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
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
  • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
  • A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
  • C08L1/02—Cellulose; Modified cellulose
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L39/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions of derivatives of such polymers
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L89/00—Compositions of proteins; Compositions of derivatives thereof
  • C08L89/005—Casein

Definitions

• the invention relates to formulations consisting of cellulose, alkali caseinate and crosslinked homopolymers or copolymers of Isf-vinyl lactams and / or polymers based on a basic N-vinyl heterocycle with a pK a value of at least 3.8, the production and use thereof for the treatment of biological liquids of vegetable origin in a non-fermented, partially fermented or fully fermented state.
• the disadvantage with the native and modified proteins and the crosslinked polymers is that they require a certain pretreatment by swelling. This means a very large amount of time. Since the vast majority of products medium is extracted together with the suspended turbidity by sedimentation, this step is also very time-consuming and can take up to 6 weeks. In addition, these products have the disadvantage that they do not remove all phenolic substances or classes of substances to the same extent, but that there is in each case a preferred interaction with a certain group of phenolic substances.
• the anfal ⁇ lumbar sediments are mostly schleimigpast Surprise masses, which is removed by a downstream treatment liquid in order to bring them into a results processed further or landfillable state.
• the invention was therefore based on the object of finding a product which does not have the disadvantages mentioned above and is able to reduce the content of different groups of phenolic compounds and at the same time also the concentration of dissolved heavy metals. At the same time, manageability should be improved by eliminating the complex preparation phase of the feed material.
• the invention relates to solid preparations consisting of
• alkali casemate (b) is understood in the following to mean above all potassium casemate, which is obtained by treating casem with potassium hydroxide solution or solutions of alkaline potassium salts of organic or inorganic acids such as e.g. Phosphoric acid or citric acid is obtained.
• Casem comes from short-term skimmed milk with a maximum fat content of 0.05%. Thickening to separate the whey is done with acids by adjusting the pH to the isoelectric point of the casein 4.5 + 0.2. After heat treatment, separation of the whey and hot water washing, the raw casa is obtained. This is further processed as a wet break or after drying to Casemat by bringing it to the solution by adding potassium hydroxide or other alkali hydroxides. The drying takes place by means of spray drying or extrusion processes.
• the products obtained which are particularly suitable for the preparation of the formulations according to the invention, have a water content of 5 to 10% and a protein content of 87% to 92% and an ash content of 3% to 8%.
• N-Vmyllactams here mean 3-methyl-N-vmylpyrrolidone, in particular N-Vmylcaprolactam and N-Vmylpyrrolidone (VP), which are used all or in a mixture with one another.
• the monomers (c) are used in an amount of 90% to 99.5%, preferably 98% to 99% by weight, based on the total polymer.
• Suitable crosslinkers are those which contain two or more radically copolymerizable Vmyl phenomenon in the molecule.
• Particularly suitable are alkylenebisacrylamides such as methylenebisacrylamide and N, N'-bisacryloylethylene diamine, also N, N '-divmylethylene urea, N, N'-divmylpropylene urea, ethylidene dis-3 - (N- inyl-pyrrolidone) and N, N' - Divmyldiimidazolyl - (2, 2 ') -1, 4-butane and 1, 1' -Bis (3, 3 '- mylbenz ⁇ m ⁇ dazol ⁇ d-2-one) 1, 4-butane.
• crosslinking agents are, for example, alkylene glycol di (meth) acrylates such as ethylene glycol di (meth) acrylate and tetramethylene glycol di (meth) acrylate, aromatic divmyl compounds such as divmylbenzene and divmyltoluene as well as alkyl acrylate, divmyldioxane, pentaerythritol and their triallyl ether. In the presence of water they are of course only polymerized suitable insofar as they are soluble in the aqueous monomer mixture.
• alkylene glycol di (meth) acrylates such as ethylene glycol di (meth) acrylate and tetramethylene glycol di (meth) acrylate
• aromatic divmyl compounds such as divmylbenzene and divmyltoluene as well as alkyl acrylate, divmyldioxane, pentaerythritol and
• the crosslinkers are used in an amount of 0.5-10, preferably 1-2% by weight, based on all the monomers of the polymer.
• Basic Vmylheterocycles are to be understood here as saturated and aromatically unsaturated heterocycles with a Vmyl distr and at least one basic tertiary Rmg atom with a pK a of at least 3.8.
• the ring can also carry alkyl groups with 1 to 4 carbon atoms, phenyl or benzyl groups or also a fused second ring. Examples include: N-Vmylimidazole (VI) and derivatives thereof we 2-methyl-l-vmyl ⁇ m ⁇ dazol, 4-methyl-l-vmyl ⁇ m ⁇ dazol, 5-methyl-l-vmyl ⁇ m ⁇ dazol,
• 2-ethyl-1-methylimidazole 2-propyl-1-vinylimidazole, 2-isopropyl-1-methylimidazole, 2-phenyl-1-methylimidazole, 1-methyl-4,5-benzimidazole.
• the following can also be used, for example: 2-methylpym, 4-methylpmdm and 2-methyl-5-methylpyrm. Mixtures of basic methyl heterocycles with one another can of course also be used.
• Preferred monomers for this are N-methylimidazole and 2-methyl-N-ylimidazole.
• These monomers are used in an amount of 50-99.5, preferably 60-96% by weight, based on the total polymer.
• the comonomers are polymerized in amounts of up to 49.5, preferably up to 30% by weight, particularly preferably up to 20% by weight, based on the total monomer mixture.
• suitable comonomers are styrene, acrylic ester, methyl ester, acrylic ide and N-methyl dihydropyridme.
• N-Vmyllactams such as 3-methyl-N-mylpyrrolidone, ms-particular N-Vmylcaprolactam and N-Vmylpyrrolidone (VP) are preferably used as comonomers.
• Suitable crosslinkers for the polymers (d) are also those which contain two or more free-radically copolymerizable methyl groups in the molecule.
• Particularly suitable are alkylenebisacrylamides such as methylenebisacrylamide and N, N'-bisacryloylethylene diamine, also N, N'-divmylethylene urea, N, N'-divmylpropylene urea, ethylidene-b ⁇ s-3 - (N-vmylpyrrolidone) and N, N'-divi- nyldumidazolyl- (2,2 ') -1,4-butane and 1,1'-bis (3,3' -vmylbenzimi-dazolid-2-one) -1,4-butane.
• crosslinking agents are, for example, alkylene glycol di (meth) acrylates such as ethylene glycol di (meth) acrylate and tetramethylene glycol di (meth) acrylate, aromatic divinyl compounds such as divinylbenzene and divinyltoluene as well as allyl acrylate, divinyldioxane, pentaerythritol triallyl ether and mixtures thereof.
• alkylene glycol di (meth) acrylates such as ethylene glycol di (meth) acrylate and tetramethylene glycol di (meth) acrylate
• aromatic divinyl compounds such as divinylbenzene and divinyltoluene as well as allyl acrylate, divinyldioxane, pentaerythritol triallyl ether and mixtures thereof.
• polymerization in the presence of water they are of course only suitable if they are soluble in the aqueous monomer
• crosslinkers are nevertheless used for the polymers (d) in an amount of 0.5-10, preferably 1-4% by weight, based on all the monomers of the polymer.
• Celluloses (a) which are particularly suitable for the use according to the invention are those which contain less than 1% water-soluble substances and have a fiber length of 20 ⁇ m to 200 ⁇ m, preferably 25 to 50 ⁇ m, and a fiber diameter of 5 ⁇ m to 50 ⁇ m, preferably have 10 to 20 ⁇ m.
• Alkalic caseinates (b) which are particularly suitable for the use according to the invention are potassium caseinates with good solubility, preferably greater than 99% and high bacteriological requirements, preferably with a total bacterial count of less than 5000 kBE / g, yeast less than 10 / g and mold less than 10 / g.
• Polymers (c) which are particularly suitable for the use according to the invention are those composed of N-vinylpyrrolidone (VP) and N, N '-divmylethyleneurea (DVEH), in particular those composed of 98-99.5% by weight of VP and 0.5 -2.0% by weight DVEH.
• VP N-vinylpyrrolidone
• DVEH N, N '-divmylethyleneurea
• Polymers (d) which are particularly suitable for the use according to the invention are those of N-vinylimidazole (VI), N-vinylpyrrolidone (VP) and N, N '-divinylethyleneurea (DVEH), in particular those of 80-90% by weight of VI, 5-15 wt% VP and 2-5 wt% DVEH.
• VI N-vinylimidazole
• VP N-vinylpyrrolidone
• DVEH N '-divinylethyleneurea
• the particle size distribution of the polymer particles (c) and (d) is usually in the range from 0.01 to 100 ⁇ m, preferably in the range from 5 to 50 ⁇ m.
• the preparation is prepared in a process variant 1 in such a way that in a solution of alkali caseinate (b), preferably in a concentration of 2% by weight to 20% by weight dry matter, the cellulose (a) and the polymers (c) and / or (d) suspended become.
• concentrations of components (c) and / or (d) are between 2% and 20% of the dry matter of the suspension.
• the suspension is spray-dried, preferably using a single-component nozzle at pressures from 50 bar to 150 bar, preferably less than 100 bar.
• process variant 2 components (a) and (b) are introduced as shown in process variant 1 by suspending the cellulose (b) in an aqueous solution of the alkali caseinate. This suspension is then atomized, the resulting primary aerosol being brought directly into contact with the powdery polymer components in the moist state and the resulting polymer-containing suspension droplets being dried. Components (c) and / or (d) are blown into the atomization zone of the tower in a correspondingly dry manner.
• powders are produced according to process variants 1 or 2, first dried in the tower to a residual moisture content of 10 to 15% by weight and to achieve an additional agglomeration effect at a powder temperature of 70 ° C up to 40 ° C, preferably from 60 ° C to 50 ° C, carried out on tape for post-drying and adjusted to a residual moisture content of 6-10% by weight at a supply air temperature of 60 ° C to 110 ° C. Post-drying at an elevated temperature results in an additional agglomeration effect.
• Partially fermented or completely fermented biological liquids of plant origin are treated with 25 to 250 g / hl, in a preferred form with 40 to 150 g / hl and in a particularly preferred application form with dosage amounts of 50 to 100 g / hl.
• Particularly suitable liquids are wine, grape must or wine-like drinks and their non-fermented musts (berry and fruit juices). All forms of solid / liquid separation, such as centrifuges, decanters, layer and diatomaceous earth filtration and membrane technologies, are suitable for separating the formulations from the application medium.
• V f filtrate volume in m 3 V f filtrate volume in m 3 , t filtration time in s, A filter area in m 2 ,
• the preparations according to the invention can be used to stabilize liquids of vegetable origin in a particularly advantageous manner against changes in color and taste.
• alkali caseinate and cross-linked! By precipitating the caseinate at the IEP in close connection with the crosslinked polymer, the polymer is increased in surface area, which has a particularly effective stabilizing effect against oxidative changes.
• a formulation consisting of 70 kg of cellulose, 20 kg of potassium casemate and 10 kg of polymer (d) with a proportion of N-vinylimidazole (VI) of 90% by weight and a proportion of N-vinylpyrrolidone (VP) of 7% by weight .-% and a proportion of N, N '-divinylethylene urea (DVEH) of 3 wt .-% was prepared by dissolving the potassium casemate in 400 l of water at 60 ° C and suspending the cellulose therein. The suspension was atomized at 185 ° C. at 70 bar through a 10-component nozzle and the polymer was blown into the atomization zone.
• a formulation consisting of 50 kg cellulose, 30 kg potassium casemate, 10 kg polymer (c) and 10 kg polymer (d) was prepared as follows:
• the potassium caseinate (b) was dissolved in 320 l of water at 60 ° C. and the cellulose (c) was suspended in it.
• the suspension was atomized at 180 ° C. at 50 bar through a single-component nozzle and a mixture of the two polymers (c) and (d) was blown into the atomization zone with a mixing ratio of 1: 1.
• Table 1 summarizes the findings immediately after treatment and bottle filling and after a storage period of 28 days at 35 50 ° C.
• 25 E absorbance at 320, 420, 520 nm; Layer thickness in cm
• the treatment reduces the browning, expressed as an absorbance value at 420 nm.
• the difference values of the extinctions at 420 nm and 520 nm show that the wine treated has a lower tendency to change color than the untreated comparison.
• Table 2 shows the results immediately after treatment and bottle filling and after a storage period of 28 days at 50 ° C. 45 The bottle was filled with a head space of 150 ml of air. Table 2
• the difference in absorbance at 420 nm confirms that the treated person has less tendency to undergo oxidative color changes than the untreated comparison.
• Table 3 shows the calculated filter medium resistance ß and the mean specific filter cake resistance ⁇ of the three batches.
• the filter properties of the must trub suspensions are significantly improved depending on the dosage of the added formulation.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
• Engineering & Computer Science (AREA)
• Polymers & Plastics (AREA)
• Life Sciences & Earth Sciences (AREA)
• Food Science & Technology (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Biochemistry (AREA)
• Nutrition Science (AREA)
• Bioinformatics & Cheminformatics (AREA)
• General Engineering & Computer Science (AREA)
• General Health & Medical Sciences (AREA)
• Genetics & Genomics (AREA)
• Wood Science & Technology (AREA)
• Zoology (AREA)
• Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
• Medicinal Preparation (AREA)
• Solid-Sorbent Or Filter-Aiding Compositions (AREA)
• Compositions Of Macromolecular Compounds (AREA)

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• 1996
  • 1996-12-18 DE DE19652697A patent/DE19652697A1/de not_active Withdrawn
• 1997
  • 1997-12-04 AU AU58540/98A patent/AU5854098A/en not_active Abandoned
  • 1997-12-04 US US09/319,878 patent/US6232373B1/en not_active Expired - Fee Related
  • 1997-12-04 WO PCT/EP1997/006779 patent/WO1998027150A1/de not_active Application Discontinuation
  • 1997-12-04 EP EP97954353A patent/EP0946636A1/de not_active Withdrawn
  • 1997-12-04 CA CA002275254A patent/CA2275254A1/en not_active Abandoned
  • 1997-12-04 NZ NZ336329A patent/NZ336329A/en unknown
  • 1997-12-16 AR ARP970105906A patent/AR010358A1/es not_active Application Discontinuation
  • 1997-12-17 ZA ZA9711304A patent/ZA9711304B/xx unknown

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