Title of Invention	THE PROCESS OF EXTRACTING TOCOPHEROL FROM DOEDOURISED DISTILLATES WHICH IS BYPRODUCT RECOVERED DURING REFINING OF SOYBEAN OIL FROM SOYBEAN SEEDS
Abstract	The process of extracting Tocopherol from deodurised distillates which is by product recovered during of Soya oil from Soya seeds comprising the steps of i) Subjecting D.O. distillates to undergo physical conversion; ii) Subjecting the resultant product at step(i) above to the Molecular Distillation; 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 s crystalizer to remove all the remaining fatty acids presents therein, and vi) Finally heating the treated resultant filtrate to distill the solvent and enable recover the pure tocopherol.

Title of Invention

THE PROCESS OF EXTRACTING TOCOPHEROL FROM DOEDOURISED DISTILLATES WHICH IS BYPRODUCT RECOVERED DURING REFINING OF SOYBEAN OIL FROM SOYBEAN SEEDS

Abstract

The process of extracting Tocopherol from deodurised distillates which is by product recovered during of Soya oil from Soya seeds comprising the steps of i) Subjecting D.O. distillates to undergo physical conversion; ii) Subjecting the resultant product at step(i) above to the Molecular Distillation; 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 s crystalizer to remove all the remaining fatty acids presents therein, and vi) Finally heating the treated resultant filtrate to distill the solvent and enable recover the pure tocopherol.

