FORM 2 PATENTS ACT, 1970 COMPLETE SPECIFICATION
(SECTION 10)
Title: - A process for fractionation of crude liquid lecithin using rectified spirit in a continuous, counter-current direction in a Rotating Disc Contactor
SONIC BIOCHEM EXTRACTIONS LIMITED,
A Limited Company under the Companies Act, 1956,
having its office at 38, Patel Nagar,
Indore, Madhya Pradesh,
India, PIN-452001.
An Indian National

The following specifications particularly describe the nature of this invention and the manner in which it is to be performed.


Title: - A process for fractionation of crude liquid lecithin using rectified spirit in a continuous, countercurrent direction and a Rotating Disc Contactor
FIELD OF INVENTION
The present invention relates to a rotating disc contactor and process of making phosphatidycholine from liquid lecithin using rotating disc contactor, by fractionation of crude liquid lecithin derived from soybean seeds using Rectified Spirit as solvent by continuous counter current process in a Rotating Disc Contactor (RDC) to manufacture Phosphatidylcholine having purity between 35 to 38 % .
BACKGROUND OF INVENTION
Lecithin is a mixture of Surface-active agents. Most of the surfactant properties of lecithin can be attributed to the phospholipids present in it. These contain a hydrophobic portion with an affinity for fats and oils and a hydrophilic portion with an affinity for water. The typical emulsifying property of phospholipids is the reason for successful use of lecithin in a variety of foodstuffs, dietetic, cosmetic and pharmaceutical preparations. The emulsification properties of different lecithin products can be assigned based on the well-known hydrophilic-lipophilic balance (HLB). HLB values reflect the size and strength of the hydrophilic (water loving or polar) and the lipophilic (oil loving or nonpolar) groups of emulsifiers.
Lecithin has a versatile function in life. It is an extremely important factor in the digestion and oxidation of fats. It helps in enhancing muscle and glandular activity thereby reducing excessive fat accumulation. Lecithin is essential not only for tissue integrity of the nervous and glandular system in all living cells, but has also been regarded as the most effective generator and regenerator of great physical, mental and glandular activity. Lecithin is an important component of the endocrine glands and the muscles of the heart and kidneys. It makes up 73 % of the total liver fat. The action of lecithin on the heart is the most important of all its proven benefits. Lecithin has the ability to break up cholesterol into small particles, which can be easily handled by the system.
There are specially two definitions used to characterize the property of lecithin. One is Acetone insoluble which is a measure of the surface-active property of the lecithin. The other is viscosity of lecithin which is evaluated with a Brookfield Viscometer, a widely used technique. When a comparison with respect to measurements is made, important factors such as spindle number, speed of rotation and sample temperature should be specified.
This material is mainly comprised of phospholipids and glycolipids. Results of viscosity are specifically reported in poise or centipoise at 25°C. The viscosity of liquid lecithin may range from 6000-15000 centipoise depending upon its composition.


CHEMICAL COMPOSITION
Lecithin is a complex mixture of Rectified spirit Insoluble phospholipids consisting mainly of Phosphatidylcholine (PC), Phosphatidylethanolamine (PE), Phosphatidylinositol (PI), and Phosphatidic acid (PA), combined with varying amounts of other substances such as triglycerides. It contains 14% to 16% of phosphatidylcholine. The composition of Standard Fluid Lecithin is given in the following image :



SOURCE OF CRUDE SOYA LECITHIN
Soybean Crude Oil is a rich source of natural Lecithin. The crude soybean oil obtained from Soybean Seeds using n-hexane is non-edible and has to be refined in a vegetable oil refinery .The first step in refining process is Water Degumming which removes water hydratable phosphatides .The phosphatides so obtained contains about 30 to 50 % moisture which is removed to get Crude Liquid Lecithin.
This present invention relates to fractionation of crude liquid lecithin to obtain one fraction rich in Phosphatidylcholine (Abbreviated as PC ) having phosphatidylcholine content between 35 to 38%,) and, more particularly, to a method in which the lecithin and the rectified spirit solvent are treated in continuous countercurrent fashion in a suitable Rotating Disc Contactor fitted with specially designed stator rings.
The conventional batch process requires large volumes of rectified spirit for producing fraction rich in Phosphatidylcholine (PC ). However the quality of the product is not consistent and sometimes it becomes difficult to achieve desired purity(PC content). This process is quite expensive, requires large inventory of rectified spirit and also the cost of plant is quite high. For example, the rectified spirit/lecithin ratios used in current batch extraction of crude lecithin are in the range of 4:1 to 5:1 which is too high.
It is desirable to find out a process for fractionation of lecithin employing least amount of solvent (rectified spirit) to make it economically viable and also to get consistent quality product having PC content more than 35 %. Thus the problems of the batch process motivated to invent a process for fractionation of lecithin using least solvent. According to the present invention, much lower lecithin to rectified spirit ratios, ranging from 1:1 to 1:1.25 are achieved, resulting in considerable savings and producing desired fraction having Phosphatidylcholine (PC) content between 35 to 38 %. This is achieved through contacting Rotating Disc Contactor having specially designed stator rings under conditions of agitation and residence time (utilizing spaced baffles) where the two reactants are flowed in continuous counter-current manner.
OBJECTIVE OF THE INVENTION
The main objective of the invention is to devise a process for fractionation of crude liquid lecithin derived from soybean seeds using rectified spirit as solvent by continuous counter current process in a Rotating Disc Contactor (RDC) to produce lecithin fraction rich in Phosphatidylcholine.
Further object of the present invention that is to find a process for fractionation of crude liquid lecithin derived from soybean seeds using least amount of rectified spirit as solvent to make the process more economically viable.
Further important object of the present invnention that to make a fraction rich in Phosphatidylcholine (PC) having purity between 35 to 38% for successful use of product for pharmaceutical preparations.


