Patent Grant
7201934
Cocoa beans are processed in large volumes into a wide variety of chocolate-related products. For example, cocoa beans can be initially processed into cocoa nibs and then into cocoa liquor, which then is further processed to separate the liquor into its cocoa butter and cocoa powder constituents. To separate cocoa butter from cocoa powder, conventional mechanical pressing of the cocoa liquor is typically used. The initial result of mechanical pressing is a press cake of cocoa solids which retains residual cocoa butter. This press cake can be cooled, milled, and classified into the cocoa powder, which still contains residual cocoa butter. The amount of residual cocoa butter can be, for example, about 10–12 wt. % (so called “10/12 cocoa powder”).
Cocoa powder can be used in many products. One major use, for example, is in beverages including drinking chocolate, chocolate-flavored milk, and instant drinks from vending machines and other sources. In these applications, ideally the powder should instantly disperse when mixed with a cold aqueous medium such as milk. However, cocoa powder is not easily wetted which can impede dispersion and result in lumping. The difficulty is exacerbated if the powder contains fat, such as residual cocoa butter, or if the dispersion is to take place in a cold liquid.
In the past, lecithination has been used to address this dispersibility problem. In this approach, cocoa powders have been further processed to include a dispersing agent such as lecithin, the dispersing agent acting as a surface active agent to reduce surface tension between the powder and the water-based liquid. Lecithin can be added at a level of about 5 wt. %. Government regulation may limit the amount of lecithin which can be added. Current lecithination technology, however, suffers from at least four disadvantages including:
(1) increased cost. Depending on cocoa powder prices, lecithin represents a considerable ingredient cost, particularly where customers demand GMO-free soya lecithin.
(2) inefficient delivery of the lecithin. Because current procedures for lecithination can be relatively inefficient, depending on a number of factors, high levels of lecithin are incorporated to achieve the dispersion behavior required of the cocoa powder. In addition to increasing cost, high levels of lecithin also can impart off-flavors, requiring the formulator to use more refined (and hence more expensive) versions.
(3) increased total fat. Lecithin is a fatty substance which becomes part of the total fat as reported in NLEA labeling requirements. Therefore, a 10/12 cocoa powder containing 5 wt. % lecithin will in fact display considerably higher values for total fat content and calories from fat per serving.
(4) issues concerning shelf life arise.
Hence, improved lecithination procedures are needed. Moreover, lecithination needs to be adapted to new procedures for production of cocoa powder. For example, liquefied gas extraction has been recently reported as an alternative to mechanical pressing to separate cocoa liquor into its cocoa butter and cocoa powder constituents as disclosed in, for example, U.S. Pat. Nos., 6,066,350 and 6,361,814. In a preferred embodiment of this process, cocoa liquor is mixed with liquefied, pressurized butane to form a slurry, and the slurry is subjected to separation on, for example, a belt filter. The belt filter retains wet cocoa solids as solvent passes through the belt filter extracting cocoa butter. The remaining wet cocoa solids, which usually retain some cocoa butter and forms a cocoa mass, are processed into cocoa powder by, among other things, breaking up any clumped particles and removing solvent (desolventization).
The present application is directed to a novel method for processing cocoa comprising the step of adding a dispersing agent such as, for example, lecithin, to a cocoa mass comprising solvent. This results, surprisingly, in improved, more uniform mixing between the cocoa mass and the dispersing agent. Advantages include lower costs, more flexibility in choice of dispersing agents, and lower fat content. The cocoa mass can be provided by reducing the fat content of cocoa mass with use of, for example, liquefied gas extraction and a belt filter to effect separation of cocoa butter. After mixing with the dispersing agent, the cocoa mass can be desolventized to yield a cocoa powder which comprises the dispersing agent. The amount of dispersing agent in the cocoa powder can be relatively low such as, for example, only about 0.5 wt. %. If desired, the cocoa powder can be further agglomerated or instantized. In one embodiment, low calorie products are prepared. Finally, improved, dispersible cocoa powder compositions are provided which are prepared by these methods.
Unless otherwise indicated, the word “a” in the present application is not exclusively limited to mean “only one” but inclusively to mean “at least one.”