Full Text	THE PATENTS ACT, 1970 FORM NO. 2 COMPLETE SPECIFICATION (Section 10) (Rule 13) THE PROCESS OF EXTRACTING TOCOPHEROL FROM DOEDOURISED DISTILLATES, WHICH IS BYPRODUCT 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 : L 6 NOV 20C6 6 THE PATENTS ACT, 1970 COMPLETE SPECIFICATION (Section 10) THE PROCESS OF EXTRACTING TOCOPHEROL FROM DOEDOURISED DISTILLATES, WHICH IS BYPRODUCT RECOVERED DURING REFINING OF SOYA OIL FROM SOYA 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 ofythis invention and the manner in which it is to be performed : This invention relates to the extraction of tocopherol from the deodourised distillates. More particularly the extraction of the tocopherol is from the deodourised distillate which is a by product recovered during refining of soya oil from soya seeds. Soya bean 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 Vidharbha in Maharashtra. The size of Crop is about 125 lacs tons per year which yields 25 lacs tons of oil. Soya Bean 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 DOC sludge and gums separated during oil refinery process are not being used for any value addition process although these contain valuable fractions. 1 ^.o^ ■/? Our R&D unit has developed the process and technology of extraction, fractionation and purification of Tocopherol. These Tocopherols are nature"s fat-soluble antioxidants. It is available in four forms viz., Alpha Tocopherol, Beta Tocopherol Gamma Tocopherol and Delta Tocopherol. The Tocopherol is used as dietary supplement and are known primarily for their antioxidant properties and are widely used where consumer preferences require the use of a natural antioxidant. Gamma and delta Tocopherols forms prediminate in Soyabean oil. Beta Tocopherols exists in the concentrations too low to have any practical significance. Tocopherols are readily soluble in fats and oils. Most fats, oils and food products derived from animal origin are low or deficient in natural antioxidants. Examples of such products are lard, tallow, poultryfat, essential oils, parafin wax. These tocopherol when used as antioxidant does not impart odour, taste or colour to fastfoods and food products. In pharmaceutical preparations, the tocopherols stabilize other substances, e.g., Vitamin A and unsaturated lipids, during shelf life. Care should be taken to prevent exposing it to high temperature, ultraviolet radiation, direct sunlight or metal contamination. The Tocopherols are used as dietary supplements and in the food technology as antioxidants to retard the development of rancidity in fatty materials. It acts as an antioxidant controlling redox reactions in a variety of tissues and organs, particularly in protecting the cellular membrance from free radicals generated during peroxidation of unsaturated lipids. Experiments with animals deficient in tocopherols have revealed perhaps the largest variety of disorders associated with the nutritional lack of any single vitamin. Tocopherols deficiency affects the reproductive system (testicular degeneration, defective development of the embryo); the muscular system ((skeletal muscular dystrophy, cardiac necrosis and fibrosis, ceroid pigment in smooth muscle); the circulatory system (exudative diathesis, erythrocyte hemolysis, anemias); the skeletal system (incisor depigmentation) and the nervous system (encephalomalacia, deposition of lipofuscin pigment). In addition, tocopherols deficiency may be manifested by a number of other conditions, such as discoloured adipose tissue, liver necrosis, lung hemorrage, kidney nephrosis and postomortem autolysis and creatinuria. Tocopherols ameleourates the adverse effects of various toxic agents (e.g., lead and chlorinated solvents), Drugs (adriamycin), and a number of soboptimal dietary (e.g., low protein) and also environmental (e.g., high oxygen, ozone or Nitrogen dioxide) conditions. Supplimentation of well balanced diets with pharmacological amounts of tocopherols enhances humoral immunity and increase phagocytosis in animals. Tocopherols also interacts metabolically with selenium. This relationship has been clarified recently by the discovery that selenium is a constituent of glutathione peroxidase, an enzyme that destroys peroxides. Tocopherols preserves integrity of red blood cell walls and protects them against haemolysis. They may also act as co-factors in enzyme sytems. Tocopherol also generally are considered to provide protection against pulmonary oxygen poisoning. Essentially all examples of clinical indication of need for tecopherols at nutritional levels are related to malnourishment on malabsorption problem and in the light of their biochemical & nutritional experience and therapeutic role, tocopherols have widely been consumed in animal and poultry feeds. Thus according to this invention the process of extracting tocopherol from the deodourised distillates which is a byproduct recovered during refining of soya oil from soya seeds comprises of the steps of; i. subjecting D.O. Distillates to undergo physical conversion; ii. subjecting the resultant product at step (I) above to the Molecular Distillation; 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 en filtrates at step (iv) with solvents in crystalizer to remove all the remaining fatty acids present therein, and vi. finally heating the treated resultant filtrate to distill the solvent and enable recover the pure tocopherol. According to another aspect of this invention, the heating of the viscous D.O. Distillates to convert into liquid form is carried out by heating coils and the D.O. 5 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. In another aspect of this invention, degassing of the liquid distillates is done whereby the low boilers 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 degree 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 degree C and then cooling to recover the major portion of the fatty acids as soap and finally once again superheating the residual liquid distillates collected at the fourth stage preferably to 240 to 250 degree C, the residue is in the form of vapours containing tocopherol with remaining fatty acids and they are collected in the collector. According to another feature of this invention, the chemical purification and mixing in this extraction process of tocopherol 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 jacketting provided therein for circulation of chilled water, so that the temperature of the residual mass comes down to the extent of minus 10 degree C to result in the form of crystal precipitates which are filtered by nutch filters. According to yet another aspect of this invention of the filtrate separated form the mass is loaded again the crystalizer and mixed with further solvents such a Isopetropyle alcohol and Sodium Carbonate for separation of the remaining fatty acids from the filtrate and finally heated in a distillation reactor to distill out the solvents used and to recover the pure tocopherol. This invention will now be described in more details with reference to the various stages for the extraction of the tecopherol from the vegetable oilseeds. 6 The plant for the extraction of tocopherol 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 and the end filtrate is filtered and then heated procure the pure tocopherol thereby distilling out the solvents. The raw material for the tocopherol is D O Distillates which is a by product of soya industry and is available in the viscous form only. This viscous D O Distillates are converted into liquid form using the heater coils and the liquid form of DO 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 vapour pressure dictates the separation of complex compound into its constituents. The D O Distillates when received from the supplier is stored into MS storage tanks of 50 tons 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 turbulance 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 turbulance 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/hours 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 D O Distillates are removed. Then this material heads towards the second stage where the temperature is maintained at 120 degree C. At this stage 15 to 20 % fatty acid converts into vapours and goes to central condenser where the temperature is maintained at 30 degree C. 70 to 75% of fatty 7 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 degree C. At this temperature, tecopherol 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 jacketting is provided for circulation of chilled water so that the temperature of the mass comes down to the extent of minus 10 degree C. Here some material is precipitated in the crystal from which is filtered by nutch filters and the filtrate is separated from the mass. This filtrate is then again loaded into another crystalizer where sodium carbonate and isopropyle alcohol are mixed for the separation of remaining fatty acid,s from the filtrate as a soap. This percipitated soap is removed and the filtrate which contains tocopherol is sent for distillation reactor where the temperature is maintained at 40 to 50 degree C. so that / the solvent is distilled and the pure tocopherol is obtained. f WE CLAIM:- j / 1. The process of extracting Tocopherol from deodourised distillates which is by product recovered during refining of soya oil from soyeTseeds comprising the steps of / /""■"i i. subjecting D.Or distillates to undergo physical conversion; ii. subjecting the resultant product at step (i) above to the Molecular Distillation; 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 present therein, and vi. finally heating the treated resultant filtrate to distill the solvent and enable recover the pure tocopherol. £ The process as claimed in claim 1 wherein step at (I) includes heating the viscous D O distillates to convert into liquid form. The process as claimed in claim 2 wherein the D O distillates are heated with heating coils to convert into the liquid form. The process as claimed in the preceding claims 1 to 3 wherein liquid D O Distillates are pumped into the distillation plant through SS Pipelines and ttv flow is kept steady preferably at 100 litres/hour with the help of flow meters control valves. \y 5. The process as claimed in preceding claims 1 & 4 wherein the degassing of liquid distillate is done by centrifugal separation. 6. The process as claimed in preceding claims 1 and 5 where in the liquid distillates are made to fall on a rotating disc placed inside the plant where by low boilers present if any in the distillates are removed. \, ^ 7. The process as claimed in claim 1 wherein step at (ii) above 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 degree C and then cooling to recover the major portion of the fatty acids as soap and finally once again superheating the residual liquid distillates collected at the fourth stage preferably to 240 to 250 degree C, the residue is in the form of vapours containing tocopherol with remaining fatty acids and they are collected in the collector. 8. The process as claimed in the claim 1 at step (iii) wherein the residue collected in collector is chemically purified in a crystalizer unit by mixing with the solvents of volume of quantity of four times to 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 degree C to result in the form of crystal precipitates. 9 9. The process as claimed in the claims 1 & 8 wherein the crystal precipitates are filtered by the nutch filters and the filtrate is separated from the mass. 10. The process as claimed in the claim 1 at the step (v), wherein the filtrate recovered from step (iv) is loaded again in the crystalizer and mixed with further solvents such as Isopropyle Alcohol and sodium carbonate for the separation of the remaining fatty acids from the filtrate as soap. 11. The process as claimed in the claim 1 wherein the resultant filtrate obtained at the step (v), is once again finally heated in a distillation reactor to the temperature of about 40 to 50 degrees C to distill the solvent and enable recover the pure tocopherol. 12. The process of extracting the tocopherol from the deodounsed distillate wh\|6h is by product recovered during refining of soya oil from soya seeqs substantially as herein before described in this complete specification. Dated this 3rd day of November, 2004. for SONIC BIOCHEM EXTRACTION LTD., SHRIKISHAN CftOITHRAM MATLANI MANAGING DIRECTOR

