Title of Invention

A PROCESS FOR DEOILING LIQUID LECITHIN USING ROTATING DISC CONTACTOR

Abstract A process for deoiling crude lecithin, introducing crude liquid lecithin into the upper part and acetone in lower part of a Rotating Disc Contactor with some of specially designed stator rings especially modified to suit viscous lecithin, under conditions of agitation, RPM ranging from 300-500 and under atmospheric pressure, in continuous countercurrent relation, the ratio of lecithin to acetone being 1: 3 to 1: 7 to provide oil free Lecithin which when dried has Acetone Insoluble in the range of 95 to 98%.
Full Text FORM 2
PATENTS ACT, 1970
COMPLETE SPECIFICATION
(SECTION 10)
TITLE OF THE INVENTION
A PROCESS FOR DEOILING LIQUID LECITHIN USING ROTATING DISC CONTACTOR
APPLICANT


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
4 AUG 2008
The following specifications particularly describe the nature of this invention and the manner in which it is to be performed.


FIELD OF INVENTION
The present invention relates to deoiling of crude liquid lecithin derived from soybean seeds using acetone as solvent by continuous countercurrent process in a Rotating Disc Contactor (RDC) to manufacture Deoiled Lecithin Powder (DLP) having acetone insoluble ranging from 95 to 98% of the final product.
BACK GROUND OF INVENTION
WHAT IS LECITHIN
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 emulsiflcation 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
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been regarded as also 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 portion of the lecithin. This material is mainly comprised of phospholipids and glycolipids. 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. Specifically results of viscosity are 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 Acetone 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. The oil-free granule or powdered form has almost all this triglycerides and fatty acids removed.
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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 remove's 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 a method for deoiling crude lecithin and, more particularly, to a method in which the lecithin and the acetone solvent are treated in continuous countercurrent fashion in a suitable Rotating Disc Contactor fitted with specially designed stator rings.
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The conventional batch lecithin deoiling process requires large volumes of acetone for extraction of oil from liquid lecithin to get lecithin of desired acetone insoluble. This process is quite expensive, requires large inventory of acetone and also the cost of plant is quite high. For example, the acetone/lecithin ratios used in current batch extraction of crude lecithin are in the range of 15:1 to 20:1 which is too high. Illustrative of the prior art batch style processing is US 3047597.
US 4803016 relates to a method for deoiling crude lecithin which includes pretreating crude lecithin with from about 5% to about 20% acetone to control viscosity variability and to facilitate breakup of solids during extraction, introducing the thus pretreated lecithin into the upper part of a contacting chamber under conditions of agitation but without flow constriction at essentially atmospheric pressure, thereafter flowing the lecithin in continuous, countercurrent relation to acetone at a rate of 3 to 10 parts acetone to one part lecithin to provide a refined lecithin having an Acetone Insolubles content in the range of about 94% to about 99.9%. Here also extra acetone is required for pretreatment of crude lecithin which increases the cost of production.
It is desirable to find out a process for deoiling of lecithin employing least amount of solvent (acetone) to make it economically viable. Thus the problems of the prior art motivated to invent a process for deoiling of lecithin using least solvent. According to the present invention, much lower lecithin to acetone ratios, ranging from 1:3 to 1:7 are achieved, resulting in considerable savings and having acetone insoluble ranging from 95 to 98% in the final product. 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.
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OBJECTIVE OF THE INVENTION
The main objective of the invention is to devise a process for deoiling of crude liquid lecithin derived from soybean seeds using acetone as solvent by continuous counter current process in a Rotating Disc Contactor (RDC) to manufacture Deoiled Lecithin Powder (DLP).
One more objective of the invention is to find a process for deoiling of crude liquid lecithin derived from soybean seeds using least amount of acetone as solvent to make the process more economically viable.
Further more objective of the invention is to make a deoiled lecithin product having acetone insoluble ranging from 95 to 98% for successful use of lecithin in a variety of foodstuffs, dietetic, cosmetic and pharmaceutical preparations.
One furthermore objective of the invention is 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 (acetone).
SUMMARY OF THE INVENTION
The present invention relates to deoiling of crude liquid lecithin derived from soybean seeds using acetone as solvent by continuous counter current process in a Rotating Disc Contactor (RDC) to manufacture Deoiled Lecithin Powder (DLP) having acetone insoluble ranging from 95 to 98% of the final product. The whole idea to achieve the object lies in the modification of the rotor rings and its inclination of the stator rings of the rotating disc contactor so that the pretreatment
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step of crude lecithin using acetone as solvent is avoided. This step decreases the consumption of solvent compared to prior art and hence become a more efficient process for deoiling lecithin using only lecithin to acetone ratio in the range of 1:3 to 1:7.
DETAILED DESCRIPTION OF THE INVENTION
The Rotating Disc Contactor as shown in the attached drawing is used for trials as mentioned in the examples below. The Annexure-1 explains different parts of the Rotating Disc Contactor.
DESCRIPTION OF THE DRA WING
In the drawing, Rotating Disc Contactor designated by numeral 100 is provided on its right side with an inlet 110 for the introduction of crude lecithin. A second inlet 104 is provided adjacent to the lower portion of the Rotating Disc Contactor 100 for the introduction of acetone. Two outlets 111 and 101 are provided wherein the upper outlet 111 is located immediately on the top left side of the Rotating Disc Contactor 100 and just below the Rotor Top 112. This outlet is for the extract, which contains acetone, acetone soluble substances and removable oils by the solvent. The lower outlet 101 which permits the removal of raffmate (deoiled lecithin) is provided at the bottom of the Rotating Disc Contactor 100.
The bulk of Rotating Disc Contactor is made up of mixing compartments with rotor 108, which is designated at the right central portion of the drawing. 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% and 60% of the total area defined by the outside diameter for maximum extraction.
