Title of Invention

A PROCESS FOR THE PREPARATION OF HIGH MELTING POINT WAX HAVING MELTING POINT OF 68-75° C FROM CRUDE WAX

Abstract

A process for the preparation of wax for use as an industrial product with high melting range is described. The product is an ester containing n-triacontanol, a growth promoter as one of the fatty alcohol. Recovery of oil (60-80%) from the crude wax was achieved using repeated extraction of cold solvent hexane. The separated solid material from miscella is added with chloroform and mixed for complete solubilisation of wax. The solution was filtered to remove insoluble material (including fine particles of hulls) under pressure. The miscella containing chloroform and chloroform solubles is concentrated and further precipitated wax with chilled acetone. Separation of wax was carried out by filtration. The wax has a melting range of max temperature 68-75 C. The product contains long chain fatty acids esterified with long chain alcohol, having n-triacontanol, a growth promoter.

Full Text

The present invention relates to a process for the preparation of high melting point wax having melting point 68-75° C from crude wax. The wax obtained from different sources of wax such as plants, animals, insects and marine origin are used in various industries. The wax obtained from edible source is used in food industries such as confectionery, coating of fruits and vegetables for storage stability and pharmaceutical purposes. Generally, preparation of wax from various sources involves extraction and isolation from other interfering substances. Separation of wax from natural sources usually is obtained by physical or chemical method. By physical method, is normally done by using adsorbents and chemical method involves organic solvents. Indian grown sunflower seed has high amounts of hulls varying from 24-32%. Majority of 2,5-3.0% wax present in the seed is situated in the hull portion. In India, the crude wax of oil refineries, tank settlings in sunflower oil industries and seed hulls are the major sources of sunflower seed wax. Wax gets extracted along with the oil if, seeds are crushed without dehulling and is responsible for turbidity in oil, which is unacceptable by consumers. Normally, dewaxing is done during refining of oil and during the process lot of crude wax is released. The oil obtained by expeller pressing and solvent extractions is stored in huge tank before refining. During storage, wax and foreign materials settle at the bottom of the tank as tank settlings/sludges. The industries with dehulling technology prior to oil extraction are left with sunflower seed hulls. In the present study a number of solvents were used to extract wax efficiently. Solvents like hexane, hexane: ethanol, carbon tetracholoride and choloroform were used. Chloroform was found to be the efficient solvent to recover wax from sunflower seed hull and from crude wax obtained in the sunflower oil refining industries. The wax extracted from crude wax of sunflower oil refining industry is comparable with the commercially available carnauba wax. The characteristics of the two waxes, such as sunflower seed wax and carnauba wax. (Table Removed) A few related processes available for the removal or preparatiori of wax from sunflower seed in different countries are described. Reference may be made to Walker and Parkin 1947, US patent No. 2,425,001 wherein winterisation of crude vegetable oils during caustic refining has been described. The winterisation was done at temperatures between 0-5 C. Method of winterisaîion is done for dewaxing sunflower oii but not extraction of wax from crude wax. Reference may be made to Young; Herbert Thomas (Cincinnati, OH) 1976, The Procter & Gamble Company (Cincinnati, OH) US patent NO. 3,943,155 wherein, simultaneous refîning and dewaxing of crude vegetable oii to get thoroughly dewaxed oii has been described. A process for refining and dewaxing crude vegetable oils using only one separation step which removes both the hydrophilic and waxy components from the crude oii. An alkali refining/dewaxing treatment is employed on crude oii at a temperature of from 15 to 45 degree F. Though this method involves only one step it is essentially an alkali refining or dewaxing employed on crude oii at a low temperature. Reference may be made to Beharry, Christopher R. 1981, The Procter & Gamble, Cincinnati, US patent No. 4,272,447 wherein crude edible oii wax removal process. This invention relates to an improved process for refining and dewaxing crude vegetable oils, consistently achieved in refining crude oils such as sunflower, safflower, and corn oii. Steps comprised of tempering the crude vegetable oii for wax nucleation at a temperature from 75 to 120 F for 24 hours, holding and coolîng temperature of crude oii for wax agglomeration at a temperature from 40 F to 70 F for 5 hours, refining and cooling of oii at a temperature from 80-90 F, with an aqueous alkali solution to provide a mixture of a wax containing aqueous phase and a refined oii phase. This method deals with improved process for refining of sunflower oii using temperature variations during the process but not the extraction of wax from crude wax. Reference rnay be made to Gibble; Walter P. (Brea, CA); Rhee; Joon S. (Anaheim, CA) 1976, Hunt-Wesson Foods, Inc. (Fullerton, CA) US patent NO. 3,994,943 wherein dewaxing of vegetable oils is described. High wax content sunflower oii is dewaxed by combining it with an aqueous treating agent containing an inorganic phosphate degumming agents and a mixture of surfactants to form an emulsion which is centrifuged to separate the waxy material. This method reveals only the removal of wax from high wax content sunflower oii but not the extraction of wax from crude wax. Reference may be made to Burnashev, V R, Rafal1 son, A B, volotovskaya, S N, Stamgya, Krishtofovich, S N, Kuznetsova, N V, Prokorova, L T, Frolova, N N 1984, Nauchno Proizvodstvennoe Ob' 'edinenie', 'Maslozhirprom' USSR patent No. SU 1 72 78 96 A, wherein, purification of sunflower seed oii or removal of wax from oii by crystallization using an adsorbant. This method is involved with temperature variation at the time of phase separation, which complicates the circuit connected with additional power loss. Reference may be made to Best, Bernd 1999, (Morfelden-Walldorf, DE), Brunner; Karlheinz (Oelde-Stromberg, DE), Hegwein,, Katja (Reinheim, DE), Ricker, Rainer (Dietzenbach, DE), Frische, Rainer (Frankfurt am Main, DE) Frische GmbH (Alzenau, DE) US patent NO.5,928,696 wherein, process for extracting native products which, are not water-soluble from native substance mixtures by centrifugal force, have been studied. This method reveals that the organic solvents used were different from the solvent used in the present investigation and also there are no of addition of water and acid binding substances in the present investigation, Reference may be made to Lake; Alan W. (Transvaal, ZA) 1976, Chemical Services (Proprietary) Limited (Johannesburg, ZA), US patent NO. 3,931,258 wherein, recovery of sugar cane wax is described. This invention relates to a process for recovering wax from filter cake derived from the treatment of sugar cane in the production of cane sugar. The process involves taking up the wax in water by forming an aqueous slurry of the filter cake, adding a surface active agent to the slurry to assist the release of wax from the fibres in the slurry and then heating the slurry to melt the wax which then passes into the water. Thereafter an extractant for the wax, such as kerosene, is added to the slurry to extract the wax whereafter the extractant is separated off, the wax is allowed to crystallize on cooling and is then recovered by filtration or centrifuging. Reference may be made to La Freniere; Lucie Y. (Brights Grove, CA); Boucher; Heather A. (Point Edward, CA) 1992, Exxon Research and Engineering Company (Florham Park, N J) US patent No. 5,084,183 wherein, fractionation of light/heavy waxes by use of porous membranes. Mixtures of light and heavy waxes are fractionated by permeation through a porous membrane at temperatures just above the cloud point of the mixture with the heavier, higher melting point waxes being the component of the mixture which selectively permeates through the porous membrane. This is physical separation of light and heavy wax from sugar cane by product. Reference may be made to Fukuyo; Kazumi (Minato-ku, JP); Fujimura; Kouji (Kisarazu, JP); Fusano; Toshiharu (Kawasaki, JP) 1999, Nippon Petrochemicals Company, Limited (Tokyo, JP) US Patent No. 5,882,114 A method of continuous extraction of crude wax and apparatus therefor is described. A method and an apparatus for continuously extracting a wax component contained in a solid residue with a solvent, in which method, the solid residue obtained from the juice of sugar cane is used as a raw material. To make the extraction time uniform and to obtain the wax at a high efficiency of extraction, the solid residue and an organic solvent for extraction are mixed under shear force and agitated in directions perpendicular to the flow direction. Reference may be made to Phukan; Amal C. (Assam, IN) 2002, Council of Scientific & Industrial Research (CSIR) (New Delhi, IN) US Patent No. 6,486,335 wherein Process for the preparation of refined hard sugarcane wax having improved qualities from press mud is described and relates to a process for the preparation of refined hard sugarcane wax having improved qualities from press mud which comprises digesting press mud with a non polar solvent in the presence of activated charcoal and separating the sugarcane wax. This invention relates to the preparation of refined hard wax of sugar cane having improved qualities from press mud using non polar solvent and activated charcoal. The main object of the present invention is to provide a process for the preparation of wax from crude wax of sunflower oii refineries, tank settlings and hulls Another object is to provide a process for recovering of wax from sunflower seed hull obtained after dehulling of seeds Yet another object is to provide a process as by-product utilization Still another object is to provide a process for a high melting point wax Another object of the present invention is to provide utilization of sunflower seed wax Another object of the present invention is to provide beneficiation of total technology of sunflower seed Another object of the present invention is to provide a low calorie wax esters Another object of the present invention is to provide a low calorie wax esters from a natural source Accordingly ,the present invention provides a process for the preparation of high melting point wax having melting point 68-75° C from crude wax, which comprises: i) removing oil from crude wax obtained from oil refining industries by conventional methods using cold hexane as solvent to obtain miscella, ii) separating miscella containing oil and hexane by known methods to obtain wax enriched material, iii) characterized in that adding chloroform to the wax enriched material and mixing to obtain solubilised wax, iv) concentrating the solubilised wax 4-15 fold, v) precipitating above said solubilised wax with chilled acetone and vi) separating wax from acetone by filtration In case of extraction of wax from hulls steps i) to iii) is not necessary. iv) involves dipping of hulls in chloroform for a short period v)filtering the insoluble materia! (fine particles of hulls) vi) concentrating miscella containing wax in chloroform vii) precipitating wax with chilled acetone and viii) separating wax from acetone by filtration Novelty Novelty steps of this invention is the development of a new process for the preparation of high melting wax from crude wax of sunflower seed oii refining industries • The novelty of the process is such that the recovery of wax from crude wax obtained from sunflower oii refineries and tank settlings • Removal of oii from crude wax • Use of cold hexane to retain wax in the residue • Separation of impurities mainly of seed huli fines • Use of chloroform for solubilisation of wax • The product has high melting point ranging 68-75 C as the process yields the wax with higher purity compared to crude wax • The wax with high temperature as the melting range is between 68-75 C is achieved by this process • The process is that the recovery of oii in such a manner, which does not affect the quality profile (acceptable) from the consumer's point of view. • Process provides non greezy wax with white colour • The wax obtained by this process contains n-triacontanol, and can be used in agricultural industry as a growth promoter The process is further illustrated by the examples given below, which shouid not however be construed to limit the scope of the invention. Example 1 A process for the preparation of wax from crude wax 1. 500 g weight of crude wax was taken 2. 1 litre of hexane extracted at room temperature (28 C) 3. Separated by decantation and filtration 4. Residue treated with chloroform (1:4) 5. Filtration under vacuum 6. Filtrate concentrated 4 fold 7. Chilled with acetone ( 8C) (1:1) Product: Oii content in the crude wax =74% Oii obtained = 60 g/100g crude wax Wax obtained = 6% Example 2 A process for the preparation of wax from crude wax 1. 