EP1628758A1 - Agent d'adsorption d'albumine dans des liquides albumineux dans le secteur des denrees alimentaires - Google Patents

Agent d'adsorption d'albumine dans des liquides albumineux dans le secteur des denrees alimentaires

Info

Publication number
EP1628758A1
EP1628758A1 EP04713056A EP04713056A EP1628758A1 EP 1628758 A1 EP1628758 A1 EP 1628758A1 EP 04713056 A EP04713056 A EP 04713056A EP 04713056 A EP04713056 A EP 04713056A EP 1628758 A1 EP1628758 A1 EP 1628758A1
Authority
EP
European Patent Office
Prior art keywords
layered silicate
protein
potassium
bentonite
content
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.)
Withdrawn
Application number
EP04713056A
Other languages
German (de)
English (en)
Inventor
Ulrich Sohling
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sued Chemie AG
Original Assignee
Sued Chemie AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE20308122U external-priority patent/DE20308122U1/de
Priority claimed from DE2003123499 external-priority patent/DE10323499A1/de
Application filed by Sued Chemie AG filed Critical Sued Chemie AG
Publication of EP1628758A1 publication Critical patent/EP1628758A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/02—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material
    • C12H1/04—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material
    • C12H1/0408—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages combined with removal of precipitate or added materials, e.g. adsorption material with the aid of ion-exchange material or inert clarification material, e.g. adsorption material with the aid of inorganic added material
    • 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

Definitions

  • the invention relates to an agent, in particular for the adsorption of protein from protein-containing liquids in the food sector, on the basis of smectic layered silicates, in particular on the basis of bentonite.
  • protein-containing liquids in the food sector from which protein substances are to be advantageously adsorbed with the aid of the agent according to the invention, primarily includes white wines.
  • a removal of residual protein from red wine or other wines, fruit juices, vinegar and beer is also possible sauces, such as Asian fish sauces, can be enhanced by adsorbing the residual protein are generally understood to mean substances and materials containing protein or oligopeptides.
  • Natural sodium bentonites are commonly used in many countries to stabilize proteins in white wines. Typical representatives of this are the so-called Wyoming bentonites. The use of these bentonites is regulated by the so-called International Oenological Codex (IOC), which limits the leaching of heavy metals from the bentonite in a 1% citric acid solution as a model substance for wine.
  • the lead leaching should be ⁇ 20 ppm and the arsenic leaching ⁇ 4 ppm. Further details regulate the magnesium and calcium leaching as well as the content of soluble iron.
  • IOC International Oenological Codex
  • the leaching of sodium from bentonites can be reduced, for example, by using natural bentonites containing alkaline earth metal, such as calcium and / or magnesium bentonite. Due to their lower swelling capacity, these bentonites show a lower protein adsorption compared to natural sodium bentonites with the same amount used. This can be explained by the fact that the calcium bentonites can never be completely delaminated into colloidal bentonite platelets, but instead form piles of bentonite platelets when dispersed, which overall provide a lower specific surface area for the adsorption of colloidal protein.
  • Laviosa Chimica Mineraria SpA, Livorno, Italy offers under the trade names "Enobent ® GK and” Enobent ® K "bentonites for the adsorption of protein from protein-containing drinks, such as wines and fruit juices, which have a low content of exchangeable sodium ions and have a high content of exchangeable potassium ions According to the chemical analysis, these bentonites contain 3.75% by weight of K 2 0 and 0.48% by weight of Na 2 0.
  • the total cation exchange capacity (IUF; cation exchange capacity, CEC) is at 52 mVal / 100 g, determined by the analysis method described below (IUF analysis)
  • the contents of metal ions which can be leached with tartaric acid are given in Table 1.
  • Table 1 Share of soluble metals in wine bentonite from Laviosa Chimica Mineraria SpA, determined by leaching with 1% tartaric acid in accordance with the German Wine Act (see below), based on bentonite with a moisture content of 10%
  • the invention has for its object to develop a means, in particular for the adsorption of protein from protein-containing liquids, in particular beverages, on the basis of smectic layer silicates, which has a high activity in the removal of colloidally dissolved proteins, but during beverage treatment only releases small amounts of metal ions, especially potassium ions and sodium ions.
  • the invention thus relates to a smectic layer silicate or an adsorbent according to claim 1.
  • Total cation exchange rate means the sum of all exchangeable cations, stated in mVal / 100 g and determined according to the IUF analysis method as explained below before the example part (IUF analysis).
  • the total cation exchange capacity thus includes, for example, the sum of all exchangeable calcium, magnesium, sodium and potassium ions.
  • the bentonite is treated with an ammonium chloride solution to determine the total cation exchange capacity. Due to the high affinity of ammonium ions for bentonite, practically all exchangeable cations are exchanged for ammonium ions. After separation and washing, the nitrogen content of the bentonite is determined and the ammonium ion content is calculated from this.
  • a stoichiometric activation (treatment) here means an activation or treatment with an amount of potassium and / or sodium ions which corresponds to the difference between the total cation exchange capacity (IUF) and the amount of monovalent cations already present in the starting material.
  • the total cation exchange capacity corresponds to a stoichiometric activation only if the smectic layered silicate, for example, contains only magnesium and calcium ions as contains exchangeable cations.
  • natural bentonites often contain sodium and, in rare cases, some potassium as exchangeable cations.
  • the amount of potassium or sodium ions required for stoichiometric activation is calculated from the total cation exchange capacity minus the amount of exchangeable sodium and possibly potassium ions in the non-activated layered silicate.
  • the agent for the adsorption of protein according to the invention when using layered silicates containing alkaline earth metal, for example, only a portion of the exchangeable alkaline earth metal ions can be replaced by potassium, ie the activation takes place under the uchiometry.
  • the smectic layered silicate is activated (treated) with potassium carbonate, in contrast to the sole activation with sodium carbonate, the maximum of the adsorption capacity is already reached with additions of potassium carbonate which are below the stoichiometric amount, based on the cation exchange capacity of the smectic layered silicate for alkaline earth metals.
  • a particularly high adsorbability of the layered silicate is achieved if the content of exchangeable potassium ions is less than 50%, preferably less than 40%, but more than 8%, preferably more than 12% of the total cation exchange capacity of the layered silicate.
  • the smectitic layered silicate is preferably a montmorillonite-containing layered silicate, in particular a bentonite. In addition to bentonites, other smectitic layered silicates, such as hectorite and nontronite, can also be used. Mixtures of the above materials can also be used.
  • the smectitic layered silicates generally, but not necessarily, have a total cation exchange capacity of about 30 to 120 meq / 100 g, preferably about 40 to 110 meq / 100 g.
  • the quantitative ratio between the potassium carbonate and the sodium carbonate used is therefore between approximately 4: 1 and approximately 1: 4, preferably between approximately 2: 1 and 1: 2.
  • the total content of exchangeable potassium and sodium ions in the treated (activated) layer silicate is less than 90%, preferably less than 80% of the total ion exchange capacity of the layer silicate.
  • the content of exchangeable potassium ions or the total content of exchangeable potassium and sodium ions is less than about 80% of the stoichiometric exchange amount of the layered silicate used as the starting material. So clearly substoichiometric amounts of potassium and optionally sodium ions are preferably used to treat the layered silicate.
  • the invention relates to an adsorbent, the content of exchangeable sodium ions being less than 70%, preferably less than 60%, particularly preferably less than 40% of the total ion exchange capacity of the layered silicate.
  • the present invention also relates to a method for producing a smectitic layered silicate or an adsorbent, in particular for adsorbing protein from protein-containing liquids in the food sector, wherein at least one smectitic layered silicate is treated with potassium carbonate and optionally sodium carbonate until the
  • the exchangeable potassium ion content is less than 50%, preferably less than 40%, but more than 8%, preferably more than 12% of the total cation exchangeability of the layered silicate.
  • preference is given to using clearly substoichiometric amounts of potassium and, if appropriate, sodium ions for the treatment of the layered silicate.
  • the content of exchangeable potassium ions or the total content of exchangeable potassium and sodium ions is preferably less than about 80% of the stoichiometric exchange amount of the starting material layered.
  • the contacting can take place in any manner known to the person skilled in the art, e.g. by producing a solid mixture, a suspension with the layered silicate and the potassium carbonate and, if appropriate, the sodium carbonate or by applying or spraying the layered silicate with a solution of the potassium carbonate and optionally the sodium carbonate.
  • the amounts of potassium carbonate or sodium carbonate to be used in order to achieve the desired contents of exchangeable potassium or sodium ions in the agent according to the invention can be easily calculated or determined by routine tests.
  • Another aspect of the present invention relates to the use of the smectic layered silicate according to the invention or the agent for removing protein from protein-containing liquids in the food sector, in particular from wine, particularly preferably from white wine.
  • the layered silicate or agent according to the invention are expressly not excluded.
  • the layered silicate to be examined was dried over a period of two hours at 150 ° C. The dried material was then reacted with an excess of aqueous 2N NH 4 C1 solution under reflux for one hour. After standing for 16 hours at room temperature, the mixture was filtered, the filter cake washed, dried and ground and the NH 4 content in the layered silicate was determined by nitrogen determination (CHN analyzer from Leco). The proportion and the type of metal ions exchanged (“exchangeable cations”) was determined spectroscopically in the filtrate according to DIN 38406, part 22.
  • the bentonite is predispersed in tap water and added to the white wine in appropriate amounts. Typically one examines the concentration range from 50 g to 200 g bentonite / hl wine. After an exposure time of 15 min. the bentonite is centrifuged off and with the help of the protein test by Dr. Nilles the residual protein content is determined photometrically via the absorbance. To determine the residual protein as a function of the addition of bentonite to represent the extinction as a function of the bentonite addition. If all residual protein is removed, a plateau occurs with low extinction coefficients that correspond to the device resolution (about 0.01). All the investigations of the clarifying properties of the bentonites according to the invention and of the comparative examples shown below were carried out using this method.
  • a calcium-containing bentonite with a water content of about 30 to 35% by weight was kneaded, dried and ground with solid sodium carbonate (comparison) or potassium carbonate (invention).
  • the raw bentonite was pre-crushed to pieces less than 3 cm in diameter. If the raw bentonite did not have the specified water content, this was adjusted by spraying with water.
  • the activation was carried out in detail as follows: 350 g of raw bentonite with a water content of about 30 to 35% by weight were placed in a mixing device (for example a Werner & Pfleiderer mixer (Kneader)) and kneaded for 1 minute. Then the corresponding amount of sodium carbonate (for the comparative experiments) or potassium carbonate, optionally together with sodium carbonate (for the products according to the invention) was added and the kneading continued for 10 min. Various amounts of sodium carbonate or potassium carbonate were added in accordance with the examples below, the amounts added being based on the anhydrous bentonite. If necessary, some distilled water was added so that the modeling clay "shears" well.
  • the modeling clay was then broken up into small pieces and dried in a forced-air drying cabinet at about 75 ° C. for 2 to 4 hours at a water content of 10 ⁇ 2%.
  • the dry material was then milled in an impact rotor mill (e.g. in a Retsch mill) over a 0.12 mm sieve.
  • the bentonite activated with sodium carbonate and obtained according to (a) as a comparison substance was kneaded, dried and ground with solid potassium carbonate at a moisture content of about 15 to 40% by weight, with the individual process variant (a ) is being worked on. 3.
  • Example 1 Activation of a natural bentonite (bentonite 1) with potassium carbonate or sodium carbonate
  • bentonite 1 A natural Ca / Mg bentonite (product name EX 0242, available from Süd-Chemie AG; hereinafter referred to as "bentonite 1") was used as the starting bentonite for Example 1, which has the characteristic data given in Table 3, column 2.
  • Bentonite powders were produced from the bentonite 1 and are activated both stoichiometrically and sub-stoichiometrically (see above). In the case of activation with sodium carbonate, an over-stoichiometrically activated sample was also prepared. Since the bentonite 1 already contains small amounts of exchangeable sodium and potassium, the stoichiometric amount of sodium ions or soda or potassium ions or potassium carbonate results from the difference between the total cation exchange capacity and the cation exchange capacity for sodium and potassium. The stoichiometric exchange amount is 61 mVal / 100 g. This speaks an amount of 3.2 wt .-% soda or 4.2 wt .-% potassium carbonate.
  • the sodium or potassium ion contents given in Table 5 relate to the total exchange capacity (IUF) of the finished adsorbent, i.e. of layered silicate treated with potassium carbonate or sodium carbonate.
  • FIGS. 1 and 2 show the test results for the activation with sodium carbonate or potassium carbonate. The curve of the non-activated bentonite is shown for comparison.
  • Table 6a Share of soluble metals in bentonite 1, determined by leaching with 1% tartaric acid in accordance with the German Wine Act, based on bentonite with a moisture content of 10%
  • Table 6b Amount of the potassium ions introduced into the bentonite 1 by activation, based on bentonite with a moisture content of 10% (water content)
  • the metal leaching from the beverage bentonites does not change significantly after activation with potassium carbonate.
  • the exception here is of course the potassium introduced during activation.
  • the values given in Tables 6a and 6b show that less than 70% of the potassium introduced by the activation is leached out with the 1% tartaric acid.
  • the protein adsorption capacity of the bentonite is greatly increased after activation, so that a lower dosage of the bentonite is required for the same protein content in the wine.
  • the entry of heavy metals into the wine is significantly reduced compared to the use of a non-activated bentonite.
  • Example 2 Activation of a bentonite mixture (bentonite 2) with potassium carbonate and mixtures of potassium carbonate / sodium carbonate
  • the stoichiometric amount of potassium carbonate i.e. the amount required for complete activation is 4.8% by weight.
  • the bentonite mixture was activated with potassium carbonate and with a mixture of potassium carbonate and sodium carbonate.
  • the proportions used for the activation are given in Table 10.
  • the proportions relate to bentonite with a moisture content of 10%.
  • Table 10 Proportions of activation reagents for the activation of a bentonite mixture (bentonite 2)
  • the sodium or potassium ion contents given in Table 10 relate to the total cation exchange capacity (IUF) of the layered silicate treated with potassium carbonate or sodium carbonate.
  • Fig. 1 shows the protein adsorption of bentonite 1 (see Example 1), activated (treated) with sodium carbonate. The percentages relate to% by weight.
  • the absorbance values plotted in the Y axis are dimensionless values which are obtained in the measurement described in the analysis method part (according to Dr. Nilles).
  • the X axis indicates the bentonite content used in g / hl of the liquid to be treated;
  • Fig. 2 shows the protein adsorption of bentonite 1 at different degrees of activation with potassium carbonate. The percentages relate are based on% by weight.
  • the extinction values plotted in the Y axis are dimensionless values which are obtained in the measurement described in the analytical method section (according to Dr. Nilles).
  • the X axis indicates the bentonite content used in g / hl of the liquid to be treated;
  • the absorbance values plotted in the Y axis are dimensionless values that are obtained from the measurement described in the analysis method part (according to Dr. Nilles).
  • the X axis indicates the bentonite content used in g / hl of the liquid to be treated.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

L'invention concerne un agent, notamment pour adsorber l'albumine dans des liquides albumineux dans le secteur des denrées alimentaires, cet agent contenant au moins un silicate stratifié smectique doté d'une capacité totale d'échange cationique d'environ 30 à 120 mVal/100g. L'invention est caractérisée en ce que la teneur en ions de potassium est inférieure à 50 %, de préférence inférieure à 40 %, mais supérieure à 8 % et de préférence supérieure à 12 % de la capacité totale d'échange cationique du silicate stratifié. La présente invention porte également sur un procédé pour réaliser un agent d'adsorption ainsi que sur son utilisation préférée.
EP04713056A 2003-05-25 2004-02-20 Agent d'adsorption d'albumine dans des liquides albumineux dans le secteur des denrees alimentaires Withdrawn EP1628758A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE20308122U DE20308122U1 (de) 2003-05-25 2003-05-25 Mittel zur Adsorption von Eiweiß aus eiweißhaltigen Flüssigkeiten auf dem Lebensmittelsektor
DE2003123499 DE10323499A1 (de) 2003-05-25 2003-05-25 Mittel zur Adsorption von Eiweiß aus eiweißhaltigen Flüssigkeiten auf dem Lebensmittelsektor
PCT/EP2004/001688 WO2004103552A1 (fr) 2003-05-25 2004-02-20 Agent d'adsorption d'albumine dans des liquides albumineux dans le secteur des denrees alimentaires

Publications (1)

Publication Number Publication Date
EP1628758A1 true EP1628758A1 (fr) 2006-03-01

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Family Applications (1)

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EP04713056A Withdrawn EP1628758A1 (fr) 2003-05-25 2004-02-20 Agent d'adsorption d'albumine dans des liquides albumineux dans le secteur des denrees alimentaires

Country Status (4)

Country Link
US (1) US20060276333A1 (fr)
EP (1) EP1628758A1 (fr)
AU (1) AU2004241700B2 (fr)
WO (1) WO2004103552A1 (fr)

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DE102005012639A1 (de) * 2005-03-18 2006-09-21 Süd-Chemie AG Verfahren zur Abtrennung von Biomolekülen aus flüssigen Medien
DE102005019089B4 (de) * 2005-04-25 2013-08-01 Süd-Chemie Ip Gmbh & Co. Kg Adsorptionsmittel zur Adsorption von Eiweiß aus eiweißhaltigen Flüssigkeiten sowie dessen Verwendung
US20090221809A1 (en) * 2005-12-09 2009-09-03 Sud-Chemie Ag Method for the sorption of at least one nucleic acid-activated phyllosilicates
DE102005060392A1 (de) * 2005-12-16 2007-06-21 Süd-Chemie AG Verfahren zur Abtrennung von Proteinen aus flüssigen Medien
DE102009023740A1 (de) * 2009-06-03 2011-07-21 Süd-Chemie AG, 80333 Verfahren zum Auftrennen von Pflanzenproteinen
US10674746B2 (en) * 2015-10-27 2020-06-09 Cytozyme Animal Nutrition, Inc. Animal nutrition compositions and related methods
EP3368498A4 (fr) * 2015-10-27 2019-06-12 Cytozyme Animal Nutrition, Inc. Compositions pour l'alimentation animale et procédés associés
JP7306961B2 (ja) * 2019-10-30 2023-07-11 水澤化学工業株式会社 塩基性アミノ酸用吸着剤

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Also Published As

Publication number Publication date
AU2004241700B2 (en) 2008-03-13
US20060276333A1 (en) 2006-12-07
AU2004241700A1 (en) 2004-12-02
WO2004103552A1 (fr) 2004-12-02

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