|Title of Invention||
THE PROCESS OF EXTRACTING STEROL FROM DEODOURISED DISTILLATES WHICH IS A BY PRODUCT RECOVERED DURING REFINING OF SOYBEAN OIL FROM SOYBEAN SEEDS
|Abstract||An industrial process of extracting sterol from deodorized distillate, which is a byproduct recovered during refining of Soybean oil from Soybean seeds. Compressing the steps of : i. Heating the viscose deodorized distillate unto liquid state by a heating coil kept inside a tank ; ii. Pumping the liquefied distillate of step (I) to molecular distillation Plant and degassing the liquefied distillate in the plant ; iii. Boiling the liquid distillate of step (ii) in the molecular distillation plant about 120oC and cooling it subsequently that removes 15 to 20% of fatty acid ; iv. Repeating the process of step (iii) thrice to recover major portion of fatty acids ; v. Superheating the residual liquid distillate after the 4th stage to about 240 -250oC and collecting the residues in form of vaporous containing sterol & fatty acids ; vi. Dissolving the content of step (v)in a crystallizer unit by a suitable solvent which is flour times the mass of the residue and cooling the system by chilled water at 10oC to precipitate the crystals & filtered to separate undesirable materials ; vii. Loading the filtrate of step (vi) to a reflex vessel and refluxing further with methanol / acetone for separation of residual fatty acids from the filtrate ; viii. Vacuum trying the filtrate of step (vii) at 50oC to remove the solvent 85 obtaining the pure sterol.|
|Full Text||FORM 3A ( 2 A)
THE PATENTS ACT, 1970
COMPLETE SPECIFICATION SECTION (10) Rule 13
THE PROCESS OF EXTRACTING STEROL
FROM DEODOURISED DISTILLATES
WHICH IS A BY PRODUCT RECOVERED DURING
REFINING OF SOYBEAN OIL FROM SOYBEAN SEEDS
SONIC BIOCHEM EXTRACTIONS LTD., A Limited Company under the Companies Act, 1956, having its office at 38, Patel Nagar, Indore, Madhya Pradesh, India, PIN 452 001.
The following specification particularly describes and ascertains the nature of this invention and the manner in which it is to be performed:-
This invention relates to the extraction of Sterol from the deodourised distillates. More particularly the extraction of the Sterol is from the deodourised distillates, which is a byproduct recovered during the refining of Soybean oil from Soybean seeds. Soybean is a natural crop having multifarious uses for the human beings. It had its origin in U.S.A and was developed in INDIA around 1980 because of its slindyness and high oil yield and its uses in improving nitrogen contents of the land. The crop had very good growth and the major portion was developed in M.P. which accounts for 70% and the rest developed in Rajasthan and some parts of Vidharba in Maharashtra. The size of crop is about 125 lac tons per year which yields 25 lacs tons of oil.
Soybean is a natural boon to humanity and it contains oils, proteins, phospholipids, Vitamin E (Tocopherol) and fatty acids. Till now conventionally in India the crop is being used only for oil extraction and Deodourised Distillate (DOD) sludge and gums separated during oil refinery process are not being used for any value addition process although these contain valuable fractions.
Our R & D unit has developed the process and the technology for fractionation and purification of Sterol. Soybean -Sterol is another important group of vegetable compounds. These group of substances bear striking similarity to cholesterol. The most important group of phytosterols found in the Soybean are beta-sitosterol, campa-sterol and stigma-sterol. Some of the application of the Soybean -sterol are as follows :-
Soybean Sterol is basic material for intermediate sterols like 17-keto sterol which has a wide applications in steroidal drugs. Sterol is used as co-emulsifier in many cosmetic preparations. It is also used in dermatological treatments like inflammatory reactions, neurodermatitis and photo-erythema.
The following sterols occur in soybean:
Beta-Sitosterol is the principal sterol of Soybean oil.
Sitosterol suspension is a mixture of plant sterol, mostly Beta-Sitosterol, which are structurally similar to cholesterol. Sitosterol may lower the
elevated serum cholesterol by interfering with the intestinal absorption of cholesterol. Mixture of plant sterols including beta-Sitosterol are among
the preparations that are absorbed to a limited extent from the intestinal tract
and compete for the absorption of both endogenous and exogenous cholesterol. For these reasons this sterol which is expensive and only of
research interest has gained limited status in the treatment of
hypercholesterolemia and artherosclerosis.
According to this invention the process of extracting Sterol from deodourised distillates which is a by-product recovered during refining of Soybean oil from the Soybean seeds, comprising the steps of;
i. subjecting deodourised distillates to undergo physical conversion;
ii. subjecting the resultant product at step (i) above to the Molecular Distillation; and
iii. subjecting the residue collected at the end of the Molecular Distillation to chemical purification and mixing, with solvents and simultaneously cooling to a very low temperature to obtain the crystal precipitates;
iv. filtering the crystal precipitates to obtain end filtrates;
v. mixing and treating the said end filtrates at step (iv) with solvents in a crystalizer to remove all the remaining fatty acids and the impurities present therein;
vi. heating the treated resultant filtrate to undergo a reflex process continuously for predetermined period thereby dissolving the waxes in a solvent and filtering the wax free crystals;
vii. subjecting the said filtered crystals to another solvent was in a centrifuge to remove any other impurities present;
viii. subjecting said resultant product at step (vii) above to vacuum drying together with simultaneous heating to obtain the pure sterol.
According to another aspect of this invention, the heating of the viscous deodourised distillates to convert into liquid form is carried out by heating coils inside the tank and the deodourised distillates are then pumped into molecular distillation plant in the liquid form through the SS Pipelines keeping their flow rate steady at 100 litres/hour with the help of flow meters and control valves and degassing of the liquid distillates is done whereby the gases present in the distillates are removed.
In yet another aspect of this invention , the molecular distillation step comprises of boiling the liquid distillates to 120 degrees C and then cooling so as to remove and recover the 15 to 20% of the fatty acids at the second stage and again at the third and fourth stage, boiling the residual liquid distillates collected at the second stage to 120 degrees C and then cooling to recover the major portion of the fatty acids and finally once again superheating the residual liquid distillates collected at the fourth stage preferably to 240 to 250 degrees C, the residue is in the form of vapours containing sterol and remaining fatty acids. They are collected in the collector.
According to another feature of this invention, the chemical purification and mixing in this extraction process of sterol comprises of chemically purifying in a crystalizer unit by mixing with the solvents of volume of quantity of 4 times the mass of the residue treated in the crystalizer, and also simultaneously cooling by jacketing provided therein for circulation of chilled water, so that the temperature of the residual mass comes down to the extent of minus 10 degrees C to result in the form of crystal precipitates which are filtered by Nutsche filters.
According to yet another aspect of this invention, the filtrate separated from the mass is loaded into a reflex vessel of SS and mixed with further solvents such as Methanol solution .For separation of the remaining fatty acids and impurities from the filtrate ,it is once again washed with other solvents such as Acetone and finally heated in a reflux vessel to dissolve all the waxes in the solvents and once again vacuum dried at a temperature of 50 degrees C in a double cone vacuum drier to recover the pure sterol.
The invention will now be described in more details with reference to the various stages for the extraction of the sterol from the deodourised distillates.
The plant for the extraction of sterol consists of mainly converter unit connected to molecular distillation unit and the residue collected from this
distillation unit is fed into a crystalizer unit where chemical purification and mixing with the solvents takes place in a reflux vessel and the end filtrate is filtered and then heated to procure the precipitated Sterol and again washing the resultant product with Acetone in a centrifuge thereby dissolving all the excess waxes in the solvents.
The raw material for the Sterol is deodourised distillate which is a by-product recovered during the refining of Soybean oil from the Soybean seeds and is available in the viscous form only. This viscous deodourised distillates are
converted into liquid form using the heater coils and the liquid form of deodourised distillates are fed into the molecular distillation unit. The
molecular distillation is a unique technology of distillation based on characteristic vapour pressure of each chemical substance and its molecular
weight. This relative difference in vapor pressure dictates the separation of complex compound into its constituents. Following table shows relative volatility of different components in deodourised Distillate:
Component Molecular Weight Relative Volatility
Fatty Acids 280 2.5
Squalene 411 5
Tocopherols 415 1
Sterols 410 0.6
Sterol Esters 675 0.04
Oil 885 Small
The deodourised distillates when received from the supplier is stored in two MS storage tanks of 50 tones each. At this stage the distillate is in the viscous form and hence to be heated to be converted into the liquid form with the help of heating coils inside the tank. This makes the loading easy in the molecular distillation plant. The raw distillates are continuously fed onto the wiped film still which consists of heaters. The fluid is spread onto the thin film by a wiper blade assembly driven at a predetermined speed. The film while being forced into turbulence by the wiper blades, progress down through the inside body wall aided by gravity and the slots in the wiper blades. During the course of flow through the heater system some degree of evaporation takes place depending upon the inside wall temperature and the system
pressure. The non-evaporated fluid forming the bottom product flows out of
the system continuously while the vapour is condensed inside & collected in the receiver. The turbulence created by the rapidly moving wiper assists in the heat transmission thereby lowering the temperature required on the inside wall of the evaporator and also the liquid exposure time to the elevated wall
temperature can be controlled within seconds. This liquid distillate is then pumped into distillation plant and flow is kept steady at 100 litres/hour with the help of flow meters and control valves. The material which is pumped into the plant at the first stage falls on a rotating disc and whatever gases present in the deodourised distillates are removed. Then this material heads towards
the second stage where the temperature is maintained at 120 degrees C.
At this stage 15 to 20% fatty acid converts into vapours and goes to central condenser where the temperature is maintained at 30 degrees C. 70 to 75% of fatty acids in the residue is recovered in the same process in the third and fourth stage of the plant. In the fifth stage the temperature is increased to 240 to 250 degrees C. At this temperature, Sterol and the remaining fatty acids convert into vapours and are collected in the collector.
At this stage process of molecular distillation is over and the mass containing the main ingredients goes for chemical purification. In chemical purification process, solvents to the tune of 4 times of the volume of mass is mixed in the crystalizer where jacketing is provided for circulation of chilled water so that the temperature of the mass comes down to the extent of minus 10 degrees C. Here some material is precipitated in the crystal iorm which is filtered by Nutsche filters and the filtrate is separated from the mass. This filtrate is then again loaded into another reflux vessel where Mathnol solution are mixed for the separation of remaining fatty acids from the filtrate. These precipitated crystals are removed and the filtrate which contains sterol is
sent into a centrifuge where the temperature is maintained at 70 degrees C, and washed with another solvent so that the remaining impurities are removed. For removal of the solvent and the moisture form pure sterol the final end product is put into a double cone vacuum drier where heat is
provided through limped coils upto 50 degree C. Finally the purified sterol is collected.
1. An industrial process of extracting sterol from deodorized distillate, which is
a byproduct recovered during refining of Soybean oil from Soybean seeds.
Compressing the steps of :
i. Heating the viscose deodorized distillate unto liquid state by a heating coil kept inside a tank ;
ii. Pumping the liquefied distillate of step (I) to molecular distillation Plant and degassing the liquefied distillate in the plant ;
iii. Boiling the liquid distillate of step (ii) in the molecular distillation plant about 120oC and cooling it subsequently that removes 15 to 20% of fatty acid ;
iv. Repeating the process of step (iii) thrice to recover major portion of fatty acids ;
v. Superheating the residual liquid distillate after the 4th stage to about 240 -250oC and collecting the residues in form of vaporous containing sterol & fatty acids ;
vi. Dissolving the content of step (v)in a crystallizer unit by a suitable solvent which is flour times the mass of the residue and cooling the system by chilled water at 10oC to precipitate the crystals & filtered to separate undesirable materials ;
vii. Loading the filtrate of step (vi) to a reflex vessel and refluxing further with methanol / acetone for separation of residual fatty acids from the filtrate ;
viii. Vacuum trying the filtrate of step (vii) at 50oC to remove the solvent 85 obtaining the pure sterol.
2. The process as claimed in claims 1 wherein liquid deodourised distillates is pumped into the distillation plant through SS pipe lines at 100 litres/hr with the help of flow meter 85 controlled valves.
3. The process as claimed in claim 1 wherein degassing of liquid distillate is carried out prior to molecular distillation for removal of gases present in the distillate.
4. The process as claimed in claim 1 wherein the crystals wherever precipitated are filtered by the notch filters and the filtrate is separated from the maso.
5. The process as claimed in step (vi) of claim 1, wherein the filtrate obtained is further heated in the distillation reactor to a temperature of about 70oC to under reflex process dissolving waxes in the solvent and enable recover of the wax free crystals.
6. The process as claimed in step (vii) of claim 1, wherein the solvent acetone is used for washing in the process of centrifuge for removal of residues from the filtrate.
7. The process as claimed in claim 1, wherein the resultant end product received from step (vii) is vacuum dried in double cone vacuum drier.
8. The industrial process of extracting the sterol from deodorized distillates which is by-product recovered during the refining of Soybean oil from Soybean seeds substantially as herein described in the complete specification.
Date 25.10.06 Signature
|Indian Patent Application Number||1177/MUM/2004|
|PG Journal Number||29/2008|
|Date of Filing||03-Nov-2004|
|Name of Patentee||SONIC BIOCHEM EXTRACTIONS LTD|
|Applicant Address||38, PATEL NAGAR, INDORE, MADHYA PRADESH, PIN-452 001 INDIA|
|PCT International Classification Number||A61K 36/00|
|PCT International Application Number||N/A|
|PCT International Filing date|