Claims:1. A composition of organic thermic fluid, the composition comprising:
v. 65-95 wt% synthetic aromatics; and
vi. 5-35 wt% poly alpha olefins or polyol esters.

2. The composition as claimed in claim 1, wherein the synthetic aromatics are selected from a group consisting of diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, p-Terphenyl and cyclohexyl benzene.

3. The composition as claimed in claim 1, wherein the synthetic aromatics are a mixture of diphenyl ether and biphenyl in a weight ratio of 73.5:26.5.

4. The composition as claimed in claim 1, wherein the poly alpha olefins or the polyol esters are present in a range of 10-12 wt%.

5. The composition as claimed in claim 1, wherein the composition further comprising an antioxidant in a range of 1-7 wt%, preferably in a range of 2-5 wt%.

6. The composition as claimed in claim 5, wherein the antioxidant is selected from a group consisting of hexamethylene bis-N-phenyl benzenamine, phenyl-[alpha]-napthalamine and phenyl–[beta]-napthalamine.

7. The composition as claimed in claim 1, wherein the composition has a thermal stability up to 320 °C for 72 hours.

8. A method for preparation of a composition of organic thermic fluid, the method comprising:
e) heating at least one synthetic aromatics at a temperature in a range of 30-50°C and stirring reaction mass to obtain a homogenous eutectic solution;
f) pouring poly alpha olefins or polyol esters to said homogenous eutectic solution to obtain the composition of organic thermic fluid.

9. The method as claimed in claim 8, wherein the synthetic aromatics are present in a range of 65-95 wt% and are selected from a group consisting of diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, p-Terphenyl and cyclohexyl benzene.

10. The method as claimed in claim 8, wherein the synthetic aromatics are a mixture of diphenyl ether and biphenyl in a weight ratio of 73.5:26.5.

11. The method as claimed in claim 8, wherein the poly alpha olefins or the polyol esters are present in a range of 5-35 wt%, preferably in a range of 10-12 wt%.

12. The method as claimed in claim 8, wherein the method further comprising an antioxidant in a range of 1-7 wt%, preferably in a range of 2-5 wt%.

13. The method as claimed in claim 8, wherein the antioxidant is selected from a group consisting of hexamethylene bis-N-phenyl benzenamine, phenyl-[alpha]-napthalamine and phenyl–[beta]-napthalamine.

14. The method as claimed in claim 8, wherein the composition obtained has a thermal stability up to 320°C for 72 hours. , Description:FIELD OF THE INVENTION:
The present invention relates to a composition of a stable organic thermic fluid and method of producing the same. Particularly, the present invention relates to a composition of a stable organic thermic fluid and method of producing the said thermic fluid which mainly consists of one or two groups of synthetic aromatics from diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, cyclohexyl benzene, p-Terphenyl and Poly Alfa olefin (PAO) or Polyol ester (POE) as major blending compound.

BACKGROUND OF THE INVENTION:
Solar energy is one of the least utilized form of unconventional energy, because of its abundancy it offers a possible solution to fossil fuel emissions and global climate change arising due to usage of conventional energy sources. Energy received by the earth from sun is approximately 1,20,000 TW of which India receives 1300 TW which is much higher than the current annual global energy consumption rate of about 15 TW. Thus, solar energy becomes an attractive option for carbon free power generation. Solar power is the conversion of energy from sunlight into electricity, either directly using photovoltaics (PV) or indirectly using concentrated solar power (CSP). Concentrated solar power systems use lenses or mirrors and tracking systems to focus a large area of sunlight into a small beam. Photovoltaic cells convert light into an electric current using the photovoltaic effect. Solar PV contributes to more than 99% of the total 26 GW installed solar capacity in India compared to CSP technologies. This variation is primarily due to lack of indigenous component manufacturing and lack of required knowledge for Operation & Maintenance of these CSP plants. However, there has been a renewed interest on CSP systems primarily because of its cost effectiveness at a large scale as compared to Solar PV and also due to lower efficiency of commercial Solar PV (14%) as compared to solar thermal (22%). Another advantage of CSP technologies is the ease of energy storage and power generation from the stored energy in the absence of source, i.e., during night or hostile weather conditions as compared to Solar PV.