Full Text

THE PATENTS ACT, 1970
FORM NO. 2
COMPLETE SPECIFICATION
(Section 10) (Rule 13)
THE PROCESS OF EXTRACTING TOCOPHEROL FROM
DOEDOURISED DISTILLATES, WHICH IS BYPRODUCT 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 :

L 6 NOV 20C6
6

THE PATENTS ACT, 1970
COMPLETE SPECIFICATION (Section 10)
THE PROCESS OF EXTRACTING TOCOPHEROL FROM
DOEDOURISED DISTILLATES, WHICH IS BYPRODUCT RECOVERED DURING
REFINING OF SOYA OIL FROM SOYA 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 ofythis invention and the manner in which it is to be performed :
This invention relates to the extraction of tocopherol from the deodourised distillates. More particularly the extraction of the tocopherol is from the deodourised distillate which is a by product recovered during refining of soya oil from soya seeds. Soya bean 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 Vidharbha in Maharashtra. The size of Crop is about 125 lacs tons per year which yields 25 lacs tons of oil.
Soya Bean 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 DOC sludge and gums separated during oil refinery process are not being used for any value addition process although these contain valuable fractions.

*1
^.o^

*■/?

Our R&D unit has developed the process and technology of extraction, fractionation and purification of Tocopherol. These Tocopherols are nature"s fat-soluble antioxidants. It is available in four forms viz., Alpha Tocopherol, Beta Tocopherol Gamma Tocopherol and Delta Tocopherol. The Tocopherol is used as dietary supplement and are known primarily for their antioxidant properties and are widely used where consumer preferences require the use of a natural antioxidant. Gamma and delta Tocopherols forms prediminate in Soyabean oil. Beta Tocopherols exists in the concentrations too low to have any practical significance.
Tocopherols are readily soluble in fats and oils. Most fats, oils and food products derived from animal origin are low or deficient in natural antioxidants. Examples of such products are lard, tallow, poultryfat, essential oils, parafin wax. These tocopherol when used as antioxidant does not impart odour, taste or colour to fastfoods and food products. In pharmaceutical preparations, the tocopherols stabilize other substances, e.g., Vitamin A and unsaturated lipids, during shelf life. Care should be taken to prevent exposing it to high temperature, ultraviolet radiation, direct sunlight or metal contamination.
The Tocopherols are used as dietary supplements and in the food technology as antioxidants to retard the development of rancidity in fatty materials. It acts as an antioxidant controlling redox reactions in a variety of tissues and organs, particularly in protecting the cellular membrance from free radicals generated during peroxidation of unsaturated lipids. Experiments with animals deficient in tocopherols have revealed perhaps the largest variety of disorders associated with the nutritional lack of any single vitamin. Tocopherols deficiency affects the reproductive system (testicular degeneration, defective development of the embryo); the muscular system ((skeletal muscular dystrophy, cardiac necrosis and fibrosis, ceroid pigment in smooth muscle); the circulatory system (exudative diathesis, erythrocyte hemolysis, anemias); the skeletal system (incisor depigmentation) and the nervous system (encephalomalacia, deposition of lipofuscin pigment). In addition, tocopherols deficiency may be manifested by a number of other conditions, such as discoloured adipose tissue, liver necrosis, lung hemorrage, kidney nephrosis and postomortem autolysis and creatinuria.

