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WO2019158756A1 - Composition en poudre, contenant un minéral argileux - Google Patents

Composition en poudre, contenant un minéral argileux Download PDF

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Publication number
WO2019158756A1
WO2019158756A1 PCT/EP2019/053981 EP2019053981W WO2019158756A1 WO 2019158756 A1 WO2019158756 A1 WO 2019158756A1 EP 2019053981 W EP2019053981 W EP 2019053981W WO 2019158756 A1 WO2019158756 A1 WO 2019158756A1
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WIPO (PCT)
Prior art keywords
clay mineral
water
range
composition according
binder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2019/053981
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German (de)
English (en)
Inventor
Christian Koepsel
Dietrich Rein
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BASF SE
Original Assignee
BASF SE
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Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Publication of WO2019158756A1 publication Critical patent/WO2019158756A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/20—Inorganic substances, e.g. oligoelements
    • A23K20/28—Silicates, e.g. perlites, zeolites or bentonites
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L11/00—Pulses, i.e. fruits of leguminous plants, for production of food; Products from legumes; Preparation or treatment thereof
    • A23L11/30—Removing undesirable substances, e.g. bitter substances
    • A23L11/34—Removing undesirable substances, e.g. bitter substances using chemical treatment, adsorption or absorption
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L7/00—Cereal-derived products; Malt products; Preparation or treatment thereof
    • A23L7/10—Cereal-derived products
    • A23L7/101—Addition of antibiotics, vitamins, amino-acids, or minerals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles

Definitions

  • the present invention relates to pulverulent compositions whose powder particles contain at least one clay mineral and at least one water-soluble, organic binder.
  • the invention also relates to a process for the preparation of such compositions and to the use of the compositions in foodstuffs, in particular in powdered foodstuffs, such as in cereal flours.
  • Aflatoxins are known to be potent carcinogens and mutagens. They are stable in food and feed, even under processing conditions. Exposure to aflatoxins in food is the cause of severe human disease such as aflatoxicosis and hepatocellular carcinoma. Especially in children, aflatoxins can cause growth disturbances and mental retardation even at low levels of exposure - see, eg. See, for example, P. Wang et al., Food Additives and Contaminants, 25 (5) (2008) 622-634 for further references. The harmful effects of aflatoxins on domestic and farm animals, especially poultry and small pets such as dogs or cats, have also been known for a long time.
  • WO 92/05706 describes the use of certain montmorillonite-based clay minerals as an aflatoxin-binding additive in feeds for animal nutrition and proposes a method of identifying clay minerals which bind aflatoxins to a particular degree.
  • WO 2007/011825 describes the use of acid-treated clay minerals as a food and feed additive for deactivating aflatoxins and for reducing the growth of mycotoxin-producing microorganisms. Preference is given to using clay minerals with a particle size below 80 ⁇ m.
  • US 2012/0328672 describes a process for the fractionation of finely divided, cadmium-containing clay minerals into a coarse fraction having an average particle size above 100 ⁇ m and a finely divided fraction having an average particle size below 100 ⁇ m, in particular in the range from 20 to 60 ⁇ m.
  • the finely divided fraction should be characterized by a lower heavy metal content and an increased binding capacity for aflatoxins.
  • clay minerals in the form of finely divided dusts adsorb mycotoxins such as aflatoxins particularly well and thus reduce their bioavailability, these dusts are difficult to handle.
  • these dusts can be incorporated only poorly or less reliably in powdered foods such as flours.
  • the problem here is that the finely divided powder particles can separate from the flour due to their higher density and fineness, resulting in an uneven distribution in the flour.
  • coarse fractions of clay minerals have the above-mentioned disadvantages of a lower binding capacity for mycotoxins and optionally a higher heavy metal content.
  • JPS-63312105 describes granules of alumina powder prepared by mixing alumina powder with an aqueous solution of a binder such as polyvinyl alcohol in a granulating drum having a plurality of rotary mixing elements.
  • a binder such as polyvinyl alcohol
  • relatively coarse-particle granules are obtained which have a mean Have diameters in the range of 170 to 840 pm and a high proportion of coarse particles.
  • the granules are proposed for use in plant protection products and fertilizers. For use in powdery foods they are unsuitable.
  • AU 548773 describes feed formulations for ruminants containing a layer silicate from the montmorillonite group.
  • the feeds can be produced in the form of granules or pellets. They are unsuitable for use in powdery foods.
  • compositions based on clay minerals which are easy to handle, which can be incorporated easily and uniformly into powdery food or feed and which do not separate and which do not lead to disadvantageous sensory properties.
  • the compositions should be easy and reproducible.
  • the compositions should not or not appreciably impair the property of the clay minerals to bind mycotoxins, in particular aflatoxins such as aflatoxin B1.
  • the powdered, clay mineral-containing compositions whose powder particles have a particle diameter in the range of 70 to 350 pm, in particular in the range of 70 to 250 pm, wherein the clay mineral in the powder particles in the form of agglomerated primary particles whose particle size distribution is characterized by a D [v, 09] value below 80 ⁇ m, in particular below 70 ⁇ m, and wherein the clay minerals contain at least one water-soluble organic binder which is mono-, di-, or di- and polysaccharides which preferably have at least one glucose unit.
  • the present invention relates to pulverulent compositions whose powder particles contain at least one clay mineral and at least one water-soluble organic binder selected from mono-, di- and polysaccharides, which preferably have at least one glucose unit, wherein at least 80 vol .-% of the powder particles contained in the composition have a particle diameter in the range of 70 to 350 pm, in particular 70 to 250 pm or 80 to 250 pm and wherein the clay mineral is present in the powder particles in the form of agglomerated primary particles whose particle size distribution by a D [v, 09] value is characterized below 80 pm, in particular below 70 pm, wherein the particle diameter specified here and the D [v, 09] value are the values determined by static laser light scattering in accordance with ISO 13320: 2009.
  • the invention also relates to a process for preparing such compositions which comprises agglomerating a clay mineral dust using an aqueous solution of the water-soluble organic binder, wherein the particle size distribution of the clay mineral dust by a D [v, 09] value below 80 gm , in particular below 70 gm, determined by static laser light scattering according to ISO 13320: 2009.
  • the invention also relates to the use of a composition according to the invention as an additive in foodstuffs and feedstuffs, in particular in powdery foods and feedstuffs, such as, for example, in flours intended for human nutrition.
  • the invention also relates to the use of a composition according to the invention for binding mycotoxins in such food and feed.
  • the invention has a number of advantages. Because of their particle size, the compositions according to the invention are easier to handle than the clay dust normally used and are easier and more uniformly incorporated into pulverulent food and feed. In these powdered food and feed they show a lower tendency to settle or to separate. In contrast to clay mineral powders of comparable particle size, they do not lead to disadvantageous sensory properties. In addition, the compositions do not or do not appreciably affect the property of the clay minerals contained therein to bind mycotoxins, in particular aflatoxins such as aflatoxin B1. Despite their comparatively large particle size they do not lead to a sensory impairment. In addition, the compositions according to the invention can be produced in a simple and easy manner and on a large scale by conventional agglomeration processes of commercially available clay mineral dusts using commercially available, water-soluble binders.
  • Clay minerals in the context of the invention are sheet silicates and minerals with a high proportion of sheet silicates of preferably at least 50% by weight, in particular at least 60% by weight, based on the clay mineral.
  • Foods according to the invention are nutrient-containing compositions for human nutrition.
  • the term foodstuffs includes food raw materials that are processed into ready-to-consume foods, as well as ready-to-eat foods made from these food commodities.
  • Feed for the purposes of the invention are nutrient-containing compositions for animal nutrition, in particular for the nutrition of domestic animals, such as dogs or cats, and poultry.
  • the powder particles contained in the composition have a particle diameter in the range from 70 to 350 ⁇ m or in the range from 80 to 350 ⁇ m, in particular in the range from 70 to 300 ⁇ m or in the range from 80 to 300 pm and especially in the range of 70 to 250 pm or in the range of 80 to 250 pm.
  • the D [v, 01] value of the particle size distribution of the composition according to the invention is generally at least 70 .mu.m and in particular at least 80 .mu.m, for example in the range from 70 to 150 .mu.m or in the range from 80 to 135 .mu.m or below Range from 80 to 125 pm.
  • the D [v, 09] value of the particle size distribution of the composition according to the invention is generally at most 350 .mu.m, in particular at most 300 .mu.m and especially at most 250 .mu.m and especially at most 200 .mu.m, and is for example in the range from 130 to 350 pm or in the range of 150 to 300 pm or in the range of 180 to 250 pm.
  • the D [v, 05] value of the particle size distribution of the compositions according to the invention is generally in the range from 80 to 240 ⁇ m, in particular in the range from 85 to 200 ⁇ m and especially in the range from 90 to 190 ⁇ m.
  • the D [v, 05] value of the particle size distribution is in the range from 80 to 180 ⁇ m, in particular in the range from 85 to 175 ⁇ m and especially in the range from 90 to 170 ⁇ m. In another group of embodiments, the D [v, 05] value of the particle size distribution is in the range from 1 10 to 240 ⁇ m, in particular in the range from 115 to 200 ⁇ m and especially in the range from 120 to 190 ⁇ m.
  • the compositions according to the invention preferably have a particle size distribution whose volume-weighted average D [4,3] is in the range from 90 to 250 ⁇ m, in particular in the range from 95 to 220 ⁇ m and especially in the range from 100 to 200 ⁇ m.
  • the surface weighted mean D [3,2] of Particle size distribution of the compositions according to the invention is generally in the range from 75 to 200 gm, in particular in the range from 80 to 180 gm and especially in the range from 85 to 160 gm.
  • all information relates to particle sizes, particle diameters and particle size distributions , including the values D [v, 01], D [v, 05], D [v, 09], D [4,3] and D [3,2] to those by static laser light scattering according to ISO
  • the value D [v, 01] means that 10% by volume of the particles of the measured sample have a particle diameter below the value indicated as D [v, 01]. Accordingly, the value D [v, 05] means that 50% by volume of the particles of the measured sample have a particle diameter below the value indicated as D [v, 05]; and the value D [v, 09] means that 90% by volume of the particles of the measured sample have a particle diameter below the value stated as D [v, 09].
  • the value D [4, 3] stands for the volume-weighted average determined by means of SLS, which is also referred to as De Brouckere mean value and which corresponds to the weight average in the particles according to the invention.
  • the value D [3, 2] stands for the surface-weighted average determined by means of SLS, which is also referred to as Sauter diameter.
  • the particle size distribution of the powder particles can also be determined by sieve analysis according to DIN 66165-1: 2016-08.
  • the inventive compositions contain less than 20 wt .-%, in particular less than 15 wt .-%, especially less than 10 wt .-% powder particles having a particle size below 63 pm.
  • the inventive compositions contain less than 15 wt .-%, preferably less than 10 wt .-% powder particles having a particle size above 250 pm.
  • the compositions of the invention contain at least 70
  • Wt .-% especially at least 80 wt .-% powder particles having a particle size in the range of 63 to 250 pm and especially in the range of 63 to 212 pm.
  • the weight-average particle diameter, hereinafter also D50, of the powder particles, as results from the particle size distribution determined by sieve analysis, is generally in the range from 70 to 200 ⁇ m, in particular in the range from 80 to 180 ⁇ m and especially in the range from 90 to 170 pm.
  • the clay minerals are present in the form of primary particles which are separated by the water-soluble organic binder. desch be held together to form larger powder particles. It is assumed that the powder particles of the compositions according to the invention decompose upon contact with aqueous liquids, for example water, but also saliva, and thus release the primary particles.
  • the water-soluble binder may also cause the primary particles to stabilize against reagglomeration. In any case, therefore, the ability of the clay mineral particles to bind mycotoxins, especially aflatoxins, is not or not appreciably reduced.
  • the particle size distribution of the primary particles is characterized by a D [v, 09] value of not more than 80 ⁇ m, in particular not more than 75 gm and especially not more than 70 ⁇ m, and is typically in the range from 20 to 80 ⁇ m, in particular in the range from 30 to 75 pm and especially in the range of 40 to 70 pm.
  • the particle size distribution of the primary particles has a D [v, 09] value in the range from 40 to 80 ⁇ m, in particular in the range from 45 to 75 ⁇ m and especially in the range from 50 to 70 ⁇ m.
  • the D [v, 05] and D [v, 01] values are only of minor importance.
  • the D [v, 05] value of the particle size distribution of the primary particles is in the range of 10 to 50 ⁇ m, especially in the range of 15 to 45 ⁇ m.
  • the D [v, 01] value will typically not fall below a value of 1 pm, in particular 2 pm, and is generally in the range from 1 to 15 pm, especially 2 to 10 pm.
  • Suitable clay minerals contained in the compositions according to the invention are naturally those which are capable of sufficiently adsorbing mycotoxins, in particular aflatoxins.
  • mycotoxins especially for aflatoxin Bi
  • the person skilled in the art can select clay minerals which are suitable as primary particles for the compositions according to the invention in a manner known per se. Methods for this purpose are known from the cited prior art, for. From WO 2007/01 1825 and from A. Marroquin-Cardona et al., Food Addit. Contam. Part A, 2009 26: 733-743 and T.D. Phillips in Toxicol.
  • suitable primary particles are those clay minerals whose suspension in water at pH 6.5 and 22 ° C. has a Qmax - Ne t for aflatoxin Bi of at least 0.1 mol / kg, especially at least 0.15 mol / kg and especially at least 0.2 mol / kg.
  • the Q max - ⁇ Ne t corresponds to the maximum possible loading of the clay minerals with aflatoxin B1 under the conditions mentioned and is calculated by extrapolation of the adsorption isotherms (Langmuir application) to high concentrations of the aflatoxin.
  • O max value The method for determining the O max value is described by A. Marroquin-Cardona et al., Food Addit. Contam. Part A, 2009 26: 733-743 and by TD Phillips in Toxicol. 1999: 52: 118-126. for aflatoxin B1 and in WO 2007/01 1825.
  • Suitable clay minerals are in particular phyllosilicates based on aluminum-containing silicates, especially based on calcium- or magnesium-containing aluminum silicates, especially those which contain water of hydration and which are referred to as hydrated aluminum silicates.
  • the term "based on” means that said specific clay mineral constitutes at least 50% by weight, in particular at least 55% by weight, of the total mass of the clay mineral.
  • examples of such clay minerals are those based on clay minerals of the Strunz classes 9. EC.05 (talc group), 9. EC.40 (montmorillonite group), 9.EC.45 (saponite group) and 9 EC.50 (vermiculite group). Of these, those based on calcium-containing montmorillonites and those based on magnesium-containing montmorillonites are particularly preferred.
  • the clay minerals used as primary particles are typically treated fractions of naturally occurring clay minerals. These usually contain other mineral constituents, which need not necessarily be clay minerals, but can act. Accordingly, the content of the here referred to as preferred clay minerals in the primary particles, based on the total mass of the primary particles, at least 50 wt .-%, in particular at least 55 wt .-%.
  • the clay minerals used can accordingly contain further mineral constituents, which, however, preferably constitute not more than 45% by weight of the particular clay mineral. Such constituents are, for example, quartz, mica, feldspar, pyrites and calcites as well as clay minerals which differ from the respective main or base sistone mineral.
  • the clay minerals contain no or only small amounts of heavy metals which are toxic to the human or animal organism when ingested, such as cadmium, lead, arsenic, nickel or chromium.
  • heavy metals which are toxic to the human or animal organism when ingested, such as cadmium, lead, arsenic, nickel or chromium.
  • the proportion of toxic heavy metals is typically below the limit values provided for this purpose. By contrast, higher iron contents are harmless.
  • clay minerals which have a content of hydrated aluminum silicates of at least 50% by weight, especially at least 55% by weight.
  • the hydrated aluminum silicates are selected from hydrati cal calcium aluminum silicates and hydrated magnesium aluminum silicates.
  • clay minerals are preferred which have a content of layer silicates from the group of montmorillonites of at least 50% by weight, especially at least 55% by weight.
  • it concerns clay minerals, which have a content of phyllosilicates from the group of calcium-containing montmorillonite of at least 50 wt .-%, especially at least 55 wt .-%.
  • Such a clay mineral based on a calcium-containing montmorillonite is the commercially available product NovaSil Plus® from BASF SE, which is a bentonite containing calcium montmorillonite.
  • finely divided clay minerals described in US 2012/0328672 in particular clay minerals, which have a content of phyllosilicates from the group of the calcium-containing montmorillonites of at least 50% by weight, especially at least 55% by weight, and whose particle size Sizes below 63 ⁇ m (mesh 250) and especially below 44 ⁇ m (mesh 325), e.g. B. sieve fractions in which at least 95% of the particles have a size in the range of 5 to 60 pm and especially 5 to 44 pm.
  • compositions according to the invention comprise at least one water-soluble organic binder which holds or glues together the primary particles to form an agglomerate.
  • the powder particles of the compositions according to the invention have an irregular structure, which is often referred to as blackberry structure.
  • water-soluble binders With regard to the water-soluble binders, the term water-soluble means that the binder has a solubility of at least 10 g / l, in particular at least 20 g / l, at 20 ° C. in deionized water.
  • the water-soluble binders are preferably suitable for use in foods or animal feeds and are especially approved for this purpose.
  • Suitable binders according to the invention are selected from food-grade mono-, di- and polysaccharides, especially those mono-, di- and polysaccharides based on glucose and / or fructose.
  • the binders are selected from glucose, fructose, sucrose, maltose, starch degradation products with a DE value in the range from 2 to 50, in particular in the range from 2 to 30, lipophilic starch derivatives and cold water-soluble starches.
  • the binders according to the invention not only have the advantage that the affinity of the clay minerals is substantially or completely retained and good compatibility with foodstuffs is ensured.
  • the formation of coarse-particle granules is less pronounced, in particular in comparison with other binders, and it is possible to set narrower particle size distributions. In this way, higher yields can be achieved.
  • starch degradation products with a DE value in the range from 2 to 50, in particular with a DE value in the range from 2 to 30, are above all starch hydrolysates and especially maltodextrins with a DE value in the range from 2 to 50, in particular with a DE value in the range of 2 to 30.
  • lipophilic starch derivatives are starches and starch hydrolysates modified with lipophilic groups, eg. For example, with alkylsuccinic acid groups and / or alkenylsuccinic acid-modified starches or their salts, in particular their sodium salts, wherein the alkyl or alkenyl radical is usually unbranched and preferably 6 to 20 and especially 8 to 18 C Carries atoms.
  • lipophilic starch derivatives are starches and starch hydrolysates which are modified with Cs-C-is fatty acids.
  • Preferred lipophilic starch derivatives are starches and starch hydrolysates which have been modified with octenylsuccinic acid and their salts, in particular their sodium salts.
  • Cold-water-soluble starches are starches which are completely soluble or swellable in water at 20 ° C. These are typically starches with a high amylose content of preferably> 50% by weight.
  • the cold-water-soluble starches may be starches which naturally have a high amylose content, eg. As waxy starches, as well as starch fractions with high amylose content.
  • binders particular preference is given to di- and oligosaccharides which have the at least one glucose unit, in particular lactose and starch degradation products, in particular maltodextrins, with one having a DE value in the range from 2 to 50, in particular with a DE value Range from 2 to 30.
  • a particularly preferred group of embodiments relates to compositions in which the binder is selected from starch degradation products, in particular maltodextrins, with one having a DE in the range from 10 to 50.
  • compositions in which the binder is selected from lactose.
  • the proportion of binder, based on the total mass of the clay mineral and the binder is generally at least 1% by weight, in particular at least 5% by weight especially at least 10% by weight.
  • the proportion of binder, based on the total mass of Tonmine- rals and the binder, 50 wt .-%, especially 40 wt .-% and especially 35% by weight does not exceed.
  • the powders according to the invention generally contain at least 50% by weight, in particular at least 60% by weight and especially at least 65% by weight, e.g. From 50 to 99% by weight, in particular from 60 to 95% by weight and especially from 65 to 90% by weight, of the clay mineral, the details in% by weight being based on the total mass of the clay mineral and the binder.
  • the powder may also contain small amounts of water due to the production.
  • the water content will generally not exceed 10 wt .-%, based on the total mass of the powder and is often in the range of 1 to 10 wt .-%, based on the total mass of the powder.
  • compositions according to the invention can be prepared analogously to agglomeration processes which are known per se and are suitable for the production of powders, for example by spray drying processes and fluidized bed agglomeration processes.
  • agglomeration processes which are known per se and are suitable for the production of powders, for example by spray drying processes and fluidized bed agglomeration processes.
  • Such methods are generally known to the skilled person, z. From H. Mollet and A. Grubenmann, "Formulation Technology", 1st Edition, Wiley VCH Verlag GmbH, Weinheim 2001, Chapters 6.2.7 and 6.2.8 and the literature cited therein and R.H. Perry et al. (Ed.) "Perry's Chemical Engineers' Handbook," 7th Edition, McGraw Hill, New York 1997, 20-77-20-79 and the literature cited therein.
  • Such a process typically comprises the agglomeration of a clay mineral dust whose particle size distribution typically corresponds to the particle size distribution of the primary particles in the powder particles of the composition according to the invention.
  • the particle size distribution of the set clay mineral dust by a D [v, 09] value, determined by static laser light scattering according to ISO 13320: 2009, below 80 gm, in particular at most 75 gm and especially at most 70 gm characterized and is typically in the range of 20 to 80 gm, in particular in the range from 30 to 75 gm and especially in the range from 40 to 70 gm.
  • D [v, 01] and D [v, 05] values of the particle size distribution of the clay mineral dust the statements made above for the particle size distribution of the primary particles apply analogously ,
  • the binder required for the agglomeration of the particles of the clay mineral dust is used here in the form of an aqueous solution of the water-soluble organic binder.
  • Such an aqueous solution usually contains the water-soluble organic binder in a concentration of 1 to 30% by weight, in particular in a concentration of 2 to 25% by weight or 5 to 25% by weight and especially 10 to 25 wt .-%.
  • the solution may also contain other constituents other than water.
  • these other ingredients may be volatile or non-volatile. These include, for example, impurities or aids, eg. As stabilizers that may be contained in the commercially available binders, but also additives that cause stabilization of the powdered composition on storage. A significant advantage of the invention is to be seen in the fact that such additional stabilizing agents are generally not required.
  • the aqueous solution preferably contains not more than 20% by weight, in particular not more than 10% by weight, based on the binder contained in the aqueous solution, of constituents which are different from the binder.
  • the type of treatment of the clay mineral dust with the aqueous solution of the water-soluble, organic binder is determined in a manner known per se according to the type of agglomeration process and is usually carried out by spraying the aqueous solution of the binder on a moving Tonmine- ralstaub or by spraying together the aqueous solution of the binder with the clay mineral dust.
  • the preparation of the compositions according to the invention is preferably carried out by a fluidized-bed agglomeration process.
  • a fluidized bed of the clay mineral dust is produced and the aqueous solution of the water-soluble organic binder is sprayed onto the clay mineral dust present in the fluidized bed.
  • a gas stream that is, a gas stream through the clay mineral lei th and thereby produce a fluidized bed of the clay mineral.
  • one will provide rotating elements to aid formation of the fluidized bed.
  • the device is operated such that the flow rate V of the gas flow in the device is at least 1.2 times, in particular at least 1.5 times, the flow rate of the gas stream required to produce the fluidized bed, which is also hereafter is referred to as V min .
  • V min the flow rate of the gas stream required to produce the fluidized bed
  • the flow velocity V will not exceed 10 times the value, in particular 5 times the value of V m in.
  • the spraying can be carried out from below and thus in cocurrent with the gas stream (bottom spray method) or from above and thus in countercurrent to the gas stream (top spray method) or tangentially to a fluidized bed (tangential spray method). Procedure). Preferred is the top spray method.
  • the fluidized bed process is carried out at temperatures above 20 ° C and below the boiling point of the aqueous solution of the binder.
  • Decisive here is the temperature in the fluidized bed, which corresponds approximately to the exhaust air temperature.
  • the process will be carried out so that the temperature in the fluidized bed is in the range of 30 to 80 ° C. Higher temperatures are also possible.
  • the temperature of the gas stream will be chosen to be in the range of from 40 to 150 ° C.
  • the temperature difference between incoming and exiting air flow is at least 10 K, z. B. 10 to 100 K.
  • the fluidized bed process makes it possible to adjust the particle size of the powder particles of the inventive composition, for.
  • the connections are known in principle, z. From RH Perry et al. (Ed.) "Perry's Chemical Engineers'Handbook,” 7th Edition, McGraw Hill, New York 1997, 20-79, Tables 20-46. The exact parameters can be determined by the skilled person via routine tests.
  • compositions according to the invention are particularly suitable as an additive in powdered foodstuffs and feedstuffs, since they are easy to incorporate, do not segregate and, moreover, are not undesirable in the ready-to-consume products prepared from the powdered foodstuffs. cause sensory effects.
  • Suitable powdered foodstuffs and feedstuffs are, above all, those foods in which there is the danger of mold being attacked or which may already contain mycotoxins, especially aflatoxins, as a result of the preparation.
  • powdery foods and feedstuffs in particular flours, especially flours of cereals or pseudo cereals such as wheat, rye, barley, oats, emmer, spelled, einkorn, millet, triticale, amaranth, rice or maize, but also to flours of nuts, nuts and oilseeds, z.
  • flours especially flours of cereals or pseudo cereals such as wheat, rye, barley, oats, emmer, spelled, einkorn, millet, triticale, amaranth, rice or maize
  • nuts nuts and oilseeds
  • z for example, peanut, walnut, Brazil nut, sesame, sunflower, pumpkin seed, apricot kernel, pea, soybean or lentil flour, flours from starchy fruits such as cassava and potato.
  • beverage powder for.
  • milk powder and dried fruit juice or tea extracts are also suitable.
  • compositions according to the invention in non-powdery, for example liquid or pasty or semi-solid products in which there is a risk of infestation by mold fungi or which may already contain mycotoxins, especially aflatoxins, as a result of the preparation.
  • non-powdery for example liquid or pasty or semi-solid products in which there is a risk of infestation by mold fungi or which may already contain mycotoxins, especially aflatoxins, as a result of the preparation.
  • non-powdery for example liquid or pasty or semi-solid products in which there is a risk of infestation by mold fungi or which may already contain mycotoxins, especially aflatoxins, as a result of the preparation.
  • mycotoxins especially aflatoxins
  • composition according to the invention required for effective additive formation depends in a manner known per se on the possible contamination of the food or feed by mycotoxins and is generally 0.1 to 2.0% by weight, in particular from 0.5 to 1.5% by weight, calculated as clay mineral and based on the total amount of the foodstuff.
  • the particle size distribution was determined by static laser light scattering of the resulting agglomerates by means of a Mastersizer 2000 from Malvern Instruments Ltd. (Sample application was carried out as a powder).
  • the particle size distribution of the powder compositions according to DIN 66165-1: 2016-08 was determined by means of a vibratory sieving machine VS 1000 from Retsch (Haan, Germany), which was equipped with 6 test sieves of the following mesh size 250 gm, 212 gm , 180 gm, 125 gm, 106 gm and 63 gm.
  • 12880 2000 by drying a sample of the powder at temperatures in the range of 105 ⁇ 5 ° C at ambient pressure to constant weight.
  • the binder content in the powders is determined from the ratio of feeds, i. submitted clay mineral and amount of sprayed binder solution, taking into account the binder concentration of the solution and the residual moisture of the powder calculated.
  • the clay mineral used was a commercial calcium bentonite having a montmorillonite content of at least 60% by weight and screened to a particle size of ⁇ 63 gm (230 mesh).
  • the starting material had the following particle size distribution:
  • clay mineral used in the following examples can also be a US 2012/0328672 by fractionation of a commercial calcium bentonite with a montmorillonite content of at least 60 wt .-% produced clay mineral, which was sieved to a particle size ⁇ 44 pm (350 mesh).
  • Binder 1 Commercial maltodextrin with a DE value of 19
  • Binder 2 Commercial, modified with octenyl succinic anhydride
  • Binder 3 Commercial maltodextrin with a DE value of 47
  • Binder 4 Lactose monohydrate - food grade
  • Binder 5 partially saponified polyvinyl alcohol (degree of hydrolysis 87-88 mol%) of which 4% strength by weight aqueous solution had a viscosity at 20 ° C., determined in accordance with DIN 53015 of 5-6 mPas (Kuraray Poval 6-88)
  • the preparation of the compositions described in the following Examples 1 and 2 was carried out by spray agglomeration.
  • the spray agglomeration was carried out in a fluidized-bed granulator GPCG 3 from Glatt, operated in top-spray mode with a compressed-air two-fluid nozzle.
  • Example 1 Spray Agglomeration with Binder 1
  • the fluidized bed was produced by means of an air flow with a temperature of 60 ° C. and a volume velocity of 77 m 3 lr 1 .
  • the spray pressure was 2 bar.
  • the exhaust valve was 33% open.
  • the product obtained was a finely divided, flowable, non-hygroscopic powder having a binder content of about 20% by weight.
  • the bulk density was 429 g / l.
  • the powder did not dust.
  • Microscopic analysis of the powder showed that the particles have an irregular shape of bonded together primary particles (blackberry structure).
  • the particle size distribution determined by means of light scattering, is given in the following Table 1.
  • the powders were prepared under the conditions given for Example 1. In this case, 1558 g of clay mineral were placed in the fluidized-bed granulator and transferred to a fluidized bed. On the fluidized bed was from above, d. H. in countercurrent to the air flow, within 151 min. With constant spray rate 3696 g of a 1 1, 2 wt .-% solution of binder 2 in water sprayed (414 g of binder 2). Then under the same conditions within 25 min. Another 804 g of 1 1, 2 wt .-% solution of binder 2 in water sprayed (90.0 g of binder 2). The product obtained was a finely divided, flowable, non-hygroscopic powder having a binder content of about 24.4% by weight. The bulk density was 303 g / l. Unlike the non-agglomerated clay mineral, the powder did not dust.
  • Examples 3 to 6 a 20 wt .-% aqueous solution of the binder 1 was used. In Examples 7 to 10, a 20 wt .-% aqueous solution of the binder 3 was used. In Examples 11 to 14, a 16% strength by weight aqueous solution of binder 4 was used. In the comparative example, a 9.5% strength by weight solution of the binder 5 was used.
  • the examples and the comparative example show that, in contrast to the binders according to the invention, the binder polyvinyl alcohol leads to very coarse-particle powders even at low use. In addition, spraying caused clogging of the spray nozzle.
  • the white maize flour with only 250 ppm of the vitamin mixture were additized in the same way and processed in the manner described to Ugali. Subsequently, the two Ugali samples were examined for their organoleptic properties.

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  • Polymers & Plastics (AREA)
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  • Inorganic Chemistry (AREA)
  • Nutrition Science (AREA)
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  • Botany (AREA)
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  • Animal Husbandry (AREA)
  • Fodder In General (AREA)

Abstract

La présente invention concerne des compositions en poudre, dont les particules de poudre contiennent au moins un minéral argileux et au moins un liant organique soluble dans l'eau. L'invention concerne également un procédé de production desdites compositions et l'utilisation des compositions dans des produits alimentaires, en particulier des produits alimentaires en poudre, par exemple des farines de céréales. Dans les compositions en poudre selon l'invention, les particules de poudre contiennent au moins un minéral argileux et au moins un liant organique soluble dans l'eau, au moins 80 % en volume des particules de poudre contenues dans la composition présentant un diamètre de particule de l'ordre de 70 à 350 µm, et le minéral argileux étant présent dans les particules de poudre sous la forme de particules primaires agglomérées dont la distribution granulométrique est caractérisée par une valeur D[v, 09] inférieure à 80 µm, le diamètre de particule et la valeur D[v, 09] indiqués dans les présentes étant les valeurs déterminées par diffraction laser statique selon la norme ISO 13320:2009.
PCT/EP2019/053981 2018-02-19 2019-02-18 Composition en poudre, contenant un minéral argileux Ceased WO2019158756A1 (fr)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU548773B1 (en) 1984-12-03 1986-01-02 David John Kingston High montmorillonite content stock feed supplement
JPS63312105A (ja) * 1987-06-15 1988-12-20 Kunimine Kogyo Kk 球状粘土基剤の製造方法
WO1992005706A1 (fr) 1990-10-01 1992-04-16 Engelhard Corporation Aliment pour animaux contenant de l'argile de montmorillonite utilisee comme additif
US5165946A (en) 1990-03-07 1992-11-24 Engelhard Corporation Animal feed additive and method for inactivating mycotoxins present in animal feeds
AT397756B (de) * 1990-08-10 1994-06-27 Interpremix Futtermittel Und P Futtermittelzusatz
WO2007011825A2 (fr) 2005-07-19 2007-01-25 Texas Enterosorbent, Inc. Aliments et aliments fourrages a preservatifs et additifs
US20120328672A1 (en) 2011-06-15 2012-12-27 Craig Conrad Composition and method of separating bentonite into particles having discrete size and density ranges capable of binding biological toxins and chemotherapeutic agents.

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU548773B1 (en) 1984-12-03 1986-01-02 David John Kingston High montmorillonite content stock feed supplement
JPS63312105A (ja) * 1987-06-15 1988-12-20 Kunimine Kogyo Kk 球状粘土基剤の製造方法
US5165946A (en) 1990-03-07 1992-11-24 Engelhard Corporation Animal feed additive and method for inactivating mycotoxins present in animal feeds
AT397756B (de) * 1990-08-10 1994-06-27 Interpremix Futtermittel Und P Futtermittelzusatz
WO1992005706A1 (fr) 1990-10-01 1992-04-16 Engelhard Corporation Aliment pour animaux contenant de l'argile de montmorillonite utilisee comme additif
WO2007011825A2 (fr) 2005-07-19 2007-01-25 Texas Enterosorbent, Inc. Aliments et aliments fourrages a preservatifs et additifs
US20120328672A1 (en) 2011-06-15 2012-12-27 Craig Conrad Composition and method of separating bentonite into particles having discrete size and density ranges capable of binding biological toxins and chemotherapeutic agents.

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Title
"Perry's Chemical Engineers' Handbook", 1997, MCGRAW HILL, pages: 20 - 77,20-79
"Perry's Chemical Engineers' Handbook", 1997, MCGRAW HILL, pages: 20 - 79
A. MARROQUIN-CARDONA ET AL., FOOD ADDIT. CONTAM, vol. 26, 2009, pages 733 - 743
A. MARROQUIN-CARDONA ET AL., FOOD ADDIT. CONTAM., vol. 26, 2009, pages 733 - 743
B. P. WANG ET AL., FOOD ADDITIVES AND CONTAMINANTS, vol. 25, no. 5, 2008, pages 622 - 634
H. MOLLET; A. GRUBENMANN: "Formulation Technology", 2001, WILEY VCH VERLAG GMBH
T.D. PHILLIPS ET AL., ADVANCES IN EXPERIMENTAL MEDICINE AND BIOLOGY, vol. 504, 2002, pages 157 - 171
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T.D. PHILLIPS ET AL., POULTRY SCIENCE, vol. 67, 1988, pages 243 - 247
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