another embodiment of the present Invention, the auxiliary component is 2,6- Di- tertbutyl-
4-methyl phenol.
In another embodiment of the present Invention, there is provided a synthetically produced
Penta cyclotetra decane.
In another embodiment of the present Invention, there is provided a process for the
production of Penta cyclotetra decane.
The invention will now be explained with the help of following examples. However, the
scope of the invention should not be limited to these examples as the person skilled in the art
can easily vary the proportion of the ingredients and combinations.
Example 1:
Cobalt containing catalyst has been extremely effective in the synthesis of the heptacyclic
NBD Dimer. An experiment was conducted for the determination of the optimum reaction
temperature. So, reaction at different temperature keeping all other parameters were fixed
under nitrogen atmosphere.
13
S. No.
1
2
3
4
5
6
Molar ratio of reactants
Co (II) Br.TPP: BF3.OEt2:
NBD
1 : 4: 200
Time hours
14 hours
Temperature
(degree
Celsius)
40
50
60
70
80
90
%
Conversion
Nil
Nil
50
60
90.8
92
%
Selectivity
Nil
Nil
82.3
84.56
84.56
80
Table 4
The above table 4 reveals that the maximum conversion to dimer is obtained at 80 degree
Celsius.
Example 2:
Another experiment was done to optimize reaction time. In the experiment, it was found that
there is no need to heat the reaction mixture for 12 to 14 hours further. The data is give in the
below table 5.
s.
No.
1
2
3
4
5
6
7
8
Molar ratio of
reactants
Co (II) Br.TPP:
BF3.OEt2: NBD
1 : 4 :
200
1: 4: 400
Time
hours
14
12
10
8
6
4
2
2
Temperature
(degree
Celsius)
80
% Conversion
90
91
90
88
87.5
85
85
84
% Selectivity
84.56
83.40
84.00
85.00
86.00
84.2
85.0
84
Table 5
14
Run no. 8 in above table 5 reveals that consistent dimer conversion with selectivity is
obtained even on upscaling the reaction.
Example 3:
Another experiment was carried out to optimize reaction time, which has been further
reduced to 0.5 hours from 2 hours under the nitrogen pressure of 7.5kg/cm , which shows that
the percent selectivity and percent conversion has been achieved with good value for the time
hours ranging from 0.5hours to 2hours.
s.
No.
1
2
3
4
5
6
7
Molar ratio of
reactants
Co (II) Br.TPP:
BF3.OEt2: NBD
1 : 4 : 400
Time
hours
2
1.5
1.0
0.5
0.5
0.5
0.5
Temperature
(degree
Celsius)
80
N2
Pressure
7.5
Kg/cm2
%
Conversion
90
88
87
86
83.2
84
84
%
Selectivity
48.5
63.40
80.00
84.00
85.00
85.00
85.00
Table 6
15
1) A jet fuel composition comprising an aviation turbine fuel having boiling temperature
ranging from 200 to 260 degree Celsius, synthetic penta cyclotetradecane,
decahydronapthalene and an auxiliary component.
2) A jet fuel composition comprising an aviation turbine fuel having boiling temperature
ranging from 200 to 260 degree Celsius, which is present in an amount ranging from
70 to 80%(v/v), synthetic penta cyclotetradecane present in an amount ranging from
15 to 20% (v/v), decahydronapthalene present in an amount ranging from 5 to 15
%(wt/wt) and an auxiliary component present in an amount of about 0.02 wt%.
3) The jet fuel composition as claimed in claim 1 or 2, wherein the density of said fuel
ranges from 0.840 to 0.845gm/cc at 20 degree Celsius.
4) The jet fuel composition as claimed in claim 1 or 2, wherein the break point
temperature of the fuel composition as per Jet Fuel Thermal Oxidation Tester
(JFTOT) is about 275 degree Celsius.
5) The jet fuel composition as claimed in claim 1 or 2, wherein the aromatic content of
said fuel is less than 10vol%.
6) The jet fuel composition as claimed in claim 1 or 2, wherein the flash point of said
fuel is more than 65 degree Celsius.
7) The jet fuel composition as claimed in claim 1 or 2, wherein said auxiliary
component is 2,6- Di- tert-butyl-4-methyl phenol.
8) The jet fuel composition as claimed in claim 1 or 2, wherein said aviation turbine fuel
is ATF K-50.
9) A process for the production of a synthetic pentacyclotetradecane, said process
comprising steps:
a) selective dimerization of bicycloheptadiene to obtain hepta cyclotetradecane,
said dimerization occurs in the presence of a catalyst which is selected from a
group comprising of cobalt bromide, Triphenylphosphine complex, Boron
Trifluoride complex etherate or combination(s) thereof and a toluene based
solvent, wherein said Triphenylphosphine complex, Boron Trifluoride
16
complex etherate and Bicycloheptadiene is present in a molar ratio of 1: 4: 200
to 400.
b) hydrogenation of Hepta cyclotetradecane resulting from step (a) to obtain
pentacyclotetradecane wherein said hydrogenation is performed in the
presence of 5% Rh/C catalyst present in a methyl cyclohexane solvent
in a ratio of about 1:2.
10) The process as claimed in claim 9, wherein said hydrogenation is performed at a
temperature ranging from 200 to 220 degree Celsius and a hydrogen pressure of about
600psi.
11) The process as claimed in claim 9, wherein said toluene based solvent comprises dry
toluene and Bicycloheptadiene in a ratio of about 1: 1 to 2.
12) The process as claimed in claim 9, wherein the reaction temperature ranges from 75
to 90 degree celsius.
13) The process as claimed in claim 9, wherein the reaction time ranges from 0.5 to 2
hours.
