EP0654527A1 - Procédé de démucilagination d'huiles végetales avec des enzymes - Google Patents

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

Info

Publication number: EP0654527A1
Authority: EP; European Patent Office
Prior art keywords: oil; enzymes; degumming; degummed; sludge
Prior art date: 1993-11-19
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.): Granted

Application number

EP94203211A

Other languages

German (de)

English (en)

Other versions

EP0654527B1 (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

Roehm GmbH Chemische Fabrik

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.)

1993-11-19

Filing date

1994-11-04

Publication date

1995-05-24

1994-11-04 Application filed by Roehm GmbH Chemische Fabrik, Metallgesellschaft AG, Roehm GmbH Darmstadt filed Critical Roehm GmbH Chemische Fabrik

1995-05-24 Publication of EP0654527A1 publication Critical patent/EP0654527A1/fr

1998-01-14 Application granted granted Critical

1998-01-14 Publication of EP0654527B1 publication Critical patent/EP0654527B1/fr

2014-11-04 Anticipated expiration legal-status Critical

Status Expired - Lifetime legal-status Critical Current

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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 process for degumming vegetable oil, adjusting the vegetable oil to a pH of 3 to 6, dispersing an aqueous enzyme solution in the oil which contains one of the enzymes phospholipase A1, A2 or B, the enzymes in the oil with stirring is allowed to act in a degumming reactor at temperatures of 20 to 90 ° C. and oil which has been degummed from the liquid drawn off from the degumming reactor is separated off.
the object of the invention is to at least partially reuse the enzymes used in the degumming process in the process mentioned at the beginning. According to the invention, this is done by adding a separating agent or a solubilizer to the liquid drawn off from the degumming reactor at temperatures of 20 to 90 ° C. before or after separating the degummed oil and obtaining an aqueous, used enzyme-containing, largely sludge-free solution which is obtained at least partially leads back to the degumming reactor and dispersed in the oil to be degummed, the proportion used, recycled enzymes in the total amount of the enzymes dispersed in the oil is at least 10%. For reasons of cost, it is advantageous if the proportion of used, recycled enzymes in the total amount of the enzymes dispersed in the oil is at least 20% or even better, at least 50%.
a variant of the second way is to add a solubilizer to the oily liquid coming out of the degumming reactor and then to separate the degummed oil from the liquid, e.g. in a centrifuge.
a solubilizer to the oily liquid coming out of the degumming reactor and then to separate the degummed oil from the liquid, e.g. in a centrifuge.
an aqueous, largely sludge-free phase is obtained which contains the used enzymes. All or part of this aqueous phase can be returned to the degumming reactor without further treatment in order to mix it with the oil to be degummed.
solubilizer or separation aid to be used can vary within a wide range; it is usually 0.1 to 100 g / l of liquid. An excess of solubilizers or release aids is not a problem.
lecithin To degum the edible oils with the help of enzymes, it is advisable to first degum the oil with water to obtain lecithin.
the phospholipases A1, A2 or B attack lecithin in the oil, so that it is expedient to lower the phosphorus content of the oil in the range from 50 to 500 ppm by pre-degumming, for example with water. This pretreatment is especially recommended for oils rich in lecithin, such as soybean oil.
the vegetable oil to be completely degummed comes from the line (1) according to Fig. 1, it is first metered from the storage container (2) into an aqueous acidic solution, e.g. Citric acid, and from the storage container (3) an aqueous alkaline solution, e.g. Sodium hydroxide solution in such amounts that the oil with a pH of 3 to 6, preferably about 5, enters the first disperser (5) through line (4).
An oil-water emulsion is produced in the disperser (5) and is passed through the line (6) into a retention tank (7).
the emulsion flows through line (8) to an addition point (9) for an aqueous enzyme solution which comes from the storage vessel (10). 10 to 100 mg of enzyme solution are added per liter of oil.
the enzymes dissolved in water are the phospholipase of type A1, A2 or B, for example with an activity of the solution of 10,000 lecitase units per milliliter.
the enzyme-containing oil is passed through a further disperser (11) and then passes through line (12) to a degumming reactor (13).
the reactor (13) consists of 1 to 5 floors, each floor having a stirring device (14) and a heater (15). There is a connecting line (16) between adjacent floors.
the reactor (13) shown has three levels (13a), (13b) and (13c) through which the oil to be treated flows from top to bottom with a certain dwell time in each level.
Different treatment temperatures can be set on each floor, it being recommended to work with the lowest temperature on the top floor (13a) and with the highest temperature on the bottom floor (13c).
the treatment temperatures in the reactor (13) are in the range from 20 to 90 ° C. with a total residence time in the reactor (13) of usually 3 to 5 hours.
the treated oil leaves the degumming reactor (13) through line (17) and is fed to a centrifuge (18).
degummed oil is obtained as a product and is discharged in line (19).
the enzyme-containing aqueous sludge phase in the line (20) is added from the storage container (21) separation aid and the whole thing is stirred intensively in the disperser (22).
the stirred phase in line (23) is placed in a retention tank (24), which is preferably provided with a stirring device (25).
the temperatures are in the range from 30 to 85 ° C. and preferably around 60 ° C., and retention times in the range from 3 to 60 minutes are ensured.
the enzymes adsorbed on the phosphatide sludge are detached and transferred to the water phase.
the liquid is transferred from the retention tank (24) to a filtration device (26), which preferably works as microfiltration. Alternatively, centrifugation can also be carried out at this point. This separates the phosphatide sludge, which is removed in line (27).
the aqueous phase containing the used enzymes is in line (28) withdrawn and fed to the storage container (10) for reuse. If necessary, fresh enzyme solution comes from the line (29). In this way, it is possible to reuse the used enzymes for degumming the oil and thus significantly reduce the operating costs of the process.
the method according to FIG. 2 corresponds between lines (1) and (17) with the method previously described together with FIG. 1.
the water-phosphatide sludge-oil mixture coming from the degumming reactor (13) is fed through line (17) to the centrifuge (18), from which oil degummed in line (19) is drawn off.
the enzyme-containing water-sludge phase of the line (30) is added from the storage container (31) solubilizer and the whole thing is stirred in the retention tank (32). This creates an aqueous, enzyme-containing solution which is returned through the line (28) to the storage container (10) for reuse; an excess of the solution can be removed in line (29).
Rapeseed oil which has been degummed with water, is degummed in various ways with enzymes in a laboratory apparatus with a single-stage reactor (13) corresponding to the drawing.
Examples 1, 5 and 6 are comparative examples in which the method according to the invention is not used.
the degummed rapeseed oil in line (19) has a residual phosphorus content of 6 ppm, the volume of the water-sludge phase is 370 ml.
the phosphorus content is a measure of the degree of degumming, well degummed oil has one Residual P content of less than 10 ppm.
Example 1 is repeated for the procedure according to the invention according to FIG. 2, 3 g / l TWEEN 80 being added to the water-sludge phase of line (30) is added and the liquid is stirred intensively for 10 min in a disperser (Ultra-Turrax). This gives a sludge-free, enzyme-containing solution without suspended particles, which is returned via line (28) to the storage container (10). Fresh enzymes are not added.
the degummed oil from line (19) has a residual phosphorus content of 5 ppm per pass.
Example 1 is repeated for the procedure according to the invention according to FIG. 2, 2.5 g of Tween 80 per liter of mixture being added via line (33) to the liquid mixture emerging from the enzyme reactor via line 17 and the mixture being separated in the centrifuge 18 . A largely sludge-free, enzyme-containing solution is thus obtained, which is fed to the storage container (10) via line (34) and line (28). Fresh enzymes are not added.
the degummed oil from line (19) has a residual phosphorus content of 5 ppm.
example 1 is repeated, adding 2 g of TWEEN 80 (manufacturer DuPont) per liter to the water-sludge phase of the line (20) and the liquids in a disperser (22) (ultra Turrax) homogenized. After a dwell time of 10 minutes, the phosphatide sludge is separated from the aqueous enzyme solution by centrifugation. The enzyme solution is returned via line (28) to the storage container (10), with fresher addition No enzyme solution whatsoever. The residual phosphorus content in the degummed oil in line (19) is 5 ppm.
Example 4 is modified in such a way that, instead of the aqueous enzyme solution, the phosphatide sludge obtained after centrifugation in line (27) and pretreated with TWEEN 80 is mixed with the oil in line (8) via the metering point (9). It is shown that this phosphatide sludge is ineffective for improving degumming since it has no enzyme activity.
Example 4 The procedure is as in Example 4, but without recycling the aqueous enzyme solution in line (28).
the phosphatide sludge from line (27) is now resuspended in distilled water and homogenized for 10 minutes at 60 ° C. using a disperser (Ultra-Turrax).
the sludge phase is then separated off by centrifugation and the aqueous phase which is produced at the same time is returned to the metering point (9).
Fresh enzyme solution is no longer added.
a residual P content of 49 ppm is found in the rapeseed oil, which proves that no enzymes have been recovered from the phosphatide sludge from line (27).
Example 1 is repeated for the procedure according to the invention, with 2 g of alginate protan (manufacturer: Pronova biopolymer, Norway) being added to the water-sludge phase of the line (20) per liter and the liquids in a disperser (22) (Ultra -Turrax) homogenized, cf. Fig. 1. After a The phosphatide sludge is separated from the aqueous enzyme solution by centrifugation for 10 minutes. The enzyme solution is returned to the storage container (10). Without the addition of fresh enzymes, the residual phosphorus content in the degummed oil in line (19) is 8 ppm.
alginate protan manufactured by Pronova biopolymer, Norway

Landscapes

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)

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
DE4339556A DE4339556C1 (de)	1993-11-19	1993-11-19	Verfahren zum Entschleimen von Pflanzenöl mittels Enzymen
DE4339556		1993-11-19

Publications (2)

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

Family

ID=6503008

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP94203211A Expired - Lifetime EP0654527B1 (fr)	1993-11-19	1994-11-04	Procédé de démucilagination d'huiles végetales avec des enzymes

Country Status (12)

Country	Link
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)

Cited By (9)

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WO1998026057A1 (fr) *	1996-12-09	1998-06-18	Novo Nordisk A/S	Limitation de la teneur en phosphore d'elements dans des huiles comestibles contenant une quantite elevee de phosphore non hydratable au moyen d'une phospholipase, phospholipase provenant d'un champignon filamenteux presentant une activite de phospholipase a ou b
US6103505A (en) *	1996-12-09	2000-08-15	Novo Nordisk A/S	Method for reducing phosphorus content of edible oils
EP1555322A1 (fr)	2000-04-28	2005-07-20	Novozymes A/S	Variant d'enzyme lipolytique
US7588925B2 (en)	2002-05-21	2009-09-15	Dsm Ip Assets B.V.	Phospholipases and uses thereof
EP2113563A2 (fr)	1998-11-27	2009-11-04	Novozymes A/S	Variants d'enzyme lipolytique
US8241876B2 (en)	2008-01-07	2012-08-14	Bunge Oils, Inc.	Generation of triacylglycerols from gums
US8460905B2 (en)	2007-09-11	2013-06-11	Bunge Oils, Inc.	Enzymatic degumming utilizing a mixture of PLA and PLC phospholipases with reduced reaction time
US8956853B2 (en)	2007-01-30	2015-02-17	Bunge Oils, Inc.	Enzymatic degumming utilizing a mixture of PLA and PLC phospholipases
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1993
- 1993-11-19 DE DE4339556A patent/DE4339556C1/de not_active Expired - Lifetime
1994
- 1994-11-04 ES ES94203211T patent/ES2111841T3/es not_active Expired - Lifetime
- 1994-11-04 DK DK94203211.1T patent/DK0654527T3/da active
- 1994-11-04 AT AT94203211T patent/ATE162210T1/de not_active IP Right Cessation
- 1994-11-04 EP EP94203211A patent/EP0654527B1/fr not_active Expired - Lifetime
- 1994-11-04 DE DE59405028T patent/DE59405028D1/de not_active Expired - Fee Related
- 1994-11-10 TW TW083110409A patent/TW279900B/zh active
- 1994-11-16 US US08/340,829 patent/US5558781A/en not_active Expired - Fee Related
- 1994-11-17 CA CA002136050A patent/CA2136050A1/fr not_active Abandoned
- 1994-11-18 BR BR9404496A patent/BR9404496A/pt not_active Application Discontinuation
- 1994-11-19 CN CN94118887A patent/CN1046760C/zh not_active Expired - Fee Related
- 1994-11-21 JP JP6311139A patent/JPH07188691A/ja active Pending
1998
- 1998-04-03 GR GR980400684T patent/GR3026501T3/el unknown

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WO1998026057A1 (fr) *	1996-12-09	1998-06-18	Novo Nordisk A/S	Limitation de la teneur en phosphore d'elements dans des huiles comestibles contenant une quantite elevee de phosphore non hydratable au moyen d'une phospholipase, phospholipase provenant d'un champignon filamenteux presentant une activite de phospholipase a ou b
EP0869167A2 (fr)	1996-12-09	1998-10-07	Novo Nordisk A/S	Réduction de substances contenant du phosphore dans les huiles comestibles à haute teneur en phosphore non-hydratable avec une phospholipase , une phospholipase issue d'un champignon filamenteux et présentant une activité de phospholipase A et/ou B
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EP0869167A3 (fr) *	1996-12-09	2001-03-14	Novozymes A/S	Réduction de substances contenant du phosphore dans les huiles comestibles à haute teneur en phosphore non-hydratable avec une phospholipase , une phospholipase issue d'un champignon filamenteux et présentant une activité de phospholipase A et/ou B
EP2287298A1 (fr)	1998-11-27	2011-02-23	Novozymes A/S	Variants d'enzyme lipolytique
EP2287297A1 (fr)	1998-11-27	2011-02-23	Novozymes A/S	Variants d'enzyme lipolytique
EP2113563A2 (fr)	1998-11-27	2009-11-04	Novozymes A/S	Variants d'enzyme lipolytique
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US7588925B2 (en)	2002-05-21	2009-09-15	Dsm Ip Assets B.V.	Phospholipases and uses thereof
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US8956853B2 (en)	2007-01-30	2015-02-17	Bunge Oils, Inc.	Enzymatic degumming utilizing a mixture of PLA and PLC phospholipases
US8460905B2 (en)	2007-09-11	2013-06-11	Bunge Oils, Inc.	Enzymatic degumming utilizing a mixture of PLA and PLC phospholipases with reduced reaction time
US8241876B2 (en)	2008-01-07	2012-08-14	Bunge Oils, Inc.	Generation of triacylglycerols from gums
US8541211B2 (en)	2008-01-07	2013-09-24	Bunge Oils, Inc.	Generation of triacylglycerols
US11142492B2 (en)	2019-08-26	2021-10-12	Wisconsin Alumni Research Foundation	Methods of isolating phenols from phenol-containing media
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TW279900B (fr)	1996-07-01
GR3026501T3 (en)	1998-07-31
DK0654527T3 (da)	1998-03-16
US5558781A (en)	1996-09-24
BR9404496A (pt)	1995-07-11
ATE162210T1 (de)	1998-01-15
CN1112156A (zh)	1995-11-22
EP0654527B1 (fr)	1998-01-14
DE59405028D1 (de)	1998-02-19
ES2111841T3 (es)	1998-03-16
DE4339556C1 (de)	1995-02-02
CN1046760C (zh)	1999-11-24
JPH07188691A (ja)	1995-07-25
CA2136050A1 (fr)	1995-05-20

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