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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 designate the distance between two adjacent stator ring. For any compartment the rotor Disc may be 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 top ten stator rings out of 38 rings (around 28 to 25%) are situated just below the lecithin feed inlet 110 have been inclined to 15° to facilitate downward movement of sticky material (the inclined stator rings are designated by numeral 115 at the right side of the drawing). The modification also helped in avoiding the slurry preparation (pre-mixing the feed with acetone) which requires 5 to 20% of additional solvent acetone as referred to in US 4803016. The modified/downward inclined top stator rings are responsible in downsizing the acetone consumption during the process carried out. Again this small inclination of 15° only does not put a restriction on the flow of acetone upward rather helps in downward movement of sticky crude lecithin.
During the countercurrent extraction operation, the treated lecithin being heavier than acetone, flows downward through the Rotating Disc Contactor while being broken up into small, deoiled particles by the Rotor Disc 109. Below the lecithin feed inlet 110, the lecithin particles are extracted in multiple compartments bounded by stator rings 105 and 106 and containing one or more turbine type Rotor Disc 109.
Acetone is introduced through the inlet designated as 104 at the bottom of Rotating Disc Contactor and it flows upward through the Rotating Disc Contactor
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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 acetone flows through the Rotating Disc Contactor, it continuously extracts oil a other acetone soluble material from the Liquid Lecithin.
As it is not possible to pump the lecithin feed into the Rotating Di Contactor chamber at low temperature, therefore, the liquid lecithin is heated 50°C. Temperature inside Rotating Disc Contactor is also maintained at 50°C providing a heating jacket designated by 119 along the Rotating Disc Contact Heating media for the heating jacket 119 is hot water, which is introduced throu; an inlet 117 shown at the bottom left side of the Rotating Disc Contactor. Numei 118 represent the mixing zone between two adjacent stator rings. The heating mec goes out through the outlet 120 provided at the top of Rotating Disc Contactor, chilled water (minus 20°C) condenser provided on the top of Rotating Di Contactor collects the acetone vapors formed inside the Rotating Disc Contactor.
Because of the nature of the raffinate (Deoiled Lecithin), it is not possible take out the same on continuous basis by any mechanical means. Therefore fre acetone (cooled to 10°C) is mixed with deoiled lecithin in the ratio 1:5 preferab 1:4 or close to 1:2.5.
A special agitator was provided at the bottom of the Raffinate receiving chamber so as not to allow deoiled lecithin to settle down at the bottom and clog the raffinate outlet 101. After removal of the slurry from the Rotating Disc Contactor through the outlet 101, the Raffinate is pumped to a decanter centrifuge. The resulting cake is then completely desolventized in a Continuous Vibro Dryer to produce dry deoiled Lecithin which can be subsequently sieved / milled / sieved to produce Lecithin Granules / Lecithin Coarse / Lecithin Powder.
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The efficiency of this continuous, counter-current extraction is superior to conventional batch extractions with respect to the acetone/lecithin ratio. The practice of the invention can be better understood from a consideration of specific examples.
EXAMPLE -1
Lecithin Liquid feed stream having Acetone Insoluble 62% was introduced to the Rotating Disc Contactor Feed Section at the rate of 6 Kg/Hr and temperature of 50°C. Acetone 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 350 rpm. The material inside Rotating Disc Contactor was maintained at 50°C by circulation of hot water in the outer jacket, deoiled Lecithin was removed from the bottom after converting to slurry with acetone.
The deoiled lecithin obtained after removing solvent had following analysis:
Acetone Insoluble = 94.07%
Fat = 5.10%
Moisture = 0.83 %
The Extract coming from the top had 10 to 11 % oil in it. With a slightly higher acetone/lecithin ratio, a significant increase in Acetone Insoluble was achieved as seen in the following example.
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EXAMPLE - 2
Lecithin Liquid feed stream having Acetone Insoluble 62% was introduced to the Rotating Disc Contactor Feed Section at the rate of 6 Kg/hr and temperature of 50°C. Acetone was introduced to the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 30 Kg/hr. The rotor was run at 350 rpm. The material inside Rotating Disc Contactor was kept at 50°C by circulation of hot water in the outside jacket. Deoiled Lecithin was removed from the bottom after converting to slurry with acetone.
The deoiled lecithin obtained after removing solvent had following analysis:
Acetone Insoluble = 97.01%
Fat =2.15%
Moisture =0.84%
The Extract coming from the top had 7 to 8% oil in it.
EXAMPLE - 3
Lecithin Liquid feed stream having Acetone Insoluble 62% was introduced to the Rotating Disc Contactor Feed Section at the rate of 6 Kg/hr and temperature of 50°C. Acetone, was introduced to the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 36 Kg/hr. The rotor was run at 350 rpm. The material inside Rotating Disc Contactor was kept at 50°C by circulation of hot water in the outer jacket. Deoiled Lecithin was removed from the bottom after converting to slurry with acetone.
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The deoiled lecithin obtained after removing solvent had following analysis:
Acetone Insoluble =97.15 %
Fat = 2.10 %
Moisture = 0.75 %
The percentage of oil in the extract was found to be 5 to 6%.
EXAMPLE - 4
Lecithin Liquid feed stream having Acetone Insoluble 62% was introduced to the Rotating Disc Contactor Feed Section at the rate of 6 Kg/hr and temperature of 50°C. Acetone was introduced to the bottom of the Rotating Disc Contactor at 30°C and a flow rate of 42 Kg/hr. The rotor was run at 350 rpm. The material inside Rotating Disc Contactor was kept at 50°C by circulation of hot water in the outer jacket. Deoiled Lecithin was removed from the bottom after converting to slurry with acetone.
The deoiled lecithin obtained after removing solvent had following analysis :
Acetone Insoluble = 97.23%
Fat -1.87%
Moisture = 0.9%
The Extract coming from the top had 5 to 5.50 % oil in it.
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From the ongoing experiments and the data generated, we can conclude as under:
1. The optimum ratio of acetone to liquid lecithin for getting smooth extraction and getting minimum 97% Acetone Insoluble in the final product is 5:1 (w/w).
2. The inclined Stator Rings on the top of the Rotating Disc Contactor reduce clogging by highly viscous liquid lecithin as well as by deoiled lecithin.
3. Maintaining temperature of 50°C inside the Rotating Disc Contactor with the help of heated jacket allow both liquid lecithin as well as deoiled lecithin flow down easily and eliminate any clogging inside the Rotating Disc Contactor.
4. As the temperature inside the Rotating Disc Contactor is 50°C and boiling point of acetone being 56 C, there is some generation of acetone vapors, therefore a chilled water condenser (minus 20 C) helps to trap any such vapors (condenser not shown in the diagram) and thus avoid building up of any pressure in the Rotating Disc Contactor.
5. That it is of advantage to take out the Raffinate from the bottom of the Rotating Disc Contactor by converting it to slurry by mixing it with acetone in a ratio of 1: 2.5 to 1:5.( Deoiled Lecithin : Acetone )
These and other modifications and 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.
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ANNEXURE-1
Description of Parts of Rotating Disc Contractor

Code Description
100 Rotating Disc Contactor
101 Raffmate Out
102 Sight Glass
103 Rotor Disc Dimension
104 Acetone In
105 Stator Ring
106 Stator Ring
107 Distance Between Two Adjacent Stator Rings
108 Rotor
109 Rotor Disc
iio Lecithin Peed In
Hi Extract Out
112 Rotor Top
113 Motor
114 RDC - Top
115 Angled Stator Ring
116 Rotor (same as 108)
117 pleating 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
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WE CLAIM
1. A process for deoiling of crude liquid lecithin using acetone as solvent in continuous, countercurrent direction in a Rotating Disc Contactor (RDC) comprising providing vertically crude liquid lecithin feed at the top, acetone feed at the bottom, rotor equipped with discs for continuous mixing and agitating the mixture of acetone and liquid lecithin, the outer shell equipped with annular stator rings for passage of liquids or partially deoiled lecithin to next mixing, the diameter of rotor discs between 40 to 60% of outside diameter of stator ring characterized in that around 26% of the stator rings which are situated on the top of the column just below the lecithin feed inlet have been inclined downward to 15° to facilitate downward movement of sticky crude liquid lecithin material so that pretreatment of crude lecithin during deoiling with 5 to 20% of extra solvent (acetone) is avoided.
2. A process as claimed in claim 1 wherein the ratio of lecithin to acetone being 1:3 to 1:7 to produce deoiled lecithin which when dried has acetone insoluble in the range of 94 to 98%.
3. A process as claimed in claim 1 wherein the viscosity of the treated lecithin is below 12,000 centipoise at 25°C.
4. A process as claimed in claim 1 wherein said crude lecithin is soya liquid lecithin having minimum 62% Acetone Insoluble and viscosity 12000 centipoise at 25°C.
5. A process as claimed in claim 1 further requires a temperature of 50°C inside the Rotating Disc Contactor is to be maintained.
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Date: 30.7.08 GIRISH MATLANI
MANAGING DIRECTOR
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6. 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.
7. A process as claimed in claim 1 further requires a specially designed agitator used at the bottom of Rotating Disc Contactor to keep the slurry from settling at the bottom and thus preventing any clogging of discharge nozzle.
8. A process as claimed in claim 1 wherein the deoiled lecithin was converted into slurry by using acetone in the ratio ranging from 2.5: 1 to 5:1 (Acetone: Deoiled Lecithin) and then pumping it out from the bottom of the Rotating Disc Contactor.
9. A process as claimed in claim 1 wherein a chilled water condenser maintained at minus 20°C is installed that helps to trap any such vapors and thus avoid building up of any pressure in the Rotating Disc Contactor.
10. A process for deoiling of crude liquid lecithin using acetone as solvent as herein described with references to the examples and disclosure in the specification.