14) The process as claimed in claim 9, wherein the initial nitrogen pressure ranges from
7.5kg/cm2to 10 kg/cm2.
15) The process as claimed in claim 9, wherein hepta cyclotetradecane conversion rate is
about 84% with about 85% selectivity.
| Section | Controller | Decision Date |
|---|---|---|
| # | Name | Date |
|---|---|---|
| 1 | 2851-del-2013-Form-3.pdf | 2014-03-12 |
| 1 | 2851-DEL-2013-RELEVANT DOCUMENTS [26-09-2023(online)].pdf | 2023-09-26 |
| 2 | 2851-del-2013-Form-2.pdf | 2014-03-12 |
| 2 | 2851-DEL-2013-RELEVANT DOCUMENTS [27-09-2022(online)].pdf | 2022-09-27 |
| 3 | 2851-DEL-2013-US(14)-HearingNotice-(HearingDate-15-10-2020).pdf | 2021-10-17 |
| 3 | 2851-del-2013-Form-1.pdf | 2014-03-12 |
| 4 | 2851-DEL-2013-RELEVANT DOCUMENTS [05-10-2021(online)].pdf | 2021-10-05 |
| 4 | 2851-del-2013-Drawings.pdf | 2014-03-12 |
| 5 | 2851-DEL-2013-IntimationOfGrant21-12-2020.pdf | 2020-12-21 |
| 5 | 2851-del-2013-Description (Complete).pdf | 2014-03-12 |
| 6 | 2851-DEL-2013-PatentCertificate21-12-2020.pdf | 2020-12-21 |
| 6 | 2851-del-2013-Correspondence-others.pdf | 2014-03-12 |
| 7 | 2851-DEL-2013-Written submissions and relevant documents [30-10-2020(online)].pdf | 2020-10-30 |
| 7 | 2851-del-2013-Claims.pdf | 2014-03-12 |
| 8 | 2851-DEL-2013-Correspondence to notify the Controller [13-10-2020(online)].pdf | 2020-10-13 |
| 8 | 2851-del-2013-Abstract.pdf | 2014-03-12 |
| 9 | 2851-DEL-2013-CLAIMS [24-07-2019(online)].pdf | 2019-07-24 |
| 9 | 2851-DEL-2013-Form-1-(24-03-2014).pdf | 2014-03-24 |
| 10 | 2851-DEL-2013-Correspondence-Others-(24-03-2014).pdf | 2014-03-24 |
| 10 | 2851-DEL-2013-FER_SER_REPLY [24-07-2019(online)].pdf | 2019-07-24 |
| 11 | 2851-del-2013-GPA-(24-06-2014).pdf | 2014-06-24 |
| 11 | 2851-DEL-2013-OTHERS [24-07-2019(online)].pdf | 2019-07-24 |
| 12 | 2851-del-2013-Correspondence-Others-(24-06-2014).pdf | 2014-06-24 |
| 12 | 2851-DEL-2013-FER.pdf | 2019-01-28 |
| 13 | 2851-del-2013-Correspondence-Others-(24-06-2014).pdf | 2014-06-24 |
| 13 | 2851-DEL-2013-FER.pdf | 2019-01-28 |
| 14 | 2851-del-2013-GPA-(24-06-2014).pdf | 2014-06-24 |
| 14 | 2851-DEL-2013-OTHERS [24-07-2019(online)].pdf | 2019-07-24 |
| 15 | 2851-DEL-2013-Correspondence-Others-(24-03-2014).pdf | 2014-03-24 |
| 15 | 2851-DEL-2013-FER_SER_REPLY [24-07-2019(online)].pdf | 2019-07-24 |
| 16 | 2851-DEL-2013-CLAIMS [24-07-2019(online)].pdf | 2019-07-24 |
| 16 | 2851-DEL-2013-Form-1-(24-03-2014).pdf | 2014-03-24 |
| 17 | 2851-DEL-2013-Correspondence to notify the Controller [13-10-2020(online)].pdf | 2020-10-13 |
| 17 | 2851-del-2013-Abstract.pdf | 2014-03-12 |
| 18 | 2851-DEL-2013-Written submissions and relevant documents [30-10-2020(online)].pdf | 2020-10-30 |
| 18 | 2851-del-2013-Claims.pdf | 2014-03-12 |
| 19 | 2851-DEL-2013-PatentCertificate21-12-2020.pdf | 2020-12-21 |
| 19 | 2851-del-2013-Correspondence-others.pdf | 2014-03-12 |
| 20 | 2851-DEL-2013-IntimationOfGrant21-12-2020.pdf | 2020-12-21 |
| 20 | 2851-del-2013-Description (Complete).pdf | 2014-03-12 |
| 21 | 2851-DEL-2013-RELEVANT DOCUMENTS [05-10-2021(online)].pdf | 2021-10-05 |
| 21 | 2851-del-2013-Drawings.pdf | 2014-03-12 |
| 22 | 2851-DEL-2013-US(14)-HearingNotice-(HearingDate-15-10-2020).pdf | 2021-10-17 |
| 22 | 2851-del-2013-Form-1.pdf | 2014-03-12 |
| 23 | 2851-DEL-2013-RELEVANT DOCUMENTS [27-09-2022(online)].pdf | 2022-09-27 |
| 23 | 2851-del-2013-Form-2.pdf | 2014-03-12 |
| 24 | 2851-DEL-2013-RELEVANT DOCUMENTS [26-09-2023(online)].pdf | 2023-09-26 |
| 24 | 2851-del-2013-Form-3.pdf | 2014-03-12 |
| 1 | 2851del2013_28-11-2018.pdf |