Title of Invention

"A PROCESS FOR THE PRODUCTION OF NUTRITIOUS RED PALM OLEIN"

Abstract

The invention relates to a process for the production of nutritious red palm olein. The red palm olein is natural carotene and vitamin E rich.. The process steps consists of; treating preheated crude palm oil with caustic soda at 70-85 deg.C, cooling the mixture to 48-65 deg.C, removing soap , washing the remaining oil with hot water, winterizing the alkali free oil by heating at 60-70 deg.C followed by cooling by using winterization unit to get crystallized mass, separating the solid mass by filtration, deodorizing by heating in the temperature range of 120-160 deg.C and cooling to obtain the product.

Full Text

This invention relates to a process for the production of nutritious red palm olein. This invention particularly relates to a process for the production of natural carotene and vitamin E rich red palm olein. Palm oil has emerged as an important source of vegetable oil in the recent years. The orange red colour of crude palm oil is due to the presence of carotenes,the content of which ranges from 500 to 700 ppm. Crude palm oil contains other minor components such as tocopherols and tocotrienols (800-1000 ppm). The carotenoids, tocopherols and tocotrienols are effective natural antioxidants. The carotenoids, particularly a and p -carotene, are also precursors of Vitamin A, which is important for vision, health of mucous membranes, skin, growth of bone and reproduction. Studies have shown that various carotenoids possess protective properties against certain types of cancers. The tocopherols and tocotrienols function as vitamin E and they have important physiological properties. Recent studies have shown that tocotrienols can lower the blood cholesterol level and also prevent aggregation of platelets in blood. So far natural carotene rich Red palm olein has not been produced in India. The products already available in Malaysia make use of the principles of molecular distillation. During normal conventional refining of Crude Palm Oil, it is processed to remove most of the carotene, making the oil, bland , colourless and nutritionally poor to meet specifications and consumer requirements. The physical and chemical refining practiced differ in treatment of the oil. A commercially viable patented Malaysian method for preserving the carotenes in palmolein makes use of the process of short path distillation (Unnithan, UR. 198-NV 586),at a temperature of 160-290°C and at pressures of 0.003-0.08 mbar whereby a high carotene rich palm olein which meets all the fully refined edible oil specifications can be obtained. Short path distillation gives low volume and high cost end product whereas the present process involves production of large quantities and is less expensive. Other Malaysian patented processes for refining of edible oil, rich in natural carotenes and Vitamin E, employs distilling the degassed degummed and bleached oil in a short path distiller at a temperature of 160-190°C and pressures of 0.003-0.08 mbar [Unnikrishnan, Ramachandran, Unnithan (Global palm products Sdn.Bhd.) United States patent US 5932 261 (1999)].Free Fatty Acids( FFA) are_removed from the oil using an internal condenser system, within the distiller which operates at a temperature greater than the m.p of Free Fatty Acids ( FFA) in the oil, typically 20-80°C. This process involves degassing, degumming and bleaching where as in the present process these steps are totally eliminated thereby retention of Vitamin E and carotenoids are improved. Another patented process describes steam blowing the oil containing carotene >500 ppm under reduced pressure ( crude palm oil followed by deacidification and deodorisation using molecular distillation. This process is also very expensive. The main objective of the present invention is to provide a process for the production of nutritionally rich red palmolein. Another objective of the present invention is to provide a method for the production of natural carotene rich red palm olein. Another objective of the present invention is to provide a method for the production of Vitamin E rich red palm olein. Another objective of the present invention is to provide a method for the production of crystalline palm stearin with maximum P' crystals with negligible Free Fatty Acids (FFA) which can be used as a by product for food formulation. Accordingly the present invention provides a process for the production of nutritious red palm olein which comprises; i) treating preheated crude palm oil at a temperature ranging 70-85°C with preheated caustic soda of concentration ranging 0.4 to 0.5% w/w dissolved in water under stirring for a period ranging 5-10 minutes, ii) cooling the mixture at a temperature ranging between 48 to 65°C under vacuum, iii) removing soap formed in above step from the oil, iv) washing the remaining oil with hot water to obtain neutralized alkali free oil, v) winterizing the alkali free oil by heating at a temperature ranging 60-70°C for a period ranging between 5-15 minutes followed by cooling between 18-28°C by controlled conditions of cooling, ranging from 10-20°C/hr by using a winterization unit to get crystallized mass, vi) separating the solid mass (palm stearin) by filtration to get clear palm olein, vii) deodorizing by heating simultaneously the palm olein obtained above to a temperature in the range of 120 - 160°C under vacuum .ranging 1-5 m bar and spraying steam at a rate of 0.2 to 0.3 kg /hr for a period of 2 hr, viii) cooling the resultant to obtain nutritious palm olein. In an embodiment of the present invention, crude palm oil is neutralized with caustic soda, using neutralizer under vacuum. In another embodiment of the present invention, winterization of the neutralized, washed palm oil is carried out by winterizer. In yet another embodiment of the present invention, crystalline solid palm stearin is separated from the olein fraction by a rotary drum vacuum filter. In another embodiment of the present invention, high colour nutritious red palm olein is obtained by the deodorisation of the above palm olein under controlled process conditions. The following procedure has been developed for the production of red palm olein and palm stearin as a by - product. The crude palm oil obtained from fresh fruit bunches (FFB) contain undesirable constituents that include free fatty acids, phosphatides, proteinaceous and odoriferous substances, all of which would interfere with subsequent processing and which contribute to undesirable flavour and appearance in the finished product. The process of refining effectively removes these contaminants. Treatment of the oil with caustic soda, followed by extensive washings results in almost complete removal of Free Fatty Acids through their conversion to water soluble soap. By using the existing process of neutralisation the carotene loss is significant due to the higher neutralisation temperature and high contact time. In the present process, treatment of crude palm oil with calculated amount of caustic soda at 70-80°C , separation of the settled soap at a reduced temperature of 48-65°C and several washings of the oil with water at elevated temperature to make it alkali free with settling durations at these temperatures, results in the maximum retention of carotene utilising high vacuum during the above process steps. Also the exposure at high temperature is minimised by cold water circulation through cooling coils in the process. In the existing process these steps are not accounted whereas in the present improved process the above conditions are established to give maximum retention of carotenes(98%). Apart from retention of caroteneJFree Fatty Acid (FFA) content is also reduced to the level of 0.25 - 0.5 percentage by weight. By this method the iron and copper content are reduced by 90% and 92% respectively. The major fractions of palm oil are palm olein (liquid fraction) and palm stearin (solid fraction). Palm oil can crystallize hi three or more polymorphic forms, stable in different; temperature ranges. Because of its large number-of different component glycerides, palm oil crystallizes in a complex manner. The crystallization is affected by many iactors including (T) the hydrolysis and oxidation products of the oil (2) the rate of cooling and the temperature of crystallization (3) agitation and mechanical disturbance during the cooling process. An optimum cooling rate only can give maximum palm olein yield and palm stern crystals in the more stable P' polymorphic form. By X-ray diffraction technique, standardization of this was arrived at by following Bragg's equation which states that nX, =2dsin0 where, n = an integer indicating order of the spectra X=wavelength d=short spacing [crystal lattice spacing of one set of planes] 0 = The angle of incidence upon this set of planes In the present winterization process neutralised palm oil is heated to 60-70°C, with a short holding time of 5-15 mints., then cooled to 18-28°C at the rate of 10-20°C/hr using chilled water, retains most of the carotenes where as hi winterization using solvent fractionation;a solvent which is a third component is utilised in rystallizing out the palm stearin fraction by which method the solvent has to be separated totally by evaporation which results hi the significant reduction of carotenes and also residual solvent would be present in the final product In the present process cooling rate of 10-20°C/hr gives maximum pahnolein yield and palmstearin in the more stable F polymorphic form. In order to achieve good separation, the crystals should be firm and uniform spherical size, which is a condition found when they are mainly in the F form Palm stearin in F polymorphic form is more favourable in palm stearin based formulations. The crystallization process as detailed above was strictly monitored in the present process by employing a winterizer which takes account of all the parameters. Filtration is an important requirement of the process which separates the olein and stearin fractions. As crystallization process is a function of rate of cooling, the entire filtration operation has to be finished at the specified temperature at which maximum crystal formation occurred. Otherwise, polymorphic transition can occur resulting in lowering of the desirable F form and palm olein yield. In the present process this has been attained by a rotary drum vacuum filter which finished the entire filtration operation within the required time of 2 hrs and at the specified temperature. The temperature and time as detailed above are strictly adhered in the filtration process. The crystalline granular stearin thus obtained was almost dry and is a usable by product The X-ray diffraction data of palm stearin shows maximum p1 polymorphic form Percentage polymorphic forms of palm stearin at different cooling rates are given in Fig. 1. Deodorisation is typically the last step in the traditional processing of oils and fats. This process removes the relatively volatile trace components from the oil which contribute to flavour, odour and colour. These components are ketones, aldehydes, alcohols and free fatty acids which are distilled off. Carotenes are heat sensitive and temperature degradable. The existing deodorisation processes,which employ a temperature of 180-220°C remove carotenes and other minor constituents almost completely. The present process, provides the oil with maximum carotene and vitamin E retention, lesser Free Fatty Acids and moisture contents, without off-flavour hi the finished product A temperature of 120-160 °C coupled with high vacuum of l-5mbar was found to give a high carotene rich red palmolien with 80% carotene retention, 85% retention of vitamin E, Free Fatty Acid content of less(|hin(.:=-((ois ture content of less than 0.1% and the resulting red palm olein has maximum stability and no off flavour, which is acceptable to the consumers and meets with the required specifications.Physico-chemical characteristics of crude palm oil and red palm olein are given in Table. 1 .Carotene and vitamin E profile of red palm olein are given in Fig2. Table.1 Physico-chemical characteristics of Crude palm oil (CPO) and Red palm oil (RPO) (Table Removed) The following examples are given by way of illustration and therefore should not be constructed to limit the scope of the present invention. Example 1 20.1 kg of crude palm oil is fed into the neutralise!/ washer by means of vacuum and heated to 70-85°c under vacuum. Calculated amount of alkali sufficient to neutralise the FFA (80-100 gms) is dissolved in water to give a 15-20° Be solution which is heated to 70- 80°C. The hot alkali is admitted into the reactor and the reaction is carried out with slow stirring for 5 -10 minutes. The soap formed is allowed to settle by reducing the temperature of the contents to 48-65°C under vacuum. After 5 hrs, 1.8 kgs of soap is removed and the remaining 18.6kgs of oil is washed with hot water for 4 to 6 times till free of alkali. The resultant neutralised palmoil {18.2kg}is taken for winterization. In another example of neutralisation, 19.6kgs of crude palm oil is fed into the neutraliser by means of vacuum and heated to70-85 °C under vacuum. Calculated amount of alkali (80-95gms) is dissolved in water and heated to 70-80°C.The hot alkali is admitted into the reactor and the reaction is carried out with slow stirring for 5-10 minutes. The soap formed is allowed to settle by gravity by reducing temperature of the contents to 48-65°C under vacuum. After 5 hrs 1.5 kgs of soap is removed and the remaining 18.5 kgs of oil is washed with hot water for 4 to 6 times till free of alkali. The resultant neutralised palm oil (18 kg) is taken for winterization. In the Illrd example of neutralisation, 20.2 kgs of crude palm oil is fed into the neutraliser by means of vacuum and heated to 70-85°C under vacuumCalculated amount of alkali (80-95 gms) is dissolved in water and heated to 70-80°C. The hot alkali is admitted into the reactor and the reaction is carried out with slow stirring for 5-10 minutes. The soap formed is allowed to settle by gravity by reduciung the temperature of the contents to 48-65°C under vacuum. After 5 hrs 2 kgs of soap is removed and the remaining 18.7kgs of palmoil is washed with hot water for 4-6 times free of alkali. The resultant neutralised palmoil (18.2kg) is taken for winterization. The neutralized palm oil obtained from the above three experiments are combined (53 kg) and fed into the winterization unit, heated to 60- 70°C by means of steam through the Jacket, the rate'of which can be controlled by PID controller with a holding time for 5-15 mints, then cooled to 18-28 °C at the rate of 10-20°C/hr by means of chilled water through the Jacket with a preprogrammed PED controller. The entire process of heating and cooling is carried out with controlled stirring. When the temperature of the oil reaches to the desired temperature the crystallized mass was taken out and filtered by means of a rotary drum vacuum filter, over a period of 2 hrs and 34 kgs of clear palm olein and 15 kgs of dry stearin is obtained with a handling loss of 1 kg. The yield of palmolein is 70% and stearin is 30%. 27kgs of neutralised, winterized palm olein thus obtained is taken for deodorisation., The deodorisation unit is evacuated first to 1-5 mm Hg. The material is fed into the vessel by means of vacuum and heated to 120-160°C under vacuum (1-5 mbar). During the heating period steam is sparged to the vessel at a rate of 0.2-0.3kg/hr and finally after 2 hrs, the product is cooled to 40- 50°C by means of cold water circulation through the internal cooling coils. 26 kgs of carotene rich red palmolein with bland flavour is obtained after deodorisation. Tabid. PFA specifications for palm olein Palm olein: means the liquid fraction obtained by fractionation of palm oil obtained from the fleshy mesocarp of fruits of oil palm (Elaeis Guineensis) tree by the method of expression or solvent extraction.lt shall be clear,free from rancidity,suspended or other foreign matter, separated water,added colouring and flavouring substances or mineral oils. It shall conform to the following standards namery> (a) Butyro-refactometer reading at 40°c 43.7-52.5 orRefiactive indexat40°c 1.4550-1.4610 (b) Iodine value (Wijs method) 54-62 (c) Saponification value 195-205 (d) Goud point Not more than 18°c (e) Unsaponifiable matter Not more ihan 12 per cent (f)Free Fatty Acids (expressed as oleic acid) Not more than 025 per cent (g) Moisture Not more than 0.1 per cent The main advantages of the present invention: (1) The novel process is cost effective forproducing carotene rich red palm olein. (2) Maximum carotene retention and Free Fatty Acid (FFA) reduction is attained during neutralisation process by employing process conditions such as vacuum and temperature;. Above 98% carotene retention is achieved by this process (3) Maximum palm olein yield of above 70% is obtained during winterization .and stable p' polyphormic forms of palmstearin crystals are also obtained as a byproduct in this process (30%). (4) Filtration of the winterized mass within a time of 2hrs has resulted in the easier separation of F crystals and carotene enriched red palm olein. (5) In the deodorisation step, by employing reduced temperature and high vacuum, high carotene and vitamin E rich red palm olein is obtained with no off flavor. We Claim: 1. A process for the production of nutritious red palm olein which comprises; i) treating preheated crude palm oil at a temperature ranging 70-85°C with preheated caustic soda of concentration ranging 0.4 to 0.5% w/w dissolved in water uader stirring for a period ranging 5-10 minutes, ii) cooling the mixture at a temperature ranging between 48 to 65°C under vacuum, iii) removing soap formed in above step from the oil, iv) washing the remaining oil with hot water to obtain neutralized alkali free oil, v) winterizing the alkali free oil by heating at a temperature ranging 60-70°C for a period ranging between 5-15 minutes followed by cooling between 18-28°C by controlled conditions of cooling, ranging from 10-20°C/hr by using a winterization unit, to get crystallized mass, vi) separating the solid mass (palm stearin) by filtration to get clear palm olein, vii) deodorizing by heating simultaneously the palm olein obtained above to a temperature in the range of 120 - 160°C under vacuum ranging 1 - 5 m bar and spraying steam at a rate of 0.2 to 0.3 kg /hr for a period of 2 hr, viii) cooling the resultant to obtain nutritious palm olein. 2. A process as claimed in claim 1 wherein easy separation of palm stearin and carotene enriched palmolein in step (VI) is effected using rotary drum vacuum filter. 3. A process as claimed in claims 1-2 wherein the free fatty acid (FFA) content is reduced to the level of 0.25 - 0.5 by weight. 4. A process as claimed in claims 1-3 wherein the iron and copper contents are reduced by 90% and 92% respectively. 5. A process for the production of nutritious red palm olein substantially as herein described with reference to the examples cited.

Documents:

407-del-2002-abstract.pdf

407-del-2002-claims(cancelled).pdf

407-del-2002-claims.pdf

407-del-2002-complete specification (granted).pdf

407-del-2002-correspondence-others.pdf

407-del-2002-correspondence-po.pdf

407-del-2002-description (complete).pdf

407-del-2002-drawings.pdf

407-del-2002-form-1.pdf

407-del-2002-form-2.pdf

407-del-2002-form-3.pdf

407-del-2002-form-4.pdf