Unless otherwise indicated, the term “cocoa mass” is used to refer to a material which includes cocoa fat and solids. One example of a “cocoa mass” would be ground cocoa nibs, before later processing, whether dutched or not. The term “cocoa liquor” is used herein to refer to cocoa mass which results from grinding cocoa nibs (whether dutched or not) but which has not been modified with respect to fat content (typically 50% or greater). Thus, as the terms are used herein, a “cocoa liquor” is one type of “cocoa mass.” The term “cocoa mass” is also intended to include within its scope material that is the result of modifying cocoa liquor. The term “wet cocoa mass” as used herein refers to a material which includes cocoa fat, cocoa solids and solvent.
Unless otherwise indicated, the phrase “suitable for human consumption of a food product” means that the composition is generally recognized as safe for eating and drinking and as not being toxic, poisonous, or otherwise harmful to humans when used in functionally useful amounts in solid and liquid food products.
Unless otherwise indicated, the phrases “uniform mixing” or “uniformly mixed” means that the majority of particles are coated with at least some dispersing agent.
Unless otherwise indicated, “functionally useful fast dispersion” means that an individual consumer is able to rapidly, in seconds, disperse the cocoa powder in the aqueous media without lumping by stirring with gentle shaking or a conventional stirring device such as a spoon or plastic rod.
Background references disclosing cocoa technology include, for example, Industrial Chocolate Manufacture and Use, 2nd Ed., Ed. S. T. Beckett, Blackie Academic, 1994; and Chocolate, Cocoa, and Confectionery: Science and Technology, 3rd Ed., B. Minifie, Van Nostrand, 1989. For example, these references discuss methods for converting raw cocoa products into cocoa mass and cocoa liquor.
A liquor extraction process can be carried out with liquid solvent, wherein the solvent is either a liquid or gas at room temperature and pressure (RTP). Liquid solvents at RTP include C6–C8 saturated alkanes such as, for example, hexane, including n-hexane and all isomers thereof (e.g., isohexane). If the solvent is a gas at RTP, the solvent is liquefied before extraction. The liquefied solvent can be, for example, saturated hydrocarbons including propane, butane, pentane, and all isomers thereof including n-butane, isobutane, n-propane, n-pentane, and isopentane. For example, the solvent can comprise at least 90% by wt. butane. Solvent molecular weight can be below 75. In addition, organic solvents such as, for example, esters and ketones and other oxygenated solvents can be used such as, for example, ethyl acetate.
Multiple references disclose liquefied gas extraction of cocoa liquor to separate cocoa butter from cocoa powder including, for example, U.S. Pat. Nos. 6,066,350; 6,361,814; and U.S. Patent Application Publication 2002/0006459 A1. These three references are incorporated herein by reference. The cocoa mass can be alkalized or non-alkalized depending on the desired application.
Conventional cocoa liquor particle sizes and distributions can be used, although relatively fine particle sizes are generally better such as, for example, mean particle sizes of about 7 microns to about 12 microns. More finely ground particle sizes can be generally useful for preparing cocoa powders having less than 1 wt. % remaining cocoa butter. In general, the particle size of the cocoa powder can be determined by the particle size of the cocoa liquor. Particle size distribution can be controlled to minimize formation of large particles and to avoid a gritty feel in the cocoa powder. Typically, 99.5% of the particles should pass through a 200 mesh screen, which means that the particles are smaller than 75 microns. Particle size distribution can be measured by methods known in the art including use of a laser defraction analyzer wherein cocoa liquor is suspended and sonicated in soybean oil in a container and then circulated over the cuvet/vial at an instrument detector. Measurements can be carried out with a Sympatec Helos-KA instrument using a low focal length lens (100 mm) when the cocoa particles consist mainly of fines. A typical cocoa powder has a steep bell-shaped curve with a mean size centered between 7–12 microns, and particle “tails” down to 0.1 micron and above 75 micron. Cocoa particle size distribution depends on parameters including grinding (e.g. combination of blade, stone, and ball mills), residence time, screening, and scalping and recycling of “overs.”
Coarse grind or flake cocoa mass can be used, although in general further grinding may be preferable.
Different types of mixers can be used to promote mixing between solvent and a cocoa mass, such as cocoa liquor. For example, static, passive, in-line, or dynamic mixers can be used to promote mixing. Fast mixing times before separation are preferred such as, for example, less than 120 seconds, including 30–110 seconds. Fast mixing can be achieved with use of, for example, static mixers including those available from Kenics.
The temperature after mixing can be, for example, 10–34° C., or alternatively, 35–60° C. In the latter temperature range, the cocoa butter is more fully softened and melted, which reduces liquor viscosity. However, the lower temperatures of the former range can provide advantages such as reduced operating pressure. Pressures can be adapted to keep solvent in the liquid or liquefied state.
In addition, the separation can be carried out with devices including, for example, a belt filter or centrifugation. Mixing and separation steps can be carried out continuously or batch-wise, although continuous operations are preferred.
The separation process results in cocoa mass which is wet with residual solvent which had been used to extract out the cocoa butter. In other words, in a typical application, cocoa liquor is defatted with the solvent to provide the cocoa mass wet with solvent. The wet cocoa mass can be removed from the separation medium for further processing and conversion to cocoa powder.
The dispersing agent which is added to the wet cocoa mass can be one or more conventional dispersing agents suitable for human consumption of food products, including drinks and chocolate products, when used in functionally useful amounts. It can function as an emulsifier, a surface active agent, and/or a wetting agent and generally improves dispersibility in aqueous media, such as cold and/or hot water and milk. The dispersing agent can be non-ionic or ionic, including anionic or cationic. It can be natural or synthetic, and preferably is relatively inexpensive. The dispersing agent can have both lipophilic and hydrophilic properties because of its molecular structure. Also, it can be in the form of a liquid, oil, or solid. It can have the capacity to be tightly bound to the particles of cocoa solids. Mixtures of dispersing agents can be used. Carriers for the dispersing agent may also be used.
The dispersing agent can be an esterified glycerol derivative, wherein the derivative is at least partially esterified with fatty acids and/or phosphate. The dispersing agent can be a monoglyceride, a diglyceride, or a triglyceride. General types of dispersing agents include surface active lipids, phospholipids, glycolipids, sorbitan esters of long chain saturated fatty acids, lactic acid or diacetyl tartaric acid esters of long chain saturated fatty acid monoglycerides, bile acids and salts including chenodeoxycholic acid derivatives, secondary deoxycholic acid derivatives, cephalin, plasmologens, animal or plant sterols, and phenolic and/or sucrose esters of long chain fatty acids.
In particular, the dispersing agent can be a lecithin-related compound including lecithin, modified lecithin, fractionated lecithin, as well as vegetable lecithin derived from vegetable sources such as, for example, soybean, safflower, corn, peanut, cotton seed, and rapeseed. Egg lecithin and deoiled lecithin can also be used. Chapter 4 of the Minifie text cited above discloses use of emulsifiers, including lecithin, in chocolate confectionary coatings and cocoa, and is hereby incorporated by reference. These emulsifiers can be used as dispersing agent. Soya lecithin, in particular, has many desirable qualities.
Chemical lecithin, which is phosphatidyl choline, is the main constituent of vegetable lecithin and can be used as dispersion agent. Page 112 of the above-noted Minifie text discloses that the approximate composition of commercial lecithin comprises the following ingredients: soyabean oil, phosphatidyl choline, phosphatidyl ethanolamine, inositol phosphatides, other phospholipids and polar lipids, carbohydrates including sterol glucoside, inositol, choline, tocopherol, biotin, folic acid, thiamin, riboflavin, pantothenic acid, pyridoxine, and niacin. The ingredients of lecithin can vary with the type of lecithin, as known to those skilled in the art.
Fractionated and modified vegetable lecithins are also known and can be used as dispersing agent. Lecithins can be modified to improve their hydrophilic properties. For example, hydroxylated lecithins can be prepared by treatment with hydrogen peroxide and lactic and acetic acid, which improves their hydrophilic properties. Modified lectithins can be used in conjunction with mono- and diglycerides. Fractionation of lecithin can be carried out by extraction of natural lecithin with alcohol to provide concentrates. Fractionated lecithins enriched in either phosphatidyl choline or phosphatidyl ethanolamine, or both can be used. Carriers can be added to these concentrates depending on their use. Carriers include, for example, cocoa butter or other vegetable oil and propylene glycol.
In addition to lecithin-related dispersing agents, synthetic phospholipids are also known and can be used as dispersing agent, and include one developed by Cadbury and called “YN.” YN is prepared from rapeseed oil and comprises ammonium salts of phosphatidic acids. In addition to YN, other phosphatides and complex glycerides can be used as dispersing agent including emargol which is 1-mono-stearin-3 monosodium sulphoacetate; phosphated monoglycerides; sucrose esters including sorbitan stearates such as sorbitan monostearate; polysorbate 60; and polyglyceryl ricinoleate, which is a partial polyglyceryl ester of interesterified castor oil fatty acids.
Still further, other types of dispersing agents which can be used include mono- and digylcerides; diacetyl tartaric acid esters of mono- and diglycerides (also referred to as DATEM); monosodium phosphate derivatives of mono- and diglycerides of edible fats or oils; lactylated fatty acid esters of glycerol and propylene glycol; polyglycerol esters of fatty acids; propylene glycol mono- and di-esters of fats and fatty acids; oat extract; mono-diglyceride; 2-stearoyl lactylate, the sodium or calcium salts thereof, and sucrose acetate isobutylate (SAIB) alone or in combination; sucrose esters such as sucrose dipalmitate; calcium-stearoyl lactoyl lactate; sorbitan monopalmitate; propylene glycol monostearate; and carrageenan, which is a polymeric saccharide derived from seaweed. Carrageenan can be used to prepare stabilized cocoa used for the production of chocolate milk. The carrageenan can prevent the cocoa from settling in the bottles or cartons.
In addition, the form of the dispersing agent is not limited to the extent facile processing is possible and the advantages of the present method can be achieved. Forms can be used which promote good adherence of the dispersing agent to the cocoa particles including cocoa butter. The dispersing agent can be, for example, in solid, oil, paste, syrup, slurry, or liquid form when it is added to the cocoa mass. The dispersing agent can be, for example, first dissolved in a solvent or carrier before adding to the wet cocoa mass. If desired, the carrier solvent can be the same solvent as the solvent present in the wet cocoa mass, such as, for example, liquefied butane. The dispersing agent can also be in the form of a mixture with a liquid carrier. For example, soya lecithin can be a mixture of phosphatides and soya oil, or the soya oil can be removed and the phosphatides redissolved in cocoa butter or other vegetable oil. In general, phosphatides can be used in conjunction with several percent oil to prevent deterioration and oxidation. In addition to solvents and carriers, temperature can also be used to control the form of the dispersing agent.
A distinction between a solvent and a carrier is that solvent will be removed during desolventization, discussed further below, whereas a carrier is not necessarily removed because it is generally less volatile.
The wet cocoa mass, to which the dispersing agent is added, typically comprises no more than about 30 wt. %, and more particularly, no more than about 20 wt. %, and more particularly no more than about 10 wt. %, and more particularly no more than about 5 wt. %, and even more particularly no more than about 1 wt. % solvent when mixed with the dispersing agent. The amount of solvent present can be sufficient to permit uniform mixing of the cocoa solids particles and the dispersing agent. For example, it can be at least about 0.01 wt. %, and more particularly, at least about 0.1 wt. %, and more particularly, at least about 1 wt. %. After addition of the dispersing agent, the wet cocoa mass may include about 0.1 wt. % to about 75 wt. % solvent, and more particularly, about 5 wt. % to about 35 wt. % solvent.
A variety of methods can be used to carry out the initial addition of dispersing agent to wet cocoa mass, and then also provide for uniform mixing of cocoa mass and dispersing agent once contact of the two components are achieved. Methods for contacting the cocoa mass with dispersing agent for subsequent mixing include injecting, spraying, and other conventional methods. The dispersing agent can be added either straight, in a liquid state, or predissolved, dispersed in solvent. Methods for mixing the two components, after initial contact, include tumbling, grinding, breaking, stirring, agitating, pulverizing, tempering, refining, sifting, milling, and other conventional methods. The pressure during mixing of wet cocoa mass and dispersing agent can be sufficient to keep the solvent in a liquefied state. The temperature during mixing can be, for example, about 15–60° and more particularly, about 20–50° C.
The mixing of cocoa mass and dispersing agent can also be done in conjunction with processes to convert the cocoa solids in the mass into a fine powder. For example, because of the cocoa butter present in the cocoa mass, cooling of the mass may be required during any processing by grinding so that the butter does not melt and cause particles to adhere and machinery to clog.
Injecting is a preferred method for adding the dispersing agent to the wet coca mass, which can be if desired further tumbled.
Mixing can result in substantially complete or complete coverage of the particle surfaces with the dispersing agent. Surface coverage can be uniform. IR and/or Raman methods, for example, can be used to analyze the uniformity of mixing.
After mixing with dispersing agent, the cocoa mass can be further processed and desolventized to yield cocoa powder mixed with dispersing agent. The amount of residual solvent in the cocoa powder produced by desolventizing, can be, for example, no more than about 250 ppm, and more particularly, no more than about 100 ppm, and more particularly, no more than 50 ppm, and more particularly no more than about 5 ppm, and more particularly, no more than 1 ppm. Residual solvent can be analyzed by head space recovery and gas chromatography.
Desolventizing can be achieved by conventional methods including reducing pressure, vacuum, heating, and sparging with gas such as, for example, nitrogen. Heating to temperatures of 60° C. to 70° C., including about 65° C., can be done. Vacuum can be pulled at constant temperature. Desolventizing can result in further mixing of the dispersing agent and cocoa mass if, for example, mixers or agitators are used.
Conventional complementary ingredients can be included with the cocoa powder if desired. For example, the cocoa powder also can be mixed with sweetening agents such as, for example, natural sweeteners such as, for example, sugars such as sucrose, sugar alcohols such as xylitol, sorbitol, erythritol, artificial sweeteners such as, for example, saccharin and aspartame, sodium cyclamate, and mixtures of sodium cyclamate and saccharin. Other examples include acesulfame-k, alitame, and sucralose. Mixtures can be used. Milk powders also can be used. Other examples of complementary ingredients include vitamins, trehalose, colors, flavors, and bulking agents. Complementary ingredients can be selected to be compatible with the solvent.
Upon desolventization, the cocoa powder can comprise no more than about 25 wt. %, and more particularly, no more than about 12 wt. % cocoa butter, and more particularly, no more than about 8 wt. % cocoa butter, and more particularly, no more than about 2 wt. % cocoa butter, and more particularly, no more than about 1 wt. % cocoa butter, and more particularly, no more than about 0.1 wt. % cocoa butter. One range of remaining cocoa butter in the cocoa powder is about 9 wt. % to about 13 wt. %, or more particularly, about 10 wt. % to about 12 wt. %. Another example is so-called breakfast cocoa powder having cocoa butter content of 22–23 wt. %. Water content can be, for example, less than about 2.5 wt. %. In measuring cocoa butter content in the cocoa powder in wt. %, the amount of dispersing agent is excluded. The amount of solvent is also excluded in measuring the amount of cocoa butter as solvent is substantially removed upon desolventization. The amount of cocoa butter remaining in the cocoa powder can be measured by soxhlet extraction methods known to those skilled in the art.
Upon desolventization, the amount of dispersing agent in the cocoa powder is typically no more than about 10 wt. %, and more particularly, no more than about 7 wt. %, and more particularly, no more than about 5 wt. %, and more particularly, no more than about 2 wt. %, and more particularly, no more than about 1 wt. %, and more particularly, no more than about 0.5 wt. %. The dispersing agent amount can be, for example, sufficient to provide functionally useful fast dispersion of the cocoa powder in aqueous media. If too high, however, off flavor can develop. The amount can be, for example, at least about 0.1 wt. %, and more particularly, at least about 0.3 wt. %. The selected amount of dispersing agent can be a function of such factors as, for example, the amount of residual cocoa butter, whether the cocoa powder is alkalized, and the particular food application. After removal of solvent, the sum of the cocoa butter content in wt. percent and the amount of dispersing agent in weight percent in the cocoa powder may be less than about 5 wt. %.
When calculating the amount of dispersing agent, the percentage of active dispersing agent in the added composition can be considered. For example, commercial natural lecithins, such as the soya lecithin, contain about 65 to about 70 wt. % of the active phospholipid. The remainder is oil natural to the source material, or it may be replaced by cocoa butter or a refined vegetable oil, and does not function as a dispersing agent. In calculating the amount of dispersing agent present, particularly with commercial lecithin, it is common practice to use the total added weight including the amount of carrier oil as dispersing agent. As employed herein, however, the “amount of dispersing agent” refers only to the amount of components which are functionally active as a dispersing agent and does not include the amount of any carrier which may be present, such as in commercially available forms of certain dispersing agents.
The cocoa powders provided herein are commonly completely capable of being dispersed in aqueous media with simple stirring with, for example, a spoon, or with moderate shaking without formation of sticky lumps. The cocoa powder also can be free flowing and can typically be poured without plugging or dusting.
Cocoa powder can be made from cocoa liquor prepared from cocoa beans which have only been roasted, i.e., from non-alkalized (non-solubilized) cocoa. In this case, the powder which is formed is referred to as natural process cocoa. However, to provide an attractive color and good dispersion characteristics in, for example, milk, cocoa powder is often made from alkalized cocoa mass.
The cocoa powders can be checked for quality including checked for color, flavor, fat percentage, moisture percentage, pH, ash on fat-free dry, alkalinity of the ash, shell percentage based on nib, percentage sieve residue on 75 microns, traces of heavy metals, pesticide residues, and microbiology.
The improved lecithination, as described above, can be combined with the process of “instantizing,” known to those skilled in the art, which joins the fine particles into agglomerates which contain tiny capillary channels which allow liquid to be drawn in, thereby producing a wetting action. Agglomeration also can affect the bulk density so that the material has a greater volume for a given weight. Cocoa powder, for example, can be agglomerated with sugar and milk powder to produce instant beverages. Instantizing is disclosed in, for example, U.S. Pat. No. 2,835,586, which is hereby incorporated by reference.
The dispersibility of the cocoa powder can be assessed based on testing methods known in the art which include the following:
(1) the time required for a predetermined amount of cocoa powder to penetrate the surface of a beverage such as, for example, cold milk or water without mixing. This measurement reflects wettability.
(2) the rate and extent of cocoa sedimentation, as visualized by the formation of bottom sediment.
(3) the presence of cocoa particles that remain on the surface (which can be called “floaters”);
(4) the formation of a surface layer resulting from cocoa butter which “oils off” and rises after a hot beverage is left to stand.
Factors (2)–(4) can be related to product defects as well.
In one embodiment, the dispersible powder composition can be formulated to be relatively low in calories. For example, the amount of cocoa butter can be reduced and low or no calorie sweeteners can be used.
In a low calorie embodiment, reducing the amount of cocoa butter content generally improves dispersibility, particularly when cocoa butter content is reduced to about 1 wt. % or less. When the amount of cocoa butter content is relatively high, then the dispersing agent becomes more important in providing good dispersibility.
When the dispersing agent is mixed with a carrier solvent such as hexane, for example, the amount of carrier solvent can be adapted based on the scale-up process parameters. For example, in some embodiments, the relative amount of carrier solvent can be reduced as the process is scaled up.
A mix was prepared by agglomeration of 80% powdered sugar and 20% alkalized cocoa powder, wherein the latter was prepared by a liquefied butane extraction of cocoa mass to reduce the cocoa buffer content to less than 1 wt. %. The wettability of this agglomerated product was analyzed by pouring dry agglomerate on the surface of cold fresh milk. The wettability time is the time needed for the powder to sink through the surface without agitation. The dispersability was evaluated in cold milk by adding 15 g to 200 mL milk at 70° C.±1° C. The wettability of cocoa powders produced by the present method may be no more than about 20 seconds, and more particularly, no more than about 15 seconds, and more particularly, no more than about 10 seconds.
Experiment 1
A. The cocoa powder product which had not been modified with lecithin almost completely sank through the surface of cold milk in 30 seconds.
B. The same cocoa powder product as in A which had been modified with lecithin at a level of 0.5 wt. % sank through the surface of cold milk in 15 seconds. Lecithin modification was carried out with use of hexane as a carrier solvent, which is removed by evaporation.
C. The same cocoa powder product as in A which had been modified with lecithin at a level of 1.0 wt. % sank through the surface of cold milk in 8 seconds. Again, lecithin modification was carried out with use of hexane as a carrier solvent, which is removed by evaporation.
Experiment 2
A conventional cocoa powder was used having 10–12 wt. % remaining cocoa butter. Lecithin was added with use of hexane as a carrier solvent. It was converted to a 80:20 agglomerated powder sugar:cocoa powder mix. The dispersability was evaluated in cold milk by adding 15 g to 200 mL milk at 7° C.±1° C.
When no lecithin was added, the powder remained on the surface of cold milk; it did not sink through the surface of cold milk. At 0.5 wt. % lecithin added, only 5 percent of the dry mix is wetted; 95% was still dry on the surface of cold milk after 30 seconds. At 1 wt. % lecithin added, only 30 percent of the dry mix is wetted; 70% was still dry on the surface of cold milk after 30 seconds. At 5 wt. % lecithin added, the mix sank through the surface of the cold milk in 8 seconds.
Although illustrated and described herein with reference to certain specific embodiments and examples, the present process is nevertheless not intended to be limited to the details shown. Rather, various modifications may be made in the details within the scope and range of equivalents of the claims and without departing from the spirit of the process.
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| 1 219 764 | Mar 1987 | CA |
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| 2059829 | Jul 1992 | CA |
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| 1050739 | Apr 1991 | CN |
| 1 934 649 | Jan 1971 | DE |
| 1934649 | Jan 1971 | DE |
| 2557056 | Jun 1977 | DE |
| 2055030 | Oct 1977 | DE |
| 2828992 | Aug 1979 | DE |
| 3318317 | Nov 1984 | DE |
| 3716227 | Dec 1988 | DE |
| 39 01 056 | Jul 1990 | DE |
| 3901056 | Jul 1990 | DE |
| 41 39 817 | Jun 1993 | DE |
| 061017 | Sep 1982 | EP |
| 171079 | Feb 1986 | EP |
| 0 252 760 | Jan 1988 | EP |
| 254610 | Jan 1988 | EP |
| 0 379 023 | Jul 1990 | EP |
| 496310 | Jul 1992 | EP |
| 252760 | Mar 1993 | EP |
| 0 574 764 | Dec 1993 | EP |
| 593833 | Apr 1994 | EP |
| 0 719 854 | Jul 1996 | EP |
| 721980 | Jul 1996 | EP |
| 0 591 981 | Dec 1996 | EP |
| 0 664 959 | Mar 1999 | EP |
| 0 943 675 | Sep 1999 | EP |
| 0 711 508 | Jul 2000 | EP |
| 1 274 872 | Oct 1961 | FR |
| 341000 | Jan 1931 | GB |
| 652619 | Apr 1951 | GB |
| 742537 | Dec 1955 | GB |
| 770843 | Mar 1957 | GB |
| 1177860 | Jan 1970 | GB |
| 1356749 | Jun 1974 | GB |
| 1356750 | Jun 1974 | GB |
| 2033721 | May 1980 | GB |
| 2 148 739 | Jun 1985 | GB |
| 2 177 107 | Jan 1987 | GB |
| 53-66473 | Jun 1978 | JP |
| 53066473 | Jun 1978 | JP |
| 54-157880 | Dec 1979 | JP |
| 54157880 | Dec 1979 | JP |
| 55135546 | Oct 1980 | JP |
| 58-146238 | Aug 1983 | JP |
| 58146238 | Aug 1983 | JP |
| 59-91845 | May 1984 | JP |
| 59091845 | May 1984 | JP |
| 62-104554 | May 1987 | JP |
| 62104554 | May 1987 | JP |
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| 62126966 | Jun 1987 | JP |
| 62272941 | Nov 1987 | JP |
| 62272941 | Nov 1987 | JP |
| EP0301278 | Jan 1989 | JP |
| 1056793 | Mar 1989 | JP |
| 01112965 | May 1989 | JP |
| 1243942 | Sep 1989 | JP |
| 3155748 | Jul 1991 | JP |
| 5015349 | Jan 1993 | JP |
| 06086637 | Mar 1994 | JP |
| 7-87892 | Apr 1995 | JP |
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| 09234018 | Sep 1997 | JP |
| 9-275905 | Oct 1997 | JP |
| 9275905 | Oct 1997 | JP |
| 10179078 | Jul 1998 | JP |
| 11113495 | Apr 1999 | JP |
| 20125767 | May 2000 | JP |
| 11-155985 | Dec 2000 | JP |
| 21069946 | Mar 2001 | JP |
| 210300 | Apr 1968 | SU |
| WO 9313035 | Jul 1993 | WO |
| WO 9415483 | Jul 1994 | WO |
| WO 9503708 | Feb 1995 | WO |
| WO 9510946 | Apr 1995 | WO |
| WO 9634535 | Nov 1996 | WO |
| WO 0182714 | Nov 2001 | WO |
| WO 02071858 | Sep 2002 | WO |
| 881378 | Feb 1988 | ZA |
| Number | Date | Country | |
|---|---|---|---|
| 20040071858 A1 | Apr 2004 | US |
