WO1994028739A1

WO1994028739A1 - Rumen-bypass fatty acid salt and protein dietary supplement for ruminants

Info

Publication number: WO1994028739A1
Application number: PCT/US1994/006329
Authority: WO
Inventors: Robert L. Jorgensen; Kenneth R. Cummings; Alfredo Vinci; M. Stephen Lajoie; Conor Rudden
Original assignee: Church & Dwight Company, Inc.
Priority date: 1993-06-16
Filing date: 1994-06-03
Publication date: 1994-12-22
Also published as: AU7100094A

Abstract

This invention provides process embodiments for the preparation of a ruminant dietary product comprising a blend of fatty acid salt and denatured protein. Ine one process embodiment, whole proteinaceous oilseed in particulate form is treated with a mixture of basic alkaline earth metal and alkali metal compounds. The oil content of the oilseed is saponified to a fatty acid salt, and the protein content is denatured into a water-insoluble form. The fatty acid salt and denatured protein ingredients of the invention ruminant dietary product have rumen-bypass properties, and are metabolized in the post-rumen digestive tract under ruminant feeding conditions.

Description

RUMEN-BYPASS FATTY ACID SALT AND PROTEIN DIETARY SUPPLEMENT FOR RUMINANTS

BACKGROUND OF THE INVENTION Conventional cattle feeds such as corn and alfalfa often fail to provide sufficient energy for cattle, especially lactating dairy cattle during periods of heavy milk production. Feed containing a high proportion of corn also has a tendency to depress the milk fat content of the milk produced by such cattle. Fat is an excellent energy source, and it is known that if the proportion of fat in cattle food is increased, lactating dairy cattle produce high milk yields without draining their reserves of body fat and without diminishing the proportion of milk fat in the milk produced.

However, it has been found that if the proportion of fat in the diet of cattle exceeds about 3-5% of the total feed solids, the feed has toxic effects upon the microorganisms in the rumen of the cattle. It appears that fat reduces the growth rate or even kills certain microorganisms which digest fiber in the cow's rumen, thereby lowering fiber digestibility. This deleterious effect on the cow's rumen is particularly true of unsaturated fats. Although the decreased fiber digestion in the rumen is partially compensated by greater fiber digestion in the lower parts of the alimentary canal, εuch later fiber digestion produces a blend of different fatty acids than that which is produced by the digestion in the rumen, and the different blend of fatty acids is less suited to the cow's metabolism.

There has been a continuing need for new fat-containing dietary supplements for animal feed which can be fed to ruminant animals without interfering with the rumen microorganisms.

United States Patent Numbers 4,642,317; 4,826,694; 4,853,233; and 4,909,138 describe the incorporation of insoluble fatty acid salts in ruminant feed as a means of increasing the fat content of the feed without deleteriously affecting the ruminant digestion cycle. A feed additive such as fatty acid calcium salt functions as a rumen- bypas≤ product, and is subsequently metabolized in the abomasum or small intestine of the ruminant. Similar effort has been directed to the prevention of protein dea ination in the rumen of polygastric animals, while preserving the capacity of protein nutrients to be assimilated in the lower regions of the ruminant alimentary tract. United States Patent Numbers 3,720,765;

3,988,480; 4,211,795; 4,225,620; and 5,064,665 describe methods for producing a protein derivative which has rumen-bypass capability. One method of providing a rumen-bypass protein is by pelleting soybean meal with lignosulfonate.

GB 2113521 describes a ruminant feedstuff comprising an animal or vegetable protein nutrient ingredient dispersed in a fatty acid alkaline earth metal salt. A feedstuff is obtained by forming a dispersion of protein meal in an aqueous solution of a water-soluble fatty acid salt, and then adding an aqueous solution of basic alkaline earth metal compound to form water-insoluble fatty acid alkaline earth metal salt which precipitates and coats the dispersed protein meal solids. The coated solids have rumen-bypass capability, and are digested in the abomasum or small intestine of ruminants.

Other methods involve the treatment of protein with formaldehyde, or the heat-treatment of protein to cause browning or crosslinking of the protein. There is sustained interest in the production of dietary feed supplement products which contain fatty acid and/or protein ingredients which exhibit rumen-bypass properties.

Accordingly, it is an object of this invention to provide a fatty acid salt/protein composition which can function as a rumen-bypass dietary supplement for ruminants, and permit a beneficial increase in the dietary fat and protein content of the feed.

It is another object of this invention to provide a fatty acid/protein animal feed supplement for ruminants, which has rumen-bypass properties and which is metabolized in the post-rumen digestive tract of ruminants.

It is another object of this invention to provide an improved process for production of a blend of fatty acid alkaline earth metal salt and denatured protein, utilizing whole oilseed meal as a starting raw material, and basic inorganic salt as a saponification reagent. Other objects and advantages of the present invention shall become apparent from the accompanying description and examples.

DESCRIPTION OF THE INVENTION One or more objects of the present invention are accomplished by the provision of a process embodiment for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 1-3 equivalents of basic alkaline earth metal compound per equivalent of oilseed fatty acid content, and (c) between about 0.1-1.5 equivalents of basic alkali metal compound per equivalent of oilseed fatty acid content, wherein the reactive admixture has a water content between about 0.2-20 weight percent; and (2) maintaining the admixture at a temperature between about 30°-130°C for a time period sufficient to convert at least about 75 percent of the total fatty acid content to fatty acid metal salt, and to denature the protein to a water-insoluble content of at least about 65 percent of the protein, thereby providing a ruminant dietary product having rumen-bypass properties.

The conversion of the total fatty acid content to fatty acid metal salt can be at least about 90 percent, and the water-insoluble content of the denatured protein can be at least about 85 percent. The dietary product of the process can contain glycerol in a quantity which is about one-third of a mole per mole of saponified fatty acid. If desired, the content of glycerol can be partially or completely removed by water extraction of the dietary product solids. The water extraction also reduces the content of water-soluble basic alkali metal byproducts contained in the dietary product solids.

Alternatively, the water-soluble basic alkali metal byproducts in the dietary product solids can be neutralized by acid treatment in an aqueous medium to a pH of about 7-9. Suitable acid reagents for the neutralization reaction include organic acids such as acetic acid, propionic acid and citric acid; and inorganic acid such as hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid, and the like.

A content of glycerol in a present invention ruminant dietary supplement product can contribute desirable properties to the product. Glycerol can reduce dust and improve the appearance and consistency of dietary product granules. Glycerol also can function as a deodorizing agent, and improve the palatability of the dietary product for ruminant feeding. In the process embodiment for production of an invention ruminant dietary product, the whole oilseed ingredient typically has an oil content between about 15-50 weight percent, and a protein content between about 20-60 weight percent. Suitable whole oilseed raw materials include soybean, cottonseed, rapeseed, linseed, sunflower seed, safflower seed, peanut, palm kernel, corn kernel , coconut (copra), and the like. The whole oilseed is ground into a meal having an average particle size between about 200-2000 microns. The whole oilseed can be ground in commercial equipment such as a Bauer mill or a Sprout-Waldron CG hammer mill. The whole oilseed also can be comminuted by high shear mixing during the step(l) blending procedure.

The whole oilseed can be ground with hulls intact or in a dehulled state. Dehulling can be accomplished by passing the whole oilseed bulk through a roller mill with fluted rolls, which are driven at different speeds. The loosened hulls are removed from the seed kernels by aspiration or by sieving.

In the invention process embodiment, the protein content of the whole oilseed ingredient undergoes a denaturation reaction, which converts water-soluble protein into denatured water-insoluble protein which exhibits rumen-bypass properties. The water-insoluble protein is assimilated in the post- rumen digestive tract of ruminants.

The protein content of a whole oilseed ingredient of the present invention process has a typical molar profile of aminoacids comprising arginine (7-11), histidine (2-4), lysine (3-7), tryptophan (0.5-3), phenylalanine (4-6), ethionine (0.5-2), threonine (3-5), leucine (4-9), isoleucine (3-7) , valine (4-7) and aspartic acid (6-12) .

The fatty acid triglyceride constituency of the oil component of the whole oilseed ingredient is different for the various oilseed sources.

Soybean has a weight percent fatty acid profile comprising lauric (0.5), myristic (0.5), palmitic (12) , stearic (4) , oleic (25) , linoleic (52) , and linolenic (6) .

Cottonseed has a weight percent fatty acid profile comprising myristic (0.7), palmitic (24), stearic (2) , palmitoleic (1) , oleic (17) , linoleic (55), and linolenic (0.3). Rapeseed has a weight percent fatty acid profile comprising palmitic (5), stearic (2), oleic (63) , linoleic (20) , linolenic (9) , and eicosenic (1) .

The basic alkaline earth metal compound ingredient can be an oxide or hydroxide of calcium or magnesium, and the ingredient can be a mixture of two or more basic alkaline earth metal compounds.

The basic alkali metal compound ingredient can be a hydroxide, carbonate, bicarbonate or phosphate of sodium or potassium metal, and the ingredient can be a mixture of two or more basic alkali metal compounds. Sodium hydroxide and potassium hydroxide are commercially available in a pellet form. In the invention process embodiment, the water content of the reactive admixture in step(l) typically is in the range between about 0.2-20 weight percent. The whole oilseed ingredient has a natural water content, so that the addition of extraneous water to the reactive admixture is not necessary. It is essential that at least a small amount of water is present in order to initiate the oilseed oil saponification reaction. After the saponification is proceeding, water is generated during the fatty acid salt-forming stage, and the saponification reaction becomes self-sustaining.

In the invention process embodiment, the step(2) reaction time can vary in the range between about 0.5-4 hours. The process is adaptable for continuous operation.

The step(2) reactive admixture can be sparged with steam to heat the admixture to a temperature between about 80°-130°C. The elevated temperature also can be achieved by utilizing a heated mixer unit, or by preheating the oilseed ingredient by mechanical friction in a comminuting extruder unit.

In another embodiment this invention provides a process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, and (b) between about 5-60 weight percent of at least one C_κ-C₂₂ fatty acid ingredient, based on the weight of oilseed fatty acid content, (c) between about 1-3 equivalents of basic alkaline earth metal compound per equivalent of total fatty acid content, and (d) between about

0.1-1.5 equivalents of basic alkali metal compound per equivalent of total fatty acid content, wherein the reactive admixture has a water content between about 0.2-20 weight percent; and (2) maintaining the admixture at a temperature between about 30°-130°C for a time period sufficient to convert at least 75 percent of the total fatty acid content to fatty acid metal salt, and to denature the oilseed protein to a water-insoluble content of at least 65 percent of the protein, thereby providing a ruminant dietary product having rumen-bypass properties.

The optional C_u-C₂₂ fatty acid ingredient can be a mixture of saturated and unsaturated carboxylic acid compounds, such as those derived from vegetable oils and animal tallow.

Palm fatty acid distillate is a commercial product produced by distilling the fatty acids present in natural palm oil. A distillate product typically has the following weight percent content:

Free fatty acids 60-90

Water <1

Triglycerides 10-40

Unsaponifiables <3

The fatty acids in the free fatty acids and the triglycerides can consist of the following weight percent:

Palmitic acid 20-60 Oleic acid 25-60

Linoleic acid 2-20

Stearic acid 1-15

Laurie acid 0-10

Beef tallow acids are available commercially as a byproduct obtained by alkaline extraction of waste beef fat and subsequent acidification, and normally contain the following weight percent of fatty constituents:

Free fatty acids 60-90 Triglycerides 10-40

Water <l

Unsaponifiables <3

The fatty acids in the free fatty acids and in the triglycerides can have the following weight percent content: Palmitic acid 20-30

Oleic acid 35-45

Linoleic acid 2-10

Stearic acid 15-25

Other ingredients optionally can be included in the invention process embodiments, such as about 0.05-20 weight percent of an additional biologically active ingredient, based on the weight of the recovered dietary product. An optional ingredient can be added during the blending procedure of the invention process.

The optional biologically active constituent utilized in the invention process can be selected from a broad variety of nutrients and medicaments, either as a single component or as a mixture of components, which are illustrated by the following listing of active molecular species:

1. C₂-C₂₂ aliphatic carboxylic acids and alkali metal, ammonium and alkaline earth metal salts which can be different or have some correspondence with the other fatty acid constituents present in the process reaction medium.

2. sugars and complex carbohydrates which include both water-soluble and water-insoluble monosaccharides, disaccharides and polysaccharides. Cane molasses is a byproduct from the extraction of sucrose from sugar cane. It is commercially available at standard 79.5° Brix concentration, which has a water content of about 21 weight percent, and a sugar content of 50 weight percent. Sugar beet byproducts also are available as low cost carbohydrate sources. Whey is a byproduct of the dairy industry.

The whey is a dilute solution of lactalbumin, lactose, fats, and the soluble inorganics from milk. Dried whey solids typically have the following composition.

Protein 12.0%

Fat 0.7%

Lactose 60.0%

Phosphorus 0.79%

Calcium 0.87% Ash 9.7%

Another source of carbohydrate is derived from the pulp and paper industry which produces large quantities of byproduct lignin sulfonates from wood during the sulfite pulping process. The carbohydrate byproduct is a constituent of the spent sulfite liquor.

3. aminoacid ingredients either singly or in combination which include arginine, histidine, isoleucine, leucine, lysine, methionine, phenylalanine, threonine, tryptophan, valine, tyrosine ethyl HCl, alanine, aspartic acid, sodium glutamate, glycine, proline, serine, cysteine ethyl HCl, and the like, and analogs and salts thereof. 4. vitamin ingredients either singly or in combination which include thiamine HCl, riboflavin, pyridoxine HCl, niacin, niacinamide, inositol, choline chloride, calcium pantothenate, biotin, folic acid, ascorbic acid, vitamin B₁₂, p-aminobenzoic acid, vitamin A acetate, vitamin K, vitamin D, vitamin E, and the like.

Trace element ingredients include compounds of cobalt, copper, manganese, iron, zinc, tin, nickel, chromium, molybdenum, iodine, chlorine, silicon, vanadium, selenium, calcium, magnesium, sodium and potassium.

5. protein ingredients as obtained from sources such as dried blood or meat meal, dried and sterilized animal and poultry manure, fish meal, liquid or powdered egg, fish solubles, cell cream, and the like.

Protein equivalent ingredients include non-protein nitrogen compounds such a urea, biuret, ammonium phosphate, and the like.

6. medicament ingredients either singly or in combination which include promazine hydrochloride, chloromadionate acetate, chlortetracycline, sulfamethazine, monensin, sodium monensin, poloxaline, and the like. Oxytetracycline is a preferred antibiotic for cattle prophylaxis.

7. antioxidants as illustrated by butylated hydroxyanisole, butylated hydroxytoluene, tocopherol, tertiary-butylhydroquinone, propyl gallate, and ethoxyquin; and suitable preservatives include sodium sorbate, potassium sorbate, sodium benzoate, propionic acid, α-hydroxybutyric acid, and the like.

8. suspension stabilizing agents which preferably are selected from nonionic surfactants, hydrocolloids and cellulose ethers. These types of chemical agents are illustrated by polyethylene oxide condensates of phenols, C₈-C₂₂ alcohols and amines; ethylene oxide reaction products with fatty acid partial esters of hexitans; alkylarylpolyoxy- ethylene glycol phosphate esters; gum arabic; carob bean gum; guar gum; tragacanth gum; ammonium, sodium, potassium and calcium alginates; glycol alginates; xanthan gum; potato agar; alkylcellulose; hydroxyalkylcellulose; carboxyalkylcellulose; and the like.

An invention process embodiment can be conducted in a batch reactor, or as a continuous operation with equipment similar to that described in U.S. 4,826,694. When conducted in a batch or continuous mode, a preferred aspect of the process is an amassment of the reactive admixture in a deep bed or heaped mound configuration, i.e., a bed or mound which is at least 10 inches in depth. The compact bulk of the reactive admixture solids minimizes loss of exothermic heat which is generated during the oilseed oil hydrolysis and salt-forming reactions. Maintenance of the reactive admixture temperature in a range between about 80°-130°C promotes the saponification reaction toward completion, and moderates denaturation of the oilseed protein ingredient.

In one type of continuous process, particulate whole oilseed and basic alkaline earth metal compound and basic alkali metal compound are blended in a continuous mixer and sparged with steam (125°-170°C) to form a hydrated reactive admixture. The admixture is transferred to a slow moving conveyor belt, in the form of a heaped mound which is about 20 inches or more in depth. Because of the reactive admixture compact bulk on the conveyor belt, the process effectively has the advantages of a continuous mode, and inherently has some attributes of a batch procedure. It is a type of continuous batch process.

The elevated temperature and alkaline pH conditions of an invention process embodiment are favorable for controlled denaturation of water- soluble proteins into water-insoluble proteins. Water-soluble proteins do not have rumen-bypass properties, and normally are digested in the rumen. Water-insoluble proteins have rumen-bypass properties, and normally are not digested in the rumen. The water-insoluble protein content of a present invention ruminant dietary supplement is metabolized in the post-rumen digestive tract of ruminants. The conditions of temperature and alkaline pH are moderate with respect to protein denaturation in the practice of the invention process. If the process conditions are overly severe, some of the protein converts into an intractable derivative which bypasses the digestive system of a ruminant and is lost as waste matter.

A further advantage derives from the temperature and alkaline pH conditions of the invention process. Any mycotoxins which are present in the whole oilseed starting material are partially or completely detoxified. An aflatoxin-contaminated oilseed meal can be completely detoxified under the invention processing conditions. In another embodiment this invention provides a process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, and (b) between about 1-3 equivalents of basic alkaline earth metal compound per equivalent of oilseed fatty acid content, wherein the reactive admixture has a water content between about 0.2-20 weight percent; and (2) maintaining the admixture at a temperature between about 40°-130°C for a time period sufficient to convert at least 70 percent of the total fatty acid content to fatty acid alkaline earth metal salt, and to denature the protein to a water-insoluble content of at least 60 percent of the protein, thereby providing a ruminant dietary product having rumen-bypass properties.

In another embodiment this invention provides a rumen-bypass dietary supplement for animals which comprises (1) between about

20-50 weight percent of at least two C₁₂-C₂₂ fatty acid alkaline earth metal salts; (2) between about 10-45 weight percent of water-insoluble vegetable protein; and (3) between about 0.1-10 weight percent of glycerol; wherein the fatty acid salt and protein ingredients are metabolized in the post-rumen digestive tract under ruminant feeding conditions.

In another embodiment this invention provides a process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 1.0-3.0 equivalents of basic alkali metal compound per equivalent of oilseed fatty acid content, and (c) between about 10-80 weight percent of an aqueous medium, based on the admixture weight; (2) maintaining the admixture at a temperature between about 25°-110°C for a time period sufficient to convert at least about 60 percent of the oilseed oil content to fatty acid alkali metal salt; (3) blending the admixture with between about 0.8-2 equivalents of basic alkaline earth metal compound per equivalent of total fatty acid content in the admixture; and (4) maintaining the admixture at a temperature between about 60°-120°C for a time period sufficient to convert at least about 70 percent of the total fatty acid content to fatty acid alkaline earth metal salt, to provide a ruminant dietary product having rumen- bypass properties. In a further embodiment the present invention provides a process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 1.0-3.0 equivalents of basic alkali metal compound per equivalent of oilseed fatty acid content, and (c) between about 10-80 weight percent of an aqueous medium, based on the admixture weight;

(2) maintaining the admixture at a temperature between about 25°C-110°C for a time period sufficient to convert at least about 60 percent of the oilseed oil content to fatty acid alkali metal salt; (3) blending the admixture with between about 0.8-2 equivalents of basic alkaline earth metal compound per equivalent of total fatty acid content in the admixture; (4) maintaining the admixture at a temperature between about 60°-120°C for a time period sufficient to convert at least about 70 percent of the total fatty acid content to fatty acid alkaline earth metal salt; and (5) acid treating the admixture medium to a pH of about 7-9, to provide a ruminant dietary product having rumen- bypass properties.

The suspension medium obtained after the step (2) oilseed oil saponification reaction can be retained and stored, and subsequently blended with the step (3) basic alkaline earth metal compound in a separate operation. As demonstrated in Example VI, the aqueous suspension medium intermediate of step (2) has utility as a convenient feed stream for supplementing a continuous fatty acid alkaline earth salt manufacturing process for production of an animal feedstuff supplement.

A present invention dietary fatty acid salt/denatured protein composition is adapted to function as a rumen-bypass dietary supplement in ruminant feed. An important advantage of a present invention dietary supplement product is the rumen- bypass protection which extends to all the biologically active ingredients of the product, such as aminoacids, vitamins, and the like, which normally are metabolized in the rumen.

The following examples are further illustrative of the present invention. The components and specific ingredients are presented as being typical, and various modifications can be derived in view of the foregoing disclosure within the scope of the invention.

EXAMPLE I This Example illustrates the continuous production of a rumen-bypass dietary fatty acid calcium salt/denatured protein product in accordance with the present invention.

Whole rapeseed meal is employed which contains about 40% oil and 27% protein. The protein content of the whole rapeseed meal starting material has a molar profile of aminoacids comprising arginine (7.2), histidine (3.2), lysine (5.4), tryptophan (2.5), phenylalanine (5.0), methionine (1.5), threonine (4.8), leucine (8.7), isoleucine (4.5), valine (6.5) and aspartic acid (11.0).

The oil content of the whole rapeseed meal starting material has a weight percent profile of fatty acids comprising oleic acid (63) , linoleic acid (20) , linolenic acid (9) , palmitic acid (5) and stearic acid (2) .

The process is operated continuously with equipment consisting of an elongated high shear mixer, in combination with a slow moving conveyor belt.

The whole rapeseed meal is introduced into the mixer from a hopper near the front end of the mixer. A mixture of calcium oxide and sodium hydroxide is introduced into the mixer from a second hopper which is adjacent to the first hopper, and the mixer is operated at a shear rate of about 1000 rpm. Near the midpoint of the mixer length, steam (150°C) is introduced into the mixer to hydrate the blended ingredients in the mixer, and to raise the temperature of the blend. The quantity of calcium oxide is about

60 lbs., and the quantity of sodium hydroxide is about 50 lbs., per 1000 lbs. of whole rapeseed meal. The steam sparging is at a rate which adds water to a total content of about 10 weight percent of the blended admixture prior to the discharge of the admixture onto the conveyor belt.

The admixture has a temperature of about 80°C as it is discharged in a heaped mound (about 20 inches deep) on the moving conveyor belt. The compact bulk of the heaped admixture minimizes heat loss as the exothermic rapeseed oil saponification reaction is proceeding. The temperature of the admixture increases to about 110°-130°C, and is maintained at this temperature for about 50 minutes on the moving conveyor belt.

The essentially dry fatty acid calcium salt/denatured protein product is cooled, passed through a sifter, and collected in bags suitable for transportation and storage. The temperature conditions of the process are sufficient to inactivate any mycotoxins originally present in the whole rapeseed starting material. The protein content of the whole rapeseed meal starting material consists of about 70 weight percent water-soluble constituents which are digestible in the rumen. The protein content of the ruminant dietary product of the process consists of about 15 weight percent of water-soluble constituents which are digestible in the rumen, and about 85 weight percent of water-insoluble constituents which bypass the rumen and are metabolized in the post-rumen digestive tract of a ruminant.

The ruminant dietary product contains about 80 weight percent of the total fatty acid content in the form of metal salt.

EXAMPLE II This Example illustrates the continuous production of a rumen-bypass dietary fatty acid calcium salt/denatured protein product in accordance with the present invention.

The oil content of the whole rapeseed meal starting material has a molar profile of fatty acids comprising oleic acid (63), linoleic acid (20), linolenic acid (9) , palmitic acid (5) and stearic acid (2) .

The high shear mixer has an alignment of two hoppers and a liquid feed pipe positioned between them at the front end of the mixer.

The whole rapeseed meal is fed into the mixer from the first hopper, a heated stream of palm fatty acid distillate (90°C) is introduced from the liquid feed pipe, and a mixture of calcium oxide and sodium hydroxide is fed into the mixer from the second hopper. The mixer is operated at a shear rate of about 1000 rpm. Near the midpoint of the mixer length, steam (150°C) is introduced into the mixer to hydrate the blended ingredients in the mixer, and to raise the temperature of the blend.

The quantity of palm fatty acid distillate is about 200 lbs. per 1000 lbs. of whole rapeseed meal.

The quantity of calcium oxide is about 60 lbs. per 1000 lbs. of whole rapeseed meal, and about 20 lbs. per 200 lbs. of palm fatty acid distillate.

The quantity of sodium hydroxide is about 50 lbs. per 1000 lbs. of whole rapeseed meal, and about 15 lbs. per 200 lbs. of palm fatty acid distillate.

The steam sparging is at a rate which adds water to a total content of about 10 weight percent of the blended admixture prior to the discharge of the admixture onto the conveyor belt.

The admixture has a temperature of about 90°C as it is discharged in a heaped mound (about 20 inches deep) on the moving conveyor belt. The compact bulk of the heaped admixture minimizes heat loss as the exothermic rapeseed oil saponification reaction is proceeding. The temperature of the admixture increases to about 110°-130°C, and is maintained at this temperature for about 50 minutes on the moving conveyor belt. The essentially dry fatty acid calcium salt/denatured protein product is cooled, passed through a sifter, and collected in bags suitable for transportation and storage. The temperature conditions of the process are sufficient to inactivate any mycotoxins originally present in the whole rapeseed starting material.

The protein content of the whole rapeseed meal starting material consists of about 70 weight percent water-soluble constituents which are digestible in the rumen. The protein content of the ruminant dietary product of the process consists of about 15 weight percent of water-soluble constituents which are digestible in the rumen, and about 85 weight percent of water-insoluble constituents which bypass the rumen and are metabolized in the post-rumen digestive tract of a ruminant. The dietary product has about 90 weight percent of the total fatty acid content in the form of metal salt.

The process is repeated with whole soybean meal starting material instead of whole rapeseed meal. The protein of the whole soybean meal starting material has a molar profile of aminoacids comprising arginine (8.3), histidine (2.6), lysine (6.8), tryptophan (1.0), phenylalanine (5.0), methionine (1.0), threonine (3.9), leucine (7.5), isoleucine (6.5), valine (5.5) and aspartic acid (6.2) . The oil content of the whole soybean meal starting material has a weight percent profile of fatty acids comprising linoleic acid (52) , oleic acid (25), palmitic acid (12), linolenic acid (6), stearic acid (4) and lauric acid (0.5).

The process is repeated with whole cottonseed meal instead of whole rapeseed meal. The protein content of the whole cottonseed meal starting material has a molar profile of aminoacids comprising arginine (10.9), histidine (2.8), lysine (3.9), tryptophan (0.9), phenylalanine (4.9), methionine (1.7), threonine (3.4), leucine (4.5), isoleucine (3.2), valine (4.1) and aspartic acid (10.0) . The oil content of the whole cottonseed meal starting material has a weight percent profile of fatty acids comprising linoleic acid (55) , palmitic acid (24), oleic acid (17), stearic acid (2), myristic acid (0.7) and linolenic acid (0.3). Each of the three process embodiments described above is repeated, except that methionine hydroxy analog is added as an ingredient during the blending stage. The added quantity provides about 2.0 weight percent of methionine hydroxy analog in the ruminant dietary product.

If the process embodiments are conducted with a bed or heaped mound of reactive admixture on the conveyor belt which is about 5 inches in depth, then the saponification of oilseed oil is less complete, and the amount of water-insoluble constituents in the protein content of the dietary supplement endproduct is about 40 weight percent. An invention fatty acid calcium salt/protein product, such as that derived from whole rapeseed and palm fatty acid distillate as illustrated above, can be incorporated as a dietary supplement in cattle feed such as hay silage or corn silage, in a quantity which will provide each animal about 1000 grams per day of fatty acid salt, and about 500 grams per day of denatured protein.

EXAMPLE III This Example illustrates the continuous production of a rumen-bypass dietary fatty acid calcium salt/denatured protein product in accordance with the present invention.

The oil content of the whole rapeseed meal starting material has a weight percent profile of fatty acids comprising oleic acid (63) , linoleic acid (20) , linolenic acid (9) , palmitic acid (5) and stearic acid (2).

The whole rapeseed meal is introduced into the mixer from a hopper near the front end of the mixer. Calcium oxide is introduced into the mixer from a second hopper which is adjacent to the first hopper, and the mixer is operated at a shear rate of about 1000 rpm. Near the midpoint of the mixer length, steam (150°C) is introduced into the mixer to hydrate the blended ingredients in the mixer, and to raise the temperature of the blend.

The quantity of calcium oxide is about 60 lbs. per 1000 lbs. of whole rapeseed meal. The steam sparging is at a rate which adds water to a total content of about 10 weight percent of the blended admixture prior to the discharge of the admixture onto the conveyor belt. The admixture has a temperature of about

80°C as it is discharged in a heaped mound (about 20 inches deep) on the moving conveyor belt. The compact bulk of the heaped admixture minimizes heat loss as the exothermic rapeseed oil saponification reaction is proceeding. The temperature of the admixture increases to about 110°-120°C, and is maintained at this temperature for about 75 minutes on the moving conveyor belt.

The essentially dry fatty acid calcium salt/denatured protein product is cooled, passed through a sifter, and collected in bags suitable for transportation and storage.

The temperature conditions of the process are sufficient to inactivate any mycotoxins originally present in the whole rapeseed starting material.

The protein content of the whole rapeseed meal starting material consists of about 70 weight percent water-soluble constituents which are digestible in the rumen. The protein content of the ruminant dietary product of the process consists of about 30 weight percent of water-soluble constituents which are digestible in the rumen, and about 70 weight percent of water-insoluble constituents which bypass the rumen and are metabolized in the post-rumen digestive tract of a ruminant.

The ruminant dietary product contains about 80 weight percent of the total fatty acid content in the form of calcium salt.

The process is repeated with whole soybean meal starting material instead of whole rapeseed meal. The protein of the whole soybean meal starting material has a molar profile of aminoacids comprising arginine (8.3), histidine (2.6), lysine (6.8), tryptophan (1.0), phenylalanine (5.0), methionine (1.0), threonine (3.9), leucine (7.5), isoleucine (6.5), valine (5.5) and aspartic acid (6.2) . The oil content of the whole soybean meal starting material has a weight percent profile of fatty acids comprising linoleic acid (52), oleic acid (25), palmitic acid (12), linolenic acid (6), stearic acid (4) and lauric acid (0.5). The process is repeated with whole cottonseed meal instead of whole rapeseed meal. The protein content of the whole cottonseed meal starting material has a molar profile of aminoacids comprising arginine (10.9), histidine (2.8), lysine (3.9), tryptophan (0.9), phenylalanine (4.9), methionine (1.7), threonine (3.4), leucine (4.5), isoleucine (3.2), valine (4.1) and aspartic acid (10.0) .

The oil content of the whole cottonseed meal starting material has a weight percent profile of fatty acids comprising linoleic acid (55), palmitic acid (24), oleic acid (17), stearic acid (2), myristic acid (0.7) and linolenic acid (0.3). Each of the three process embodiments described above is repeated, except that methionine hydroxy analog is added as an ingredient during the blending stage. The added quantity provides about 2.0 weight percent of methionine hydroxy analog in the ruminant dietary product. If the process embodiments are conducted with a bed or heaped mound of reactive admixture on the conveyor belt which is about 6 inches or less in depth, then the saponification of oilseed oil is less complete, and the amount of water-insoluble constituents in the protein content of the dietary supplement endproduct is about 40 weight percent.

An invention fatty acid calcium salt/protein product, such as that derived from whole rapeseed as illustrated above, can be incorporated as a dietary supplement in cattle feed such as hay silage or corn silage, in a quantity which will provide each animal about 1000 grams per day of fatty acid salt, and about 500 grams per day of denatured protein. EXAMPLE IV This Example illustrates the alkaline treatment of whole soybean meal to produce an aqueous suspension medium which contains fatty acid salt and denatured protein.

Whole soybean which contains 18% oil and 36% protein is ground into a meal by passage of the whole soybean through a mix mill with a 3/16" screen. A ribbon band mixer is filled with

30 gallons of water at a temperature of 60°C. Sodium hydroxide pellets (6 lbs) are added to the water, and stirring is commenced. Whole soybean meal (155 lbs) is added to the alkaline aqueous medium, and stirring is continued until saponification of the soybean oil is completed (2 hours) .

The aqueous suspension medium has a content of fatty acid sodium salt, water-insoluble denatured protein, and glycerol.

The protein of the whole soybean meal starting material has a molar profile of aminoacids comprising arginine (8.3), histidine (2.6), lysine (6.8), tryptophan (1.0), phenylalanine (5.0), methionine (1.0), threonine (3.9), leucine (7.5), isoleucine (6.5), valine (5.5) and aspartic acid (6.2) . The procedure is repeated with whole cottonseed instead of whole soybean. The protein content of the whole cottonseed meal starting material has a molar profile of aminoacids comprising arginine (10.9), histidine (2.8), lysine (3.9), tryptophan (0.9), phenylalanine (4.9), methionine (1.7), threonine (3.4), leucine (4.5), isoleucine (3.2), valine (4.1) and aspartic acid (10.0). The procedure is repeated with whole rapeseed instead of whole soybean. The protein content of the whole rapeseed meal starting material has a molar profile of aminoacids comprising arginine (7.2), histidine (3.2), lysine (5.4), tryptophan (2.5), phenylalanine (5.0), methionine (1.5), threonine (4.8), leucine (8.7), isoleucine (4.5), valine (6.5) and aspartic acid (11.0).

EXAMPLE V This Example illustrates the preparation of mixtures of fatty acid salt and denatured protein from whole oilseed meal. Whole rapeseed which contains 40% oil and

27% protein is ground in a Bauer Mill with water using a 3:1 water to rapeseed weight ratio to yield a slurry of whole rapeseed meal.

A portion of the slurry (1550 g of rapeseed meal) is charged to a ribbon band mixer, and potassium hydroxide pellets (120 g) are added. Stirring is commenced, and continued until saponification of the rapeseed oil is completed at ambient temperature (about 72 hours) . The aqueous suspension medium has a content of fatty acid potassium salt, water- insoluble denatured protein, and glycerol.

A. One liter of the aqueous suspension medium is transferred to a Berk ring dryer, and the water is removed to provide a dry solids product.

B. A second liter of the aqueous suspension medium is placed in a reactor, and calcium oxide (15 g) is added. The reaction mixture is heated to 60°C, and the reaction mixer temperature is maintained for about two hours with stirring.

The product aqueous suspension medium has a content of fatty acid calcium salt, water- insoluble denatured protein, glycerol, and potassium hydroxide. The pH of the aqueous suspension medium is about 11.

A portion of the product aqueous suspension medium (500 ml) is neutralized with hydrochloric acid to a pH of 7-8, and the suspension medium is dried under vacuum to yield a dry solids fatty acid calcium salt/denatured protein product which has utility as a ruminant dietary supplement product having rumen-bypass properties.

EXAMPLE VI

This Example illustrates the continuous production of a rumen by-pass dietary fatty acid calcium salt/denatured protein product in accordance with the present invention.

The fatty acid component is a palm fatty acid distillate of the following composition:

Lauric acid 2.3%

Palmitic acid 49.9%

Stearic acid 5.4%

Oleic acid 35.0%

Linoleic acid 7.4%

The process is operated continuously with equipment which is essentially the same as described and illustrated with reference to Fig. 1 of U.S. 4,826,694 by W. McAskie.

Calcium oxide from a hopper and hot palm oil distillate (96°C) from a supply line are mixed in predetermined proportions in a mixing pump. An aqueous suspension medium is added to the reactant admixture via a supply line.

The aqueous suspension medium is an admixture prepared by a procedure similar to that described in Example I. The aqueous suspension medium contains about one pound of fatty acid sodium salt and about two pounds of protein per gallon of aqueous medium. Water is supplied to the continuous process at a rate of about 20 weight percent, based on the total weight of fatty acid components. The calcium oxide is supplied to the continuous process in a quantity of 1.2 equivalents per equivalent of palm oil fatty acid and the fatty acid sodium salt in the added aqueous suspension medium.

The hydrated mixture formed in the continuous process is passed through a mixing pump and the resultant semi-liquid reaction medium at about 100°C is discharged as a spread layer onto a continuously moving conveyor belt. Steam evolves from the conveyor transported reaction mass.

At the end of the conveyor belt solid lumps of reaction product fall through a sizing machine onto a second conveyor belt. In this conveying zone the salt-forming reaction and evolution of water proceed to completion. The essentially dry fatty acid calcium salt/denatured protein product is passed through a sifter, and collected in bags suitable for transportation and storage.

The residence time on the first conveyor is about 30 minutes, and the overall production time from reactant mixing to collection of the dry granulated product is about 2.5 hours. The final product has a fatty acid calcium salt content of 73 weight percent, a denatured protein content of about 12 weight percent, and a water content of about 5 weight percent. The invention fatty acid calcium salt/protein product can be incorporated as a dietary supplement in cattle feed such as hay silage or corn silage, in a calculated quantity which will provide each animal about 1000 grams per day of fatty acid salt, and about 165 grams per day of denatured protein.

Claims

WHAT IS CLAIMED IS:

1. A process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 1-3 equivalents of basic alkaline earth metal compound per equivalent of oilseed fatty acid content, and (c) between about 0.1-1.5 equivalents of basic alkali metal compound per equivalent of oilseed fatty acid content, wherein the reactive admixture has a water content between about 0.2-20 weight percent; and (2) maintaining the admixture at a temperature between about 30°-130°C for a time period sufficient to convert at least about 75 percent of the total fatty acid content to fatty acid metal salt, and to denature the protein to a water-insoluble content of at least about 65 percent of the protein, thereby providing a ruminant dietary product having rumen-bypass properties.

2. A process in accordance with claim 1 wherein the oilseed ingredient has an oil content between about 15-50 weight percent, and a protein content between about 20-60 weight percent.

3. A process in accordance with claim 1 wherein the basic alkaline earth metal compound is an oxide or hydroxide of calcium or magnesium, or a mixture of compounds.

4. A process in accordance with claim 1 wherein the basic alkali metal compound is a hydroxide, carbonate, bicarbonate or phosphate of sodium or potassium metal, or a mixture of compounds.

5. A process in accordance with claim 1 wherein the step (1) blending procedure includes between about 0.05-20 weight percent of an additional biologically active ingredient, based on the weight of the recovered dietary product.

6. A process in accordance with claim 1 wherein in step (2) the reactive admixture is sparged with steam to heat the admixture to a temperature between about 80°-130°C.

7. A ruminant dietary product produced by the process of claim 1.

8. A ruminant dietary product produced by the process of claim 1, which has been acid treated in an aqueous medium to a pH of about 7-9.

9. A ruminant dietary product produced by the process of claim 1, which has been contacted with an aqueous medium to remove water-soluble alkali metal compounds by extraction.

10. A process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 5-60 weight percent of at least one C_u-C₂₂ fatty acid ingredient, based on the weight of oilseed fatty acid content, (c) between about 1-3 equivalents of basic alkaline earth metal compound per equivalent of total fatty acid content, and (d) between about

11. A process in accordance with claim 10 wherein the oilseed ingredient has an oil content between about 15-50 weight percent, and a protein content between about 20-60 weight percent.

12. A process in accordance with claim 10 wherein the C_u-C₂₂ fatty acid ingredient is palm fatty acid distillate.

13. A process in accordance with claim 10 wherein the basic alkaline earth metal compound is an oxide or hydroxide of calcium or magnesium, or a mixture of compounds.

14. A process in accordance with claim 10 wherein the basic alkali metal compound is a hydroxide, carbonate, bicarbonate or phosphate of sodium or potassium metal, or a mixture of compounds.

15. A process in accordance with claim 10 wherein the step(l) blending procedure includes between about 0.05-20 weight percent of an additional biologically active ingredient, based on the weight of the recovered dietary product.

16. A process in accordance with claim 10 wherein in step(2) the reactive admixture is sparged with steam to heat the admixture to a temperature between about 80°-130^βC.

17. A ruminant dietary product produced by the process of claim 10.

18. A ruminant dietary product produced by the process of claim 10, which has been acid treated in an aqueous medium to a pH of about 7-9.

19. A ruminant dietary product produced by the process of claim 10, which has been contacted with an aqueous medium to remove water-soluble alkali metal compounds by extraction.

20. A process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, and (b) between about 1-3 equivalents of basic alkaline earth metal compound per equivalent of oilseed fatty acid content, wherein the reactive admixture has a water content between about 0.2-20 weight percent; and (2) maintaining the admixture at a temperature between about 40°-130°C for a time period sufficient to convert at least 70 percent of the total fatty acid content to fatty acid alkaline earth metal salt, and to denature the protein to a water- insoluble content of at least 60 percent of the protein, thereby providing a ruminant dietary product having rumen-bypass properties.

21. A process in accordance with claim 20 wherein the oilseed ingredient has an oil content between about 15-50 weight percent, and a protein content between about 20-60 weight percent.

22. A process in accordance with claim 20 wherein the basic alkaline earth metal compound is an oxide or hydroxide of calcium or magnesium, or a mixture of compounds.

23. A process in accordance with claim 20 wherein the step(l) blending procedure includes between about 0.05-20 weight percent of an additional biologically active ingredient, based on the weight of the recovered dietary product.

24. A process in accordance with claim 20 wherein in step(2) the reactive admixture is sparged with steam to heat the admixture to a temperature between about 80°-130°C.

25. A ruminant dietary product produced by the process of claim 20.

26. A rumen-bypass dietary supplement for animals which comprises (1) between about 20-50 weight percent of at least two C₁₂-C₂₂ fatty acid alkaline earth metal salts; (2) between about

10-45 weight percent of water-insoluble vegetable protein; and (3) between about 0.1-10 weight percent of glycerol; wherein the fatty acid salt and protein ingredients are metabolized in the post-rumen digestive tract under ruminant feeding conditions.

27. A ruminant dietary supplement in accordance with claim 26 which contains between about 0.05-20 weight percent of an additional biologically active ingredient.

28. A process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 1.0-3.0 equivalents of basic alkali metal compound per equivalent of oilseed fatty acid content, and (c) between about 10-80 weight percent of an aqueous medium, based on the admixture weight;

(2) maintaining the admixture at a temperature between about 25°-110°C for a time period sufficient to convert at least about 60 percent of the oilseed oil content to fatty acid alkali metal salt;

(3) blending the admixture with between about 0.8-2 equivalents of basic alkaline earth metal compound per equivalent of total fatty acid content in the admixture; and (4) maintaining the admixture at a temperature between about 60°-120°C for a time period sufficient to convert at least about 70 percent of the total fatty acid content to fatty acid alkaline earth metal salt, to provide a ruminant dietary product having rumen-bypass properties.

29. A process in accordance with claim 28 wherein the oilseed ingredient has an oil content between about 15-45 weight percent, and a protein content between about 20-40 weight percent.

30. A process in accordance with claim 28 wherein the basic alkali metal compound is a hydroxide, carbonate, bicarbonate or phosphate of sodium or potassium metal, or a mixture of compounds.

31. A process in accordance with claim 28 wherein the basic alkaline earth metal compound is an oxide or hydroxide of calcium or magnesium, or a mixture of compounds.

32. A process in accordance with claim 28 wherein the step (3) blending procedure includes between about 0.05-20 weight percent of an additional biologically active ingredient, based on the weight of the recovered dietary product.

33. A ruminant dietary product produced by the process of claim 28.

34. A process for the preparation of a fatty acid salt and denatured protein ruminant dietary product which comprises (1) forming a ^' reactive admixture of ingredients comprising (a) whole proteinaceous oilseed ingredient in comminuted form, (b) between about 1.0-3.0 equivalents of basic alkali metal compound per equivalent of oilseed fatty acid content, and (c) between about 10-80 weight percent of an aqueous medium, based on the admixture weight; (2) maintaining the admixture at a temperature between about 25°C-110°C for a time period sufficient to convert at least about 60 percent of the oilseed oil content to fatty acid alkali metal salt; (3) blending the admixture with between about 0.8-2 equivalents of basic alkaline earth metal compound per equivalent of total fatty acid content in the admixture; (4) maintaining the admixture at a temperature between about 60°-120°C for a time period sufficient to convert at least about 70 percent of the total fatty acid content to fatty acid alkaline earth metal salt; and (5) acid treating the admixture medium to a pH of about 7-9, to provide a ruminant dietary product having rumen- bypass properties.

35. A ruminant dietary product produced by the process of claim 34.