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1, 21
The mechanical separation=of the denser phase from
the lighter phase by virtue ofitheir diiferences'in- speci?c
2,759,956 gravities can suitably be. accomplished by decantation. or
RICE WAX EXTRACTION centrifugation. Centrifugation is preferred:
In one preferredembodiment of the inventionthe': rice
Joseph Pominski, Henry L. E. Vix, and Paul H. Eaves, bran is heat treated in the manner described above; the
New Orleans, La, assignors to theUnited' States of so treated bran is contacted with the oil solvent. at attem
America asrepresented by the-Secretary of Agriculture
perature of about from 35 to 60-9 F;, until a portion of
No Drawing. Application November 3,1953, the oil is selectively dissolved in the solvent;:the oil- rich
Serial N0. 390,100 miscella so formed is removed from contact with the rice
14 Glaims. (c1; 260M123) bran; the so treated rice bran is contacted with. fresh oil
solvent at a temperature of about from 70? to: 220 F.,
(Granted under Title 35, U. S. Code (1952), see. 266) until wax dissolves; and the wax containing miscella; is
treated in the manner described above.
A non-exclusive, irrevocable; royaltyefree license in the The proportion of-ther oil which is selectively extracted
invention herein described, for all governmental pur prior to the extractionof the wax can suitably range from
poses, throughout'the world, with the power togrant sub 0 to 100%. Since waxes consist of complex mixtures
licenses for such purposes, is hereby granted to the Gov containing many components: closely resembling oils, the
ernment of the United Statesof America. selective extraction-of all of they oil prior to the selective
This invention relates to the production of av hard 20 extraction of the wax removes an appreciable amountof
rice wax. A 7 components which would ordinarily be components: of
Rice bran contains in the order of 15 to 20% lipides. the wax. The selective extraction of at least the bulk
The rice bran lipides consist essentially of rice oil, wax, of the oil, and preferably from about 90 to 98% of the
free fatty acids and phosphatides. As heretofore prac oil; prior to the extraction of the wax,.is preferred.
ticed, the solvent extraction of rice branremove's from In another preferred embodiment, the wax containing
about 90 to 95% of the lipides. When the ,oil obtained miscella is washed: several: times with water at- a. tem
by such a solvent extraction is freed of oil solvent and perature of about from>7OPto 220 F. The denser water
allowed to stand, an oil insoluble tank settling precipi solutions of water soluble components areme'chanically
tates. Such tank settlings amount to about3 1 to 2% by separated from the lighter hydrocarbon solution and; the
' weight of the oil1 and consist1 essentially of oil, a rela 30 water solutions are sent to a phosphatide'i treatment
tively soft wax fraction; free fatty acids and phospha system.
tides. In another preferred embodiment, the rice wax phase;
The solid and liquid portions of such tank settlings which is mechanically isolated from the wax containing
cannot readilybe separated by ?ltration- Dilution with miscella after'the miscella has. been cooled until an oil
liquid hydrocarbons such as hexane, heptane and the solvent insoluble phase separates,.is washed several times
like provides little if any improvement in their ?ltra with a liquid hydrocarbon- at a temperature ofv about
tion characteristics However, by puri?cation and frac from 35v to 70 F. The lighter hydrocarbon solutions
tional crystallization from isopropyl alcohol, a hard rice of hydrocarbon soluble components are' mechanically
bran wax which is comparable'tocarnauba wax in' many separated from. the heavier wax phase and the hydro
of its properties, can-be~ isolated from rice branoil tank 40 carbon' solutions-are sent to-an: oil recovery system.
settlings. When. the rice b'ra'nito be: extracted contains less. than
An object of the presentiinvention is to providev a proc about. 14% moisture prior to- the heat treatment of the
ess of solvent extracting wax from rice branim amariner bran, the moisture content can suitably be adjusted to
in which av hard; essentially oilifree rice wax is- isolated about from 14 to 35% prior to or during the heating.
from the extractingsolvent; Another objectiisitoiprovide 45 The adjustment is preferably made during the initial
a process of solvent extracting'the lipides from rice bran, stages of the heating. The moisture content ot the? rice
in which process, an oil of goodv re?ning character is bran1 is preferably adjusted- to- about 20% while. the bran
selectively extracted? from the bran and then a hard wax is being heated. to about from 170 to- 210 F. and, ad~
is extracted from the bran; Another'object- isi to provide justed- during the: subsequent heating. to a moisture con
aproce'ss of producing av hard wax from rice branby a 50 tent of aboutrf-rom' 8 to 3.0% during, the final stages of
process which can be applied to the tanle settlings of. rice the heating, at which time the temperature is rising: to
oil which was solvent extracted from rice bran' which about fromZlO to 225 F.
