Source: http://www.google.com/patents/US4181709?dq=patent:5992892
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Patent US4181709 - Rumen-stable pellets - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsPellets adapted to be orally administered to ruminants are disclosed. The pellets have a core comprising a nutrient and/or medicament, and a coating which protects the core in the environment of the rumen is also provided to allow utilization of the core in the abomasum and/or intestine. The coating...http://www.google.com/patents/US4181709?utm_source=gb-gplus-sharePatent US4181709 - Rumen-stable pelletsAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS4181709 APublication typeGrantApplication numberUS 05/830,281Publication dateJan 1, 1980Filing dateSep 2, 1977Priority dateSep 2, 1977Also published asCA1104495A, CA1104495A1, DE2838298A1Publication number05830281, 830281, US 4181709 A, US 4181709A, US-A-4181709, US4181709 A, US4181709AInventorsClarence C. DannellyOriginal AssigneeEastman Kodak CompanyExport CitationBiBTeX, EndNote, RefManPatent Citations (6), Referenced by (51), Classifications (29), Legal Events (1) External Links: USPTO, USPTO Assignment, EspacenetRumen-stable pellets
US 4181709 AAbstract
Pellets adapted to be orally administered to ruminants are disclosed. The pellets have a core comprising a nutrient and/or medicament, and a coating which protects the core in the environment of the rumen is also provided to allow utilization of the core in the abomasum and/or intestine. The coating comprises a polymeric matrix which is resistant to the mildly acidic environment of the rumen, a hydrophobic substance, a flake material, and reactive acid dispersed throughout the continuous matrix. The core may contain a neutralizer if desired. The continuity of the polymeric matrix is destroyed in the more acidic environment of the abomasum.
1. A pellet adapted for oral administration to a ruminant comprising a core material having a pH greater than about 5.68, said core material being beneficial to the ruminant postruminally, and a coating surrounding said core material which protects the core material in the rumen and releases it in the abomasum, said coating comprising(a) a film-forming polymeric material containing at least one basic amino group in which the nitrogen content is from 3 to 14% by weight of the total molecular weight of the polymeric material, said polymeric material comprising cellulose propionate morpholinobutyrate, or at least one polymer, copolymer or blend of polymers derived from monomers selected from 2-vinylpyridine, 4-vinylpyridine, 2-methyl-5-vinylpyridine, and 2-ethyl-5-vinylpyridine, (b) from about 2 to about 40% based on the weight of said polymeric material, of a hydrophobic material dispersed in said polymeric material selected from fatty acids having from 12 to 32 carbon atoms, aluminum salts of fatty acids having from 12 to 32 carbon atoms, or polycarboxylic acids having a ratio of from 10 to 22 carbon atoms per carboxyl group and a molecular weight of from 400 to 1000, (c) from about 10 to about 200%, based on the weight of said polymeric material, of a physiologically acceptable flake material dispersed in said polymeric material, and (d) from about 5 to about 40% by weight based on the weight of said polymer, of a reactive fatty acid,said coating making up about 5 to about 50% of the weight of said pellet, and having a sticking temperature of at least about 50° C. 2. A pellet according to claim 1 wherein said reactive acid is selected from the group consisting of dimer acid, oleic acid, stearic acid, and palmitic acid.
3. A pellet according to claim 1 wherein said core material is selected from the group consisting of glucose, bacitracin, thyrotropin releasing factor and inositol.
4. A pellet according to claim 1 wherein said polymeric material is a copolymer of 2-methyl-5-vinylpyridine and styrene.
5. A pellet according to claim 3 wherein said polymeric material is a copolymer consisting essentially of about 80% 2-methyl-5-vinylpyridine and about 20% styrene.
6. A pellet according to claim 1 wherein said hydrophobic material is aluminum oleate.
7. A pellet according to claim 1 wherein said hydrophobic material is stearic acid.
8. A pellet according to claim 1 wherein said hydrophobic material is dimer acid.
9. A pellet according to claim 1 wherein said flake material is selected from the group consisting of metal flake, mineral flake, and crosslinked organic polymer.
10. A pellet according to claim 9 wherein said flake material is selected from the group consisting of aluminum flake, talc, graphite, and ground mica.