Majorly, two types of Heat Transfer fluids (HTFs) are being used for solar thermal applications and those are Organic Heat Transfer fluid (OHTF) and Inorganic HTF (molten salt). Molten salts are generally solids at room temperature and can be used at temperature greater than 550 oC. Due to its high thermal stability, they are used as binary, ternary or quaternary mixtures to reduce its melting point. The main advantage of OHTF is that it avoids problems associated with prior heating and solidification of liquid in operational loop. Limitations of a OHTF is its stability at elevated temperatures and that of molten salt is its high melting point. It is well known that heat to power conversion will be more efficient at higher temperatures thus making it preferable. However, the current heat transfer fluids capable of performing at such higher temperatures (>450 oC) are mostly solids at low temperatures (~100 oC) resulting in significant issues such as chocking in flow systems and secondary start-up system, while the ones in liquid phase at low temperatures are not suitable for such high temperature operations because of their poor thermal stability.

US3907696A discloses new heat transfer agents containing at least three components consisting of by volume 5 to 90% of diphenyl oxide, 5-50% of biphenyl and 5 to 90% of polyphenyl ether having 3 or 4 aromatic nuclei, alkylated biphenyl or diphenyl oxide having 1-4 methyl or ethyl substituents, ethylbenzene oil and mixtures thereof.

US5075022 discloses a heat transfer fluid which maintains a low hydrogen permeation rate at temperatures of 350°-400° c. or higher and its pumpability at temperatures of -10° C. or lower is provided. The fluid is especially useful in solar energy collection applications. A method of reducing fluid impurities from polyphenyls.

WO2015122830A1 relates to dielectric fluids for transformers, and more particularly to the use of certain aromatic compounds as additives to a dielectric liquid in order to reduce the viscosity and especially low temperature viscosity thereof. The invention also relates to the use of such low-viscosity dielectric liquid in a transformer.

Still, there is a need for an organic thermic fluid which can overcomes the limitations of the prior-art documents by having good thermophysical properties, good oxidation stability and high thermal stability simultaneously.

Surprisingly, the inventors of the present invention have found more effective organic thermic fluid with combination of:
• Diphenyl Ether, Biphenyl and Poly Alpha olefins
• Diphenyl Ether, Biphenyl and Polyol Esters
in broad proportion synthesized and shows the good thermophysical properties and thermal stability up to 320°C which has potential competitor in current organic thermic fluid market.

OBJECTIVES OF THE INVENTION:
It is a primary objective of the invention to provide a composition of stable organic thermic fluid and method of producing the said thermic fluid which mainly consists of one or two groups of synthetic aromatics from diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, cyclohexyl benzene, p-Terphenyl and Poly Alfa olefin (PAO) or Polyol ester (POE) as major blending compound.

A further objective of the present invention is to provide a synthetic organic thermic fluid with good oxidation stability and thermal stability up to 320 °C, consists of 5-35% saturated poly alpha olefin and 65-95% synthetic aromatics which consists of at least two groups from diphenyl oxide, biphenyl, cyclohexyl benzene, p-Terphenyl, o-terphenyl and m-terphenyls.

A further objective of the present invention is to provide a stable organic thermic fluid which can be used as heat transfer fluid medium for primary and secondary heating in process heating application up to 320 °C.

Another objective of the present invention is to produce a formulation or composition with stable synthetic aromatic and Poly alpha olefin/Polyol ester to form uniform homogeneous mixture with good oxidation stability, thermal conductivity and overall heat transfer characteristics.

SUMMARY OF THE INVENTION:

The present invention discloses a composition of organic thermic fluid, the composition comprising:
i. 65-95 wt% synthetic aromatics; and
ii. 5-35 wt% poly alpha olefins or polyol esters.

The present invention further discloses a method for preparation of a composition of organic thermic fluid, the method comprising:
a) heating at least one synthetic aromatics at a temperature in a range of 30-50°C and stirring reaction mass to obtain a homogenous eutectic solution;
b) pouring poly alpha olefins or polyol esters to said homogenous eutectic solution to obtain the composition of organic thermic fluid.

In a feature of the present invention, the synthetic aromatics are selected from a group consisting of diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, p-Terphenyl and cyclohexyl benzene.

In a feature of the present invention, the synthetic aromatics are a mixture of diphenyl ether and biphenyl in a weight ratio of 73.5:26.5.

In a feature of the present invention, the poly alpha olefins or the polyol esters are present in a range of 5-35 wt%, preferably in a range of 10-12 wt%.

In a feature of the present invention, the composition further comprising an antioxidant in a range of 1-7 wt%, preferably in a range of 2-5 wt%.

In a feature of the present invention, the antioxidant is selected from a group consisting of hexamethylene bis-N-phenyl benzenamine, phenyl-[alpha]-napthalamine and phenyl–[beta]-napthalamine.

In a feature of the present invention, the composition has a thermal stability up to 320 °C for 72 hours.

In a feature of the present invention, the synthetic aromatics are present in a range of 65-95 wt% and are selected from a group consisting of diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, p-Terphenyl and cyclohexyl benzene.

DETAILED DESCRIPTION OF THE INVENTION

In one aspect, the present invention relates to a composition of organic thermic fluid, the composition comprising:
iii. 65-95 wt% synthetic aromatics; and
iv. 5-35 wt% poly alpha olefins or polyol esters.

In another aspect of the present invention, the present invention discloses a method for preparation of a composition of organic thermic fluid, the method comprising:
c) heating at least one synthetic aromatics at a temperature in a range of 30-50°C and stirring reaction mass to obtain a homogenous eutectic solution;
d) pouring poly alpha olefins or polyol esters to said homogenous eutectic solution to obtain the composition of organic thermic fluid.

In an embodiment of the present invention, the synthetic aromatics are selected from a group consisting of diphenyl ether, biphenyl, o-Terphenyl, m-Terphenyl, p-Terphenyl and cyclohexyl benzene.

In an embodiment of the present invention, the synthetic aromatics are a mixture of diphenyl ether and biphenyl in a weight ratio of 73.5:26.5.

In an embodiment of the present invention, the poly alpha olefins or the polyol esters are present in a range of 5-35 wt%, preferably in a range of 10-12 wt%.

In an embodiment of the present invention, the composition further comprising an antioxidant in a range of 1-7 wt%, preferably in a range of 2-5 wt%.

In an embodiment of the present invention, the antioxidant is selected from a group consisting of hexamethylene bis-N-phenyl benzenamine, phenyl-[alpha]-napthalamine and phenyl–[beta]-napthalamine.

In an embodiment of the present invention, the composition has a thermal stability up to 320 °C for 72 hours.

The present invention relates to development of thermic fluid formulation with one component being stable synthetic aromatic and in blending of alpha olefin in 5-35% results in high oxidation stability and better heat transfer characteristics as commercial with thermally stable up to 320 °C.

The term Poly Alfa Olefin used here refers to hydrocarbon formed by oilgomerization of α-olefin.
CH2 = CHR
where R can be Hydrocarbyl group such as aryl, alkyl or arylalkyl.

The poly Alfa olefins obtained in accordance with embodiments of the present invention may be hydrogenated.

In accordance with present invention, there is provided synthetic organic thermic fluid with good oxidation stability and thermal stability up to 320 °C, consists of 5-35% saturated poly alpha olefin and 65-95% synthetic aromatics consists of at least two groups from diphenyl oxide, biphenyl, cyclohexyl benzene, p-Terphenyl, o-terphenyl and m-terphenyls.