may be cooked in the de?ned mannerprior to" the solvent The extraction can. suitably be conducted in a batch
extraction. wise or continuous manner. ontinuous operation- is
In general, one variation of thepresent invention com 55 preferred. A wide1 variety of solvent extraction proce
prises: heatingl rice bran in contact with about from 14 dures and apparatus can suitably be used in. conducting
to 35% of its weight of water at at temperature of- about the extraction of rice wax in accordance with. this in?
from 70 to 235v F. for about from? 15' to 70 minutes vention. The procedures and apparatus described irr the
and adjusting the moisture content of the bran, during co-pending application of G'astroclt, Vix,.DAquin, Graci,
the heating, to- producev a ?nal moisture content of at 60 and Spada-ro, Serial. No. 314,234, ?led. October 10, 1952,
least about from 5 to 7%, and preferably to' produce a now U. 8-. Patent 2,727,914,. issued. December 20,, 1955,
?nal moisture content of- about fromv 8'- to 30%; con can suitably be used. In. using them, the rice bran is
tacting the so heated rice brain with a normally liquid oil preferably heated. as de?ned above, then: crisped as
solvent having a boiling- point? of- about- from 100 to 220 de?ned in that patent application, and thus converted to
F, at a temperature of about from 70 to 220'0 F.,- until 65 relatively friable particles which are particularly adapted
wax dissolves; cooling: the hot. wax containing miscella to be solvent. extracted by slurrying. the. particles: with
so formed, until an immiscible; wax>rich phase, consist an oil/Wax solvent, supporting the rice bran- particles
ing essentially of rice wax,.tis obtained;v andlmechanically on a ?lter bed and Washing. them with substantially sep
separating. the denser phase, consisting. essentially of arate portions of an, oil solvent, in the- manner de?ned
rice wax, from the lighter phase, consisting essentially of 70 in that patent. application. The so treated; rice bran
the oil solvent, by virtue- of their differences in speci?c particles are preferably slurried at low temperature; sup
gravity. ported on the ?lter bed, then contacted ?rst with portions
2,759,956
3 4
of the oil solvent at the relatively low temperature range about 40 F. The immiscible wax-rich phase which
de?ned above and then ?nally with portions of the oil formed was centrifugally separated using a relative cen
solvent at the relatively high temperature range, de?ned trifugal force of about 800 times gravity.
above, with the recycling of portions of the oil solvent The cool miscella was not ?lterable at a temperature
being arranged to concentrate the oil in the portions of 38 F.
which contact the rice bran particles at low temperature The wax obtained by the centrifugation dried to a
and with the wax being removed by cooling and cen hard wax, melting at 785 C. This wax was comparable
trifuging the portions of the oil solvent which contact to the isopropanol puri?ed wax described in Journal of
the bran particles at the higher temperatures. The wax the American Oil Chemists Society, 30, 9-14. January
is preferably recovered by cooling the wax containing - 1953. The yield of wax was 0.254% based on the weight
miscella to a temperature at which a liquid or solid of rice bran or 1.5% based on weight of oil.
phase of the wax becomes immiscible with the solvent The oil obtained by the above extraction at 37 to 39
and mechanically separating the wax in the manner de F. was recovered by subjecting the miscella to ?ltration,
?ned above. _ concentration, and stripping in the usual manner. The
In the case of wax-rich miscellas containing from about 15 re?ning character of this oil was compared to that ob
2 to 10% of oil, a solid phase of the wax becomes im tained by subjecting similarly treated rice bran to a
miscible at about 35 to 60 F., temperature and cen similar extraction and oil recovery in which the tem
trifugation separates a hard rice wax which is suitable perature during the extraction was about 85 F. and
for many applications without further puri?cation. wax was not isolated from the miscella so obtained.
Normally liquid oil solvents boiling at about from The following table illustrates the important character
100 to 220 F. which can suitably be used in the present istics of the two oils. The re?ning losses of the oil ex
process include the commercial hexanes and heptanes, tracted in accordance with the process of the present in
the trimethyl pentanes, the chlorinated hydrocarbon sol vention were about 25% less than those of the oil ob
vents and the like. The commercial hexanes are pre tained by the conventional hot extraction.
ferred. 25
In cooling the wax-containing miscellas, i. e., rice Re?ning data on cold extracted rice oil
wax dissolved in the above liquids at about from 70 to
220 F., to a temperature at which an immiscible wax Lovibond Color
Re?n- Excess
rich phase separates the miscellas are preferably cooled Oil FFA, Lye. iDE'. Lye.
at the rate of from about 2 to 4 degrees per minute. 30 percent B Loss, per- Re?ned Bleached
percent cent Oil,1 Oil,2
Where a wax-containing rice oil is produced by the Red 70 Y Red 35 Y
solvent extraction of a rice bran cooked in the manner
de?ned above prior to the extraction, the wax contained Extracted at 14 15.3 0. 5
in the oil can suitably be recovered in accordance with 38 F _______ _, 3. 24 16 14. 8 0.5