250 g weight of crude wax taken 2. 1000 ml of hexane added at cold temperature 3. extraction repeated 5 times 4. separated by decantation and filtration 5. residue treated with chloroform (1:4) 6. filtration was done under vacuum 7. filtrate concentrated under vacuum 8 fold 8. chilled with acetone (8 C) (1:1) Oii content in the crude wax =74% Oii obtained = 73 g/100g crude wax Wax obtained = 9 % Impurities = 18% Example 3 A process for the preparation of wax from crude wax 1. 5 kg weight of crude wax taken 2. 15 litres of hexane added at cold ternperature 3. extraction repeated 5 times 4. separated by decantation and filtration 5. residue treated with chloroform (1:4) 6. filtration was done under vacuum 7. filtrate concentrated under vacuum 15 fold 8. chilled with acetone ( 8C) (1:1) Oii content in the crude wax =74% Oii obtained = 72 g/100g crude wax Wax obtained = 10% Impurities = 18% Example 4 A process for the preparation of wax from crude wax 1. 250 g weight of crude wax taken 2. 1000 ml of hexane added 3. extraction at cold ternperature for 6-8 hrs 4. extraction repeated 3 times 5. separated by decantation and filtration 6. residue treated with chloroform (1:6) 7. filtration was done under vacuum 8. filtrate concentrated under vacuum 8 fold 9. chilled with acetone (1:1) at 8 C 10. wax is passed through charcoal Oii content in the crude wax =74% Oii obtained = 73 g/100g crude wax Wax obtained = 9 % (before passing through charcoal) Impurities = 18% Wax after passing through charcoal gave a very poor recovery. Example 5 A process for the preparation of wax from tank settlings 1. 500 g weight of tank settlings was taken 2. 2 litre of hexane extracted at room temperature 6-8 hrs 3. Separated by decantation and filtration 4. Residue treated with chloroform (1:4) 5. Filtration under vacuum 6. Filtrate concentrated 8 fold 7. Chilled with acetone (1:1) Product: Oii obtained in the settlings = 62 g/100 g Wax obtained = 3.0 g/100 g Impurities = 34 g/100 g Example 6 A process for the preparation of wax from seed hulls 1. 500 g weight of hulls was taken 2. Coarse ground 3. Dipping the hulls taken in cotton cloth for 300 seconds in chloroform (1:6 w/v) 4. Filtration to remove fine particles of hulls 5. Filtrate concentrated 10 fold 6. Chilled with acetone (1:1)at8C Product: Oii content in the huli = 2.6 g/100 g huli Wax obtained = 1.5 g/100 g huli Impurities = 94. O g/100 g huli Advantages: The main advantages of the present invention are » The product having high melting point wax for industrial use » Non-greezy white wax * Partially it can replace other vegetable wax having similar melting range for usage in industry * The wax obtained by this process contains n-triacontanol, and which can be used in agricultura! industry as a growth promoter * Total technology for sunflower industry * By-product utilization of sunflower oii refining industry * The method of processing consists of reasonable processing steps We claim: 1. A process for the preparation of high melting point wax having melting point 68-75°C from crude wax, which comprises: i) removing oil from crude wax obtained from oil refining industries by conventional methods using cold hexane as solvent to obtain miscella, ii) separating miscella containing oil and hexane by known methods to obtain wax enriched material, iii) characterized in that adding chloroform to the wax enriched material and mixing to obtain solubilised wax, iv) concentrating the solubilised wax 4-15 fold, v) precipitating above said solubilised wax with chilled acetone and vi) separating wax from acetone by filtration 2. A process as claimed in claim 1, wherein crude wax is from sunflower oil refineries,tank settlings and hulls. 3. A process for the preparation of high melting point wax having melting point 68- 75° C from crude wax substantially as herein described with reference to the examples.

Documents:

440-DEL-2003-Abstract-(24-09-2008).pdf

440-del-2003-abstract.pdf

440-DEL-2003-Claims-(24-09-2008).pdf

440-del-2003-claims.pdf

440-DEL-2003-Correspondence-Others-(24-09-2008).pdf

440-del-2003-correspondence-others.pdf

440-del-2003-correspondence-po.pdf

440-DEL-2003-Description (Complete)-(24-09-2008).pdf

440-del-2003-description (complete).pdf

440-del-2003-form-1.pdf

440-del-2003-form-18.pdf

440-DEL-2003-Form-2-(24-09-2008).pdf

440-del-2003-form-2.pdf

440-DEL-2003-Form-3-(24-09-2008).pdf

440-del-2003-form-3.pdf