11. A composition adapted for use in coating pellets orally administrable to a ruminant which protects the core material in the rumen and releases it in the abomasum comprising(a) a film-forming polymeric material containing at least one basic amino group in which the nitrogen content is from 3 to 14% by weight of the total molecular weight of the polymeric material, said polymeric material comprising cellulose propionate morpholinobutyrate, or a polymer, copolymer or blend of polymers derived at least in part from monomers selected from 2-vinylpyridine, 4-vinylpyridine, 2-methyl-5-vinylpyridine, and 2-ethyl-5-vinylpyridine, and (b) from about 2 to about 40%, based on the weight of said polymeric material, of a hydrophobic material dispersed in said polymeric material selected from fatty acids having from 12 to 32 carbon atoms, aluminum salts of fatty acids having from 12 to 32 carbon atoms, or polycarboxylic acids having a ratio of from 10 to 22 carbon atoms per carboxyl group and a molecular weight of from 400 to 1000, and (c) from about 10 to about 200%, based on the weight of said polymeric material, of a physiologically acceptable flake material dispersed in said polymeric material, and (d) from about 5 to about 40% by weight, based on the weight of said polymer, of a reactive fatty acid,said coating having a sticking temperature of at least about 50° C. 12. A composition according to claim 11 wherein said polymeric material is a copolymer of 2-methyl-5-vinylpyridine and styrene.
13. A composition according to claim 11 wherein said polymeric material is a copolymer consisting essentially of about 80% 2-methyl-5-vinylpyridine and about 20% styrene.
14. A composition according to claim 11 wherein said hydrophobic material is aluminum oleate.
15. A composition according to claim 11 wherein said hydrophobic material is stearic acid.
16. A composition according to claim 11 wherein said hydrophobic material is dimer acid.
17. A composition according to claim 11 wherein said flake material is selected from the group consisting of metal flake, mineral flake, and crosslinked organic polymer.
18. A composition according to claim 17 wherein said flake material is selected from the group consisting of aluminum flake, talc, graphite, and ground mica.
19. A pellet adapted for oral administration to a ruminant comprising a core material having a pH greater than about 5.68, said core material being beneficial to the ruminant postruminally, and a coating surrounding said core material which protects the core material in the rumen and releases it in the abomasum, said coating comprising(a) a film-forming copolymer of about 80% 2-methyl-5-vinylpyridine and about 20% styrene by weight, (b) from about 2 to about 40% based on the weight of said polymeric material, of a hydrophobic material dispersed in said polymeric material selected from aluminum oleate, dimer acid, stearic acid or oleic acid, (c) from about 10 to about 200%, based on the weight of said polymeric material, of at least one physiologically acceptable flake material dispersed in said polymeric material selected from the group consisting of talc, aluminum flake and graphite, and (d) from about 5 to about 40% by weight, based on the weight of said polymer, of a reactive fatty acid,said coating making up about 5 to about 50% by weight of said pellet, and having a sticking temperature of at least about 50° C. Description
In ruminants, ingested feed first passes into the rumen, where it is pre-digested or degraded by fermentation. During this period of fermentation the ingested feed may be regurgitated to the mouth via the reticulum where it is salivated and ruminated. After a period of fermentation regulated by natural processes and variable depending on the animal and the feedstuff, adsorption of digested nutrients starts and continues in the subsequent sections of the digestive tract by the ruminant animal. This process is described in detail by D. C. Church, "Digestive Physiology and Nutrition of Ruminants", Vol. 1, O.S.U. Book Stores, Inc., of Corvallis, Ore.
In accordance with the present invention, a polymeric coating having a hydrophobic substance, a flake material, and reactive acid dispersed therein, which is resistant to environmental conditions of the rumen but releases the core material under the environmental conditions of the abomasum, provides a very desirable utilization efficiency by ruminants. The core material may also contain a neutralizer to provide a pH above about 5.5.
Difficulty has been encountered with known coated pellets in attaining the necessary characteristics of protection and release at efficiencies required in commercial applications. When pellets are coated in accordance with the present invention, a surprisingly high percentage of the coated pellets are found (1) to be protected in the environment of the rumen for the required time, and (2) to release the core material in the environment of the abomasum within the required time. It was unexpected that the coating described herein would demonstate such an increased efficiency. For example, at least 60%, and normally at least 75% and frequently higher percentages of the pellet core material will be protected by the coating for the required time in the mildly acidic environment of the rumen and be released by the coating within the required time in the more acidic environment of the abomasum. This increased efficiency may be due to the acid sensitivity characteristics of the coating, the resistance to abrasion in handling and/or the resistance to sticking under relatively high heat and humidity conditions which may damage the coating.
The coating material has the ability to withstand environmental conditions of the rumen, and the ability to expose the core material of the pellet in the environment of the abomasum. Thus, the coating material is resistant to pH conditions of about 5.5 for at least about 24 hours. The coating material releases the core material upon exposure to abomasum environmental conditions having a pH of about 3.5 after a time of about 10 minutes to about 6 hours. The exposure of the core may occur by the coating becoming permeable to the fluids therein or by dissolving or disintegrating. Another requirement for the coating material is to have the ability to withstand storage conditions of relatively high heat and/or humidity without a significant amount of blocking.
______________________________________Amino Acids Solubility and pH of Saturated Solutions            Solubility g./100 g. water            at 25° C.                      pH______________________________________DL - Alanine       16.7        6.2L - Asparagine     3.1         4.7L - Arginine       21.6        11.8L(-) - Cysteine    0.01        3.7DL - Methionine    4.0         5.7L(-) - Lencine     2.0         4.8L(-) - Tyrosine    0.05        7.3DL - Phenylalanine 3.0         5.6______________________________________
Other suitable active core materials include glucose, bacitracin, thyrotropin releasing factor and inositol. Proteins from various sources are valuable for practice of the invention. Generally, proteins are polymers derived from various combinations of amino acids. Proteins are amphoteric substances which are soluble or suspendable in aqueous media either more acidic or more basic than the particular protein being considered.
The core material may be made ready for coating by the following method. The nutrient, medicament, or the like, and core neutralizer, if used, are mixed with water, binders, a basic substance for adjusting the core pH, and sometimes inert inorganic substances added to adjust the specific gravity of the pellet and the resulting plastic dough-like mass is extruded or rolled to obtain suitable size particles. Adhesive binders are added to strengthen the pellet and can be nontoxic vegetable gums, starches, cellulose derivatives, animal gums and other similar substances well-known in the art of food thickening and tablet making. Inorganic additives used to adjust the specific gravity of the pellet include such substances as insoluble, nontoxic pigment-like materials such as metal sulfates, oxides and carbonates having a relatively high density. The final desirable range of specific gravity for the rumen protected pellets is from 1.0 to 1.4. After creating suitable size pellets by extrusion, rolling or other suitable means, the pellets are dried to remove the water. The pellets are then coated by contacting them with a solution of the protective coating material in a suitable solvent or mixture of solvents as hereinafter described. Typical solvents of value include lower alcohols, ketones, esters, hydrocarbons, and chlorinated hydrocarbons.
Core materials may be raised in pH to a predetermined degree by mixing a basic neutralization substance therewith or by coating the core with a basic neutralization substance. The acidity is modified by adding nontoxic, insoluble, basic substances such as alkaline earth oxides, hydroxides, or carbonates, to the core material before the pellet forming step. Basic compounds of aluminum such as the various forms of hydrated alumina, aluminum hydroxide, and dibasic aluminum salts of organic acids, having less than 6 carbon atoms, such as dibasic aluminum acetate may also be used. These basic substances are added to the pellets by mixing the core material, basic substance, and binders as described above before adding water. The amount used depends on both the solubility and relative acidic nature of the proteinaceous substance, on the coating composition used to obtain rumen protection and on the thickness of the coating applied. The amount of basic substance used is that quantity which will theoretically neutralize or raise the pH at least to 5.68, preferably to about 7.