Tocopherols ameleourates the adverse effects of various toxic agents (e.g., lead and chlorinated solvents), Drugs (adriamycin), and a number of soboptimal dietary (e.g., low protein) and also environmental (e.g., high oxygen, ozone or Nitrogen dioxide) conditions. Supplimentation of well balanced diets with pharmacological amounts of tocopherols enhances humoral immunity and increase phagocytosis in animals. Tocopherols also interacts metabolically with selenium. This relationship has been clarified recently by the discovery that selenium is a constituent of glutathione peroxidase, an enzyme that destroys peroxides. Tocopherols preserves integrity of red blood cell walls and protects them against haemolysis. They may also act as co-factors in enzyme sytems. Tocopherol also generally are considered to provide protection against pulmonary oxygen poisoning.
Essentially all examples of clinical indication of need for tecopherols at nutritional levels are related to malnourishment on malabsorption problem and in the light of their biochemical & nutritional experience and therapeutic role, tocopherols have widely been consumed in animal and poultry feeds.
Thus according to this invention the process of extracting tocopherol from the deodourised distillates which is a byproduct recovered during refining of soya oil from soya seeds comprises of the steps of;
i. subjecting D.O. Distillates to undergo physical conversion;
ii. subjecting the resultant product at step (I) above to the Molecular Distillation;
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 en filtrates at step (iv) with solvents in crystalizer
to remove all the remaining fatty acids present therein, and vi. finally heating the treated resultant filtrate to distill the solvent and enable
recover the pure tocopherol.
According to another aspect of this invention, the heating of the viscous D.O. Distillates to convert into liquid form is carried out by heating coils and the D.O.
5

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.
In another aspect of this invention, degassing of the liquid distillates is done whereby the low boilers 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 degree 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 degree C and then cooling to recover the major portion of the fatty acids as soap and finally once again superheating the residual liquid distillates collected at the fourth stage preferably to 240 to 250 degree C, the residue is in the form of vapours containing tocopherol with remaining fatty acids and they are collected in the collector.
According to another feature of this invention, the chemical purification and mixing in this extraction process of tocopherol 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 jacketting provided therein for circulation of chilled water, so that the temperature of the residual mass comes down to the extent of minus 10 degree C to result in the form of crystal precipitates which are filtered by nutch filters.
According to yet another aspect of this invention of the filtrate separated form the mass is loaded again the crystalizer and mixed with further solvents such a Isopetropyle alcohol and Sodium Carbonate for separation of the remaining fatty acids from the filtrate and finally heated in a distillation reactor to distill out the solvents used and to recover the pure tocopherol.
This invention will now be described in more details with reference to the various stages for the extraction of the tecopherol from the vegetable oilseeds.
6

The plant for the extraction of tocopherol 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 and the end filtrate is filtered and then heated procure the pure tocopherol thereby distilling out the solvents.
The raw material for the tocopherol is D O Distillates which is a by product of soya industry and is available in the viscous form only. This viscous D O Distillates are converted into liquid form using the heater coils and the liquid form of DO 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 vapour pressure dictates the separation of complex compound into its constituents. The D O Distillates when received from the supplier is stored into MS storage tanks of 50 tons 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 turbulance 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 turbulance 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/hours 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 D O Distillates are removed. Then this material heads towards the second stage where the temperature is maintained at 120 degree C. At this stage 15 to 20 % fatty acid converts into vapours and goes to central condenser where the temperature is maintained at 30 degree C. 70 to 75% of fatty
7

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 degree C.
At this temperature, tecopherol 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 jacketting is provided for circulation of chilled
water so that the temperature of the mass comes down to the extent of minus 10
degree C. Here some material is precipitated in the crystal from which is filtered by
nutch filters and the filtrate is separated from the mass. This filtrate is then again
loaded into another crystalizer where sodium carbonate and isopropyle alcohol are
mixed for the separation of remaining fatty acid,s from the filtrate as a soap. This
percipitated soap is removed and the filtrate which contains tocopherol is sent for
distillation reactor where the temperature is maintained at 40 to 50 degree C. so that /
the solvent is distilled and the pure tocopherol is obtained. f
WE CLAIM:- j /
1. The process of extracting Tocopherol from deodourised distillates which is by
product recovered during refining of soya oil from soyeTseeds comprising the
steps of /
/""■"i
i. subjecting D.Or distillates to undergo physical conversion;
ii. subjecting the resultant product at step (i) above to the Molecular
Distillation; 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 present therein, and vi. finally heating the treated resultant filtrate to distill the solvent and
enable recover the pure tocopherol.
£

The process as claimed in claim 1 wherein step at (I) includes heating the viscous D O distillates to convert into liquid form.
The process as claimed in claim 2 wherein the D O distillates are heated with heating coils to convert into the liquid form.
The process as claimed in the preceding claims 1 to 3 wherein liquid D O Distillates are pumped into the distillation plant through SS Pipelines and ttv flow is kept steady preferably at 100 litres/hour with the help of flow meters control valves.

\y

5. The process as claimed in preceding claims 1 & 4 wherein the degassing of liquid distillate is done by centrifugal separation.
6. The process as claimed in preceding claims 1 and 5 where in the liquid distillates are made to fall on a rotating disc placed inside the plant where by low boilers present if any in the distillates are removed. \, ^
7. The process as claimed in claim 1 wherein step at (ii) above 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 degree C and then cooling to recover the major portion of the fatty acids as soap and finally once again superheating the residual liquid distillates collected at the fourth stage preferably to 240 to 250 degree C, the residue is in the form of vapours containing tocopherol with remaining fatty acids and they are collected in the collector.
8. The process as claimed in the claim 1 at step (iii) wherein the residue collected in collector is chemically purified in a crystalizer unit by mixing with the solvents of volume of quantity of four times to 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 degree C to result in the form of crystal precipitates.
9

9. The process as claimed in the claims 1 & 8 wherein the crystal precipitates are filtered by the nutch filters and the filtrate is separated from the mass.
10. The process as claimed in the claim 1 at the step (v), wherein the filtrate recovered from step (iv) is loaded again in the crystalizer and mixed with further solvents such as Isopropyle Alcohol and sodium carbonate for the separation of the remaining fatty acids from the filtrate as soap.
11. The process as claimed in the claim 1 wherein the resultant filtrate obtained at the step (v), is once again finally heated in a distillation reactor to the temperature of about 40 to 50 degrees C to distill the solvent and enable recover the pure tocopherol.
12. The process of extracting the tocopherol from the deodounsed distillate wh|6h is by product recovered during refining of soya oil from soya seeqs substantially as herein before described in this complete specification.
Dated this 3rd day of November, 2004.
for SONIC BIOCHEM EXTRACTION LTD.,
SHRIKISHAN CftOITHRAM MATLANI MANAGING DIRECTOR

Documents:

1176-mum-2001-abstract.doc

1176-mum-2001-claims.doc

1176-mum-2001-description[granted].doc

1176-mum-2001-form 2[granted].doc

1176-mum-2004-abstract.pdf

1176-mum-2004-cancelled page(25-11-2004).pdf

1176-mum-2004-claims.pdf

1176-mum-2004-correspondence(ipo).pdf

1176-mum-2004-correspondence.pdf

1176-mum-2004-description(granted).pdf

1176-mum-2004-form 1(03-11-2004).pdf

1176-mum-2004-form 1.pdf

1176-mum-2004-form 19.pdf

1176-mum-2004-form 2 6-11-2006.pdf

1176-mum-2004-form 2(granted).pdf

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Patent Number

214169

Indian Patent Application Number

1176/MUM/2004

PG Journal Number

13/2008

Publication Date

28-Mar-2008

Grant Date

05-Feb-2008

Date of Filing

03-Nov-2004

Name of Patentee

SONIC BIOCHEM EXTRACTIONS LTD.

Applicant Address

38, PATEL NAGAR, INDORE-452 001

Inventors:

#	Inventor's Name	Inventor's Address
1	SHRIKISHAN CHOITHRAM MATLANI	38, PATEL NAGAR, INDORE-452 001
2	GIRISH SHRIKISHAN MATLANI	38, PATEL NAGAR, INDORE-452001

PCT International Classification Number

A61K31/00 A01P5/48

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA