Claims:We claim:
1. A process for the preparation of policosanol comprising:
a) providing a crude rice bran wax;
b) refluxing said rice bran wax using an organic solvent to separate oil, wax and resinous matter;
c) saponifying said resinous matter at desired temperature forming a soap;
d) drying said soap in oven;
e) extracting said soap using acetone to form a acetone soluble and sodium soap of fatty acids;
f) crystallizing acetone soluble at desired temperature for about 12 hours; and
g) removing said crystallized acetone soluble by filtration to get a final product.
2. The process of as claimed in claim 1, wherein said organic solvent is ethanol.
3. The process of as claimed in claim 1, wherein said refluxing is performed for 2 to 5 times at about 800 C to about 100 0C.
4. The process of as claimed in claim 1, wherein said saponification is performed at about 100 0C.
5. The process of as claimed in claim1, wherein said crystallization is performed at about 24 0C.
6. The process of as claimed in claim 1, wherein said final product comprises about 30% to about 38% policosanol with about 15% to about 20% triacontanol and about 7% to about 11% octacosanol.
7. The process of as claimed in claim 1, wherein said crude rice bran wax contains between 10% to 40% oil by weight.
8. The process of as claimed in claim 1, wherein said crude rice bran wax contains between 30% to 50% wax by weight.
, Description:FIELD OF INVENTION
The invention relates to a process for the preparation of policosanol from crude rice bran wax. It particularly relates to the use of residue left after wax refining for the preparation of policosanol after the removal of wax and oil from crude rice bran wax using an alcohol.

BACKGROUND
Rice is one of the most important grains in the world and India is second largest producer of rice in the world. Rice bran is valuable byproduct of rice milling industry because it contains about 12-25 % of oil depending on quality. The oil extracted from rice bran is called rice bran oil and is available in both grades (i.e. edible and non-edible). An important step in the processing of the oil is the removal of waxes present in the oil. Rice bran wax is a byproduct of the rice bran oil refining and it is a source of value added chemicals such as wax ester and oils. Rice bran wax mainly consist of saturated monoesters (C-46 to C-60) of long chain fatty acids (C-22 to C-26) and long chain fatty alcohols (C-26 to C-30) with ester. Rice bran oil has the highest wax content among vegetable oils and can reach up to 5%. Rice bran wax is a hard non tacky wax. The refined and bleached rice bran wax has melting point 78-82°c, saponification value 70-120 and iodine value 4 to 10. Crude rice bran wax is refined by removing oil and resinous matter. Refined rice bran wax is used in many industries like food, pharmaceuticals, polishes and cosmetics.
Policosanol is a major component of wax ester of rice bran wax. Policosanol is a mixture of higher chain length of fatty alcohols. Out of all the fatty alcohol triacontanol (C30) and octacosanol (C28) are commercially important. Octacosanol is used as a nutraceutical compound, whereas triacontanol is mainly used as plant growth regulator.
Triacontanol is characterized in being effective in very small concentrations as hormones. The mechanism of action is primarily by an increase the rate of photosynthesis and thereby to improve the productive capacity of the plants. Triacontanol activates the plant's genes controlling the photosynthesis; these genes in turn produce the enzymes controlling the dark reactions of photosynthesis leading to increase in the photosynthetic activities.
Octacosanol helps in improving human body's natural ability to process and use oxygen. It is used to treat various disease conditions and as a dietary supplement. It helps the body process oxygen and increase the amount of oxygen that is in the blood and flowing to the muscles. It increases strength and stamina, as well as reaction time. It is used in the treatment of a myriad of diseases, including Parkinson's and amyotrophic lateral sclerosis, or Lou Gehrig's disease. It is also used to treat herpes, skin infections, high cholesterol and hardening of the arteries.
Current invention discloses a method for simultaneous production of refined rice bran wax and policosanol from the crude rice bran wax. In prior art, extraction of policosanol from waxes is reported. Said policosanol are obtained from rice bran wax by saponifying either the crude or deoiled wax. This method is complicated and needs larger handling of raw materials. However, refining of rice bran wax followed by preparation of policosanol from leftover resinous matter containing some wax, in a same process is not reported. The main object of the present invention is to develop a process to refine the crude rice bran wax and prepare policosanol from remaining resinous matter which is novel and economical process.

DETAILED DESCRIPTION OF THE INVENTION
The present invention provides a process for the preparation of policosanol from the residue remained after refining the rice bran wax and oil from crude rice bran wax using ethanol as a solvent. Said process is a commercial alternative as it gives refined rice bran wax, crude rice bran oil and policosanol as a three major product.
The disclosed process further utilizes ethanol as an organic solvent over known methods providing economic advantages. The present invention further provides a method for purifying crude rice bran wax comprising mixing of wax with ethanol to refine it by selective removal of oil and resinous matter. The disclosed method further produced policosanol from left resinous matter containing some wax, by a process of the invention disclosed herein, the said wax is useful in food or cosmetic preparations and said policosanol is mixture of triacontanol and octacosanol which is useful as a plant growth regulator and octacosanol is useful in pharmaceuticals.
In one embodiment of the present invention, disclosed is a process for the preparation of policosanol comprising: providing a crude rice bran wax; refluxing said rice bran wax using an organic solvent to separate oil, wax and resinous matter; saponifying said resinous matter at desired temperature forming a soap; drying said soap in an oven; extracting said soap using acetone to form a acetone soluble and sodium soap of fatty acids; crystallizing acetone soluble at desired temperature for about 12 hours; removing said crystallized acetone soluble by filtration to get a final product. These steps lead to the preparation of oil, rice bran wax and policosanol of a wax of higher purity as compared to known methods.
In another embodiment of the invention, the process comprises crude rice bran wax obtained during refining process of rice bran oil. The crude rice bran wax contains oil and wax with resinous matter. Said wax is mixed with about 99% ethanol to form a mixture of oil, wax and resinous matter in ethanol. Next said mixture is refluxed at desired temperature and for a desired time to dissolve said wax into about 99% pure ethanol. The resultant mixture allowed to stand idle at desired temperature for about 30 to about 60 minutes, and then separating the undissolved matters from liquid fraction. Said liquid fraction containing oil, ethanol and wax is decanted in second reactor and said undissolved matter contains resinous matter, oil and wax. So to separate remaining oil and wax from undissolved matter, the above procedure is repeated two to four times with said undissolved matters to extract remaining wax in ethanol and separated out resinous matter from oil, wax and ethanol in a reactor. Next, obtained resinous matter along with some unreacted wax is used further for high pressure saponification. Said saponification is carried out at desired condition for desired hours. Obtained soap is decanted from the reactor and dried in an oven for the removal of moisture. Said dried soap is used for solid liquid extraction using acetone in the soxhlet apparatus for desired hours to form an acetone soluble and sodium soap of fatty acids. Said acetone soluble fraction is allowed to crystallize at about 24 0C for about 12 hours. Said crystallize mass is then filtered using Buchner funnel to separate it from filtrate. Said crystallize mass is dried in vacuum oven to get final policosanol product. Said final product comprises about 30 % to about 38 % policosanol. After preparation said product is analyzed to check the quantity of triacontanol and octacosanol in it with other policosanol.
In another embodiment of present invention the refluxing of said wax and ethanol mixture is performed for at least one hour at temperature about 800C to about 1000C. The total amount of ethanol used is between 2 to 5 times the amount of wax used depending upon the number reflux cycles used.
In another embodiment of present invention the saponification is performed at temperature about 1000C.
In another embodiment of present invention the crude rice bran wax contains between 30 % to 50 % oil by weight and between 30 % to 50 % wax by weight.
In another embodiment of present invention, said process afforded about 30% to about 38% policosanol with about 15% to about 20% triacontanol and about 7% to about 11% octacosanol.

ADVANTAGES OF THE DISCLOSED PROCESS
• The disclosed process is carried out systematically for selectively separation of oil, refined wax and policosanol from crude rice bran wax.
• The disclosed process gives refined rice bran wax, policosanol and rice bran oil as major products.
• 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 process.
• Ethanol can be reused by simple pretreatment.
EXAMPLES
Examples provided below give wider utility of the invention without any limitations as to the variations that may be appreciated by a 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 1000 gm of crude rice bran wax containing wax, oil and resinous matter was taken in a jacketed reactor having reflux condenser along with about 5000 ml (99.8%) ethanol. Said mixture was re-fluxed for about 1 hour at 80 0C to dissolve the wax and then allowed to stand idle at room temperature for half an hour to settle the resinous matter at the bottom of the reactor and then top liquid fraction containing oil, ethanol and wax was decanted in second reactor. This entire procedure was repeated four times in first reactor with 4000 ml, 3000 ml, 2000 ml and 3000ml ethanol and separated out all the four fractions of resinous matter, oil, wax and ethanol. Said process produces about 210 g resinous matter along with 350 g of oil and 426 g of refined wax. Next, obtained resinous matter was used further for high pressure saponification. Said saponification was carried out using about 25 g of NaOH and about 227 g of water under 4 kg/m3 nitrogen pressure for about 4 hours. Obtained soap was decanted further from the reactor and dried in an oven for the removal of moisture. Said dried soap was used for solid liquid extraction using about 1000 ml acetone in the soxhlet apparatus for about 12 hours to form an acetone soluble and sodium soap of fatty acids. Said acetone soluble was allowed to crystallize at about 24 0C for about 12 hours. Said crystallize mass was then filtered using Buchner funnel to separate it from filtrate. Said crystallize mass was dried in vacuum oven to get final policosanol product. This process afforded about 22 g of policosanol having 21% triacontanol and about 11% octacosanol in it.
EXAMPLE 2
About 1000 gm of crude rice bran wax containing wax, oil and resinous matter was taken in a high pressure reactor along with about 5000 ml (99.8%) ethanol. Said mixture was vigorously stirred at about 100 °C and using about 2 bar pressure for about 1 h to dissolve the wax part and then allowed it to stand idle at about 73 °C for 30 min to settle the resinous matter at the bottom of reactor. Next, settled resinous matter was removed from the bottom valve and top liquid fraction containing mostly wax and oil was collected in a separate vessel. This entire procedure was repeated in a high pressure reactor by treating the formed resinous matter with 5000 ml ethanol and separated out all the four fractions of resinous matter, oil, wax and ethanol. Said process produces about 280 g resinous matter along with 355 g of oil and 350 g of refined wax. Next, obtained resinous matter was used further for high pressure saponification. Said saponification was carried out using about 33 g of NaOH and about 330 g of water under 4 kg/m3 nitrogen pressure for about 4 hours. Obtained soap was decanted further from the reactor and dried it oven for the removal of moisture. Said dried soap was used for solid liquid extraction using about 1000 ml acetone in the soxhlet apparatus for about 12 hours to form an acetone soluble and sodium soap of fatty acids. Said acetone soluble was allowed to crystallize at about 24°C for about 12 hours. Said crystallize mass was then filtered using Buchner funnel to separate it from filtrate. Said crystallize mass was dried in vacuum oven to get final policosanol product. This process afforded about 88 g of policosanol having 20% triacontanol and about 8% octacosanol in it with other policosanol.
EXAMPLE 3
About 1000 gm of deoiled rice bran wax containing about 3-5 % oil was taken into a high pressure reactor along with about 5000 ml (99.8 %) ethanol. Said mixture was refluxed at about 100 °C and using about 2 bar pressure for about 1 h to dissolve the wax part and then allowed it to stand idle at 73° C for 30 min to settle the resinous mattes at the bottom of reactor. Next, settled resinous matter was removed from the bottom valve and top liquid fraction containing mostly wax and oil was collected in a separate vessel. This entire procedure was repeated two times in high pressure reactor by treating the formed resinous matter with 5000 ml, 3000 ml ethanol and separated out all the four fractions of resinous matter, oil, wax and ethanol. Said process produces about 600 g resinous matter along with 50 g of oil and 350 g of refined wax. Next, obtained resinous matter was used further for high pressure saponification. Said saponification was carried out at using about 72 g of NaOH and about 650 g of water under 4 kg/m3 nitrogen pressure for about 4 hours. Obtained soap was decanted further from the reactor and dried it oven for the removal of moisture. Said dried soap was used for solid liquid extraction using about 2000 ml acetone in the soxhlet apparatus for about 12 hours to form a acetone soluble and sodium soap of fatty acids. Said acetone soluble was allowed to crystallize at about 24°C for about 12 hours. Said crystallize mass was then filtered using Buchner funnel to separate it from filtrate. Said crystallize mass was dried in vacuum oven to get final policosanol product. This process afforded about 128.6 g of policosanol having 15.5% triacontanol and about 12% octacosanol in it with other policosanol.
EXAMPLE 4
About 1000 gm of crude rice bran wax was saponified using about 120 g of NaOH and about 1080 g of water under 4 kg/m3 nitrogen pressure for about 4 hours. Obtained soap was decanted further from the reactor and dried in an oven for the removal of moisture. Said dried soap was used for solid liquid extraction using about 3000 ml acetone in the soxhlet apparatus for about 12 hours to form an acetone soluble and sodium soap of fatty acids. Said acetone soluble was allowed to crystallize at about 24 0C for about 12 hours. Said crystallize mass was then filtered using Buchner funnel to separate it from filtrate. Said crystallize mass was dried in vacuum oven to get final policosanol product. This process afforded about 198 g of policosanol having 18% triacontanol and about 14% octacosanol in it with other policosanol.
While the invention has been particularly shown and described with reference to embodiments listed 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 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.