FORM 2
THE PATENT ACT 1970 & THE PATENTS RULES, 2003
COMPLETE SPECIFICATION
(See section 10 and rule 13)
1. TITLE OF THE INVENTION
METHOD FOR THE PURIFICATION OF CRUDE SUNFLOWER WAX
2. APPLICANT
(a) NAME: PRAJ INDUSTRIES LIMITED
(b) NATIONALITY: Indian Company
(b) ADDRESS: PRAJ Tower, 274-275, Bhumkar
Chowk - Hinjewadi Road, Hinjewadi, Pune-411057, INDIA
3. PREAMBLE TO THE DESCRIPTION
The following specification particularly describes the invention and the manner in which it is to be performed.

4. DESCRIPTION
FIELD OF INVENTION
The invention relates to a method for the purification of crude sunflower wax using an alcohol as a purifying solvent. It particularly relates to the use of ethyl alcohol as said solvent for efficient and economic purification of crude sunflower wax into economically valuable high purity wax products.
BACKGROUND
The waxes are organic compounds that characteristically consist of long alkyl chains. The natural waxes comprise esters of carboxylic acids and long chain alcohols or mixtures of unsubstituted and substituted hydrocarbons, such as higher alkanes, long chain fatty acids and primary alcohols. These waxes are synthesized by several plants and animals. The plant origin waxes contain the mixtures of unesterified hydrocarbons. The waxes of camauba, rice bran, and sunflower are some examples of the vegetable waxes.
The sunflower oil is one of the most important edible oils in the world and India is a largest consumer of it. The sunflower oil contains about 1 % waxy materials called sunflower oil wax, which is a byproduct of the sunflower oil refining process. The crude wax has certain low value applications; however if purified to certain higher degree it

forms a valuable product as being used in cosmetics and food preparations.
Chemically the sunflower wax is a heterogeneous product with made up of saturated monoesters of long chain fatty acid [C-38 to C-42] and long chain fatty alcohols [C-38 to C-42]. Up on refining or purification the wax becomes a relatively homogenous mixture having physical characters like melting point of about 78 °C to 82 °C , saponification value of about 70 to 90 units, acid value of about 1 to 10 units and iodine Value of about 10-20 units.
This purified wax then has many industrial applications like leather polishes, crayons, candles, shoe creams, paper coatings, carbon papers, lubricants etc. Other major applications are in food industry like in chocolate enrobes, vegetable coatings and wax emulsions for fruit preservation. It is further used in pharmaceuticals products like tablets, ointments, suppositories and cosmetic products like moisturizing lotions, lipsticks, skin creams etc.
The sunflower wax is recovered during sunflower oil refining. It contains a high quantity of fatty acids, both monounsaturated and polyunsaturated. It further contains long chain saturated esters, an organic compound that has replaced the hydrogen content. There are several types of sunflower oils produced based on the sunflower cultivar varieties. Upon refining or purification the wax form hard and relatively homogenous mixture having physical characters like melting point of about 78-80 °C, saponification value of about 80

units, acid value of about 1-10 units and iodine value of about 10-20 units. The purified sunflower wax is thermally stable, therefore, excellently suitable for light coloured, practically odourless and tasteless lip balms, lipsticks and other oil gel products.
In the prior art, in one of the methods, the crude sunflower wax is purified or refined is by removing the residual oil from it by hydraulic pressing to maximum extent possible, followed by extracting it in solvents like hexane with water. However, these extractions are costly for recycling of hexane * in the process is expensive and efficiency of the process is limited. The disclosed invention describes a novel method of purification of crude sunflower wax to high' purity waxes.
BRIEF DESCRIPTION OF THE INVENTION
The disclosure provides a method for purifying crude sunflower wax comprising: mixing said wax with ethanol forming a mixture; refluxing said mixture for a desired time dissolving said wax; allowing said mixture to stand idle for desired time; separating undissolved matters from liquid fraction; cooling said liquid fraction allowing formation of crystallised wax; removing said crystallised wax by filtration; washing said crystallised wax by ethanol; repeating steps above up to three times with said undissolved matters to extract remaining wax; and pooling and drying said crystallised wax under vacuum forming a final

product that is a purified sunflower wax with consistent characters of physical and chemical properties
DETAILED DESCRIPTION OF THE INVENTION
In an embodiment of the invention, the crude sunflower wax obtained as a byproduct of the sunflower oil refining process is dissolved in absolute ethyl alcohol. In the first step, about five parts of ethanol and one part the wax is refluxed at about 75 °C in a reflux vessel for about 1 hour to allow dissolution of said wax into ethanol leaving impurities undissolved in the mixture. The oil present in the crude is also dissolved in ethanol. After refluxing the mixture, the liquid fraction is decanted and allowed to cool to room temperature for the wax to crystallize, out from the solution. Then the solid wax is removed by filtration under vacuum, once washed with ethanol, optionally decoloured with an oxidizing agent, and dried to get the white to pale yellow solid mass of purified sunflower wax having consistent physical and chemical properties like meltfng temperature and purity. The impurities/ residues obtained are further subject to ethanol refluxing to recover remaining wax up to 3 times, if required. On average, the crude sunflower wax contains up to 40% oil, which is obtained as a byproduct of the process disclosed herein. Further remaining residues may also be as crude waxy material.

In another embodiment of the invention, ethanol used as the solvent for refluxing of the crude sunflower wax is absolute ethanol or ethanol at least 99% pure by volume. Any reduction in the purity of ethanol below 99% leads to drastic reduction in the final yield of purified rice bran wax as the presence of water in ethanol leads to reduction in dissolution of wax in ethanol.
In yet another embodiment of the invention, the refluxing of said wax and ethanol mixture is performed for at least one hour at temperature about 75 °C with an efficient condenser to prevent loss of the solvent.
In further embodiment of the invention, the purified sunflower wax is used in preparation of pharmaceutical or cosmetic products that required unique characters of the wax like its melting temperature, texture, colour, etc.
ADVANTAGES OF THE DISCLOSED PROCESS:
• The disclosed process is simple, carried out in two vessels, and hence is scalable for the large volume applications.
• The steps used for recovery are simple and efficient due to simplicity of the process.
• The disclosed process is substantially more economical compared with earlier processes.

• Ethanol is,recycled in the process after simple pre-treatment.
EXAMPLES
Examples provided below give wider utility of the invention without any limitations as to the variations that may be appreciated by the person skilled in the art. A non-limiting summary of various experimental results is given in the examples, which demonstrate the advantageous and novel aspects of the process disclosed herein.
EXAMPLE 1
About 10G g of crude sunflower wax containing residual oil impurity was taken in a refluxing vessel with about 500 mL of ethanol [99.9% pure by volume] forming a mixture. Then said mixture was refluxed at about 75 °C for about 1 h to dissolve the wax part and then allowed to stand idle at room temperature for about 30 min to settle the resinous mattes at the bottom of reactor. Next, the top liquid fraction containing mostly wax and oil was decanted and collected in a vessel. The undissolved wax along with impurities was again subjected to the above refluxing steps with reduced amounts of ethanol at each subsequent repeat at 400 mL and 300 mL respectively to recover the undissolved wax. The liquid fractions after each step were collected and pooled. Next, said liquid fraction pool was cooled

at room temperature, allowed to stand idle for dissolved wax to crystallize out from oil and other impurities, and then separated by vacuum filtration. Said crystallized wax was once washed with about 100 ml_ of ethanol and dried under vacuum to form the final wax product [purified rice bran wax]. These steps afforded about 48 g of highly pure final wax product with acid value of about 1.5 units, saponification value of about 87 units and iodine value of about 27 units with white to white colour. This product has a melting point of about 80 °C. Further, about 37 g of oil and about 8 g of solid impurities were recovered as byproducts.
EXAMPLE 2
About 100 g of crude sunflower wax containing residual oil impurity was taken in a refluxing vessel with about 500 mL of ethanol [98% pure by volume] forming a mixture. Then said mixture was refluxed at about 75 °C for about 1 h to dissolve the wax part and then allowed to stand idle at room temperature for about 30 min to settle the resinous mattes at the bottom of reactor. Next, the top liquid fraction containing mostly wax and oil was decanted and collected in a vessel. The undissolved wax along with impurities was again subjected to the above refluxing steps with reduced amounts of ethanol at each subsequent repeat at 400 mL, 300 mL, 200 mL, and 300 mL respectively to recover the undissolved wax. The liquid fractions after each step were collected and pooled. Next, said liquid

fraction pool was cooled at 10 °C temperature, allowed to stand idle for dissolved wax to crystallize out from oil and other impurities, and then separated by vacuum filtration. Said crystallized wax was once washed with about 100 ml of ethanol and dried under vacuum to form the final wax product [purified rice bran wax]. These steps afforded about 31 g of highly pure final wax product with acid value of about 2 units, saponification value of about 71 units and iodine value of about 30 units with white to white colour. This product has a melting point of about 78 °C. Further, about 33 g of oil and about 33 g of solid product were recovered as byproducts.
EXAMPLE 3
About 100 g of crude sunflower wax containing residual oil impurity was taken in a refluxing vessel with about 500 mL of ethanol [95% pure by volume] forming a mixture. Then said mixture was refluxed at about 75 °C for about 1 h to dissolve the wax part and then allowed to stand idle at room temperature for about 30 min to settle the resinous mattes at the bottom of reactor. Next, the top liquid fraction containing mostly wax and oil was decanted and collected in a. vessel. The undissolved wax along with impurities was again subjected to the above refluxing steps with reduced amounts of ethanol at each subsequent repeat at 400 mL, 300 mL, 200 mL, and 300 ml_ respectively to recover the undissolved wax. The liquid fractions after each step were collected and pooled. Next, said liquid

fraction pool was cooled at 10 °C temperature, allowed to stand idle for dissolved wax to crystallize out from oil and other impurities, and then separated by vacuum filtration. Said crystallized wax was once washed with about 100 mL of ethanol and dried under vacuum to form the final wax product [purified rice bran wax]. These steps afforded about 24 g of highly pure final wax product with acid value of about 4 units, saponification value of about 135 units and iodine value of about 61 units with white to white colour. This product has a melting point of about 78 °C. Further, about 26.6 g of oil and about 54.2 g of solid product were recovered as byproducts.
While the invention has been particularly shown and described with reference to embodiments enlisted in examples, it will be appreciated that several of the above disclosed and other features and functions, or alternatives thereof, may be desirably combined into many different systems or applications. Also that various presently unforeseen and unanticipated alternatives, modifications, variations, or improvements therein may be subsequently made by those skilled in the art which are also intended to be encompassed by the following claims. Although the invention has been described with reference to specific preferred embodiments, it is not intended to be limited thereto; rather those having an ordinary skill in the art will recognize that variations and modifications may be made therein.

which are within the spirit of the invention and within the scope of
the claims. . -

5. CLAIMS
We Claims:
1. A method for purifying crude sunflower wax comprising:
. a) mixing said wax with ethanol forming a mixture;
b) refluxing said mixture for a desired time dissolving said -
wax;
c) allowing said mixture to stand idle for desired time;
d) separating undissolved matters from liquid fraction;
e) cooling said liquid fraction allowing formation of crystallised wax fraction;
f) removing said crystallised wax fraction by filtration;
g) washing said crystallised wax fraction by ethanol;
h) repeating steps (a) to (g) up to five times with said undissolved matters to extract remaining wax; and
i) pooling said crystallised wax fractions and drying under vacuum forming a final product.
2. A method of claim 1, wherein purity of ethanol is not less than 95%
by volume.
3. A method of claim 1, wherein said refluxing is performed for at
least for one hour.
4. A method of claim 1, wherein said refluxing is performed at about
75 "C. '

5. A method of claim 1, wherein said liquid fraction is gradually cooled to room temperature to about 10 °C.
6. A method of claim 1, wherein said crystallised wax fraction is filtered by vacuum filtration,
7. A method of claim 1, wherein said crude sunflower wax contains between up to 40% oil by weight.
8. A method of claim 1, wherein said final product is clear white to pale yellow in colour upon vacuum drying.
9. A wax product according to claim 1, used in cosmetic or food preparations.