Further more important object of the present invention that to modify the rotating disc contactor that helps to perform the process of the invention to achieve the desired product in an economical way employing least solvent (rectified spirit).
SUMMARY OF THE INVENTION
The present invention relates to fractionation of crude liquid lecithin derived from soybean seeds using rectified spirit as solvent by continuous counter current process in a Rotating Disc Contactor (RDC) to manufacture desired fraction having Phosphatidylcholine (PC) content from 35 to 38 %.
DETAILED DESCRIPTION OF THE INVENTION
The present invention relates to a process of making phosphatidycholine from liquid lecithin using rotating disc contactor, by fractionation of crude liquid lecithin derived from soybean seeds using Rectified Spirit as solvent by continuous counter current process in a Rotating Disc Contactor (RDC) to manufacture Phosphatidycholine having purity between 35 to 38 % comprising, the said Rotating Disc Contactor designated by numeral(lOO) provided on its right side with an inlet (110) for the introduction of crude lecithin. A second inlet (104) is provided as shown in the figure adjacent to the lower portion of the Rotating Disc Contactor (100) for the introduction of rectified spirit Two outlets (111) and (101) as shown in the figure are provided wherein the upper outlet (111) is located immediately on the top left side of the Rotating Disc Contactor and just below the Rotor Top (112). The said outlet is ment for the extract, containing rectified spirit and soluble fraction rich in phosphatidylcholine. The lower outlet (101) which permits the removal of raffinate (fraction poor in phosphatidylcholine having PC content from 5% to 9%) is provided at the bottom of the Rotating Disc Contactor.
The above Rotating Disc Contactor is made up of mixing compartments of rotor (108), which is fixed at the right central portion of the contactor. Each compartment includes an upper and lower stator ring (106) and (105) respectively, in the form of annular ring. The inner diameter of each stator ring ranges between 40% to 60% of the total area defined by the outside diameter for maximum extraction. The Rotor Disc (109) is interposed in each compartment and is driven by a motor (113), provided at the top of the Rotating Disc Contactor. The number (107) designated the distance between two adjacent stator rings. For any compartment the Rotor Disc is designed to yield specific mixing intensities which may be different from those in other compartments.
The liquid-liquid extraction column used in the experiments was laboratory model- Rotating Disc Contactor having diameter of 100 mm, the number of stages is 38, the stator rings designated as 106 and 105. The Rotor Plan is given in Fig denoated with no. (124). During the countercurrent extraction operation, the fraction poor in Phosphatidylcholine flows downward through the Rotating Disc Contactor and the fraction rich in Phosphatidylcholine goes to the top of the RDC column .
Rectified spirit is introduced through the inlet designated as 104 at the bottom of Rotating Disc Contactor and it flows upward through the Rotating Disc Contactor 100 making intimate contact with lecithin and then exits from the Rotating Disc Contactor Top 114 at the outlet for extract designated by numeral 111. As the rectified spirit flows through the Rotating Disc Contactor, it continuously enriches the extract with Phosphatidylcholine.


