CA1137352A - Method of treating whole seeds to incorporate solid materials - Google Patents

Abstract

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.

Description

~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 ~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 ~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 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 ~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.

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-- 13a - 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 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 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 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 ~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 - ~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~

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 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.

- , 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.

~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 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.

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 -~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.

Claims (14)

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, 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.

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.

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