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Sommaire du brevet 1137352 

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Disponibilité de l'Abrégé et des Revendications

L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 1137352
(21) Numéro de la demande: 1137352
(54) Titre français: METHODE DE TRAITEMENT DE GRAINES ENTIERES POUR L'ABSORPTION DE SOLIDES
(54) Titre anglais: METHOD OF TREATING WHOLE SEEDS TO INCORPORATE SOLID MATERIALS
Statut: Durée expirée - après l'octroi
Données bibliographiques
(51) Classification internationale des brevets (CIB):
(72) Inventeurs :
  • BARHAM, HAROLD N., JR. (Etats-Unis d'Amérique)
  • BARHAM, HAROLD N., SR. (DECEASED) (Etats-Unis d'Amérique)
(73) Titulaires :
(71) Demandeurs :
(74) Agent: BERESKIN & PARR LLP/S.E.N.C.R.L.,S.R.L.
(74) Co-agent:
(45) Délivré: 1982-12-14
(22) Date de dépôt: 1979-05-18
Licence disponible: S.O.
Cédé au domaine public: S.O.
(25) Langue des documents déposés: Anglais

Traité de coopération en matière de brevets (PCT): Non

(30) Données de priorité de la demande:
Numéro de la demande Pays / territoire Date
907,834 (Etats-Unis d'Amérique) 1978-05-19

Abrégés

Abrégé anglais


ABSTRACT OF THE DISCLOSURE
A method for sorption of solids by the tissues
of whole seeds to enhance the available nutritional value
of the whole seeds, to provide nutritional requirements
for a ruminant feed, to provide new superimposed processes,
to make more effective precent superimposed processes, to
provide innoculation with viable organisms, to provide means
to reduce explosion hazzards from grain dust, and other
advantages accruing from encapsulation of solids, the method
comprising contacting the whole seeds with a synergetic
mixture of solid materials and an oleaginuous vehicle and
maintaining contact until the synergetic mixture has been
sorbed by the grain.

Revendications

Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.


The embodiments of the invention in which an exclusive
property or privilege is claimed are defined as follows:
1. A method for treating grains or seeds comprising
contacting the whole grains or whole seeds with a mixture
of a fine solid material and an oleaginous vehicle until
the mixture has been sorbed by the seeds, the components
of the mixture being synergistic with respect to their
sorption by the grains or seeds.
2. The method of claim 1, wherein the particles of
the fine solid material pass through a U.S.60 mesh screen.
3. The method of claim 1, wherein the oleaginous vehicle
is selected from oils, fats or greases of animal, vegetable
and mineral origin.
4. The method of claim 3, wherein the oleaginous vehicle
is mineral oil, soya oil, corn oil, peanut oil, cotton seed
oil, coconut oil,oleomargarine, white petroleum jelly,
animal fat, or olive oil.
5. The method of claim 1, wherein the grains or seeds
are cereal grain or legume seeds.
6. The method of claim 5, wherein the grains or seeds
are barley, corn, grain sorgham, millet, oats, rice, rye,
31

triticale, wheat, pinto beans, northern beans, soybeans
and peanuts.
7. The method of claim 1, wherein the fine solid
material is a non-protein nitrogenous material and the
total equivalent protein of the treated seeds is increased
to about 50 per cent; or a chemical reactive with the
tissues in the seed to increase tissue availability and/or
endosperm uniformity for subsequent use; or a chemical
reactive with the endosperm tissues whereby the treated
endosperm tissues become more available, hydratable and
more easily digested; or dust associated with the seeds
and the hazards arising during handling or storage of
the seeds is reduced.
8. The method of claim 6, wherein the fine solid material
is selected from sodium, tetraborate, calcium oxide or its
hydrate, chloral hydrate, sodium hydroxide, sodium formate,
calcium formate, sodium sulfite, sodium chloride, sulfur,
sucrose, glucose, bentonite clay, ammonium sulfate, urea,
borax, diethyl stilbestrol, potassium, gibberellate,
yeast, ammonium biphosphate, sodium sulfate, lysine,
manganese sulfate, zinc oxide, ferrous sulfate, ferric
carbonate, copper sulfate, ethylene diamine dihydroiodide,
cobalt carbonate, niacin, pantothenic acid or vitamins
A, D, C, B1, B2, B6, B12, or E.
32

9. The method of claim 1, wherein the ratio of the fine
solid material to the oleaginous vehicle in the synergistic
mixture varies from about 1:1 to about 10:1 by weight.
10. The method of claim 9, wherein the said ratio varies
from about 1:1 to about 6:1 when the fine solid material
is a non-protein nitrogenous material or a reactive
chemical and from about 3:1 to about 9:1 when the fine
solid material is dust.
11. The method of claim 1, wherein the fine solid material
is urea and the treated grains or seeds are converted into
a concentrated nitrogen source with a total equivalent
protein content of at least 70 per cent, moisture free basis.
12. The method of claim 1, further comprising subsequent
processing which comprises subjecting the treated grains
or seeds to infrared heat to increase endosperm uniformity
and availability, when the file solid material is calcium
oxide or its hydrate, or subjecting the treated grains
or seeds to superatmospheric steam pressure to produce a
product with increased water solubility and adhesive
properties.
13. The method of claim 1, wherein substantially all of
the synergistic mixture is sorbed into the the whole seed
structure within up to a time period of about five minutes.
33

14. Grains or seeds when treated by a process according
to claim 1 .
34

Description

Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.


~13~3S2
This invention relates to a method of treating
whole seeds to incorporate solid materials into them.
The method can be used to alter their nutritive
content, or to encapsulate chemicals within the berry
tissues preparatory to subsequent and superimposed
processes, or both. In particular the method can be
used to incorporate solids into whole seeds to enhance
their nutritive values for food and feed purposes, and/or
to enhance personnel and property safety in grain
handling.
According to the present invention there is
provided a method for treating grains or seeds comprising
contacting the whole grains or whole seeds with a
mixture of a fine solid material and an oleaginous
vehicle until the mixture has been sorbed by the seeds,
the components of the mixture being synergistic with
respect to their sorption by the grains or seeds.
As used herein, the term "seeds" refers to all cereal
and legume seeds and includes barley, corn, grain sorghum,
millet, oats, rice, rye, triticale, wheat and soybeans,
peanuts, various edible beans, and others in these
categories. The term "whole seed" means seeds which are
essentially whole, whether previously processed or raw.
It also includes seeds of a single type or mixed types,
varieties, hybrids, and the like. The process is
particularly applicable to whole seeds due to the unusual
and obvious utility. A11 of the examples were carried out
with whole seeds, including the usual amount of chaff,
broken kernels and other debris, in order to illustrate
the efficacy of incorporation of chemicals without the
necessity of comminution.
The term "sorption" includes adsorption and absorption,
or both, and is used interchangeably with "incorporation" or
"encapsulation", including variations thereof. The term

1~3735~
"solids" includes mixtures of solids.
It has been found that solids, in the presence of
oleaginous liquids or semi-solids, result in the very
rapid sorption of both phases. Normally oils, fats and
greases of animal, vegetable and mineral origin are sorbed
by the grain sparingly,by the seeds,if at all. With the
exception of extremely reactive solid chemicals, which
react with seed tissues in the presence of even the low
normal water content, solids are not accepted by the whole
seed in measurable quantities and usually not at all. In
aqueous solutions containing chemicals which are soluble,
reaction, or "loading", at sorption sites occurs, which
prevents further adsorption. Thus, the unexpectedness of
the oil-solids relationship is very apparent.
Methods according to the invention will now be
particularly described by way of example only.
All oils, fats and greases of all sources are appli-
cable to the process. Such oleaginous compounds are herein-
after referred to as a "vehicle" or "carrier" and may consist
of combinations of various oils, fats or greases from all
sources. Although there are no limitations, the oils, fats
and greases with relatively higher melting ranges, or
higher aggregate molecular weight or other pertinent
configurations, are usually more efficient vehicles, but
such differences are small. Choice of vehicles for
commercial application will center around the relative costs
and intended usage. For instance, the use of animal fat,
including products of widely varying physical and chemical
characteristics, has been a frequent choice because of
nutritional value and price, a factor of considerable
importance for uses of very high tonnage and rigid economic
perimeters. The oleaginous material may ~e a non-edible
type such as an inexpensive petroleum type oil for use in
-- 2 --

~13735Z
a synergetic mixture with a solid chemical such as borax,
useful to produce an oil well drilling adjunct by means
of a steaming process superimposed on the treated grain.
It is believed that the mesomorphic state, or "liquid
crystal" concept, may be at least a partial explanation for
the synergetic phenomenon. Neither the solids nor the
vehicle has the capability of responding to the unbalanced
forces within the seeds, but together the solids and
vehicle move rapidly into the seeds. Thus, the behavior
of the mixture is distinctly different from the separate
components It is believed that the metastable state of
the seed, resulting from an imbalance of vector forces
caused by the polar and nonpolar areas of the structure,
and attendant attempt to reach maximum stability, are
responsible. Pertinent to the phenomenon is the fact that
in every case the sorption of the two-phase system of oil
and solids was significantly more rapid and extensive than
simple adsorption of water. Furthermore, the size and
shape of the solid crystals preclude an explanation based
on particle size because of the size of very large
polymers and the relatively large crystals of solids with
low molecular weights which are easily sorbed. By no
means is solubility a factor because the majority of the
solids are not soluble in fats and oils and some are barely
soluble in any frequently used solvent Chemical reaction
is not a factor and does not occur. In the "liquid
crystal" concept, crystals may change size and shape but
continue to exhibit some of the properties of solid crystals
such as birefringence to polarized light.
The ratios of weight of solids to vehicle vary and are
influenced by several factors, although such variance is
usually low. As stated, particle size must be such that the
synergetic effect is attained. Generally, the particle size

' ~1373S2
of the solids used has been that which would pass through
a U. S. Wire No. 60, or would pass through an aperture of
250 microns. However, particles of some solids used have
been larger than 250 microns in at least one dimension.
Individual solids affect the synergetic relationship of
vehicle to solids, as well as the particular mixture of
solids. The relationship of solids to vehicle is usually
from 1:1 to 6:1, with 4.5:1 a common ratio. It is readily
apparent that the relatively low amount of vehicle required
in the relationship obviates solubility as a criterion.
Almost unlimited flexibility of operation is incor-
porated into the process. In commercial application the
proper ratio of solid(s) to vehicle to be incorporated will
be known and will be dependent on the factors listed above.
However, if the amount of carrier is deficient most of the
solids will be carried into the whole seeds rapidly but with
some of the solids remaining on the seed pericarp. The
remaining vehicle requirement may be added later when
convenient with results substantially the same as if it had
been added together. Likewise, more solids may be added if
a surplus of vehicle has been used in the first addition.
More probably, various batches of processed whole seeds
would be mixed together in a manner which would ensure the
proper amounts of the vehicle and solids incorporated.
When the synergetic two-phase system is properly balanced
quantitatively, neither the solids nor the vehicle are
present on the seed peripheries when sorption is complete,
and as much as about 35 per cent of such a mixture has been
sorbed, based on the dry weight of the whole seed. Even the
grain dust, always accompanying country-run grain, is
incorporated, leaving only large debris such as sticks,
straws, stones, known as "foreign matter" (f.m.), and other
particles too large to be adsorbed. Moreover, the apparatus
-- 4 --

~13735Z
used for mixing the grain with the mixture components
becomes clean, lacking evidence of either of the added
physical phases.
Flexibility, simplicity, and the very high rate of
sorption of the synergetic mixture are factors inherent in
the process and which lend the process to treatment of
enormous quantities of seeds at extremely low cost. Accurate
liquid and solids metering devices, mixers, screw conveyors,
and the like, are readily available. Many grain storage
facilities have such equipment in operation or could
quickly and economically acquire such devices. The
aforegoing advantages are imperative in such high volume
business areas, including preparation of legumes and cereals
for feed and food purposes.
In the present procedure, seeds may be treated with a
variety of possible vehicles to suit the intended purposes
and virtually eliminate grain dust hazards at the same time.
Corn, for example, may be treated with corn oil to adsorb
corn dust. Likewise, soybeans could be treated with soya
oil. Oils are commonly extracted from these seeds and
purity of such oils produced from treated seeds could be
preserved if desired. Where seeds are to be used for
animal feeds, a choice migh~ well be one with the best
combination of nutrition and economy. Besides elimination
of dust emissions, seed handling operators may retain the
weights of dust otherwise lost or collected, as well as
retention of the very small weight of the vehicle added.
The process is effective on seeds of widely varying
moisture content and is therefore not restricted to any
particular moisture content or range Generally, seeds with
natural moisture content are used because of the
practicality, readily apparent. Occasionally, the moisture
content may be increased either before or after the sorption

11373SZ
of solids when unusually large amounts of solids are to be
sorbed, or to cause or facilitate subsequent reactions, or
both. Seeds containing saturation moisture have been shown
to be efficacious to the process, if there is no water on
the seed surfaces. Even so, the attraction by the seeds for
the synergetic mixture is so strong water may be rejected
from the grain to accommodate adsorption of the synergetic
mixture. However, adsorption of the synergetic mixture
into substantially dehydrated seeds has shown the phenomenon
to be largely independent on the incident moisture level.
An obvious expedient is usage of the prevailing physical
conditions whatever they may be.
The following specific examples are given by way of
illustration
In each of the examples listed, the seeds were weighed
into a glass Jar, followed by weighed additions of components
of the synergetic mixture, the jar hermetically sealed by a
screw-type metal lid, then shaken. By such procedure, the
sorption of the synergetic mixture could be observed
visually. Moreover, since the metal lid and glass jar could
not possibly adsorb the mixture, it was obvious that the
mixture was sorbed by the whole seeds. In addition to
visual observation and measured weights, three of the examples
were measured for total nitrogen. Such additional proof
was actually more of a check on analytical procedure than
on proof of sorption.
Treated whole seeds in many of the examples were
selected at random and cut in two, both laterally and longi-
tudinally. Kernel structures, thus exposed, could be
visually examined to ascertain uniformity of endosperm, as
compared to seeds from the same lot before treatment. The
endosperm of the principal feed grains are almost always
nonuniform, with a portion of the endosperm "corneous" or
"vitrious" and the remainder "floury", usually white. An
-- 6 --

~13735~
increase in uniformity toward homogeneity is known to
provide increased tissue availability for the ultimate use.
In no instance were any of the solids or vehicle so
introduced in visual evidence in the sectioned seeds.
The sorption of large quantities of salt or urea, for
example, tended to mask the taste of the solids so
introduced.
In the table listing the examples, all weights are
in grams and percentages based on the seed dry weight.
Numbers in parentheses indicate the order of applications.
Figures after the vehicle, water or solids used, indicate
the time lapsed after the next previous addition, with
letters such as "m", "h" and "d" indicating minutes, hours
and days. Small letters preceding listings refer to foot-
notes. The observed maximum time for disappearance is, by
no means, an accurate figure since visual observation is
approximate and difficult when seeds are in motion. Usually,
the times listed are greater than those actually occurring.
Protein contents were determined by analyzing the nitrogen
content by the standard ~jeldahl method, then the nitrogen
content was multiplied bya factor of 6.25 and reported as
protein or equivalent protein content, a standard
procedure in the animal feeding industry.