It is not possible to pump the lecithin feed into the Rotating Disc Contactor chamber at low temperature; therefore, the liquid lecithin is heated to 50°C. Temperature inside Rotating Disc Contactor is also provided and maintained at 50°C by providing a heating jacket designated as (119) along the Rotating Disc Contactor. Heating media for the heating jacket 119 is hot water, which is introduced through an inlet (117), shown at the bottom left side of the Rotating Disc Contactor. Numeral (118) represents the mixing zone between two adjacent stator rings. The heating media goes out through the outlet (120) provided at the top of Rotating Disc Contactor.
The efficiency of this continuous, counter-current extraction is superior to conventional batch extractions with respect to the rectified spirit/lecithin ratio. The practice of the invention can be better understood from a consideration of specific examples.
EXAMPLE - 1
Lecithin Liquid feed stream having 14.05% PC content, Acetone Insoluble 62% and viscosity of 12000 centipoise was introduced to the Rotating Disc Contactor Feed Section at the rate of 12 Kg/Hr and temperature of 50°C. Rectified spirit (Moisture content = 5%) was introduced at the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 18 Kg/hr. The rotor was run at 400 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket.
The Extract obtained after removing solvent had following analysis:
PC Content = 35.10%
A.I =52.75%
The raffinate ( Fraction obtained from bottom of LLE) after removing solvent had following analysis:
PC Content = 7.05%
A.I =65.05%
The recoveries of Extract and Raffinate (Based on FEED to LLE ) were as under :
RAFFINATE: 75.05% EXTRACT: 24.95% EXAMPLE - 2
Lecithin Liquid feed stream having 14.05% PC content , Acetone Insoluble 62% and viscosity of 12000 centipoise was introduced to the Rotating Disc Contactor Feed Section at the rate of 15 Kg/Hr and temperature of 50°C. Rectified spirit (Moisture content = 5%) was introduced at the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 15 Kg/hr. The rotor was run at 400 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket.
The Extract obtained after removing solvent had following analysis:


PC Content = 38.05%
A.I = 54.05 %
The raffinate ( Fraction obtained from bottom of LLE) after removing solvent had following analysis:
PC Content =5.15%
A.I = 65.02 %
The recoveries of Extract and Raffinate (Based on FEED to LLE) were as under:
RAFFINATE: 72.1% EXTRACT: 27.9%
EXAMPLE -3
Lecithin Liquid feed stream having 14.05% PC content , Acetone Insoluble 62% and viscosity of 12000 centipoise was introduced to the Rotating Disc Contactor Feed Section at the rate of 10 Kg/Hr and temperature of 50°C. Rectified spirit (Moisture content = 5%) was introduced at the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 20 Kg/hr. The rotor was run at 400 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket.
The Extract obtained after removing solvent had following analysis:
PC Content = 32.95%
A.I =51.24%
The raffinate (Fraction obtained from bottom of LLE) after removing solvent had following analysis:
PC Content = 8.98%
A.I = 64.87 %
The recoveries of Extract and Raffinate (Based on FEED to LLE) were as under:
raffinate: 78.85% EXTRACT: 21.15%
EXAMPLE - 4
Lecithin Liquid feed stream having 14.05% PC content , Acetone Insoluble 62% and viscosity of 12000 centipoise was introduced to the Rotating Disc Contactor Feed Section at


the rate of 16 Kg/Hr and temperature of 50°C. Rectified spirit (Moisture content = 5%) was introduced at the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 12 Kg/hr. The rotor was run at 400 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket.
The Extract obtained after removing solvent had following analysis:
PC Content =31.09%
A.I =55.02%
The raffiante (Fraction obtained from bottom of LLE) after removing solvent had following analysis:
PC Content = 8.65%
A.I =64.19%
The recoveries of Extract and Raffmate (Based on FEED to LLE) were as under :
RAFFINATE: 75.95% EXTRACT: 24.05%
EXAMPLE - 5
Lecithin Liquid feed stream having 14.05% PC content , Acetone Insoluble 62% and viscosity of 12000 centipoise was introduced to the Rotating Disc Contactor Feed Section at the rate of 16 Kg/Hr and temperature of 50°C. Rectified spirit (Moisture content = 5%) was introduced at the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 20 Kg/hr. The rotor was run at 400 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket.
The Extract obtained after removing solvent had following analysis:
PC Content =36.17%
A.I =54.18%
The RAFFINATE (Fraction obtained from bottom of LLE) after removing solvent had following analysis:
PC Content =5.31%
A.I =65.11%
The recoveries of Extract and Raffmate (Based on FEED to LLE ) were as under :
RAFFINATE: 71.68% EXTRACT: 28.32%


EXAMPLE - 6
Lecithin Liquid feed stream having 14.05% PC content, Acetone Insoluble 62% and viscosity of 12000 centipoise was introduced to the Rotating Disc Contactor Feed Section at the rate of 12 Kg/Hr and temperature of 50°C. Rectified spirit was introduced at the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 14.Kg/hr. The rotor was run at 400 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket.
The Extract obtained after removing solvent had following analysis:
PC Content = 38.75%
A.I = 52.17%
The RAFFINATE (Fraction obtained from bottom of LLE) after removing solvent had following analysis:
PC Content =5.04%
A.I =65.71%
The recoveries of Extract and Raffinate (Based on FEED to LLE) were as under:
RAFFINATE: 72.45% EXTRACT: 27.55%
From the ongoing experiments and the data generated, we can conclude as under:
1. The optimum ratio of rectified spirit to liquid lecithin for getting smooth extraction and getting minimum 35% PC content in the final product and optimum yield is 1:1.17 to 1:1.25.
2. Maintaining temperature of 50°C inside the Rotating Disc Contactor with the help of heated jacket allow both liquid lecithin flow down easily and also help in better fractionation of lecithin to get required PC content in extract.
3. The ratio is so designed that it enables fractionation of liquid lecithin to get PC rich fraction having purity 35 to 38%. The rotor design is shown in the attached drawing.
These and other modifications along with variations to the present invention may be practiced by those of ordinary skill in the art, without departing from the spirit and scope of the present invention, which is more particularly set forth in the appended claims. In addition, it should be understood that aspects and various embodiments may be interchanged both in whole and in part. Furthermore, those of


ordinary skill in the art will appreciate that the foregoing description is by way of example only, and is not intended to limit the invention so further described in such appended claims.
ANNEXURE-1
Description of Parts of Rotating Disc Contractor

Code Description
100 Rotating Disc Contactor
101 Raffinate Out
102 Sight Glass
103 Rotor Disc Dimension
104 Rectified spirit In
105 Stator Ring
106 Stator Ring
107 Distance Between Two Adjacent Stator Rings
108 Rotor
109 Rotor Disc
110 Lecithin Feed In
111 Extract Out
112 Rotor Top
113 Motor
114 RDC - Top
115 Angled Stator Ring
116 Rotor (same as 108)
117 Heating Media in (Hot Water)
118 Mixing Zone Between Two Adjacent Stator Rings
119 Heating Jacket
120 Heating Media Out (Hot Water)
121 Sight Glass
122 Lifting Lug
123 Skirt Pipe
124 R.otor Plan


WE CLAIM
1. A process for fractionation of crude liquid lecithin using rectified spirit in a
continuous, countercurrent direction and a Rotating Disc Contactor (RDC)
for performing the process comprising, the said device designated as numeral
(100) as shown in right side of fig. with an inlet (110) for the introduction of
crude lecithin, a second inlet (104) is provided as shown in the figure adjacent
to the lower portion of the Rotating Disc Contactor (100) for the introduction
of rectified spirit, two outlets (111) and (101) as shown in the figure are
provided , the upper outlet (111) is located immediately on the top left side of
the Rotating Disc Contactor and just below the Rotor Top (112), an outlet is
meant for the extract, of rectified spirit and soluble fraction rich in
phosphatidylcholine, the lower outlet (101) which permits the removal of
raffinate (fraction poor in phosphatidylcholine having PC content from 5% to
9%) is provided at the bottom of the Rotating Disc Contactor,
2. A process and device as claimed in claim 1, wherein a device is made up
of mixing compartments such as a rotor (108), is fixed at the right central
portion of the contactor, each compartment includes an upper and lower stator
ring (106) and (105) respectively, having an annular ring, and inner diameter
of each stator ring ranges between 40% to 60% of the total area for maximum
extraction,
3. A process as claimed in claim 1, wherein the Rotor Disc (109) is interposed
in each compartment and driven by a motor (113), provided at the top of the
Rotating Disc Contactor, a distance between two adjacent stator rings
designated with (107),
4. A process and device as claimed in claim 1, wherein a liquid-liquid extraction column having diameter of 100 mm, is being used, for obtaining fraction rich in phosphatidylcholine,
5. A process as claimed in above claims, wherein the RDC is provided a heating media with a heating Jacket (119) and a mixing zone (118) to maintain temperature of the process,
6. A process for fractionation of crude liquid lecithin using rectified spirit as solvent in continuous, countercurrent direction as claimed in above claims,


the said process comprising , providing vertically crude liquid lecithin feed at the top, rectified spirit feed at the bottom, rotor equipped with discs for continuous mixing and agitating the mixture of rectified spirit and liquid lecithin, the outer shell equipped with annular stator rings for passage of liquids to next mixing, the diameter of rotor discs between 40 to 60% of outside diameter of stator ring characterized in that a ratio of lecithin to rectified spirit being 1:1.17 to 1:1.25 to produce lecithin fraction having Phosphatidylcholine content between 35% to 38%,
7. A process as claimed in claim 6, wherein the viscosity of the treated lecithin is below 12,000 centipoise at 25°C.
8. A process as claimed in claim 7, wherein said crude lecithin is Soya liquid lecithin having minimum 62% Acetone Insoluble and 12000 centipoise viscosity at25°C,
9. A process as claimed in claim 6 to 8 wherein the temperature of process is maintained 50°C inside the Rotating Disc Contactor,
10. A process as claimed in claim 1 wherein the rotating motors are maintained at 300-500 revolutions per minute (RPM) and the column is operated under atmospheric pressure,
11. A process for fractionation of crude liquid lecithin and a device using rectified spirit as solvent as described herein with references to the examples and drawings.