EP0654527B1 - Procédé de démucilagination d'huiles végetales avec des enzymes - Google Patents

Procédé de démucilagination d'huiles végetales avec des enzymes Download PDF

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Publication number
EP0654527B1
EP0654527B1 EP94203211A EP94203211A EP0654527B1 EP 0654527 B1 EP0654527 B1 EP 0654527B1 EP 94203211 A EP94203211 A EP 94203211A EP 94203211 A EP94203211 A EP 94203211A EP 0654527 B1 EP0654527 B1 EP 0654527B1
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EP
European Patent Office
Prior art keywords
oil
enzymes
degumming
sludge
degummed
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.)
Expired - Lifetime
Application number
EP94203211A
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German (de)
English (en)
Other versions
EP0654527A1 (fr
Inventor
Henning Dr. Buchold
Rudolf Dr. Boensch
Joerg Dr. Schroeppel
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.)
GEA Group AG
Roehm GmbH Darmstadt
Original Assignee
Metallgesellschaft AG
Roehm GmbH Darmstadt
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.)
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Publication date
Application filed by Metallgesellschaft AG, Roehm GmbH Darmstadt filed Critical Metallgesellschaft AG
Publication of EP0654527A1 publication Critical patent/EP0654527A1/fr
Application granted granted Critical
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Anticipated expiration legal-status Critical
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/003—Refining fats or fatty oils by enzymes or microorganisms, living or dead

Definitions

  • the invention relates to a method for degumming Vegetable oil, whereby the vegetable oil is adjusted to a pH of 3 to 6, an aqueous enzyme solution dispersed in the oil, which contains one of the enzymes phospholipase A1, A2 or B, which Enzymes in the oil with stirring at temperatures from 20 to 90 ° C in a degumming reactor can act and from the Degumming reactor withdrawn liquid degummed oil separates.
  • the invention is based, at the beginning mentioned processes the used enzymes in Degumming process at least partially to reuse. According to the invention, this is done in that the liquid withdrawn from the degumming reactor at temperatures of 20 to 90 ° C before or after the separation of the degummed oil a release agent or a Solubilizer admits and an aqueous, used enzyme containing, largely sludge-free solution that one at least partially leads back to the degumming reactor and dispersed in the oil to be degummed, the proportion used, recycled enzymes in total the enzyme dispersed in the oil is at least 10%. For cost reasons, it is advantageous if the share used, recycled enzymes in total of the enzymes dispersed in the oil at least 20% or more better, at least 50%.
  • a variant of the 2nd way is that of the Degumming reactor coming oily liquid admit a broker and then that separate degummed oil from the liquid, e.g. in a centrifuge. You get next to that degummed oil an aqueous, largely sludge-free Phase that contains the used enzymes. This The aqueous phase can be wholly or partly without further Treatment, before returning the degumming reactor, to mix them with the oil to be degummed.
  • solubilizer to be used or Release aids can vary widely, they is usually 0.1 to 100 g / l liquid. A Excess solubilizer or separation aid is not disturbing.
  • the vegetable oil to be completely degummed comes in accordance with Fig. 1 from the line (1), it is dosed from the Storage container (2) first an aqueous acidic solution, e.g. Citric acid, and one from the storage container (3) aqueous alkaline solution, e.g. Caustic soda, in such Amounts that the oil has a pH of 3 to 6 preferably about 5, through line (4) into one first disperser (5) occurs. In the disperser (5) an oil-water emulsion is created, which can be Line (6) in a retention tank (7) passes.
  • aqueous acidic solution e.g. Citric acid
  • aqueous alkaline solution e.g. Caustic soda
  • the reactor (13) shown has three levels (13a), (13b) and (13c), through which the oil to be treated with a certain dwell time on each floor from top to bottom flows.
  • Each floor can have different Treatment temperatures can be set, it is recommends on the top floor (13a) with the lowest temperature and on the lowest floor (13c) to work with the highest temperature.
  • the Treatment temperatures in the reactor (13) are in the range from 20 to 90 ° C with a total residence time in Reactor (13) of usually 3 to 5 hours.
  • the treated oil leaves the degumming reactor (13) through line (17) and becomes a centrifuge (18) given up.
  • the centrifuge is used as a product degummed oil obtained in the line (19) dissipates.
  • the enzyme-containing aqueous sludge phase in the Line (20) is given from the storage container (21) Separation aid and stir the whole thing in Disperser (22) intensive. Then you give the stirred phase in line (23) one Indwelling container (24), preferably with a Stirring device (25) is provided.
  • the temperatures are in the range from 30 to 85 ° C and preferably at about 60 ° C and man ensures dwell times in the range of 3 to 60 minutes.
  • 2 is correct between the Lines (1) and (17) with the previously together with Fig. 1st described method. 2 is also that coming from the degumming reactor (13) Water-phosphatide sludge-oil mixture through the Line (17) fed to the centrifuge (18), from which one withdraws degummed oil in line (19). Of the enzyme-containing water-sludge phase of the line (30) there one from the reservoir (31) solubilizer to and stir the whole thing in the retention tank (32). Here creates an aqueous, enzyme-containing solution, which one by the line (28) in the reservoir (10) to Reuse returns; an excess of the solution can be removed in line (29). In place the retention tank (32) can also be a Disperser (22), cf. Fig. 1.
  • rapeseed oil which with Water has been degummed in various ways Enzymes degummed.
  • Examples 1, 5 and 6 are Comparative examples in which the invention Procedure is not applied.
  • the degummed rapeseed oil in line (19) has one remaining phosphorus content of 6 ppm, the volume of Water-sludge phase is 370 ml.
  • the phosphorus content is a measure of the level of degumming, good degummed oil has a residual P content of less than 10 ppm.
  • Example 1 For the procedure according to the invention according to FIG. 2 Example 1 is repeated, with the Water-sludge phase of line (30) 3 g / l TWEEN 80 adds and the liquid 10 min in a disperser (Ultra-Turrax) stirs intensely. You get one sludge-free, enzyme-containing solution with no suspended Particles that one in the line (28) in the Returns storage container (10). On adding fresher Enzymes are avoided. The degummed oil of the Line (19) has a residual phosphorus content of 5 ppm per run.
  • a disperser Ultra-Turrax
  • Example 1 For the procedure according to the invention according to FIG. 2 Example 1 is repeated, the one from the Enzyme reactor exiting via line 17 Liquid mixture via line (33) 2.5 g Tween 80 per liter of mixture and the mixture in the Centrifuge 18 separates. You largely get one sludge-free, enzyme-containing solution that can be piped (34) and line (28) to the reservoir (10). Fresh enzymes are not added.
  • the degummed oil in line (19) has one Residual phosphorus content of 5 ppm.
  • Example 1 For the procedure according to the invention according to FIG. 1 Example 1 is repeated, with the Water-sludge phase of the line (20) per liter 2 g TWEEN 80 (manufacturer DuPont) adds and the Liquids in a disperser (22) (Ultra-Turrax) homogenized. After a dwell time of 10 minutes the phosphatide sludge by centrifuging the aqueous enzyme solution separated. The enzyme solution will via the line (28) into the storage container (10) traced back, adding fresher addition No enzyme solution whatsoever. The residual phosphorus content in the degummed oil of line (19) is 5 ppm.
  • Example 4 is modified so that instead of aqueous enzyme solution after centrifugation in the Line (27) occurring, pretreated with TWEEN 80 Phosphatide sludge via the dosing point (9) with the oil the line (8) is mixed. It turns out that this Phosphatide sludge to improve degumming is ineffective because it has no enzyme activity.
  • Example 1 For the procedure according to the invention Example 1 is repeated, taking the water-sludge phase the line (20) 2 liters of alginate protan per liter (Manufacturer: Pronova-Biopolymer, Norway) adds and the liquids in a disperser (22) (Ultra-Turrax) homogenized, cf. Fig. 1. After a The phosphatide sludge becomes a residence time of 10 minutes by centrifuging the aqueous enzyme solution severed. The enzyme solution is in the Storage container (10) returned. Without adding fresh enzymes the residual phosphorus content in degummed oil of line (19) 8 ppm.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Microbiology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biochemistry (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Enzymes And Modification Thereof (AREA)
  • Treatment Of Sludge (AREA)

Claims (8)

  1. Procédé pour la démucilagination d'huile végétale, dans lequel on règle le pH de l'huile végétale à une valeur de 3 à 6, on disperse dans l'huile une solution aqueuse enzymatique qui contient une des enzymes phospholipases A1, A2 ou B, on laisse agir les enzymes dans l'huile tout en agitant à des températures de 20 à 90°C dans un réacteur de démucilagination et on sépare l'huile ayant subi une démucilagination du liquide extrait du réacteur de démucilagination, caractérisé en ce qu'on ajoute au liquide extrait du réacteur de démucilagination, à des températures de 20 à 90°C, avant ou après la séparation de l'huile ayant subi une démucilagination, un adjuvant de séparation et/ou un solubilisateur, et on récupère une solution aqueuse exempte de boue dans une large mesure, qui contient les enzymes ayant déjà servi, que l'on recycle au moins partiellement en amont du réacteur de démucilagination et que l'on disperse dans l'huile qui doit être soumise à une démucilagination, la fraction des enzymes recyclées ayant déjà servi représentant au moins 10% de la quantité totale des enzymes dispersées dans l'huile.
  2. Procédé selon la revendication 1, caractérisé en ce qu'on sépare du liquide extrait du réacteur de démucilagination l'huile ayant subi une démucilagination et on obtient en l'occurrence une phase eau-boue dans laquelle on disperse des adjuvants de séparation à des températures dans le domaine de 20 à 90°C, dans lequel on agite la phase eau-boue dans un récipient de séjour, on sépare de la phase eau-boue agitée une phase aqueuse exempte de boue dans une large mesure et contenant des enzymes ayant déjà servi et on la recycle au moins partiellement en amont du réacteur de démucilagination.
  3. Procédé selon la revendication 1, caractérisé en ce qu'on sépare du liquide extrait du réacteur de démucilagination l'huile ayant subi une démucilagination et on obtient en l'occurrence une phase eau-boue à laquelle on ajoute des solubilisateurs à des températures dans le domaine de 20 à 90°C et on obtient, tout en agitant, une solution aqueuse contenant les enzymes ayant déjà servi et exempte de boue dans une large mesure, que l'on recycle au moins partiellement en amont du réacteur de démucilagination.
  4. Procédé selon la revendication 1, caractérisé en ce qu'on ajoute des solubilisateurs au liquide extrait du réacteur de démucilagination, on guide le liquide à travers un mécanisme de séparation et on obtient de l'huile ayant subi une démucilagination et, séparée de cette dernière, une solution aqueuse contenant les enzymes ayant déjà servi et exempte de boue dans une large mesure, dans lequel on recycle la solution au moins en partie en amont du réacteur de démucilagination.
  5. Procédé selon la revendication 1 ou selon une quelconque des revendications ultérieures, caractérisé en ce qu'on utilise, comme adjuvant de séparation et comme solubilisateur,
    a) des esters d'acides gras de polyéthylène-sucre,
    b) de l'éthoxylate de ricin,
    c) du palmitate éthoxylé,
    d) un alcool primaire synthétique éthoxylé,
    e) de l'alcool laurylique éthoxylé,
    f) un alcool gras de suif éthoxylé ou
    g) un agent tensioactif hydrophobe.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce qu'on utilise, comme adjuvant de séparation, au moins
    h) un composé actif par voie anionique ou
    i) un composé non ionogène.
  7. Procédé selon la revendication 1 ou selon une quelconque des revendications ultérieures, caractérisé en ce qu'on ajoute l'adjuvant de séparation ou le solubilisateur, par litre de liquide, en une quantité de 0,1 à 100 g.
  8. Procédé selon une quelconque des revendications 1 à 4, caractérisé en ce que la fraction d'enzymes ayant déjà servi représente au moins 20% de la quantité totale des enzymes dispersées dans l'huile qui doit être soumise à une démucilagination.
EP94203211A 1993-11-19 1994-11-04 Procédé de démucilagination d'huiles végetales avec des enzymes Expired - Lifetime EP0654527B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4339556 1993-11-19
DE4339556A DE4339556C1 (de) 1993-11-19 1993-11-19 Verfahren zum Entschleimen von Pflanzenöl mittels Enzymen

Publications (2)

Publication Number Publication Date
EP0654527A1 EP0654527A1 (fr) 1995-05-24
EP0654527B1 true EP0654527B1 (fr) 1998-01-14

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US (1) US5558781A (fr)
EP (1) EP0654527B1 (fr)
JP (1) JPH07188691A (fr)
CN (1) CN1046760C (fr)
AT (1) ATE162210T1 (fr)
BR (1) BR9404496A (fr)
CA (1) CA2136050A1 (fr)
DE (2) DE4339556C1 (fr)
DK (1) DK0654527T3 (fr)
ES (1) ES2111841T3 (fr)
GR (1) GR3026501T3 (fr)
TW (1) TW279900B (fr)

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US7807398B2 (en) 2003-01-17 2010-10-05 Danisco A/S Method of using lipid acyltransferase
US7906307B2 (en) 2003-12-24 2011-03-15 Danisco A/S Variant lipid acyltransferases and methods of making
US7955814B2 (en) 2003-01-17 2011-06-07 Danisco A/S Method
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US8012732B2 (en) 2004-03-12 2011-09-06 Danisco A/S Fungal lypolytic and amylase enzyme composition and methods using the same
US8030044B2 (en) 2003-12-24 2011-10-04 Danisco A/S Lipid acyltransferases
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USRE43341E1 (en) 1995-06-07 2012-05-01 Danisco A/S Method of improving the properties of a flour dough, a flour dough improving composition and improved food products
US7972638B2 (en) 1998-07-21 2011-07-05 Danisco A/S Foodstuff
US7718204B2 (en) 1998-07-21 2010-05-18 Danisco A/S Foodstuff
US7781001B2 (en) 1998-07-21 2010-08-24 Danisco A/S Foodstuff
US8163315B2 (en) 1998-07-21 2012-04-24 Danisco A/S Foodstuff
USRE43135E1 (en) 2001-05-18 2012-01-24 Danisco A/S Method of improving dough and bread quality
US8278062B2 (en) 2003-01-14 2012-10-02 Dupont Nutrition Biosciences Aps Method of using lipid acyltransferase
US8003095B2 (en) 2003-01-17 2011-08-23 Danisco A/S Method of using lipid acyltransferase
US7955814B2 (en) 2003-01-17 2011-06-07 Danisco A/S Method
US7955813B2 (en) 2003-01-17 2011-06-07 Danisco, A/S Method of using lipid acyltransferase
US7807398B2 (en) 2003-01-17 2010-10-05 Danisco A/S Method of using lipid acyltransferase
US7718408B2 (en) 2003-12-24 2010-05-18 Danisco A/S Method
US8030044B2 (en) 2003-12-24 2011-10-04 Danisco A/S Lipid acyltransferases
US7906307B2 (en) 2003-12-24 2011-03-15 Danisco A/S Variant lipid acyltransferases and methods of making
US8440435B2 (en) 2003-12-24 2013-05-14 Dupont Nutrition Biosciences Aps Method for reducing 1,2-diglyceride content of an edible oil
US8012732B2 (en) 2004-03-12 2011-09-06 Danisco A/S Fungal lypolytic and amylase enzyme composition and methods using the same
US7666618B2 (en) 2004-07-16 2010-02-23 Danisco A/S Lipolytic enzyme: uses thereof in the food industry
US8192782B2 (en) 2004-07-16 2012-06-05 Danisco A/S Enzymatic oil-degumming method
US8535900B2 (en) 2004-07-16 2013-09-17 Dupont Nutrition Biosciences Aps Lipolytic enzyme uses thereof in the food industry
US8889371B2 (en) 2004-07-16 2014-11-18 Dupont Nutrition Biosciences Aps Lipolytic enzyme: uses thereof in the food industry
US7960150B2 (en) 2007-01-25 2011-06-14 Danisco A/S Production of a lipid acyltransferase from transformed Bacillus licheniformis cells
US8652809B2 (en) 2007-08-17 2014-02-18 Dupont Nutrition Biosciences Aps Method for producing ultra-heat treatment milk

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Publication number Publication date
DE4339556C1 (de) 1995-02-02
ES2111841T3 (es) 1998-03-16
BR9404496A (pt) 1995-07-11
DE59405028D1 (de) 1998-02-19
TW279900B (fr) 1996-07-01
CN1046760C (zh) 1999-11-24
US5558781A (en) 1996-09-24
DK0654527T3 (da) 1998-03-16
GR3026501T3 (en) 1998-07-31
EP0654527A1 (fr) 1995-05-24
JPH07188691A (ja) 1995-07-25
ATE162210T1 (de) 1998-01-15
CN1112156A (zh) 1995-11-22
CA2136050A1 (fr) 1995-05-20

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