11373SZ
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1137352
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1~37352
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- 14 -

1~37352
The efficacy of various vehicles is shown in Examples
1 through 9, in which the primary variable was the vehicle.
Three of the vehicles, animal fat (example 2), oleomargarine
(Example 5) and white petroleum jelly (Example 7), may be
classified, roughly, as semisolids. The animal fat, obtained
from a large cattle feeding enterprise where it is added to
the ration, was not a uniform product. However, no difficulties
were encountered with incorporation into the grain. Two
carriers, white petroleum jelly, "Vaseline" (Example 7), and
mineral oil (extra heavy) (Example6) are of mineral source;
six of the vehicles are from a vegetable source, corn oil
(Example 1), olive oil (Example 4), peanut oil (Example 8),
coconut oil (Example 9), soya oil (Examples 57, 58, 59, 60,
66 and 67), cottonseed oil (Example 64), and oleomargarine
made from corn oil (Example 5); one is an essential oil,
anise oil (Example 3) from a vegetative source; and one is
from an animal source, animal fat (Example 2).
Two of the vehicles were unrefined, cottonseed oil
(Example 64) and soya oil (Example 66), and the mineral oil
in Example 58 had no preservative. Anise oil was adsorbed
both prior to and after addition of the salt (NaCl). Corn
oil was added after the salt had been mixed with the grain.
h'ith all vehicles, the sorption was rapid.
A variety of solids, representing widely variable
chemical types have been sorv~d, as shown by the examples.
NaOH, a very reactive alkali was readily sorbed (Examæle 10)
by the grain with normal moisture. Kernels sectioned later
revealed a significantly improved endosperm uniformity. About
l; minutes after encapsulation, the grain sample darkened,
indicating reaction throughout the berries between various
tissues and the alkali, and involving water associated
-- 15 --

13~352
with l~rain tissues
Elemental sul~ur (Example 11), sublimed flowers of
sulfur of pharmaceutical purity, was sorbed wi~h ease. One
per cenL o~ sucrose (~xample 12) was readily adsorbed, then
suhjec~e(l ~o infrared héating, causing an aroma resemblin~,
fresh bread clnd an cndosperm with much iml)roved uniformity.
Very similar re~ults were achieved when CaO and glucose were
sorbed, then heated by infrared ener~y (Example 59). Endo-
sperm uniIormity improvcments were even greater in Example
13 in which a reducing agent, sodium formate, was sorbed,
tllen tlle ~,rain subjected to a brief but intcnse infrared
exposure. Calcium oxide was sorbed by corn (Example 14)
usiny, corn oil as the vehicle. Subseguent infrared heating
improved t11e endosperm quality somewhat. CaO or Ca(Ol1)2 is
uséd in the process of cooking corn to make tortilla flour.
Lysine, an essential amino acid in which most féed grains are
deficient was sorbed by grain sorghum (Example 15) USitlg corn
oil WhiCil was mixed with the grain before addition of the
amino acid and added twice after addition of tllat solid. In
Example 16, NaCl was encapsulated in grain sorghum and then
~ e moisLure was increased to more than 20 per cent. The
subs~c~uent wa~er adsorption rate was very similar to that of
the same grain wi~hou~ the NaCl.
Very l~rge, complex, and dissimilar mo]ecular aggre-
gates were sor~)ed by grain sorghum, using corn oil as the
vehicle. Casein, milk protein (Example 17), was sorbed in
one minute or less. Pearl corn starch (Exam~le 18), whose
granules ~enerally vary in diameter from eig~t to 15 microns,
were very readily adsorbed. Bentoni~e (Example 19), an
aluminum silicate clay of tlle montmorillonite type, was
also rapidly sorbed by the grain. Bentonite is fre~luently
- 16 _

1~37;~52
used in animal ~ee~s because oE its inorganic content.
Examples 20 and 21 show the efficacy of adding various
solids, one at a time, with intervening ad~itions of the
vellicle. In I,xample 20, phcnol red was sori~ed by the grain
to illus~ratc the ex~ent of sorption. Eollowing sorption,
several kernels were sectioned to expose the largest amount
of endosperm. Tiny drops of dilute alkaline solution were
applicd to the center of the exposed elldosperm in a manner
which precluded contact with the outer regions. The instant
development of a pink color indicated sorption of the dye in
Lhe cellter of the kernel structure. Later, CaO was subse-
quently sorbed into the grain. In Example 21, (N1~4)2S03-H20,
an N~N cornpound wi~h strong reducing power, was sorbed into
the grclin, followed in about five hours by the sorption of
urea. Subsequent infrared heat treatment resulted in much
increased endosperm uniformity.
As noted with other chemicals in water solution,
borax (Na2B407 1~l~20), frequently used in connection with
starch utilization, is sorbed nonuniformly by wh~le cereal
2() graill. ln l,xample 22, borax, a powerful swelling agent for
s~arch in tl~e presence of water, was readily adsorbed by
whole grain sorgllum seeds and using corn oil as the vehicle.
I~atcr wa~s ~hen ad.sorbed by the grain to the 25 per cent level,
thcn heaLed at 65C for 12 hours. After drying to the
normal moi.sture con~ent, the seeds were sectione(~ showing
endosperms which were nearly uniform.
Die~thylstilbestrol (DES), a synthetic hormone
frequellLly use~ in animal therapy and in steer feeding rations,
was sorbed in grain sorghum (Example 23) U.Sillg corn oil as
the vellicle. 'rlle amount sorbed wa.s massive in contcxt witll
steer rat~enin~ but it is obvious that lesscr amoullts can be

113~7;~5Z
incorpora~ed. There is a curr~nt controversy between govern- -
mèntal regulation agencies and cattle feeders due to possible
toxic meat produced from DES fed animals. Ilowever, tlle
erficacy of any partieular fee~ additive, whe~her drug or
otherwise, is not an objective of this invention. Rather,
tlle eE~icacy lies in methods to encapsulate solids into
wllole see~s within the obvious confines of official regula-
tions, pruclence, and application efficacy, to produce highly
desira~le feeding and other materials for a v~riety of
l~urposes.
Chloral hydrate, a reactant used to produce a modi-
fied starch product experimentally, and reported as a methane
production inhibitor in ruminant feeding, was incorporated
very rapidly in grain sorgllum (Example 24), using corn oil
as a vehicle. Thus, a relationship of reactor and reactant
was fa.shioned which is suitable for subsequent treatment.
Yeast cells (saccharomyces cerevisiae), viable,
dried atld simp]e plant cells, were readily incorporated into
grain sorghum using corn oil as the carrier (I,xample 25)
Subseguent ad~itions of water, followed by incubation at
37 C for 12 hours, caused gas production in amounts consis-
tent with available sugar present in t he normal grain. An
obvious variation would be the simultaneous incorporation
of yeast foo~s or appropriate enzymes, or bo~h
Exarnple 26 illustrates the ease of incorporation of a
vitamin-mineral mixture into grain sorghum, though somewhat
excessive in amount. Tl~e encapsulation Or the same vitamin
mix, including a large number of other solids and using
anotller vehicle, are inclu~ed in otller exam~les.
In ~xample 27, a household meat tenderizer, includ-
ing seasonings and papain, a prot:eolytic enzymc from t he

37352
papaya plant, was encapsulated in grain sorghum using corn
oil as the vehicle. The treated grain was subsequently in-
creased in moisture content to 25 per cent, followed by heating
for 24 hours at 65~C., an optimum temperature for activity
of papain. Sectioned kernels revealed a much increased endo-
sperm uniformity. After drying and cooling other randomly
selected sectioned kernels also showed increased endosperm
uniformity. It can be seen that degredation of the protein
matrix increases starch availability to removing a significant
portion of the inhibiting characteristics of that matrix.
At the same time, the protein availability may be increased.
Nutritionists have calculated starch and protein availability
to be about 65 to 80percent, depending on the animal and
method of expression. When these percentages are multiplied
by the huge tonnage of grains used for animal feeding,
possible increases in animal utilization are of enormous
economic importance.
In Example 28 a commercial preparation, Gibrel, con-
taining 1.65 per cent of potassium gibberellate and the
remainder a filler of unknown origin was sorbed into the grain
sorghum sample using corn oil as a carrier. The plant metabo-
lite is known to stimulate the germination processes of seeds
under appropriate sprouting conditions.
Examples 29 through 38 and 57 illustrate the pr~cess
efficacy by encapsulation of inordinately large quantities
of chemicals into whole seeds, necessary for the production
of pro~ucts containing concentrated chemical sources for
feeding and a variety of other processes. Generally, the
grains containing relatively large amounts of solids and
carrier did not increase in volume in proportion to amounts
of additives, thus increasing the density. The increase
-- 19 --

1~37;~52
in den~si~y, unlil;e ~hat resultin~ from water adsorption,
is hi~hly indicative of sorption in heretofore unavailble
areas of the seed, and is tantamount to proof of sorption
in all seed tis~sues since it is impossil)le to sorl) such
quanLities in ~he pericarp and germ areas only.
Examples 2~, 30 and 31 illustrate mc~ ods for sorb-
ing into a cereal seed 15 per cent of calcined lime (CaO).
Typical of many calcium compounds, lime is on]y very spar-
in~].y solu~lc in water (less than 0.2 per cent). CaO was
ad~ed to the grain-vehicle mixture all at once in two exam-
ples, using ex~ra heavy mineral oil in Example 29, and corn
oil as the carri.er in ~xample 30. In Example 31, CaO and
corn oil were addcd to the grain alternately in l.3 or l.4
~,ranl ancl ~.3 and 0.4 gram increments, respectively.
Altl-ou~ll vehiclllar efficiency was increased somewhat the
ratio of .solid to carrier chan~e was minor.
Exalllples 32, 33 and 58 illustrate well the effi-
ciency of sorbil-g urea in large quantities, t-hus providing
a novel, si.mple ~nd economic method to provide a product with
a very hi~ ecluivalent protein value for ruminant feeding.
Condensal:ion of llrea with cereal grain polymer.s is an old
objective, but one which has not been achieve(l in a manner
which i~ econolnically attractive. Certainly, there are no
me~hods presently available to those in the art which provide
for encal)sulation of that chemical in the ~h~e seed in
whicll the gross integrity of the seed is nlaintained. Using
the prescnt process, such as ~hat of Example 32, wllercin
15 per cent of urea was adsorbed by the whole grain, the
resultant product had an analyzed total ~r~-c~l protein
e(luivaLellcy of 39.~8 per cent and a inal moi.s~lre content
of 11.l per cent. It may be expected that thc urca ~so
- 20 -

~3~35Z
introduced will condense to some degree with the berry tissues
at ordinary temperatures. However, the presence of heat,
such as that normally used to prepare rations for ruminant
animals in large feedlots, would increase still further the
extent of condensation. Such condensation, observed in the
steam flaking or "micronizing" process, the latter being a
process involving infrared heating immediately followed by
rolling, together with encapsulation itself, serve to inhibit
the rate of chemical release to more closely conform to the
rate of availability of the remaining nutrients.
In Example 33, the grain moisture was increased to
20.5 per cent, then corn oil added in 0.2 and 0.3 gram incre-
ments, and urea in 1.5 gram increments, added alternately
over a period of time. The analyzed equivalent protein was
58.96 per cent with 15.96 per cent moisture, based on total
solids. Equivalent protein on a dry basis was 70.15 per cent.
Equivalent protein in this example (33) was higher than oil-
seed protein concentrates and clearly shows the flexibility
of the method.
Examples 34 and 35 illustrate the rapid addition
of glucose (Example 34) and sucrose (Example 35), appropriate
for readily available energy for food or feed, or the availa-
bility to microorganisms such as yeast cells.
Similarly, NH4H2PO4, an excellent and commonly used
source of NPN and phosphorous, was incorporated into grain
sorghum using corn oil as the vehicle in Example 36. The
vehicle and solid, 3.75 and 15.0 per cent of the dry grain
weight, respectively, were incorporated in less than 60
seconds, with most of the two-phase system disappearing within
26 15 seconds after introduction of the solids. The total
equivalent protein content was determined to be 17.53
- 21 -

- ~137352
per cent and Lhe phosphosous content was calculated to be
3.02 per c~nt, both based on total solids and final moisture
eontent.
Sodium chloride (Example 37) was sorhed by grain
sor~hum in quantity, lS per cent by dry grain wei~ht,~ which
gro~ssly exceecls the amount wllich can be sorbed into the
seec~coat layers from aq~leous solutions of any concentration.
Su~se~uent water adsorption was fairly rapid and only
sliglltly inhi~ited by the presence of the large guantities
of tl~e syner~e~ic ~wo-phase system, ~urther support for the
eonviction of nonpolar area sorption.
Example 38 illustrates the ease in fasllioning a
trace mineral concen~rate in grain sor~hum USillg corn oil
as the vehicle. The lS per cent used represents about 300
times ~he trace mineral requirement by t~le ruminant animal
in a straigllt ratiotl.
In Exalllple 39, sufficient urea and eorn oil was
eneapsulaLed into whc)le corn kerllels to increase the total
equivaletlt T)rotein level to about 11 per cent, sufficient
fc)r the avera~e cattle feedin~ ration whicll usually varies
rrom al~o-lt 10.5 to 12 per cent, dependillg on the age o~ the
animal.
~ry northern beans, sometimes called "navy beans",
were usecl in Ixamples 40 and 41, whereby 0.4 ~rams of calcium
oxide W<IS encapsulated ~herein, using corn oil as the carrier.
'~he beans in Example ~0 were then cooked by conventional
boiling. The cooking time necessary was clecreased, as
compared to untreated beans, ancl yielded a product which
tencled to be firmer ancT resisted mushiness. Turther, the
prc>duct seemed to be easier to cligest. In Example 41, t}~e
treatment was the same except that a 30-seconcl infrare(l heat
- 22 _

``- ~ 1~3'735Z
treatment was superinl~osed on the chemi.cal treatrnent. The
resultatlt pro~uct exhibited further decrease in cooking
time, firmer beans, and were notably easier to digest.
Very ~imilar resul~s were observed when dried
pinto bcans (I.xample 42) were treated with CaO, corn oil
and subse~uent heat from an inErared source. The beans
re~-ained ~hilpe and the desiral)le firmness, cooked in signifi-
can~ly less ~ime and were observed to digest with less di~fi-
cul.ty as compare~ to untreated cooke~ pinto beans.
Example 43 shows the utility of incorporating all
of the required nutrients, not already furnished by the
~rain, into wllole grai.n sorghum to fashion what is consid-
ered to be a complete ration for steer fattening. Subse~uent
infrare~ heating significantly increase~ endosperm uniformity.
In Example 44, two per cent NaC1 was incorpolated
inLo the seed structure of raw peanuts, using corn oil as
the vehicle.
~,xamples ~5 througll 53 clearly il]ustrate the
e~icacy of encapsulati.on of a large variety of solids into
a variety of seeds whicll inc.lude barley, corn, grain sorghum,
oats, rice, rye, triticale, wheat and soyl~eans. In ttlese
examples animal Lat, because of its utility and economy,
was used as the vehicle, and the solid additive combination
was i~enti.cal in al]. examples. Also, the moisture was
adjusted to the ~ame level (14 per cent) in eacll example.
As noted, the sorption of the synergetic combination of
animal fat an~l solids varied from a few secon~s to about
30 seconds. Considering the low protein gr.lirls, corn and
grain sorghum, the re~uirements for an all-concentrate
cattle finishing raLion llave been attainé~, a1LI10Ugh the B
complex vitamins and vitamin E are no~ normally required b~
- 23 -

3735Z
ruminants since they have the ability to syntllesize those
entities. l`he products have been prepared for immediate
processing by the feedlot operator; only the amount of
roughage, if any, reguired by the operator may ~e added.
In addition, other advantages to the fecl animal are included,
~uch as ~low N~N release and uniformity of feed ingredients
which cannot stratify and separate.
Examples 54 and 55 have been included to show the
ac3vantage o~ sorption of chemicals appropriate for super-
impose(l steam processing. In Example 54, 1.~ grams of Na2SO3
(equivalent to 0.395 per cent of sulfur dioxide) was encap-
sulated in grain sorghum prior to sorption oE sulfur dioxide,
which was accompli.shed by way of processes in U. S. Patent
Nos. 3,725,081 and 3,911,147. It was an objective to place
a chemical reclucing compound in both polar and nonpolar
areas of sorption. Af~er steaming for four minutes at 150
psig, tlle grain was dried and ground. The product was 77.23
per cent cold water ~oluble, an improvement over a sample o~
identical grain and iderltica].ly treated except Lhat t~e
cot~trol experiment had no Na2SO3 and oil encapsulated.
In ~xample 55, one per cent of calcium formate and
0.28 per cent of mineral oil vehicle was sor~ed by the grain
sorghum, thell steamed for four minutes at 15(~ psig. The
resultant product was 71.28 per cent cold water soluble and
exhibitecl the highly adhesive characteristics recluired of a
feed pellet binder, wall board adhesive, charcoal briquette
adhe~sive, and ~he like.
IllusLraLin~ the advantage of incorporating a solid
in previously processed whole grain, gelatini~ed corn, 0.4
~rams of corn oil and two grams of urea were simultaneously
adsorbed ~y the cooked grain (Example 56). Such adsorption
- 24 -

1~.3735Z
sllows ~he in~erllal vector forces to be intact to cause the
<~dsorption of the syner~etic mixture even tllougll gelatini~ed.
Predictal)ly, samples identical with Examples 54 and 55,
wllicll had been chemically degraded to des~roy most of ~he
internal primary vect:or forces, would not a~sorb the syner-
gc L ic mixtures.
Examples 60 - 69 clearly reveal Lhe embodiments of
~he invention clirected toward the adsorption Or seed dust by
various seeds and using variou.s appropriate oleaginous
vehicles. 'rhe examples set forth were selected from a large
number of experimental examples which includ~d all of the
commodi~y seeds, dust and mixtures o~ dust rrom various seeds,
and oleaginous vehicles and mixtures of these vehicles. In
most cases, tlle dust (through a U. S. 60 mesh screen) had
been si.fted from the grain, then added back in ~roportions
shown to ensure known amounts of dust. In all cases tlle
"dust" inclucled substantial amounts of particles smaller
tllan 37 microns. In all of the illustrative ~xamples the
amount of cdu~st a(lded respresented su~stalltially more than
that normally found i.n any of the seed commodities, all of
which yield dust duri.ng normal handling to cause a number
- of serious problems.
Ex~mi)le 60 was included to illustrate the efficiency
of the process even under extreme an~ unreasona~le circum-
stance:;. 'I'l~e three per cent dust (2.h6 per cent, hased on
"as is" grain weight) represents an amount 15 to 50 times
more ~han normally found wi~h the wheat, according to various
sources and depending on age and condition of the grain. ln
thi~s example ~he ratio of solids (dust) to vehicle in the
synergetic mix~ure was only 3:1. Thus trea~ed, the san-ple
was milled into flour and ~aked by an inclel)el-dent laboratory.
- 25 - -

- ,
1~37~}52
Water adsorption by the treated wheat (tempering), mill
extraction (flour yield from the grain), and most baking
characteristics (loaf volume and bread grain and texture)
were normal as compared to identical but untreated wheat
("control"). However, flour color, ash content and flour
odor were adversely affected, reflecting the high content
of synergetic mixture adsorbed into the grain endosperm.
The "musty" odor reported was caused by the dust.
The wheat in Example 61 was mixed with one-third
of the total dust added, then the vehicle mixed vigorously
with the extremely dusty grain resulting in the very rapid
and simultaneous adsorption of both phases of the synergetic
mixture. Another third of the dust was mixed with the wheat
seeds to simulate the issue of new dust caused by additional
handling. The final third of the dust was then mixed with
the grain for the same reason. The total amount of dust added
was about triple that normally encountered. In each case
the dust adsorption occurred as rapidly as the big glass
container could be shaken. Prior to addition of the mineral
oil vehicle, the jar atmosphere was extremely hazy and opaque.
After all of the synergetic mixture had been added, there
was no visible dust whatever. Subsequent milling of the wheat,
and baking of the resultant flour, produced results which
were considered to be normal as compared to the "control"
graln .
~5 ~ The wheat used in Example 62 was dehydrated to 1.49
per cent moisture specifically for the purpose of demonstrating
the independence of the process efficacy from grain moisture
content. No difference in rate of sorption of the two phases,
corn oil and wheat dust, was observed as compared to wheat
with a normal moisture content.
- 26 -

~3735Z
Grain sorghum dust (one-half the total) was mixed
with the grain sorghum before addition of the corn oil vehicle
(Example 63) and the rest after the synergetic mixture had
been adsorbed. The adsorption of the latter is always signifi-
cantly faster because the vehicle has already been dispersed.
In Example 64 wheat dust was used in conjunction
with whole grain sorghum and unrefined cottonseed oil to
illustrate the irrelevance of a particular source of dust
with any special seed type. Grain elevators commonly handle
various commodities with the inevitable mixing of dust types
and even mixing of seed types to some extent.
The synergetic mixture of corn dust and corn oil
was used in conjunction with corn in Example 65, an obvious
expedient when the intended use includes the production of
corn oil. When intended for animal feeds where most corn is
used, any of the oleaginous vehicles may be appropriately
used, such asthe unrefined soya oil in Example 66.
Virtually all soybeans are processed into two primary
products, soybean meal and soya oil. As shown in Example
67, soybean dust was mixed with soybeans, then mixed with
unrefined soya oil, resulting in the very rapid sorption of
the synergetic mixture. Two more equal additions of soybean
dust were then mixed with the beans. No atmospheric dust
could be observed when the sample was shaken. By such practice
a soybean supplier or processor could protect the purity of
his oil product if desired, even though the amount of the
oleaginous vehicle added would be extremely small in most
cases.
One-third of the rice dust added was mixed with the
whole grain rice (Example 68), followed by the mixing of all
0 of the food grade mineral oil used. Simultaneous adsorption
- 27 -

1J.3735Z
of both phases of the rice was, typically, remarkably rapid~The remaining dust, as with the aforegoing examples, was added
in two equal Aliquots to simulate the issue of new dust caused
by further grain handling. As shown in the Table of Examples,
adsorption of all dust additions was very rapid.
Sixty-five degrees C. animal fat was used as the
vehicle in Example 69 along with barley dust in conjunction
with whole barley. The speed and efficiency of adsorption
of the synergetic mixture approximated that of the other
examples.
Obviously, all of the oleaginous vehicles dislcosed
herein are operative with seed dust or the other disclosed
solids.
In general, a solids (dust)-to-oleaginous vehicle
ratio of 3:1 to 4.5:1 was required for the simultaneous and
total adsorption of the synergetic mixtures. However, in
every instance where a deficiency in vehicle was used, relative
to that required for total adsorption of both phases, excellent
dust control resulted due to the preferential adsorption of
the smaller particles. Larger particles are not the cause
of explosive conditions. Thus, in the practical application
of the process, ratios of 6:1 to 10:1 were found to exhibit
excellent process efficacy. Since the quantities of dust
are generally very small compared to grain weight, the
necessary quantity of vehicle used is minute. For control
of wheat dust, for example, 250 to 500 p.p.m. (0.025 to 0.050
per cent, based on dry grain weight) of the vehicle is
ade~uate. In the event that an excess of the vehicle was
applied to a given lot of grain, that grain may be mixed with
similar but untreated grain. Conversely, if too little
vehicle was applied to adsorb the dust present, an obvious
expedient would be to apply additional vehicle to the grain.
- 28 -

1~.3735~
From the aforegoing discussion and examples, it isevident that an array of novel processes and products have
been provided by the present invention which is predicate~
on the surprising discovery of the phenomenon of sorption
by whole seeds of the synergetic mixture of solids and oleagi-
nous vehicles. The process provides for the encapsulation
of large amounts of solids in virtually limitless combinations,
and in a manner which provides component availability which
more closely parallels that of the tissues of the seeds and
which precludes its subsequent resolution into original
components. Further, it has been shown in the selected
examples, by their reaction to a dye, reactions following
adsorption, reactions in subsequent superimposed processes,
large quantities of solids sorbed, bread baking tests, and
the like, that the gross structure of all seed tissues are
involved in sorption of the synergetic mixture. Also illustra-
ted is the efficacy in the sorption of solids, which vary
widely in chemical composition and physical configuration,
to provide significantly enhanced whole seed nutritional
quality.
Provided are methods which obviate many seed utili-
zation processes which are dependent upon seed comminution.
The method for processing utilizes the natural seed structure
intact to utilize the grain marketing channels, present and
future, and provides the various seed consuming entities with
an energy source better balanced nutritionally. Embodiment
of very rapid and accurate processing, at a cost which approxi-
mates a theoretical minimum, provides the seed with reactive
chemicals, catalysts, viable cells, and the like, for
0 subsequent and superimposed processing. Further, a method
- 29 -

-
~3735Z
is provided to sorb solids into whole seed tissues to provide
that which is regarded as a complete ruminant ration. In
addition, an extremely effective and inexpensive method is
provided for the adsorption of dust to eliminate grain ware-
house explosions, reduce fire hazards, and vastly improveenvironmental conditions for involved employees and the general
public. All of such products of~ the method will immediately
indicate to those skilled in the seed utilization arts that
the properties for subsequent use or treatment have been
significantly enhanced.
- 30 -

Dessin représentatif

Désolé, le dessin représentatif concernant le document de brevet no 1137352 est introuvable.

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S.O.
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HAROLD N., JR. BARHAM
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Revendications 1994-02-28 4 84
Dessins 1994-02-28 1 5
Abrégé 1994-02-28 1 19
Description 1994-02-28 31 1 102