Another method of core neutralization is based on the concept that, whereas the coating is permeable to water and acidic water borne molecules, not all of the pellet interior is required to be neutralized. In this method of practicing the invention, the nontoxic inorganic basic substances are deposited on the surface of the core material prior to application of the coating. In practice, the preformed pellets are placed in a fluidized bed or other coating apparatus and a dispersion of an oxide, hydroxide, carbonate, or basic salt of magnesium, calcium, or aluminum in water or an organic liquid is sprayed on the pellet. The dispersion of basic substance preferably contains a binder and may also contain a protective colloidal substance wherein the ratio of binder plus protective colloidal substance to basic substance is less than about 1:3. The amount of basic substance coated onto the pellet is normally from about 1 to about 20% of the weight of the core material. The binder and protective colloidal substance can be the same substance or different and are preferably soluble or dispersible in water and in the organic liquid used to suspend the basic substance. Such binder materials as relatively low molecular weight cellulose derivatives, synthetic polymers, and natural gums known to the art of tablet making are suitable for the practice of the invention. The organic liquid can be any having suitable solvent power and boiling in the range of from 40°-140° C.
Another requirement for the coating material is its ability to withstand abrasion in handling and storage conditions of relatively high heat and/or humidity without a significant amount of blocking or sticking. It should have a sticking temperature of greater than about 50° C. Sticking temperature is defined as the temperature at which an applied force of 0.25 Kg/cm2 for 24 hours causes the coating of pellets to adhere to the coating of adjacent pellets strongly enough to cause rupture of the coating when the pellets are forceably separated. Also, the coating material is preferably soluble or dispersable in organic solvents having boiling points of between about 40° C. and 140° C. to permit conventional coating processes such as spray coating to be used. Particularly suitable solvents include methylene chloride, chloroform, ethanol, methanol, ethyl acetate, acetone, toluene, isopropanol or mixtures of these.
The coating or film forming material according to this invention includes a mixture or blend of at least one polymeric substance, at least one hydrophobic substance, and at least one flake material. Generally, the more acidic and more soluble core materials require greater ratios of hydrophobic substance and flake material to polymeric substance, while more basic and less soluble core materials require lesser ratios of hydrophobic substance and flake material to polymeric substance within this range. The hydrophobic substance and flake material are normally dispersed in the polymeric matrix. The hydrophobic substance is normally present in amounts of between about 2 and about 40% and the flake material is normally present in amounts between about 10 and 200%, based on the weight of the polymeric material. The coating normally accounts for from 5 to about 50% by weight of the pellet.
The polymeric substances which are useful in the coatings of this invention include those which, in combination with the hydrophobic substance described hereinafter, are physiologically acceptable and resistant to a pH of greater than about 5 but capable of releasing the core of the pellets at a pH of less than about 3.5, at the normal body temperature of ruminants (about 37° C.).
The polymeric substances are macromolecules of sufficient molecular weight to have film-forming properties when the polymer is deposited from a solution and after removal of a solvent, dispersing medium or on cooling from a melt. Typical molecular weights will be in the range of from about 5,000 to about 300,000.
Polymeric substances having the characteristics defined herein include certain modified natural polymers, homo- and interpolymers, containing at least one basic amino group in which the nitrogen content is from 3 to 14% by weight of the total molecular weight of the polymeric material. The polymeric material is at least one polymer, copolymer, or blend of polymers selected from the group consisting of cellulose propionate morpholinobutyrate, poly(vinylpyridine), and polymeric derivatives of vinylpyridine specifically, polymer comprising 2-vinylpyridine, 4-vinylpyridine, 2-methyl-5-vinylpyridine and 2-ethyl-5-vinylpyridine. Especially preferred is a copolymer of about 75-85% by weight 2-methyl-5-vinylpyridine and about 15-25% by weight styrene, and in particular about 80% by weight 2-methyl-5-vinylpyridine and about 20% by weight styrene.
Preferred also are copolymers of vinylpyridine and acrylonitrile, and in particular, the copolymer of about 55-65% by weight 2-methyl-5-vinylpyridine and about 35-45% by weight acrylonitrile. These copolymers are commercially available or may be produced by conventional techniques well known in the art. Conventional additives such as plasticizers may be used in the polymer.
Useful hydrophobic substances which are physiologically acceptable are commercially available. The polymer and hydrophobic substance should have a degree of compatability to permit the film to remain intact in the rumen environment, but to permit permeation of the abomasal fluid to the core while the pellet is in the abomasum.
Suitable hydrophobic substances include fatty acids, dimer acids, trimer acids, and aluminum salts of fatty acids. The useful hydrophobic substances are fatty acids having from 12 to 32 carbon atoms such as, for example, oleic acid and stearic acid. Aluminum salts of such acids, for example, aluminum oleate, aluminum stearate, aluminum dimerate, are also useful. Also, the hydrophobic material may be one or more polycarboxylic acids having a ratio of from 10 to 22 carbon atoms per carboxyl group and a molecular weight of from about 400 to about 1000. Blends of these acids and/or salts are also useful.
FUNCTIONAL FLAKE MATERIAL
In accordance with this invention, a physiologically acceptable flake material is dispersed throughout the polymeric matrix. The flake material is substantially inert with respect to the environment of the rumen.
REACTIVE ACIDS
In accordance with this invention, one or more fatty acids are used with the inert flake material to form a coating resistant to the environment of the rumen, but which will permit permeation of the abomasum contents into the core material. These acids react with the flake material to join adjacent flakes and bind the flakes together to form a strong barrier against the acidic environment of the rumen.
Acids which may be used include fatty acids having 12 to 32 carbon atoms, and polyfunctional carboxylic acids having a ratio of from 10 to 22 carbon atoms per carboxyl group and a molecular weight greater than 300.
Especially preferred are dimer acid, oleic acid, stearic acid, and palmitic acid.
Such acids may conveniently be used in amounts of 5 to 40 percent by weight, based on the weight of the polymer.
In reference to FIG. 1, the coating apparatus is designated in general at 10 and includes a vertically disposed first hollow column 12 of regular shape. By "regular shape" is meant that it may be cylindrical, octagonal, hexagonal or of other configurations, so long as the hollow column is generally symmetrical with respect to its central axis. The hollow column contains therewithin the practicle storage, coating, drying and deceleration zones, which will be described herein.
The upper surface of the gas shaping or areodynamic structure is centrally disposed within and extends generally horizontally across the cross-section of the vertically disposed hollow column. In other words, it has a cross-sectional plane generally perpendicular to the vertical axis of the vertically disposed hollow columns. The outer edge of the upper surface is equally spaced from the wall surface of the hollow column and defines therebetween with the wall surface of the hollow column a reduced pressure region for acceleration in velocity of the upwardly flowing gases in such manner that the upwardly flowing gases form a boundary layer that is directed away from the wall surface of the hollow column and that adheres to the upper surface of the gas shaping or aerodynamic structure for flow across a portion thereof.
The cross-sectional configuration of an annular airfoil in a plane described from the center of the cross-sectional area of the coating apparatus to a point, p1, on the lower rim of the airfoil to a point, p2, in the upper rim of the airfoil is teardrop, or similar to the cross-sectional shape of a lifting aerodynamic shape, and having the thicker cross section on the forward part with reference to the direction facing the upwardly flowing gases. The thickest part is located about two-fifths (2/5) to about one-half (1/2) of the height in the vertical direction. In other words, the height (H) of the thickest part (T), or HT is equal to about 2/5 H to about 1/2H. The thickest cross section (T) is from about one-sixth (1/6) to about two-fifths (2/5) of the height (H) of the airfoil; or T is equal to about 1/6 H to about 2/5 H.
The following examples are submitted for a better understanding of the invention. Generally, pellets are prepared from the nutrients indicated to a size of between about 8 and 12 sieve size. The nutrients are mixed with conventional additives such as microcrystalline cellulose, binders, inert consistency adjusting substances such as water, etc. The pellets are formed by a conventional pelletizer, dried, sieved, and coated using a coater as described herein. Upon formation of an imperforate coating on the pellets, they are tested for resistance to pH conditions resembling those of the rumen and abomasum by agitating in buffer solutions of pH 2.9 for 0.5 hours and 5.4 for 24 hours. Recovery and protection figures cited for active core ingredients herein contain in them all materials of the original coated pellet that are not completely dissolved in the pH 2.9 buffer, including any undissolved active ingredient in the original core. For the sake of simplicity, abbreviations are used in the examples as follows:
2M5VP--2-methyl-5-vinylpyridine
Where coating ratios are used, the first number indicates the number of parts polymer, the second number indicates the number of parts hydrophobic substance, and the third number indicates the number of parts inert flake material. Unless otherwise specified, a coating ratio of 70/30/10, wherein the flake material is aluminum or graphite, is used, and 25% of the hydrochloride of the lycine.HCl is neutralized using calcium carbonate. Dimer Acid 1010 is a trademark for dimer acid marketed by Emery Industries.
Table I compares results obtained using actual abomasal and duodenal fluid extracted from a ruminant with artificial test fluid. In this table, the polymeric material used is an 80/20 copolymer of 2-methyl-5-vinylpyridine and styrene (I.V.=1.23). The core material is 90.9% methionine, 3.6% sodium carboxymethyl cellulose and 5.5% sucrose. The pellets are made by first dry mixing 500 g. of methionine, 20 g. sucrose and 10 g. sodium carboxymethyl cellulose. Water (135 g.) is added and mixed to obtain an extrudable wet powder. The mixture is extruded and chopped to obtain pellets to pass 8 mesh screen and remain on 12 mesh. Ten grams sucrose and 10 g. sodium carboxymethyl cellulose are dry mixed, and added to the wet pellets. The pellets are then tumbled to obtain a uniform coating. Tumbling is continued in hot air to obtain dry pellets.
The coatings are made using the ingredients indicated dissolved or suspended in acetone at 5% solids level. An air suspension coater is used to coat the pellets.
In the examples, the coating comprises 31.5% polymer, 3.5% stearic acid, and aluminum flake and talc as indicated. Ten percent coating, based on the weight of the core, is used unless otherwise indicated. pH of the abomasum simulated fluid is 2.9. pH of the rumen simulated fluid is 5.4. Release is measured after one hour periods.
TABLE I__________________________________________________________________________            pH, Actual                   pH, Actual                         % Release                               % Release                                     % Release                                             % Release                                                   % ProtectionExample Aluminum        Talc,            Abomasum                   Duodenum                         Abomasum                               Duodenum                                     Abomasum plus                                             Abomasum                                                   Rumen TestNo.   Flake, %        %   Fluid  Fluid Fluid Fluid Duodenal Fluid                                             Test Fluid                                                   Fluid__________________________________________________________________________1     0      65  2.8    2.9   32    34    66      75    692     5      60  2.8    2.9   26    43    69      --    723     10     55  2.8    2.9   28    40    68      77    844     15     50  2.8    3.0   29    37    78      74    865     25     40  2.8    3.0   28    --    73      73    896     30     35  2.8    3.0   29    46    76      71    92Z__________________________________________________________________________
TABLE II__________________________________________________________________________Effects of Humidity and Temperature on Abomasal Release of RumenProtected Glucose After 7 Days Storage                      Percent Recovered From pH 2.9 Buffer                      0%        80%      100%     Stored                      Relative Humidity                                Relative Humidity                                         Relative Humidity                                                  Over WaterExample Coating Composition                Original                      25° C.                            60° C.                                60° C.                                         25° C.                                              60° C.                                                  25°                                                      60°__________________________________________________________________________                                                      C.7     70 parts 60/40 2M5VP/AN                23.2  27.9  30.3         27.2 30.4                                                  26.2 30 parts Dimer Acid 1010 30 parts talc-stearic acid8     70 parts 60/40 2M5VP/AN                25.4  26.4  29.6         28.4 30.8                                                  28.4 30 parts Dimer Acid 1010 30 parts talc-oleic acid9     70 parts 60/40 2M5VP/AN                7.9   8.3   7.8 8.0      7.6  7.9 7.1 9.7 30 parts Dimer Acid 101010    70 parts 60/40 2M5VP/AN                10.1  9.7   11.3                                10.8     9.3  10.7                                                  9.6 8.4 30 parts Dimer Acid 1010 10 parts Al__________________________________________________________________________
TABLE III__________________________________________________________________________Effects of Humidity and Temperature on Coated Glucose After 7 DayStorage                Percent Recovered From pH 5.4 Buffer                      0%        80%      100%     Stored                      Relative Humidity                                Relative Humidity                                         Relative Humidity                                                  Over WaterExample Coating Composition                Original                      25° C.                            60° C.                                60° C.                                           25° C.                                              60° C.                                                  25°                                                      60°__________________________________________________________________________                                                      C.11    70 parts 60/40 2M5VP/AN                91.3  91.3  96.4         86.4 91.7                                                  87.9 30 parts Dimer Acid 1010 30 parts talc-stearic acid12    70 parts 60/40 2M5VP/AN                90.2  89.6  95.0         89.4 93.1                                                  86.7 30 parts Dimer Acid 1010 30 parts talc-oleic acid13    70 parts 60/40 2M5VP/AN                93.3  93.1  93.6                                93.1     90.6 94.1                                                  85.6                                                      23.6 30 parts Dimer Acid 101014    70 parts 60/40 2M5VP/AN                93.1  92.8  97.0                                95.0     90.1 96.0                                                  88.2                                                      27,5 30 parts Dimer Acid 1010 10 parts A1__________________________________________________________________________
TABLE IV__________________________________________________________________________Effect of Mechanical Tumbling in a Heated Drum on the Coated Glucose(Drum Temperature = 80° C.)              Percent Recovered                        Percent Recovered              From pH 5,4 Buffer                        From pH 2.9 Buffer              Heatine Time, hrs.                        Heating Time, hrs.ExampleCoating Composition              0   1  2  0    2__________________________________________________________________________15   70 parts 60/40 2M5VP/AN              91.3                  93.3                     95.0                        23.2 23.830 parts Dimer Acid 101030 parts talc-stearic acid16   70 parts 60/40 2M5VP/AN              90.2                  93.6                     95.9                        25.4 29.530 parts Dimer Acid 101030 parts talc-oleic acid17   70 parts 60.40 2M5VP/AN              93.3                  95.7                     96.9                        7.9  7.630 parts Dimer Acid 101018   70 parts 60/40 2M5VP/AN              93.1                  96.0                     96.0                        10.1 10.030 parts Dimer Acid 101010 parts Al__________________________________________________________________________
TABLE V______________________________________Recovery of Coated Glucose Pellets(coating components: 70 parts60/40 2M5VP/AN, 30 parts Emphol 1010and 30 parts talc-fatty acid mixture)           %      % Recovered FromExample  Talc:Fatty Acid Ratio                 coating  pH 2.9                                pH 5.4______________________________________19     300:10 stearic 21.5     26.8  90.320     300:50 stearic 18.6     26.1  81.721     300:10 oleic   20.5     25.7  90.922     300:50 oleic   19.9     30.7  74.4______________________________________
TABLE VI______________________________________Glucose Pellet Protection with Varying Amounts of60/40 2M5VP/AN, Dimer Acid 1010 and Aluminum Flake  Coating %         % Recovered FromExample  Ratio     Coating   pH 2.9  pH 5.4______________________________________23       70/30/10  16.2      12.2    92.324       70/20/10  18.1      10.7    93.625       70/10/10  16.6      10.4    84.026       70/30/5   20.0      10.4    72.9______________________________________
TABLE VII______________________________________Glucose Pellet Protection with Varying Amounts of60/40 2M5VP/AN, Dimer Acid 1010 and Talc-Oleic Acid Mixture  Coating %         % Recovered FromExample  Ratio     Coating   pH 2.9  pH 5.4______________________________________27       70/30/30  19.4      25.2    94.628       70/20/30  18.1      24.1    89.629       70/30/20  15.3      22.4    94.230       70/20/20  19.1      16.8    95.431       70/26/10  19.9      14.1    92.932       70/20/10  18.6      22.3    92.833       70/10/20  19.7      17.2    95.434       70/10/10  19.2      18.8    82.4______________________________________
The fluid used to simulate environmental conditions of the rumen (at pH 5.5) is prepared by making 11.397 grams of sodium acetate with 1.322 grams of acetic acid and diluting this mixture with demineralized water to 1 liter.
Unless otherwise specified, all ratios, percentages, etc., are by weight, and the ratio of flake material to reactive acid in the examples is 300:30.
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