Documents:

1657-MUM-2008-ABSTRACT(GRANTED)-(25-4-2011).pdf

1657-mum-2008-abstract.doc

1657-mum-2008-abstract.pdf

1657-MUM-2008-CLAIMS(GRANTED)-(25-4-2011).pdf

1657-mum-2008-claims.doc

1657-mum-2008-claims.pdf

1657-MUM-2008-CORRESPONDENCE(25-4-2011).pdf

1657-MUM-2008-CORRESPONDENCE(30-7-2008).pdf

1657-MUM-2008-CORRESPONDENCE(7-3-2011).pdf

1657-MUM-2008-CORRESPONDENCE(IPO)-(25-4-2011).pdf

1657-mum-2008-correspondence.pdf

1657-mum-2008-description(complete).doc

1657-mum-2008-description(complete).pdf

1657-MUM-2008-DESCRIPTION(GRANTED)-(25-4-2011).pdf

1657-MUM-2008-DRAWING(GRANTED)-(25-4-2011).pdf

1657-mum-2008-drawing.pdf

1657-mum-2008-form 2.doc

1657-MUM-2008-FORM 1(24-01-2011).pdf

1657-MUM-2008-FORM 1(4-8-2008).pdf

1657-mum-2008-form 1.pdf

1657-mum-2008-form 13(8-4-2011).pdf

1657-mum-2008-form 18.pdf

1657-MUM-2008-FORM 2(GRANTED)-(25-4-2011).pdf

1657-MUM-2008-FORM 2(TITLE PAGE)-(25-4-2011).pdf

1657-MUM-2008-FORM 2(TITLE PAGE)-(4-8-2008).pdf

1657-MUM-2008-FORM 2(TITLE PAGE)-(GRANTED)-(25-4-2011).pdf

1657-mum-2008-form 2(tittle page).pdf

1657-mum-2008-form 2.pdf

1657-MUM-2008-FORM 3(24-01-2011).pdf

1657-MUM-2008-FORM 3(4-8-2008).pdf

1657-mum-2008-form 3.pdf

1657-MUM-2008-FORM 5(24-01-2011).pdf

1657-MUM-2008-FORM 5(4-8-2008).pdf

1657-mum-2008-form 5.pdf

1657-mum-2008-form 9(4-8-2008).pdf

1657-MUM-2008-REPLY TO EXAMINATION REPORT(24-01-2011).pdf

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FORM9.TIF


Patent Number 247578
Indian Patent Application Number 1657/MUM/2008
PG Journal Number 17/2011
Publication Date 29-Apr-2011
Grant Date 25-Apr-2011
Date of Filing 04-Aug-2008
Name of Patentee GIRISH MATLANI
Applicant Address 38, PATEL NAGAR, INDORE, INDIA
Inventors:
# Inventor's Name Inventor's Address
1 GIRISH MATLANI 38, PATEL NAGAR, INDORE-452 001,
PCT International Classification Number A23CL1/164
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA