Title of Invention

A PROCESS FOR THE UPGRADATION AND BLEACHING OF CRUDE RICE BRAN WAX

Abstract The present invention relates to a process for upgradation and bleaching of crude bran wax, by treating crude rice bran wax with isopropyl alcohol (IPA) containing 1 to 15 % by volume water to form an IPA-wax suspension to allow precipitation of resinous matter thus formed from the IPA-wax suspension to obtain clear IPA wax solution containing upgraded wax, then the upgraded wax is bleached by adding sodium chlorite or sodium borohydride to IPA-wax suspension and the molten wax is bleached by adding 30% hydrogen peroxide to remove from clear by ketonic solvents(methyl ethyl ketone).The rice bran oil and the soft wax present in clear solution is separated by treating the clear solution by acetone and methyl ethyl ketone.
Full Text Field of the Invention:
The present invention relates to a process for the up-gradation and bleaching of crude rice bran wax, obtained during refining of crude rice bran oil. More particularly, the present invention relates to a process for refining and purification of crude rice bran wax obtained during de-waxing stage of refining process of rice bran oil to an essentially wax ester product which involves, a) removal of the triglycerides oil, b) removal of polymeric resinous material, c) bleaching of upgraded wax to obtain a pale yellow colored product that has potential in food, cosmetic and pharmaceutical applications. Depending on the intended application, some of these process steps may be omitted; for example, if the intended application is for industrial uses such as polishes, carbon paper, etc, the color may not be a great hindrance.
Background and Prior Art of the Invention:
About 3.8 lakh tons of crude rice bran oil is processed in India every year (India is the world's largest producer of rice bran oil) and an important step in the processing of the oil is the removal of waxes present in the oil (de-waxing). Rice bran oil has the highest wax content among vegetable oils and can reach up to 5% [F.T. Orthoefer, in Bailey's Industrial Oil and Fat Products edited by Y.H. Hui, John Wiley & ONS, Inc., New York p.393 (1996)]. Thus, there is a potential of about 28,000 tons of wax with a multitude of potential applications including paper coating, candles, waterproofing polish (floor, furniture and shoe), carbon paper, printing inks, adhesives, fruit and vegetable coatings, cosmetics, pharmaceutical preparations, etc. Purified rice bran also can at least partially substitute camauba wax, which is totally imported. The crude wax separated from the oil retains about 25% or more amount of oil, so the crude wax produced in the country is estimated to be around 35,000 to 60,000 tons. This product is presently underutilized for want of suitable processing technologies. The present invention provides for such a technology. A large number of industrial crude wax samples have been processed by the present process to test its efficacy.
There have been sporadic attempts to purify the crude rice bran wax. These have generally been restricted to removal ot the oil present along with the wax. while the exact composition of the wax is not known, there have been reports on the possible


presence [V.K. Belavadi and D.N. Bhowmick, J. Amer. Oil Chem. Soc. 65: 241-245 (1988)] of polymeric compounds in the wax. Removal of these components is of immense importance in the refining process so that the final product is acceptable for use in food pharmaceutical and cosmetic products. Earlier methods have not been successful in total removal of such compounds (hereafter referred to as "resinous matter"). The wax after removal of oil has an unacceptable dark color, largely due to these resinous materials. Physical methods of color removal such as adsorption onto bleaching clays and carbon are not effective and chemical methods, mainly oxidative bleaching, have been resorted to, frequently under drastic conditions that may chemically alter the wax components. For bleaching to be effective, it is essential that the resinous matter is totally removed from the wax as reported in the present invention. Mild conditions can then be employed, as shown in the present invention, for bleaching the wax.
As stated before, earlier attempts have largely been restricted to removal of the oil from the crude wax followed by bleaching. Chung - Sung et al, used isopropanol to remove the resinous matter from rice bran oil filter mud (Chemistry Taipei, 1961, 185-7, CA: 58: 3619) at 65°C in a ratio of 8:1. Eventhough the researchers tried to separate some resinous matter from rice bran oil filter mud, it was not possible to separate resinous matter quantitatively at 65°C when the wax is not dissolved completely in the isopropanol at this temperature. This procedure was also not tried for commercially produced crude rice bran wax obtained during the de-waxing step of rice bran oil processing.
Bleached rice bran wax was prepared by dissolving rice wax in methyl ethyl ketone at 76-77°C and cooled to 55°C followed by bleaching using a number of bleaching agents such as hydrogen peroxide, sodium chlorite, oxalic acid, sorbitan sesquioleate in sequence [Ishii Masakatsu, JP: 76,30,204 (1976)]. In this process at least five bleaching agents were used in sequence and hence may not be a commercially feasible process.
Cousins., et al [JAOCS, 30: 9-14 (1953)] reported some protocols to process a typical sample of tank settling from crude rice bran oil in various ways to obtain a hard, non tacky wax fraction. The procedures consists of removal of the oil from the tank settlings by washing with acetone, destruction of the phosphatides through hydrolysis

or saponification, and subsequent purification by fractionation from isopropanol; another involved hydration of the tank settlings, followed by separation of the aqueous and oil phases, and fractionation of oil phase from isopropanol solution. The waxes were bleached by hydrogen peroxide and by chromium trioxide in the presence of H2SO4 solution or by combination of these reagents Chung - Sung et al (Chemistry Taipei, 1961, 185-7, CA: 58: 3619) also purified the wax by heating it with CrO3 and 40% H2SO4 in a ratio of 1:1.5 (wt/wt) at 95°C for 2 hr. In another report acetone fractionated rice bran wax was bleached with 0.5 parts by wt. of H2O2 as well as 0.5 and 1 part by wt. of chromium trioxide with 4.5 to 5 parts of sulphuric acid for every part of wax (S. D. Tirumala Rao and K.V. Rao, Indian Oil & Soap Journal 29, (1964) 177). In all the above processes, rice bran wax was bleached with hydrogen peroxide followed by chromium trioxide in presence of sulphuric acid which are strong oxidizing agents and difficult to remove their traces from the wax and not clean and environmental friendly processes.
Rice bran wax was de-gummed by precipitation from melt (at 100-120°C) or solution followed by ozonization at 12°C for 4 hr. to give de-gummed and bleached wax [Y. Yoshihiro et al., JP, 79,100,404 (1979)]. Crude rice bran wax was also oxidized with cone. HNO3 to a light yellow wax [Rao, B., et al., Indian Patent 119747 (1970)]. Ozonization and nitric acid treatments are also environmentally not clean processes.
Thus the processes reported were not aimed at the complete removal of resinous matter from the crude rice bran wax obtained during the de-waxing stage of rice bran oil processing. Methodologies were needed for complete removal of the oil and the resinous matter present along with the wax esters. While de-oiling can be accomplished by a variety of organic solvents, a process for the complete removal of resinous matter does not exist. The aim of the present invention was to evolve such a process of removal of oil and the resinous matter present along with the wax ester.
Objects of the Present Invention:
The main objective of the present invention is to provide an efficient and simple commercially viable process with mild conditions and reagents for the up-gradation and bleaching of crude rice bran wax obtained during refining process of rice bran oil, which obviates the drawbacks of the processes, described above.

Another objective of the present invention is to remove the oil and resinous matter present in crude rice bran wax samples quantitatively by incorporating few volume percentages of water into IPA.
Yet another objective of the present invention is bleaching the upgraded rice bran wax in solvent medium particularly in IPA containing various amounts of water at the reflux temperature of the solvent.
A further object of the present invention is to use sodium borohydride to bleach rice bran wax.
Yet another objective of the present invention is to bleach the wax by adding hydrogen peroxide solution to molten wax after removal of residual solvent from the wet upgraded wax cake.
Detailed Description of the Invention:
Accordingly, the present invention provides a process for upgrading crude rice bran wax, said process comprising:
a) treating crude rice bran wax with isopropyl alcohol (IPA) containing 1 to 15%
by volume water to form an IPA-wax suspension;
b) allowing the IPA wax suspension to stand to allow precipitation of resinous
matter;
c) separating the resinous matter thus formed from the IPA-wax suspension to
obtain clear IPA-wax solution containing upgraded wax, oil and soft wax;
d) separating the upgraded wax from clear solution of step (c), and
e) optionally bleaching the upgraded wax before or after its is removed from the
clear solution.
In an embodiment of the present invention, the crude rice bran wax is a by-product obtained during dewaxing stage of refining process of rice bran oil.
In another embodiment of the present invention, the crude rice bran wax contains 25-70% of oil.

In yet another embodiment of the present invention, wherein in step (a), the ratio (weight: volume) of crude rice bran wax to aqueous IPA is 1:3 to 1:6.
In still another embodiment of the present invention, wherein in step (a), the reaction between the IPA and the crude bran wax is carried at 70-77° C.
In a further embodiment of the present invention, wherein in step (a), the IPA-wax suspension is further refluxed for 0.25 to 1 hour.
In one more embodiment of the present invention, the EPA-wax suspension is refluxed for 0.50 hours.
In one another embodiment of the present invention, wherein in step (b), the IPA-wax suspension us allowed to stand for 1-5 minutes to allow precipitation of resinous matter.
In an embodiment of the present invention, the hot IPA-wax suspension having temperature of 75-77° C is allowed to stand for 3-5 minutes to allow precipitation of resinous matter.
In another embodiment of the present invention, the resinous matter precipitates out in the form of dark brown liquid.
In yet another embodiment of the present invention, wherein in step (c), the resinous matter is removed from the clear IPA-wax solution by filtering.
In still another embodiment of the present invention, wherein in step (d), the upgraded wax is crystallized and separated from the clear solution containing upgraded wax, rice bran oil and soft wax.
In a further embodiment of the present invention, the upgraded wax is crystallized by cooling the clear solution to 30-35° C.
In one more embodiment of the present invention, the upgraded wax is separated by filtration.

In one another embodiment of the present invention, the clear solution obtained after filtering crystallized wax contains rice bran oil and soft wax.
In an embodiment of the present invention, the upgraded wax may be further upgraded by repeating steps (a) to (d) of claim 1 using the upgraded wax as the starting material.
In another embodiment of the present invention, the physical and chemical characteristics of upgraded wax thus obtained depend upon the source of the crude rice bran wax.
In yet another embodiment of the present invention, the physical and chemical
characteristics of upgraded wax thus obtained are:
(i) Color: around 18+ (Gardner scale in 1 cm cell);
(ii) M.P.: around 78-79°C;
(iii) A.V.: around 1-10;
(iv) S.V.: around 80 - 95 and
(v) I.V.: around 13-18.
In still another embodiment of the present invention, bleaching of the upgraded wax may be done with the IPA-wax suspension after removing the resinous matter.
In a further embodiment of the present invention, bleaching of the upgraded wax may be done with the IPA-wax suspension if the crude rice bran wax contains up to 40% oil.
In one more embodiment of the present invention, the upgraded wax is bleached by adding sodium chlorite or sodium borohydride to the IPA-wax suspension.
In one another embodiment of the present invention, the bleached upgraded wax may be separated from the clear solution by cooling the contents to 30-35°C and filtering the wax.
In an embodiment of the present invention, the solvent in the wet upgraded or bleached cake may be removed by distillation.

In another embodiment of the present invention,'any residual solvent may be removed by vacuum distillation.
In still another embodiment of the present invention, the bleaching of the upgraded wax can be done after separating it from the clear solution containing upgraded wax, oil and soft wax.
In yet another embodiment of the present invention, the upgraded wax may be separated and bleached if the crude bran wax contains greater than 40% oil.
In a further embodiment of the present invention, the upgraded wax may be bleached by adding 30% hydrogen peroxide to molten upgraded wax.
In one more embodiment of the present invention, the physical and chemical characteristics of the bleached wax are:
(a) - Color: around 11.8 - 14.3 (Gardner scale in 1 cm cell);
(b) M.P.: around 79-80°C;
(c) A.V.: around 1 -8;
(d) S.V.: around 75 -85, and
(e) I.V.: around 8-13.
In one another embodiment of the present invention, the rice bran oil and the soft wax present in the clear solution may be separated by treating the clear solution with ketone solvents.
In an embodiment of the present invention, the ketone solvents may be selected from the group acetone and methyl ethyl ketone.
The present invention also provides an upgraded rice bran wax prepared in
accordance with the aforesaid process and having the following the physical and
chemical characteristics:
Color: around 18+ (Gardner scale in 1 cm cell);
M.P.: around 78-79°C;
A.V.: around 1-10;
S.V.: around 80 - 95 and
I.V.: around 13-18.

The present invention further provides a bleached, upgraded rice bran wax prepared in
accordance with the aforesaid process and having the following the physical and
chemical characteristics:
Color: around 11.8 - 14.3 (Gardner scale in 1 cm cell);
M.P.: around 79-80°C;
A.V.: around 1 -8;
S.V.: around 75-85, and
I.V.: around 8-13.
More particularly, the present invention provides an efficient process for the up-gradation and bleaching of crude rice bran wax, said process comprises:
a) treating crude rice bran wax with isopropyl alcohol (IPA) containing 5 to 15%
volume percentages of water to precipitate resinous matter present;
b) separating the resinous matter thus formed;
c) cooling the IPA wax suspension to around 30 to 35°C followed by separation of
upgraded wax from IPA solubles;
d) separating soft wax and oil from IPA solubles using ketone solvents like acetone
and methyl ethyl ketone;
e) bleaching the upgraded wax using bleaching agents such as sodium chlorite or
sodium borohydride in IPA containing various volume percentages of water or by
optionally treating the molten upgraded wax with hydrogen peroxide solution, and
f) separating bleached wax after cooling to 30 to 35°C in case the bleaching is
carried out in IPA medium.
In an embodiment of the present invention a simple process is developed for the upgradation and bleaching of crude rice bran wax obtained during dewaxing stage of refining process of rice bran oil in aqueous IPA medium using sodium brorohydride or sodium chlorite or by treating the molten upgraded wax with hydrogen peroxide as bleaching agents.
In another embodiment of the present invention the resinous matter present in the crude rice bran wax is separated out quantitatively when water is incorporated into IPA.

In yet another embodiment of the present invention the separation of resinous matter and oil is achieved in a single step if the oil content of crude rice bran wax is less than 40%.
In still another embodiment of the present invention the removal of resinous matter and oil, and also bleaching is carried out continuously in the same vessel if the oil content in the crude wax is up to 40%.
In still another embodiment of the present invention the bleaching of upgraded wax is carried out in aqueous isopropanol medium to prepare good quality wax with minimum ash content.
In still another embodiment of the present invention the oil recovered in the upgradation step can be added to the crude rice bran oil for refining process thereby reducing oil loss to the vegetable oil industry.
In still another embodiment of the present invention provides a very simple and efficient filtration in both upgradation and bleaching steps.
In still another embodiment of the present invention upgraded and bleached wax obtained in the present invention is a uniform melting wax with about 78-80°C
In still another embodiment of the present invention the aqueous IPA can be re-used in the process by adjusting the required water content in the solvent.
The broad applicability of the invention was examined by upgrading and bleaching the crude rice bran wax in aqueous IPA using sodium borohydride or sodium chlorite as bleaching agents.
Preferably, the upgradation of crude rice bran wax is carried out using aqueous IPA with a water content ranging from 5 to 15% on the basis of wax.
Preferably, there is employed 3 to 6 times volume of IPA based on the crude rice bran wax for upgradation.
Preferably, there is employed a reaction time of 0.5 to 3 hours for upgradation of crude rice bran wax.

Preferably the bleaching is carried out using sodium chlorite or sodium borohydride. Preferably 1 to 3 weight per cent of sodium chlorite or 0.5 to 3% of sodium borohydride based on the upgraded wax.
Preferably sodium chlorite bleaching of upgraded wax is carried out in IP A containing 0.2 to 2% of water whereas sodium borohydride dissolved in equal weight of water and added to IPA.
Preferably the sodium chlorite and sodium borohydride bleaching is carried out in 5 to 7 volumes of IPA based on the weight of upgraded wax.
Preferably hydrogen peroxide (30% solution) bleaching is carried out by taking it 5 to 10 volume percent of the weight of the upgraded wax without organic solvent medium.
The Gas Chromatographic (GC) composition of wax esters and physical and chemical properties of a typical bleached wax sample is given below.
(Table Remove)The aim of the invention is to remove resinous matter from the crude rice bran wax by increasing the polarity of IPA by adding water to settle down the resinous matter from IPA solution followed by chemical bleaching. In the bleaching step oxidants like sodium chlorite and hydrogen peroxide and reducing agents like sodium borohydride were employed. The physical and chemical characteristics of the crude, upgraded and bleached waxes are given in Table 1. FDA specifications of rice bran wax are also given for comparison. The ranges of characteristics of upgraded and bleached waxes obtained in this invention are matching with the FDA specifications.
Table 3: Physical and chemical characteristics of crude, upgraded and bleached rice bran wax(Table Remove)The Inventors have found that from a hot solution of the de-fatted wax in isopropanol, the resinous matter can be separated by the addition of a few volume percentage of water. The resinous matter would settle as a dark layer at the bottom, which can be easily separated. Thus, the undesirable material can be removed without any chemical treatment. A further advantage is that the resinous matter takes with it a good portion of the components that impart the dark color to the wax, so that removal of the resinous matter greatly improves the color of the wax.
Bleaching steps are generally ineffective when the resinous matter is present and this.. explains why drastic reagents (chromium trioxide, sulphuric acid, nitric acid etc.,) and conditions described in prior art were necessary to achieve some color reduction.
A large number of samples with varying oil content, obtained from commercial refining plants were processed by the present process. In initial trials, the Inventors used hexane as the de-fatting solvent. Although hexane is effective for oil removal, filtration rate for the resulting wax suspension was exceedingly slow. In later experiments the inventors have carried out de-fatting and removal of resinous matter using isopropanol (IPA) in presence of various volume percents of water. The
Inventors have further discovered that both de-fatting and removal of resinous matter can be carried out in a single step provided the oil content of the crude wax low (less than 40%). In other cases, de-fatting and resinous matter removal was carried out in separate steps. After removal of the resinous matter, the product was ready for bleaching. It should be further noted that the earlier attempts at chemical bleaching were restricted to oxidative bleaching only. The inventors have found that reductive bleaching by using sodium borohydride was very effective. High cost of the reagent could be a negative factor. Hence the use of cheaper reagents was sought. Both sodium chlorite and hydrogen peroxide were found to be satisfactory. Sodium chlorite bleaching was carried out in isopropanol medium while hydrogen peroxide bleaching was carried out on the molten wax without any solvent medium.
The resinous matter starts separating out from IPA soluble wax solution as a solid gummy material when IPA contains water. Then the resinous matter can be separated out from the wax solution very easily in hot condition. Removal of this resinous^ matter from crude rice bran wax enhances the bleaching efficiency and improves the quality of bleached wax.
Eventhough sodium chlorite was reported for the bleaching of rice bran wax it was used in combination with a number of other bleaching agents [Ishii Masakatsu, JP: 76,30,204 (1976)]. In the present study sodium chlorite alone could exhibit efficient bleaching capability when the bleaching was carried out in IPA medium in presence of various amounts of water.
The following examples are given by way of illustration and therefore should not be construed to limit the scope of the present invention.
Example 1:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (1.5 liters) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hrs. and allowed to settle for 3 minutes at 75°C. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) ur ' - -eflux conditions. The pooled IPA soluble portion which contains upgraded oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax
with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (302.5 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (184.5 g). The yield of the resinous matter obtained was 12.4 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 2:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2 liters) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 3 minutes at 75°C. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner runnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (302.5 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (185.3 g). The yield of the resinous matter obtained was 12.2 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 3:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 3 minutes at 75°C. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 33°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax wnh about 500 ml of IPA. The residual IPA present in wet upgraded wax .was removed by vacuum distillation to obtain dried upgraded wax (299.5 g). The IP A
soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (185 g). The yield of the resinous matter obtained was 15.5 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 4:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (3.0 liters) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hrs. and allowed to settle for 3 minutes at 75°C. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux, conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (303 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (183 g). The yield of the resinous matter obtained was 14 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 5:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (25 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hrs. and allowed to settle for 4 minutes at 76°C. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 35°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (301 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil

along with soft wax (174.5 g). The yield of the resinous matter obtained was 24.5 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 6:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 4 minutes at 76°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (291.3 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (174.5 g). The yield of the resinous matter obtained was 34 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax was found to be 18+ and 78 - 79°C respectively.
Example 7:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (75 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 4 minutes at 76°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (270.8 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (173.5 g). The yield of the resinous matter obtained was 55.6 g. The amount of resinous matter is comparatively high as

considerable amount of wax came out along with resinous matter. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 8:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for one hour and allowed to settle for 3 minutes at 77°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion, which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (297.5 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (170 g). The yield of the resinous matter obtained was 32.5 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax was found to be 18+ and 78 - 79°C respectively.
Example 9:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 3 hrs. and allowed to settle for 3 minutes at 77°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion, which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA
present in wet upgraded wax was removed by vacuum distillation to obtain dried
upgraded wax (295 g). The IPA soluble potion was concentrated using a rotary evaporator to recover the oil along with so (172 g). The yield of the resinous

matter obtained was 33 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax were found to be 18+ and 78 - 79°C respectively.
Example 10:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 3 minutes at 76°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2x100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (336.9 g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (132.1 g). The yield of the resinous matter obtained was 30.1 g. The color (Gardner scale in 1.0 cm cell) and melting point of the upgraded wax was found to be 18+ and 78 - 79°C respectively.
Example 11:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 3 minutes at 76°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The residual IPA present in wet upgraded wax was removed by vacuum distillation to obtain dried upgraded wax (122.5g). The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (367.4g). The yield of the resinous matter obtained was 9.1g. The color (Gardner scale in 1,0cm cell) and melting point of the upgraded wax was found to be 18+ and 78-79°C respectively.

Example 12:
The IP A solubles (lOOg) obtained during the upgradation of crude rice bran wax was taken in a 1 liter round bottomed flask and dispersed in acetone (500ml). The contents were refluxed for a period of one hour and cooled to about 15°C. The crystallized wax was centrifuged and decanted the clear acetone soluble fraction. The wax was washed with chilled acetone (2x 50 ml) and dried to obtain soft wax (4.9 g). The acetone soluble fraction was concentrated using rotaevaporator to recover the oil (95 g).
Example 13:
The IP A solubles (100 g) obtained during the upgradation of crude rice bran wax was taken in a 1 liter round bottomed flask and dispersed in methyl ethyl ketone (500 ml). The contents were refluxed for a period of one hour and cooled to about 15°C. The crystallized wax was centrifuged and decanted the clear methyl ethyl ketone soluble fraction. The wax was washed with chilled methyl ethyl ketone (2 x 50 ml) and dried to obtain soft wax (5.1 g). The methyl ethyl ketone soluble fraction was concentrated using rotaevaporator to recover the oil (94.7 g).
Example 14:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (17.5 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (2.5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.2 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (13.2 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 3.9 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 12.9 and 79 - 80°C respectively.

Example 15:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (17.5 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 4 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite started settling down in the flask. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.6 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (13.4 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 5.8 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 11.9 and 79 - 80°C respectively.
Example 16:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (17.5 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (7.5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 5 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during • this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 33°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (234.8 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (13.7 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium

chlorite was 8.9 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 11.9 and 79 - 80°C respectively.
Example 17:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (35 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (2.5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (234.3g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (13.6g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 4.4 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 12.8 and 79 - 80°C respectively.
Example 18:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (35 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 35°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with EPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.2 g). The filtrate was concentrated using a rotary

evaporator to recover the residual oil (13.5 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 6.1 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 11.8 and 79 - 80°C respectively.
Example 19:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (35 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (7.5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite started settling down in the flask. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (234.9 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (14.1 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 8.1 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 11.8 and 79 - 80°C respectively.
Example 20:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (3.5 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite started settling down in the flask. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized b , d wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet

bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.Ig). The filtrate was concentrated using a rotary evaporator to recover the residual oil (12.9g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 6.9 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 13 and 79 - 80°C respectively.
Example 21:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.25 lit.) and water (25 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (240.2g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (8.3g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 6.3 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 12.8 and 79 - 80°C respectively.
Example 22:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.5 lit.) and water (30 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was

treated with fresh IPA (2x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (236.7g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (6.4 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 6.4 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 12.4 and 79 - 80°C respectively.
Example 23:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (35 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5 grams) was added and the reflux was continued for another one hour. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.3g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (13.4g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 6.2 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 12.3 and 79-80°C respectively.
Example 24:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and water (35 ml) and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (5g) was added and the reflux was continued for another 3 hours. After completion of the reaction time the contents were allowed to settle for 3 minutes at hot temperature. Residual resinous matter and

undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.5 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (13.2 g), with small amounts of soft wax and sodium chlorite. The yield of the resinous matter along with the unreacted sodium chlorite was 6.1 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 11.8 and 79 - 80°C respectively.
Example 25:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 3 minutes at 75°C temperature. Resinous matter started settling down in the flask during this period. The clear hot IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The yield of the resinous matter obtained was 33.5 g. The pooled IPA soluble portion, which contains upgraded wax and oil was taken back to 5 lit round bottomed flask and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (6 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time allowed to settle for 3 minutes at 75°C. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (290.4 g). The filtrate was concentrated using a rotary evaporator to recover the oil (174.5 g), with small amounts of soft wax and sodium chlorite. The weight of the resinous matter along with the unreacted sodium chlorite was 7.3 g. The color (Gardner scale in 1.0 cm

cell) and melting point of the bleached wax were found to be 12.8 and 79 - 80°C respectively.
Example 26:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hrs. and allowed to settle for 3 minutes at 75°C temperature. Resinous matter started settling down in the flask during this period. The clear hot IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The yield of the resinous matter obtained was 33.9 g. The pooled IPA soluble portion, which contains upgraded wax and oil was taken back to 5 lit round bottomed flask and heated on an isomantle to make uniform solution. When the reflux started, sodium chlorite (9 grams) was added and the reflux was continued for another 2 hrs. After completion of the reaction time allowed to settle for 3 minutes at 75°C. Residual resinous matter and undissolved sodium chlorite were started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (289.5 g). The filtrate was concentrated using a rotary evaporator to recover the oil (174.7 g), with small amounts of soft wax and sodium chlorite. The weight of the resinous matter along with the unreacted sodium chlorite was 7.3 g. The color (Gardner scale in 1.0 cm
cell) and melting point of the bleached wax were found to be 11.8 and 79 - 80°C
/ respectively.
Example 27:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and heated on an isomantle to make uniform solution. When the reflux started, sodium borohydride (1.25 g , a 2.5 ml water) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the

contents were allowed to settle for 4 minutes at hot temperature. Residual resinous • matter was started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The" residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.8 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (9.1 g), with small amount of soft wax. The yield of the resinous matter was 6 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 13 and 79 - 80°C respectively.
Example 28:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and heated on an isomantle to make uniform solution. When the reflux started, sodium borohydride (2.5 grams in 5 ml water) was added and the reflux was continued for another 2 hrs. After completion of the reaction time the contents were allowed to settle for 4 minutes at hot temperature. Residual resinous matter was started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (235.1 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (9.5 g), with small amount of soft wax. The yield of the resinous matter was 6.7 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 13 and 79 - 80°C respectively.
Example 29:
Upgraded wax (250 grams) was taken in a 3 liter round bottomed flask along with IPA (1.75 lit.) and heated on an isomantle to make uniform solution. When the reflux siirted, sodium borohydride (5 grams in 10 ml water) was added and the ref! •, was continued for another 2 hrs. After completion of the reaction time the contents were

allowed to settle for 4 minutes at hot temperature. Residual resinous matter was started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the resinous matter was treated with fresh IPA (2 x 50 ml) under hot conditions. The pooled IPA soluble portion was cooled to around 30°C. The crystallized bleached wax was filtered using Buchner funnel and washed the wax with IPA (2 x 125 ml). The residual IPA present in wet bleached wax was removed by vacuum distillation to obtain dried bleached wax (234.3 g). The filtrate was concentrated using a rotary evaporator to recover the residual oil (12.4 g), with small amount of soft wax. The yield of the resinous matter was 7.7 g. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 13 and 79 - 80°C respectively.
Example 30:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform solution. The contents were further refluxed for 0.5 hours and allowed to settle for 4 minutes at 76°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (174.8 g). The yield of the resinous matter obtained was 34.1 g. The residual IPA present in wet upgraded wax was removed by vacuum distillation. When the molten wax was free of solvent and moisture, 25 ml of hydrogen peroxide (30% solution) was added and stirred the contents for 2 hours. The moisture and hydrogen peroxide were distilled out under vacuum and obtained 291.1 g of bleached wax. The color (Gardner scale in 1.0 cm cell) and melting point of the bleached wax were found to be 14.3 and 79 - 80°C respectively.
Example 31:
Crude rice bran wax (500 grams) was taken in a 5 lit round bottomed flask along with IPA (2.5 liters) and water (50 ml) and heated on an isomantle to make uniform

solution. The contents were further refluxed for 0.5 hours and allowed to settle for 5 minutes at 76°C temperature. Resinous matter started settling down in the flask during this period. The clear IPA soluble portion was decanted into a beaker and the settled resinous matter in the flask was treated with fresh IPA (2 x 100 ml) under reflux conditions. The pooled IPA soluble portion which contains upgraded wax and oil was cooled to around 30°C. The crystallized upgraded wax was filtered using Buchner funnel and washed the wax with about 500 ml of IPA. The IPA soluble portion was concentrated using a rotary evaporator to recover the oil along with soft wax (174 g). The yield of the resinous matter obtained was 34.3 g. The residual IPA present in wet upgraded wax was removed by vacuum distillation. When the molten wax was free of solvent and moisture, 50 ml of hydrogen peroxide (30% solution) was added and stirred the contents fro 2 hours. The moisture and hydrogen peroxide were distilled out under vacuum and obtained 291. 7g of bleached wax. The color (Gardner scale in 1.0 ^m cell) and melting point of the bleached wax were found to be 13.7 and 79 -~ 80°C respectively.
The main advantages of the present invention are:
a) The present invention is a simple process for the upgradation and bleaching of
crude rice bran wax obtained during dewaxing stage of refining process of rice
bran oil.
b) In the present invention the resinous matter present in the crude rice bran wax
is separated easily by incorporating water into IPA.
c) The present invention describes an easy process for the separation of resinous
matter and oil in a single step.
d) The removal of resinous matter and oil, and also bleaching is carried out
continuously in the same vessel if the oil content in the crude wax is upto
40%.
e) In the present invention bleaching operation is carried out in aqueous
isopropanol medium to prepare good quality wax with minimum ash content.
fj The rice bran oil recovered in the upgradation step can be added to the crude oil for refining process thereby reducing oil loss to the vegetable oil industry.
g) The present invention provides a very simple and efficient filtration in both upgradation and bleaching steps.

h) Upgraded and bleached wax obtained in the present invention is a uniform
melting wax at about 78-80°C i) The aqueous IPA can be re-used in the process by adjusting the required water
content in the solvent.





We Claims:
1. A process for upgrading crude rice bran wax, said process comprising:
a) treating crude rice bran wax with isopropyl alcohol (IPA) containing 1 to
15 % by volume water to form an IPA-wax suspension;
b) allowing the IPA wax suspension to stand to allow precipitation of
resinous matter;
c) separating the resinous matter thus formed from the IPA-wax suspension
to obtain clear IPA -wax solution containing upgraded wax, oil and soft
wax by ketonic solvents;
d) separating the upgraded wax from clear solution of step (c).