In view therefore, the objective of the present invention is to provide stable organic thermic fluid which can be used as heat transfer fluid medium for primary and secondary heating in process heating application up to 320° C.

Poly alpha olefin (PAO) is formulated by the oligomerisation of petrochemical Alpha olefins (C6-C20) or simple alkene monomer such as 1–Decene/1-Octene. Olefin oligomerisation is the process of forming heavy carbon Alpha olefin with the cationic oligomorisation in presence of Lewis acids such as AlCl3, BF3, FeCl3 results in olefin oligomer. Feed contains olefin monomers and unsaturated compounds with oligomerisation results in formation olefin oligomer and non-reacted compounds so upon separation and hydrogenation of product under catalyst, saturated Poly alpha olefins will be formed. Petrochemical olefins are wax free, with high oxidation stability and good flow properties.

Polyol esters are formulated by transesterification of vegetable oils, fatty acid esters.

Present invention relates to a formulation with stable synthetic aromatic (65-95%) and Poly alpha olefin/Polyol ester (5-35%) to form uniform homogeneous mixture with good oxidation stability, thermal conductivity, and overall heat transfer characteristics.

Individual constituents and proportions of proposed organic thermic fluid shown in Table.1

Table 1: Weight Proportion-Constituents
S. No. Constituents Proportion (%W/W) In-house chemical name
1.
Diphenyl Ether 66.15 OHTF-δ
Biphenyl 23.85
Poly Alpha Olefin - 4 10.00
2.
Diphenyl Ether 66.15 OHT-ζ
Biphenyl 23.85
Polyol Ester-1 10.00
3. Diphenyl Ether 66.15 OHTF-ω
Biphenyl 23.85
Polyol Ester-2 10.00

PREPARATION
DPO + BP Eutectic Mix
Take the crystal sample of Diphenyl Ether or Diphenyl Oxide (DPO) and heat the compound in indirect heating above 30°C using water bath to get liquefied for mixing. Slowly add finely grounded biphenyl (BP) with 99% purity mixture to DPO solvent with mechanical stirring in the specified weight ratio (DPO: BP as 73.5:26.5). Ultrasonicate the solution at 20KHz for 15 to 30 minutes for uniform dispersion of biphenyl and followed by uniform mixing. Kept the solution on hot plate at 50°C with magnetic stirring of 500 RPM for 20 to 30 minutes to obtain a homogeneous solution.
DPO + BP + PAO/POE
Pour the blending solvent PAO/POE (10% W/W) slowly on the eutectic mix with simultaneous mechanical stirring with bulk temperature at 50 °C. Ultrasonicate the solution at 20KHz for 15 minutes to obtain a homogeneous solution.

Proposed thermic fluids with thermophysical properties is shown in Table 1.
Table 1: Thermophysical Properties
Formulation 1 Formulation 2 HP-OHTF-ζ HP-OHTF-ω HP-OHTF-δ
Composition
(w/w %) DPO + BP Synthetic Aromatics DPO + BP + POE - 1 DPO + BP +
POE - 2 DPO + BP + PAO - 4
Density
(gm/cc) 25 oC 1.055 1.07 1.045 1.049 1.025
100 oC 0.994 1.007 0.983 0.985 0.967
Viscosity
(mPa-sec) 25 oC 3.71 11.5 4.37 3.76 3.704
100 oC 0.97 1.61 0.99 0.87 0.80
Pour Point (oC) 12 -18 13 15 15
Flash Point (oC) 113 132 116.5 117.2 122.5
Oxidation Stability (RSSOT-D7545) 126.5 125 - 160 Minutes 165 minutes
Max. operating Temperature
(Inert Atmosphere) (oC) 400 380 320* 320* 320
Specific Heat Capacity
(kJ/kg k) @100°C 1.8 1.769 1.16 1.54 1.56
Neutralization No
(mg KOH/gm) <0.2 0.2 0.02 0 0.14
Thermal Conductivity
(W/m-k) @100°C 0.1259 0.13 N.T 0.118 0.201
Thermal Diffusivity (m2/s) 0.07036E-6 0.0729E-6 N.T 0.161E-6 0.295E-6
Copper Strip Corrosion @40°C 1A N.T 1A 1A 1A
Sulfur Content (ppm) 325 402 250 580 37
Moisture Content (ppm) N.T 200 207 95 206
Surface Tension (Dyne/cm) 40.10 N.T 29.20 25.23 26.80
Reynolds Number* at 100°C (v = 1 m/s, tube ID = 4.57 mm) 4683 2858 4537.6 5174 5523.9
OHTC (W/m2-k) at 100°C 178.2 182 175 184 197

Table 3
DPO+BP+PAO - 4 (10%)
S. No. Compound 1
(DPO + BP) Compound 2
(PAO - 4) Flash Point (°C) Kinematic Viscosity (cSt)-
40°C Oxidation Stability (ASTMD7545) Thermal Stability (ASTMD - 6743) Miscibility MCRT OHTC
(w/m2-K)
YES NO
1. 0 100 219 4 58 ☒
☐
0
2. 100 0 124 2.48 15 Up to 420 Degree Celsius ☒
☐
0 178.2
3. 90 10 122.5 3.704 165 PASS ☒
☐
0 197
4. 80 20 119.5 ☒
☐
0
5. 70 30 112 3.848 <300 ☒
☐
0 192

Table 4
DPO + BP + POE - 2 (10%)
S. No. Compound 1
(DPO + BP) Compound 2
(POE-II) Flash Point Kinematic Viscosity (cSt) Oxidation Stability (ASTMD 7545) - in Minutes Thermal stability (@320 °C) Miscibility MCRT OHTC
(W/m2-K)
YES NO
1. 0 100 ☒
☒

2. 100 0 124 2.48 126.5 Up to 420 °C ☒
☐
178.2
3. 90 10 117.2 3.76 160 PASS ☒
☐
184
4. 80 20 109 ☒
☐

5. 70 30 97 5.475 <300 ☒
☐
179

SPECIFIC HEAT CAPACITY
It is the quantity of heat required to raise the temperature of unit mass of a substance by one Kelvin, unit of Cap is J/kgK. In other words, it denotes the amount of heat a substance can hold before bringing about change in temperature of the substance. This implies that the substance with higher specific heat capacity is better suited to heat transfer process. This is one of the reason why water (Cp =4.186kJ/kgK) is most commonly used in heat transfer applications. It is well known that the driving force behind any heat transfer process is the temperature difference between the systems involved, when this is high the heat transfer will be better and also the material can store more heat for unit change in temperature. Now if a substance with low specific heat capacity is used, the rise in temperature of the substance will be higher than that of a substance with high specific heat capacity for the same heat transferred to the system. This causes the temperature difference to drop rapidly for the system involving substance with low specific heat capacity resulting in lower heat transfer.

Specific heat capacity (Cp) has been measured using NETZSCH simultaneous thermal analyzer (STA) 449 F3 Jupiter, Platinum crucible has been used for specific heat capacity measurement. For Cp measurement using DSC, three simultaneous experiments have been performed.

HEAT TRANSFER COEFFICIENT
The heat transfer coefficient is the proportionality constant between the heat flux and the thermodynamic driving force for the flow of heat. Heat transfer performance is generally quantified by heat transfer coefficient, heat-transfer coefficient is a function of the Reynolds number, the Prandtl number, and the tube diameter. These can be further broken down into the following fundamental parameters: physical properties (namely viscosity, thermal conductivity, and specific heat), tube diameter and mass velocity. Unlike other parameters ‘h’ is a cumulative function of other physical properties, hence this can be used to quantify the overall performance of HTF. A high value of ‘h’ indicates that HTF has properties which boosts the heat transfer performance and vice-versa. Here Overall heat transfer coefficient ‘U’ is estimated in-place of ‘h’ by using High temperature solar loop manufactured by Biojenik Engineering with 2 L tank capacity, working under argon pressure.

THERMAL STABILITY STUDIES
Since most of the Organic HTF undergo boiling before thermal decomposition it becomes inappropriate to measure decomposition temperature by using Thermogravimetric Analysis (TGA). Hence decomposition studies were carried out in autoclave in batch mode. The fluid is initially taken in the autoclave and is then subjected to leak test at 30 bar for 45 minutes. Once no leak was observed the chamber is pressurized with nitrogen to about 10bar and is then heated, once the set temperature is reached the chamber is maintained in isothermal condition for 2 hours. The heater is then switched off and is allowed to reach equilibrium with ambient. Once the temperature reaches desired value the autoclave is vented to remove the gases, the sample is then collected from the autoclave and is weighed. Further studies on physical properties indicate potential decomposition of HTF. To study the variation in physical properties before and after heating an HTF with known decomposition temperature is taken and is subjected to heating as mentioned above. Dowtherm A whose decomposition temperature is 425oC is also subjected to decomposition study so as to quantify the results of in-house HTF.

KEY PARAMETERS
Synthesized Organic Thermic Fluids OHTF-ζ, OHTF-ω and OHTF-δ shows thermal stability (ASTMD-6743) up to 320 °C with evaluation in batch reactor isothermal conditions under nitrogen blanketing and Heat transfer coefficient found to be in the similar range of formulations fluid under similar test conditions of 100°C. Thermophysical properties are also quite good and in the appreciable range of reported thermic fluids.

In the heat medium composition of the present invention, the production method is not particularly limited to petrochemical Olefin produced by synthesizing oligomers of either 1-decene or 1-dodecene. Since petrochemical olefins are free from waxy, sulphur and nitrogen compounds and having good viscosity index, oxidation stability and flow properties, homogeneous solution of these compounds with diphenyl oxide and biphenyl shows good antioxidant and stability characteristics. Petrochemical esters are belonging to Group-V produced by reaction of carboxylic acid and alcohols. Esters are widely used as lube additives due to having excellent lubricity and antioxidant properties. Diphenyl ether normally produced by a phenol bimolecular reaction with zeolite. Biphenyls are produced by oxidative dehydrogenation of benzene.

Table 5
Name Weight (gm) Flash Pt (oC) Viscosity (Pa-s)
25 °C 100 °C
B.
Exp A.
Exp B.
Exp A.
Exp B.
Exp A.
Exp dev. % B.
Exp A.
Exp dev. %
HPTherm-ζ 125 124 119 118.2 0.004370 0.00428 -2.05 0.00099 0.000988 0.2
HP Therm-ώ 120 116 117.2 115.3 0.003760 0.0036 -4.2 0.00087 0.000865 -0.57
HP Therm-δ 125 121 122.5 113.2 0.003704 0.0037 -1.07 0.00080 0.00082 2.5

EXAMPLES:
Synthesis of PAOs
Example-1A:
To a stirred solution of 1-octene (30 mL), AlCl3 (6 g) followed by catalytic amount of de-ionized water (100 µL) is added. This flask is quickly set-up with condenser and the reaction was continued at 50°C for 16 h. After the reaction stopped, reaction is cooled to room temperature and reaction contents are transferred into separating funnel which is then quenched with water (20 mL). The separated water-layer (bottom layer) from the separating funnel is collected and discarded. The top layer in the separating funnel is washed again with water (2 X 20 mL) and the separated water layer is discarded. Top layer is then collected and dried over anhydrous sodium sulfate and then filtered. Collected filtrate was concentrated using rotary evaporator to afford polyalphaolefin Product-1 given below.
Viscosity of PAO-1 @ 40 oC: 35.279 cSt
Viscosity of PAO-1 @ 100 oC: 6.4363 cSt
Pour point of PAO-1: -66 oC
Example-2A:
To a stirred solution of olefin-rich refinery stream (Delayed coaker naphtha) (400 mL), AlCl3 (6 g) followed by catalytic amount of de-ionized water (200 µL) is added. This flask is quickly set-up with condenser and the reaction was continued at 50 oC for 16 hours. After the reaction stopped, the reaction mass is cooled to room temperature and the reaction mass/contents are transferred into separating funnel which is then quenched with water (200 mL). The separated water-layer (bottom layer) from the separating funnel is collected and discarded. The top layer in the separating funnel is washed again with water (2 X 100 mL) and the separated water layer is discarded. Top layer is then collected and dried over anhydrous sodium sulfate and then filtered. Collected filtrate was concentrated using rotary evaporator to afford polyalphaolefin Product-2.

Viscosity of PAO-2 @ 40 oC: 9.614 cSt
Viscosity of PAO-2 @ 100 oC: 2.542 cSt
Pour point of PAO-2: -71 oC
Example-3A:
To a stirred solution of olefin-rich refinery stream (Delayed coaker naphtha) (500 mL), AlCl3 (6 g) followed by catalytic amount of de-ionized water (200 µL) is added. This flask is quickly set-up with condenser and the reaction was continued at 50oC for 16 hours. After the reaction stopped, the reaction mass is cooled to room temperature and the reaction mass/contents are transferred into separating funnel which is then quenched with water (200 mL). The separated water-layer (bottom layer) from the separating funnel is collected and discarded. The top layer in the separating funnel is washed again with water (2 X 100 mL) and the separated water layer is discarded. Top layer is then collected and dried over anhydrous sodium sulfate and then filtered. Collected filtrate was concentrated using rotary evaporator to afford polyalphaolefin Product-3.

Viscosity of PAO-3 @ 40 oC: 46.2 cSt
Viscosity of PAO-3 @ 100 oC: 7.8 cSt
Pour point of PAO-3: -75 oC
Example-4A:
To a stirred solution of olefin-rich refinery stream (Delayed coaker naphtha) (430 mL), AlCl3 (5 g) followed by catalytic amount of de-ionized water (200 µL) is added. This flask is quickly set-up with condenser and the reaction was continued at 50oC for 16 hours. After the reaction stopped, the reaction mass is cooled to room temperature and the reaction mass/contents are transferred into separating funnel which is then quenched with water (200 mL). The separated water-layer (bottom layer) from the separating funnel is collected and discarded. The top layer in the separating funnel is washed again with water (2 X 100 mL) and the separated water layer is discarded. Top layer is then collected and dried over anhydrous sodium sulfate and then filtered. Collected filtrate was concentrated using rotary evaporator to afford polyalphaolefin Product-4.

Viscosity of PAO-4 @ 40 oC: 16.8 cSt
Viscosity of PAO-4 @ 100 oC: 3.8 cSt
Pour point of PAO-4: -75 oC

Synthesis of POEs
Example-1B:
To a reaction flask containing pentaerythritol (50 mmol), oleic acid (205 mmol) in toluene (200 ml), p-toluene sulfonic acid (10 mmol) was added, and dean-stark set up was placed on the reaction flask. The reaction mixture was stirred under reflux conditions for 16 hours. After the reaction stopped, reaction is cooled to room temperature and reaction contents are transferred into separating funnel which is then quenched with water (50 mL). The separated water-layer (bottom layer) from the separating funnel is collected and discarded. The top layer in the separating funnel is washed again with water (2 X 50 mL) and the separated water layer is discarded. Top layer is then collected and dried over anhydrous sodium sulfate and then filtered. Collected filtrate was concentrated using rotary evaporator to afford poly-ol-ester Product-1.
Viscosity of POE-1 @ 40 oC: 68 cSt
Viscosity of POE-1 @ 100 oC: 12.3 cSt
Pour point of POE-1: -21 oC
Example-2B:
To a reaction flask containing pentaerythritol (50 mmol), oleic acid (102 mmol), 2-ethylhexanoic acid (102 mmol) in toluene (200 ml), p-toluene sulfonic acid (10 mmol) was added, and dean-stark set up was placed on the reaction flask. The reaction mixture was stirred under reflux conditions for 16 h. After the reaction stopped, reaction is cooled to room temperature and reaction contents are transferred into separating funnel which is then quenched with water (50 mL). The separated water-layer (bottom layer) from the separating funnel is collected and discarded. The top layer in the separating funnel is washed again with water (2 X 50 mL) and the separated water layer is discarded. Top layer is then collected and dried over anhydrous sodium sulfate and then filtered. Collected filtrate was concentrated using rotary evaporator to afford poly-ol-ester product-2.
Viscosity of POE-2 @ 40 oC: 50.65 cSt
Viscosity of POE-2 @ 100 oC: 8.15 cSt
Pour point of POE-2: -42 oC
Synthesis of Organic Thermic fluid
EXAMPLE 1C:
A 300 mL flask with magnetic stir bar was cleaned with acetone and dried in oven at 90°C after thoroughly evacuated by purging with dry compressed air to eliminate contaminants. The flask was charged with diphenyl ether and indirect heating at 40°C using water bath. Finely grounded biphenyl added to the reaction flask with the weight ratio of 73.5:26.5 (Diphenyl ether: biphenyl). Kept the reaction flask on hot plate and stirred using magnetic stir and continued mechanical stirring at 500 rpm and temperature maintained at 50°C for about half an hour result in eutectic solution. Ultrasonicate the formed eutectic solution at 20 KHz for 15 minutes using Probe ultrasonicator for uniform mixing of the two compounds. Now pour the blending compound PAO/POE (10% w/w) into the reaction mixture with simultaneous mechanical stirring 500 rpm and temperature 50°C. Ultrasonicate the formed homogeneous solution at 20 KHz for 15 minutes. Analysis of prepared thermic fluid by Rapid small scale oxidation test shows significant improvement in oxidation stability as compared to commercial synthetic thermic fluids. Thermal stability tested in batch reactor as per ASTMD-6743 at 320 °C for 72 hours shows good thermal stability as commercial synthetic thermic fluids.

EXAMPLE 2C:
The procedure was essentially same as Example-1C, except there is additional antioxidant (2%) from group of methyl and phenyl based such as but not limited to Hexamethylene bis-N-Phenyl Benzenamine, Phenyl-[alpha]-and/or phenyl–[beta]-napthalamine.

EXAMPLE 3C:
The procedure was essentially same as Example-1C, except there is additional antioxidant (5%) from group of methyl and phenyl based such as but not limited to Hexamethylene bis-N-Phenyl Benzenamine, Phenyl-[alpha]-and/or phenyl –[beta]-napthalamine.

EXAMPLE 4C:
The procedure was essentially same as Example-1C, except there is additional antioxidant (5%) from group of methyl and phenyl based such as but not limited to Hexamethylene bis-N-Phenyl Benzenamine, Phenyl-[alpha]-and/or phenyl–[beta]-napthalamine. Blending compound PAO/POE in the weight ratio of (12%) instead (10%).

EXAMPLE 5C:
The procedure was essentially same as Example-1C, except, there is additional antioxidant (5%) from group of methyl and phenyl based such as but not limited to Hexamethylene bis-N-Phenyl Benzenamine, Phenyl-[alpha]-and/or phenyl–[beta]-napthalamine. Blending compound PAO/POE in the weight ratio of (12%) instead (10%). Base solution consists of Diphenyl Ether (70%), Biphenyl (22%) and finely grounded o-terphenyl (8%) by weight and mixing temperature 65°C instead 50°C and blending with PAO/POE at 50°C.