US3754961A - Method of preventing the caking of hardened oil coated particles - Google Patents

Method of preventing the caking of hardened oil coated particles Download PDF

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Publication number
US3754961A
US3754961A US00164717A US3754961DA US3754961A US 3754961 A US3754961 A US 3754961A US 00164717 A US00164717 A US 00164717A US 3754961D A US3754961D A US 3754961DA US 3754961 A US3754961 A US 3754961A
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caking
hardened oil
particles
hardened
coated particles
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R Ueno
T Miyazaki
S Inamine
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Ueno Fine Chemicals Industry Ltd
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Ueno Fine Chemicals Industry Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/30Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using agents to prevent the granules sticking together; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • A23P10/35Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/40Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added
    • A23P10/43Shaping or working of foodstuffs characterised by the products free-flowing powder or instant powder, i.e. powder which is reconstituted rapidly when liquid is added using anti-caking agents or agents improving flowability, added during or after formation of the powder
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/48Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals

Definitions

  • This invention relates to a method of preventing the caking of particles consisting of a core material coated with a coating agent whose principal ingredient is a hardened oil.
  • Hardened oils have been used for such purposes as the prevention of moisture absorption, maintenance of effectiveness of prevention of reaction of such drugs and chemicals as medicines for man as well as animals, agricultural chemicals, food additives, etc., by serving as a surface coating with these drugs and chemicals as the core material.
  • a food additive is the core material
  • the application of a hardened oil coating has been frequently practiced to achieve a unique end, i.e., to prevent the additive from eluting at room temperature but permitting it to elute during the step of heating the food product, in order to prevent the decomposition of the core material in the foodstuff material and any adverse effect of the core material on the foodstuff material.
  • a hardened oil to be used for the above described purposes is one having a melting point ranging from 45 to 85C.
  • a hardened oil whose melting point is below the foregoing range, there is the possibility of its softening at high temperatures experienced in summer.
  • Especially desirable hardened oils are, for example, hardened beef tallow (m.p. 59 61C.), hardened whole oil (m.p. 55 60C.), hardened rape seed oil (m.p. 50 62C.), hardened soybean oil (m.p. 60 69C.), hardened cottonseed oil (m.p. 55 61C.) and hardened castor oil (m.p. 82 85C.)
  • the spraying method which comprises heatmelting the hardened oil, dispersing the core material therein and thereafter spraying this dispersion into a gas of a melting point below that of the hardened oil (e.g. air, nitrogen and carbon dioxide) thereby accomplishing the coating of the core material and at the same time the cooling and solidification of the particles.
  • a gas of a melting point below that of the hardened oil e.g. air, nitrogen and carbon dioxide
  • the coating pan method in which the coating of the particles is carried out by repeating an operation consisting of placing the core material in a coating pan, spraying a solvent-dissolved hardened oil onto the core material while tumbling same in the pan, and thereafter evaporating and removing the solvent by blowing, for example, hot air against the coated particles.
  • the suspensiomin-air coating method which comprises floating the core material in a stream of air and coating the so floating core material by spraying a solution of a hardened oil against the material.
  • the vacuum vaporization method which'comprises heating the hardened oil in a vacuum and evaporating it against the core material to thereby effect the vapor deposition of the hardened oil onto the surface of the core material.
  • the electrostatic coating method which comprises impressing the particles of the core material and the particles of the hardened oil solution with opposite electric charges to thus unite these particles.
  • meltable-dispersion method which comprises heat-melting the hardened oil in a liquid which does not dissolve the same, dispersing the core material in the melt, forming the dispersed core material into small particles, and thereafter cooling and solidifying the same.
  • these coated particles consisting of a core material coated with a hardened oil
  • the coated particles are usually prepared so as to have a suitable particle diameter ranging from 50 to 2,000 microns. It is most desired that these coated particles are independent from each and have fluidity. If the coated particles are caked and in a lumpy state, their use is not only inconvenient but also this makes them unfit for use at times.
  • the core material happens to be a food additive, it is necessary that these particles are uniformly mixed in the foodstuff material. Therefore, a food additive in which the particles are in a caked state rather than achieving its purpose has the opposite effect of degrading the quality of the food, since it becomes incorporated in the food product in a nonuniform state.
  • the object of the present invention is to therefore provide hardened oil coated particles in which the hereinbefore noted caking does not occur.
  • the particles consisting of a core material which have been coated with a coating agent whose principal ingredient is a hardened oil of a melting point 45 C. are allowed to stand for at least 20 hours at a temperature higher than 25C. but lower than the softening point of the hardened oil, thereby stabilizing the crystal structure of the hardened oil, following which the particles are incorporated with a caking inhibitor, in an amount of 0.3 5 percent by weight based on the weight of the coated particles.
  • the solidified mass of hardened oil is made up of a plurality of crystals, i.e., a congregation of small crystals and, thus, changes in the crystal structure take place as a result of the temperature history of these small crystals.
  • the solid hardened oil obtained by either cooling and solidifying or precipitating from a solvent a hardened oil which is in a molten state as a result of heating is of a structure in which a plurality of small crystals in an unstable form are collected together in a relatively loose arrangement.
  • FIG. 1 is a graph illustrating the results of a different thermal analysis of hardened beef tallow.
  • FIG. 2 is a graph illustrating the results of an infrared absorption analysis of hardened beef tallow.
  • A, B and C forms The crystal forms of the hardened oil which pro vide these three classes of differential thermal curves are referred to as A, B and C forms.
  • the A form crystal is a crystal form obtained when a heat-melted hardened oil is rapidly cooled and solidified in cold water, and while it is stable at low temperatures, it gradually transform to the B form crystal when the temperature rises finally becoming transformed to the C form crystal.
  • the B form crystal is one which is obtained when the hardened oil has been cooled and solidified under relatively mild conditions, i.e.
  • the B form crystal is obtained without passing through the A form crystal stage.
  • the B form crystal as in the case with the A form crystal, is unstable and therefore gradually transforms to the C form crystal.
  • the C form crystal is a crystal form'which is obtained when the A and B form crystals have been allowed to stand either for or more days at C. or 3 or more days at C. This C form crystal being exceedingly stable does not change at temperatures below the softening point. Further, concurrently with this transformation, a change in the disposition of the small crystals from a loose arrangement to an orderly arrangement takes place. Therefore, not only is the crystal form stabilized but also the stability of the overall structure is increased. Referring to the graph of FIG.
  • the maximum peak temperature of the A form crystal is 68C.
  • that of the B form crystal is 64C.
  • that of the C form crystal is 70C., that of the C form crystal being the highest, while that of the B form crystal being the lowest. That is, in the case of the hardened beef tallow, the transformation takes place first from the A form crystal to the Bform crystal having a lower maximum peak temperature and then to the C form crystal which is the most stable. This sort of transformation is a phenomenon which is generally seen in the case of the higher fatty acids and higher alcohols.
  • graph I illustrates the infrared analysis results of the C form crystal and graph II shows that of the A form crystal.
  • the form of graph I is more complicated than that of graph II, and it can be clearly seen a difference exists.
  • the hardened oils precipitated from a solvent are of the C form crystal, but in this case it is still an unstable C form crystal.
  • its crystal structure is also one not disposed in an orderly manner but is one which is of loose arrangement.
  • this hardened oil is allowed to stand at above a certain temperature, the crystals are changed to C form crystals having stability and its crystal structure becomes one which has an orderly arrangement.
  • Graph III of FIG. 2 is the result of an informed analysis of hardened beef tallow which has been crystallized by the evaporation of chloroform from a chloroform solution at 20C., a clear difference being seen from this graph when compared with graphs l and II.
  • this hardened oil crystal is allowed to stand at above a certain temperature, it changes to a stable crystal equalling that of graph I.
  • the speed with which the crystal structure transforms from the A or B form to C form is influenced by the temperature at which the crystals stand, the speed becoming faster in proportion as the temperature becomes higher. At low temperatures at which the transformation does not progress (generally, the speed becomes very slow when the temperature falls to below 15C.), caking of the particles coated with a hardened oil of the A form or B form crystals does not take place even though the particles are allowed to stand fora prolonged period of time.
  • the caking of the hardened oil coated particles which takes place when the crystal structure transforms from the A or B form to the C form, can be explained as being a phenomenon wherein particles combine by mutually taking in the crystals of the other particles at the surfaces thereof during the time when the transformation of the A form and B form crystals to the stables C form crystal is taking place or when a change in the loose disposition of the small crystals to an orderly arrangement is taking place.
  • the hardened oil coated particles are suitably allowed to stand at a temperature above 25C., and preferably above 30C. At low temperature of below 25C., either the speed of transformation is has occurred during the transformation is eliminated.
  • the particles which have in this way been rendered independent of each other, as then incorporated with 0.3 5 percent by weight, and preferably 0.5 3 percent by wieght, based on the particles, of a caking inhibitor, and as a result the product of the present invention of improved fluidity, which does not cake at temperatures lower than the softening point of the hardened oil, and is therefore of high merchandise value is obtained.
  • any substance may be used as the aforesaid caking-inhibitor as long as it is one which does not impede the function of the core material, usually silica, magnesium alumino silicate, magnesium carbonate, calcium tertiary phosphate, calcium stearate or magnesium stearate is conveniently used.
  • the operation for carrying out the stabilization treatment is simple.
  • the coated particles immediately after their preparation need only be allowed to stand in a room of a temperature higher than 25C.
  • EXAMPLE 1 Four kg of hardened beef tallow were heat-melted and maintained at a temperature of 70C. After adding 1 kg of powdered sorbic acid to the melted hardened beef tallow, the mixture was mixed with thorough stirring using a homo-mixer to obtain a homogeneous dispersion. The dispersion was sprayed into air of 20C., and on cooling and solidification hardened oil coated sorbic acid particles useable as a food preservative were prepared. The following caking test was carried out on the so obtained coated particles.
  • the several classes of caking inhibitors indicated in Tables l--l to 1-5 were added separately to the coated particles, following which the coated particles were allowed to stand under the various conditions indicated in Tables l-l to [-5. This was followed by packing the coated particles in a cylindrical tube 40 mm in diameter and mm in height and subjecting the particles to a pressure by placing a 500-gram weight atop the packed particles. The particles were allowed to stand for 7 days in this state at the prescribed test temperatures indicated in Tables ll to 1-5. Next, the coated particles contained in the tube were taken out therefore ensuring that in doing so the caked condition of the particles was not disturbed, after which the so withdrawn particles were lightly sieved with a lO-mesh sieve.
  • the amount of coated particles remaining on the sieve relative to the total amount was then calculated and expressed in percent. This value, which is' designated the degree of caking is indicated in Tables l'-l to l-5. The larger this value is, the greater the caking of the particles. Also shown in Tables ll to l5 are the crystal forms of the hardened beef tallow before and after the test.
  • EXAMPLE 2 The three kilograms of hardened castor oil (m.p. 80 85C.) were heat-melted. After adding 4 grams of soya-lecithin thereto as a surfactant, one kg of finely divided fumaric acid was added, following which the mixture was commingled with thorough stirring to obtain a dispersion. While maintaining this dispersion at 90C., it was sprayed into air of C., wherefrom it was cooled and solidified. As a result hardened castor oil coated fumaric acid particles were prepared.
  • coated particles were incorporated separately with the various caking inhibitors indicated in Table 2 to adhere the caking inhibitors to the surface of the hardened caster oil coated fumaric acid particles, and a caking test was carried out as in Example 1 under the various conditions indicated in Table 2. The results obtained are shown in Table 2.
  • the hardened castor oil coated fumaric acid particles are added to the starting food material, and by preventing the elution of the fumaric acid at room temperature but by causing the acid to elute during the heating step, they are used for the purpose of lowering the pH of the food product. Since as shown in Table 2 the degree of caking of the invention coated particles is low, they are especially suitable for this purpose.
  • a glutamic acid powder of 40-mesh was placed in a coating pan and while being tumbled the powder was sprayed with a 30 percent chloroform solution of hardened beef tallow (mp. 59 61C.) After continuing the tumbling of the powder particles for a while and having accomplished the uniform wetting of the surface of the glutamic acid powder particles, the chloroform was evaporated by means of hot air. The foregoing operation was repeated until the content of the hardened beef tallow in the particles became 40 percent. As a result coated glutamic acid particles which could be used as a seasoning as well as a pH lowering agent of food products were prepared.
  • a method of preventing the caking of hardened oil coated particles which comprises allowing particles consisting of a core material coated with a coating agent predominantly of a hardened oil having a melting point of 45-85C., to stand for at least 20 hours at a temperature exceeding 25C. but lower than the softening point of said hardened oil and thereafter adding to the stabilized hardened oil-coated particles a cake inhibitor, in an amount of 0.3-5 percent by weight based on the weight of the stabilized hardened oil-coated particles.
  • caking inhibitor is a finely divided inorganic substance.
  • caking inhibitor is an alkaline earth metal salt of a higher fatty acid.

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Plant Pathology (AREA)
  • Epidemiology (AREA)
  • Toxicology (AREA)
  • Agronomy & Crop Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Bioinformatics & Cheminformatics (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Pest Control & Pesticides (AREA)
  • Animal Behavior & Ethology (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Biophysics (AREA)
  • Molecular Biology (AREA)
  • Fodder In General (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)
  • Formation And Processing Of Food Products (AREA)
  • Medicinal Preparation (AREA)
  • Glanulating (AREA)
  • Fertilizers (AREA)
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US00164717A 1970-07-24 1971-07-21 Method of preventing the caking of hardened oil coated particles Expired - Lifetime US3754961A (en)

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JP (1) JPS5015742B1 (enrdf_load_stackoverflow)
AU (1) AU464264B2 (enrdf_load_stackoverflow)
BE (1) BE770382A (enrdf_load_stackoverflow)
DE (1) DE2136978C3 (enrdf_load_stackoverflow)
FR (1) FR2103335A5 (enrdf_load_stackoverflow)
GB (1) GB1339830A (enrdf_load_stackoverflow)
NL (1) NL168716C (enrdf_load_stackoverflow)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4267198A (en) * 1978-06-27 1981-05-12 Daicel Ltd. Melt-coated preparation containing sorbic acid
US4469710A (en) * 1982-10-14 1984-09-04 The Procter & Gamble Company Pourable solid shortening
US5698186A (en) * 1992-08-17 1997-12-16 Clairol, Inc. Methods of controlling dust and compositions produced thereby
US5894029A (en) * 1994-03-21 1999-04-13 Purebred Pet Products, Inc. Method of making pet snack food
US20040109927A1 (en) * 2002-11-27 2004-06-10 Ang Jit Fu Carbonate-based anti-caking agent with reduced gas release properties
US20040223999A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Mold inhibitor integrated within a matrix and method of making same
US20040224063A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Pet food treat and method of making same
US20040224065A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Pet food treat and method of making same
US20040224053A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Habitat for caged animals and method of improving animal environment
US20050256234A1 (en) * 2002-06-24 2005-11-17 Asahi Denka Co., Ltd Flame retardant composition and flame retardant resin composition containing the composition

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI56925C (fi) * 1979-01-29 1980-05-12 Serlachius Oy Foerfarande foer att foerhindra agglomereringen av lignosulfonathaltigt bindemedel foer granulering av foderblandningar
FR2518426A1 (fr) * 1981-12-18 1983-06-24 Grp Etud Rech Charges Traitement de produits fins pulverulents par des charges antimottantes
FR2627955B1 (fr) * 1988-03-02 1991-12-06 Roquette Freres Adjuvant de congelation pour aliments a base de chair hachee et son procede de fabrication
US5626893A (en) * 1994-10-18 1997-05-06 Reddy; Malireddy S. Method of treating a divided cheese product for anticaking
EP0953282A1 (en) * 1998-03-02 1999-11-03 Novartis AG Pesticidal compositions
EP1879469B1 (en) * 2005-05-11 2011-11-09 Hill's Pet Nutrition, Inc. Methods for enhancing palatability of compositions for animal consumption
CN115551363A (zh) * 2020-05-29 2022-12-30 上野食品科技株式会社 食品用包覆有机酸粉末和食品用保质期改善剂
AU2022289117A1 (en) * 2021-06-10 2023-11-30 Givaudan Sa Flavour composition

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4267198A (en) * 1978-06-27 1981-05-12 Daicel Ltd. Melt-coated preparation containing sorbic acid
US4469710A (en) * 1982-10-14 1984-09-04 The Procter & Gamble Company Pourable solid shortening
US5698186A (en) * 1992-08-17 1997-12-16 Clairol, Inc. Methods of controlling dust and compositions produced thereby
US5894029A (en) * 1994-03-21 1999-04-13 Purebred Pet Products, Inc. Method of making pet snack food
US20050256234A1 (en) * 2002-06-24 2005-11-17 Asahi Denka Co., Ltd Flame retardant composition and flame retardant resin composition containing the composition
US20040109927A1 (en) * 2002-11-27 2004-06-10 Ang Jit Fu Carbonate-based anti-caking agent with reduced gas release properties
WO2004049821A1 (en) * 2002-11-27 2004-06-17 International Fiber Corporation Carbonate-based anti-caking agent with reduced gas release
US20040224063A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Pet food treat and method of making same
US20040224060A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Mold inhibitor integrated within a matrix and method of making same
US20040224065A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Pet food treat and method of making same
US20040224053A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Habitat for caged animals and method of improving animal environment
US20050065308A1 (en) * 2003-05-06 2005-03-24 Markham Joseph P. Mold inhibitor integrated within a matrix and method of making same
US6894136B2 (en) 2003-05-06 2005-05-17 Joseph P. Markham Mold inhibitor integrated within a matrix and method of making same
US6939937B2 (en) 2003-05-06 2005-09-06 Joseph P. Markham Mold inhibitor integrated within a matrix and method of making same
US6965005B2 (en) 2003-05-06 2005-11-15 Markham Joseph P Mold inhibitor integrated within a matrix and method of making same
US20040223999A1 (en) * 2003-05-06 2004-11-11 Markham Joseph P. Mold inhibitor integrated within a matrix and method of making same
US20060153948A1 (en) * 2003-05-06 2006-07-13 Markham Joseph P Habitat for caged animals and method of improving animal environment

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Publication number Publication date
AU464264B2 (en) 1975-08-21
AU3160371A (en) 1973-01-25
DE2136978C3 (de) 1974-01-24
GB1339830A (en) 1973-12-05
BE770382A (fr) 1971-12-01
DE2136978B2 (de) 1973-06-28
NL7110221A (enrdf_load_stackoverflow) 1972-01-26
NL168716C (nl) 1982-05-17
FR2103335A5 (enrdf_load_stackoverflow) 1972-04-07
JPS5015742B1 (enrdf_load_stackoverflow) 1975-06-07
DE2136978A1 (de) 1972-02-17

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