2. A process as claimed in claim 1, wherein the crude rice bran wax is a byproduct
obtained during dewaxing stage of refining process of rice bran oil.
3. A process as claimed in claim 1, wherein the crude rice bran wax contains
25- 70% of oil.
4. A process as claimed in claim 1, wherein step (a), the ratio (weight: volume)
of crude rice bran wax to aqueous IPA is 1:3 to 1:6.
5. A process as claimed in claim 1, wherein step (a), the IPA contains 5-15% by
volume of water.
6. A process as claimed in claim 1, wherein step (a), the reaction between the IPA
and the crude bran wax is carried at 70-77° C.
7. A process as claimed in claim 1, wherein step (a), the IPA-wax suspension is
further refluxed for 0.25 to 1 hour.
8. A process as claimed in claim 7, wherein the IPA-wax suspension is refluxed
for 0.50 hours.
9. A process as claimed in claim 1, wherein step (b), the IPA-wax suspension is
allowed to stand for 1-5 minutes to allow precipitation of resinous matter.
10. A process as claimed in claim 9,wherein the hot IPA-wax suspension having
temperature of 75-77° C is allowed to stand for 3-5 minutes to allow
precipitation of resinous matter.
1 1. A process as claimed in claim 9 and 10 , wherein the resinous matter precipitates out in the form of dark brown liquid.

12. A process as claimed in claim 1, wherein in step (c), the resinous matter is
removed from the clear IPA-wax solution by filtering.
13. 'A process as claimed in claim 1, wherein in. step (d), the upgraded wax is
crystallized and separated from the clear solution containing upgraded wax.
rice bran oil and soft,wax
14. A process as claimed in claim 13, wherein the upgraded wax is crystallized by
cooling the clear solution to 30-35° C.
15. A process as claimed in claim 13, wherein the upgraded wax is separated by
filtration.
16. A process as claimed in claim 13, wherein the clear solution obtained alter
filtering crystallized wax contains rice bran oil and soft wax.
17. A process as claimed in claim 1, wherein bleaching of the upgraded wax is
.done with the IPA-wax suspension after removing the resinous matter.
18. A process as claimed in claim 18, wherein bleaching of the upgraded wax is
done with the IPA-wax suspension if the crude rice bran wax contains up to
40% oil.
19. A process as claimed in claim 17, wherein the upgraded wax is bleached by
adding sodium chloride or sodium borohydride to the IPA-wax suspension
20. A process as claimed in claim 19, wherein the bleached upgraded wax is
separated from the clear solution the contents to 30-35° C and filtering the wax
21. A process as claimed in claim 19, wherein the solvent in wet upgraded or
bleached cake is removed by distillation.
22. A process as claimed in claim 21, wherein any residual solvent is removed by
vacuum distillation.
23. A process as claimed in claim 1. wherein the bleaching of the upgraded wax is
done after separating it from the clear solution containing upgraded wax, oil
and soft wax.

24. A process as claimed in claim 23, wherein the upgraded wax is bleached by
adding 30% hydrogen peroxide to molten upgraded wax.
25. A process as claimed in claim 1, wherein the ketone solvents is selected from
the group acetone and methyl ethyl ketone.

26. A process for the upgradation and bleaching of crude rice bran wax
substantially as herein described with reference to examples accompanying this specification.

Documents:

155-DEL-2003-Abstract-(19-11-2008).pdf

155-del-2003-abstract.pdf

155-DEL-2003-Claims-(19-11-2008).pdf

155-DEL-2003-Claims-(26-11-2008).pdf

155-del-2003-claims.pdf

155-DEL-2003-Correspondence-Others-(09-01-2009).pdf

155-DEL-2003-Correspondence-Others-(19-11-2008).pdf

155-del-2003-correspondence-others.pdf

155-del-2003-correspondence-po.pdf

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

155-DEL-2003-Descripton (Complete)-(19-11-2008).pdf

155-DEL-2003-Form-1-(09-01-2009).pdf

155-del-2003-form-1.pdf

155-del-2003-form-18.pdf

155-del-2003-form-2.pdf

155-DEL-2003-Form-3-(19-11-2008).pdf

155-del-2003-form-3.pdf

155-DEL-2003-Petition-137-(19-11-2008).pdf


Patent Number 228674
Indian Patent Application Number 155/DEL/2003
PG Journal Number 08/2009
Publication Date 20-Feb-2009
Grant Date 06-Feb-2009
Date of Filing 19-Feb-2003
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110001, INDIA
Inventors:
# Inventor's Name Inventor's Address
1 SAMIR KUMAR ROY IICT, DELHI, INDIA.
2 THENGUMPILLIL NARAYANA BALAGOPALA KAIMAL IICT, DELHI, INDIA.
3 RACHAPUDI BADARI NARAYANA PRASAD IICT, DELHI, INDIA.
4 BETHALA LAKSHMI ANU PRABHAVATHI DEVI IICT, DELHI, INDIA.
5 BHAMIDIPATI VENKATA SURYA KOPPESWARA RAO IICT, DELHI, INDIA.
PCT International Classification Number C11B 3/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA