EP2592133A1 - Dégommage enzymatique - Google Patents
Dégommage enzymatique Download PDFInfo
- Publication number
- EP2592133A1 EP2592133A1 EP11188382.3A EP11188382A EP2592133A1 EP 2592133 A1 EP2592133 A1 EP 2592133A1 EP 11188382 A EP11188382 A EP 11188382A EP 2592133 A1 EP2592133 A1 EP 2592133A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- temperature
- range
- acid
- aqueous mixture
- vegetable oils
- 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.)
- Granted
Links
- 230000002255 enzymatic effect Effects 0.000 title description 9
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000003925 fat Substances 0.000 claims abstract description 16
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 16
- 239000008158 vegetable oil Substances 0.000 claims abstract description 16
- 102000004190 Enzymes Human genes 0.000 claims abstract description 13
- 108090000790 Enzymes Proteins 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 125000005456 glyceride group Chemical group 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 40
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 102000015439 Phospholipases Human genes 0.000 claims description 6
- 108010064785 Phospholipases Proteins 0.000 claims description 6
- ZIIUUSVHCHPIQD-UHFFFAOYSA-N 2,4,6-trimethyl-N-[3-(trifluoromethyl)phenyl]benzenesulfonamide Chemical compound CC1=CC(C)=CC(C)=C1S(=O)(=O)NC1=CC=CC(C(F)(F)F)=C1 ZIIUUSVHCHPIQD-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 102000014384 Type C Phospholipases Human genes 0.000 claims description 2
- 108010079194 Type C Phospholipases Proteins 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000003921 oil Substances 0.000 description 23
- 235000019198 oils Nutrition 0.000 description 23
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 229960004106 citric acid Drugs 0.000 description 4
- 150000003904 phospholipids Chemical class 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 235000020238 sunflower seed Nutrition 0.000 description 3
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010685 fatty oil Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 235000019774 Rice Bran oil Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229960002303 citric acid monohydrate Drugs 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- -1 gums Chemical class 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000008165 rice bran oil Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
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
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- 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
-
- 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
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
-
- 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
- C11B3/10—Refining fats or fatty oils by adsorption
Definitions
- fatty oils - of vegetable or animal origin - contain impurities which must be removed before the oil is suitable for consumption. Also fatty oils for technical use often have to be purified to some extent to make them suitable for their purpose.
- the removing of impurities could be carried out by a degumming and/or winterization process and may be combined into one process a so-called cold degumming process.
- the traditional cold degumming process is not always successful because:
- the present invention solves the above mentioned technical problems by the new inventive method.
- the present invention relates to a new method for treating vegetable oils and/or animal fats to reduce the content of impurities, such as various phospholipids i.e. gums, wax and/or high melting glycerides.
- impurities such as various phospholipids i.e. gums, wax and/or high melting glycerides.
- One aspect of the invention to provide a method for efficiently removing both the phospholipids and the high melting glycerides by phospholipase at the same time.
- Another aspect of the invention to provide a method for utilizing the enzyme reaction feature such as the reacted gum has lower viscosity and less emulsification strength to achieve less oil loss.
- the main purpose of a degumming process is to remove phospholipids from the oil.
- oil types such as sunflower seed oil, rice bran oil, corn oil, winterization process is needed to remove the high melting glycerides to avoid problems in the use of the oils at lower temperature or in later process.
- the enzymatic degumming process has been proven effective in gum removal.
- the phospholipids are converted to lyso-phospholipids and free fatty acids i.e. FFA.
- the lyso-phospholipids have much less emulsion capacity and lower viscosity. So, it is expected that the separation at lower temperature in enzymatic degumming process is much better than in a conventional process.
- lyso-phospholipids are water-soluble, it is expected that most lyso-phospholipids will stay in the water phase during wax crystallation and crystal growth, so that the inhibition due to the presence of gums is eliminated.
- the cold enzymatic degumming process will provide the possibility of making degumming and dewaxing simultaneously, and with significant low loss of neutral oil
- the new method for treating vegetable oils and/or animal fats according to the invention comprises the following steps:
- step (i) the temperature of the vegetable oils and/or animal fats may be adjusted within the range from about 60 to about 90°C.
- the vegetable oils and/or animal fats may be treated with acid from about 1 to about 60 minutes, preferably from about 5 to about 60 minutes, most preferred from about 20 to about 40 minutes.
- the pH in step (iii) may be adjusted with lye to a pH within a range from about 4 to about 8 at a temperature preferably from about 40 to about 60°C.
- the lye in step (iii) is selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium silicate, sodium carbonate, calcium carbonate, and a combination thereof, preferably sodium hydroxide or potassium hydroxide. According to the invention the mixing of the lye in step (iii) may be continued within the range from about 1 min to about 4 hours.
- the temperature of the aqueous mixture in step (v) may be adjusted by a cooling rate and by a residence time to optimize crystallisation, preferably by a cooling rate within the range of from about 0.5 degrees per hour to about 5 degrees per hour, and a residence time within the range of from about 4 to 24 hours, preferably from 6 to 12 hours.
- the temperature of the aqueous mixture in separation step (vi) may be adjusted to facilitate separation, preferably the temperature is within the range of from about 15 to about 50°C.
- the enzyme in treatment step (iv) may be a phospholipase enzyme, preferably one or more phospholipase A enzymes, or one or more phospholipase C enzymes, or a combination thereof.
- the acid used in step (ii) is selected from the group consisting of phosphoric acid, acetic acid, citric acid, tartaric acid, succinic acid, and a mixture thereof, preferrably phosphoric acid or citric acid.
- the equipment used in this experiment was an oil bath, Erlenmeyer flasks 500 ml, magnetic stirrer with heating and temperature control, an Ultra Turrax, a laboratory centrifuge.
- FFA is analyzed according to method according to American Oil Chemists' Society, AOCS, Ca 5a-40, moisture is analyzed according to method AOCS Ca 2b-38, and phosphorus is analyzed according to method DIN EN 14107.
- the crude sunflower seed oil was heated in oven to 70°C to ensure all the wax crystals are melted and dissolved in the oil.
- A normal enzymatic deep degumming
- B cold enzymatic deep degumming
- a citric acid solution i.e. 5 ml
- a sodium hydroxide solution was prepared, i.e. 5 ml, by dissolving 0,5075g sodium hydroxide pellets in distilled water.
- the oil bath for flask A is heated to 80°C to inactivate the enzyme; while flask B was moved together with the magnetic agitator to fridge (7 - 8°C), and the agitation was kept at ca. 40 rpm for an overnight.
- flask B and the magnetic agitator were removed from the fridge, and the agitation was kept at room temperature (about 22°C) for ca. 15 min.
- the oil from flask B was centrifuged for 5 min. at 2000X g and the moisture, FFA and phosphorus content in the light phase were analysed.
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP20110188382 EP2592133B1 (fr) | 2011-11-09 | 2011-11-09 | Dégommage enzymatique |
| ES11188382.3T ES2495991T3 (es) | 2011-11-09 | 2011-11-09 | Desengomado enzimático |
| ARP120104221 AR088812A1 (es) | 2011-11-09 | 2012-11-08 | Desgomado enzimatico |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP20110188382 EP2592133B1 (fr) | 2011-11-09 | 2011-11-09 | Dégommage enzymatique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP2592133A1 true EP2592133A1 (fr) | 2013-05-15 |
| EP2592133B1 EP2592133B1 (fr) | 2014-06-04 |
Family
ID=44992680
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP20110188382 Active EP2592133B1 (fr) | 2011-11-09 | 2011-11-09 | Dégommage enzymatique |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP2592133B1 (fr) |
| AR (1) | AR088812A1 (fr) |
| ES (1) | ES2495991T3 (fr) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014067569A1 (fr) * | 2012-10-31 | 2014-05-08 | Alfa Laval Corporate Ab | Démucilagination enzymatique |
| CN106459119A (zh) * | 2014-06-04 | 2017-02-22 | 生命纳米科学有限责任两合公司 | 用于从脂样相获得糖基甘油脂和糖鞘脂的装置和方法 |
| US10344246B2 (en) | 2017-05-24 | 2019-07-09 | Arisyne Systems, Inc. | Oil degumming systems |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9340749B1 (en) | 2015-05-06 | 2016-05-17 | Arisdyne Systems, Inc. | Method for degumming triglyceride oils |
| BR112017023635B1 (pt) * | 2015-05-06 | 2021-11-30 | Archer-Daniels-Midland Company | Método para degomar um óleo de triglicerídeo |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB382946A (en) * | 1931-07-23 | 1932-10-24 | Leslie William Mapson | Improvements in or relating to the manufacture of concentrated edible products |
| US5558781A (en) * | 1993-11-19 | 1996-09-24 | Metallgesellschaft Aktiengesellschaft | Process for enzymatically degumming vegetable oil |
| EP1876222A1 (fr) * | 2006-07-06 | 2008-01-09 | Cognis IP Management GmbH | Procede de production d 'acides gras, d'esters d'acides gras et d'esters de sterol à partir de solution savonneuse |
| WO2008094847A1 (fr) * | 2007-01-30 | 2008-08-07 | Bunge Oils, Inc. | Dégommage enzymatique utilisant un mélange de phospholipases pla et plc |
| US20100240917A1 (en) * | 2009-03-19 | 2010-09-23 | N.V. Desmet Ballestra Engineering S.A. | Enzymatic oil recuperation process |
-
2011
- 2011-11-09 EP EP20110188382 patent/EP2592133B1/fr active Active
- 2011-11-09 ES ES11188382.3T patent/ES2495991T3/es active Active
-
2012
- 2012-11-08 AR ARP120104221 patent/AR088812A1/es active IP Right Grant
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB382946A (en) * | 1931-07-23 | 1932-10-24 | Leslie William Mapson | Improvements in or relating to the manufacture of concentrated edible products |
| US5558781A (en) * | 1993-11-19 | 1996-09-24 | Metallgesellschaft Aktiengesellschaft | Process for enzymatically degumming vegetable oil |
| EP1876222A1 (fr) * | 2006-07-06 | 2008-01-09 | Cognis IP Management GmbH | Procede de production d 'acides gras, d'esters d'acides gras et d'esters de sterol à partir de solution savonneuse |
| WO2008094847A1 (fr) * | 2007-01-30 | 2008-08-07 | Bunge Oils, Inc. | Dégommage enzymatique utilisant un mélange de phospholipases pla et plc |
| US20100240917A1 (en) * | 2009-03-19 | 2010-09-23 | N.V. Desmet Ballestra Engineering S.A. | Enzymatic oil recuperation process |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014067569A1 (fr) * | 2012-10-31 | 2014-05-08 | Alfa Laval Corporate Ab | Démucilagination enzymatique |
| US10329514B2 (en) | 2012-10-31 | 2019-06-25 | Alfa Laval Corporate Ab | Enzymatic degumming |
| CN106459119A (zh) * | 2014-06-04 | 2017-02-22 | 生命纳米科学有限责任两合公司 | 用于从脂样相获得糖基甘油脂和糖鞘脂的装置和方法 |
| US10239906B2 (en) * | 2014-06-04 | 2019-03-26 | Nanoscience For Life Gmbh & Cokg | Apparatus and method for obtaining glycoglycerolipids and glycosphingolipids from lipid phases |
| CN106459119B (zh) * | 2014-06-04 | 2019-10-25 | 生命纳米科学有限责任两合公司 | 用于从脂样相获得糖基甘油脂和糖鞘脂的装置和方法 |
| US10344246B2 (en) | 2017-05-24 | 2019-07-09 | Arisyne Systems, Inc. | Oil degumming systems |
Also Published As
| Publication number | Publication date |
|---|---|
| AR088812A1 (es) | 2014-07-10 |
| ES2495991T3 (es) | 2014-09-18 |
| EP2592133B1 (fr) | 2014-06-04 |
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