WO2016167638A1 - Procédé d'élimination d'acides gras libres d4une huile végétale brute - Google Patents

Procédé d'élimination d'acides gras libres d4une huile végétale brute Download PDF

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Publication number
WO2016167638A1
WO2016167638A1 PCT/MY2016/000007 MY2016000007W WO2016167638A1 WO 2016167638 A1 WO2016167638 A1 WO 2016167638A1 MY 2016000007 W MY2016000007 W MY 2016000007W WO 2016167638 A1 WO2016167638 A1 WO 2016167638A1
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WIPO (PCT)
Prior art keywords
oil
vegetable oil
aqueous discharge
crude
process according
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Ceased
Application number
PCT/MY2016/000007
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English (en)
Inventor
Chien Lye @ Mervin CHEW
Ahmad Jaril ASIS
Yosri MOHD SIRAN
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Sime Darby Malaysia Bhd
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Sime Darby Malaysia Bhd
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Publication of WO2016167638A1 publication Critical patent/WO2016167638A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases

Definitions

  • the present invention relates to a process of removing free fatty acids (FFA) from crude vegetable oil. More particularly, the present invention provides a process of removing FFA from crude vegetable oil by mixing crude vegetable oil with a biologically treated aqueous discharge from oil milling process, and separating the mixture into treated vegetable oil and soap-containing aqueous liquor.
  • FFA free fatty acids
  • the invention also relates to a vegetable oil obtained by the aforementioned refining process.
  • RBD refined, bleached and deodorised
  • FFA free fatty acids
  • Alkali refining refers to a refining step in which crude oil is treated with an alkali such as caustic soda (sodium hydroxide).
  • the feed can be crude oil, but the oil may also have been degummed before being alkali refined.
  • the purpose of the alkali refining process is manifold.
  • the alkali refining process should remove them.
  • the process should remove free fatty acids present by converting them into soaps that are oil-insoluble and can be separated from the oil by settling or centrifugal separation.
  • the process should remove colouring compounds and/or their precursors so that bleaching the alkali-refined oil requires less bleaching earth and colour fixation during subsequent high temperature treatments is avoided.
  • Palm oil is an edible oil that is widely used in the food industry. Palm trees bear fruit in the third year after planting and continue producing for about 25 years. Fruit bunches of 4 to 20 kg contain 200 to 2000 individual fruits and are harvested throughout the year. The fruit bunches are transported to palm oil mills where crude palm oil (20 to 24%) is produced by mechanical and physical extraction processes along with palm kernels from which a further 2 to 4% of palm kernel oil (based on weight of palm fruits) can be produced. Crude palm oil is obtained from palm fruits by steaming at 95°C to loosen the fruits in the fruit bunch and to deactivate the lipase present in the fruits, followed by centrifugation or hydraulic pressing to release the oil. So called neutralised, bleached and deodorised (NBD) palm oil is produced from this crude palm oil by successively subjecting the oil to degumming, alkali refining, bleaching and deodorising.
  • NBD neutralised, bleached and deodorised
  • Palm oil mill effluent Typically, 1 t of crude palm oil production requires 5-7.5 1 of water; over 50% of which ends up as POME.
  • This wastewater is a viscous, brownish liquid containing about 95-96% water, 0.6-0.7% oil and 4-5% total solids. It is acidic (pH 4-5), hot (80-90°C), nontoxic and has a high organic content (COD 50,000 mg/l, BOD 25,000 mg/l).
  • US 2012/0040442 describes a method for use in treating palm oil mill effluents (POME) to generate a biogas with high methane content, the method comprising the steps of:
  • WO 2013/169091 describes a zero discharge treatment technology in handling a palm oil milling waste; comprises the following steps:
  • the IAAB achieved highest overall Chemical Oxygen Demand (COD), Biochemical Oxygen Demand (BOD) and total suspended solids removal efficiencies of > 99% at optimum organic loading rates (OLR) of 12.8 g COD L '1 d “1 , mixed liquor volatile suspended solids in anaerobic compartments (MLVSS an ) of 40,600 mg L "1 , and mixed liquor volatile suspended solids in aerobic compartments (MLVSS a ) of 18,700 mg L "1 .
  • OLR organic loading rates
  • a particular biologically treated aqueous discharge from an oil milling process can suitably be used to reduce the FFA content of crude vegetable oils.
  • This particular aqueous discharge has been biologically treated to reduce suspended and dissolved solids and has a total alkalinity of at least 1 ,000 mg CaC0 3 per litre.
  • the present invention provides a process of treating crude vegetable oil, said process comprising the steps of:
  • biologically treated aqueous discharge from an oil milling process, said biologically treated aqueous discharge having a water content of at least 80 wt.% and a total alkalinity of at least 1 ,000 mg CaC0 3 per litre;
  • the present process can suitably be employed in oil mills to produce crude vegetable oils with a reduced FFA content. These crude vegetable oils may subsequently be refined by means of ordinary oil refining processes.
  • the present process can advantageously be used to reduce the FFA content of various crude vegetable oils, including crude palm oil and crude palm kernel oil.
  • the present process offers the advantage that it enables the preparation of a crude vegetable oil with reduced FFA content without using chemicals such as caustic soda. Furthermore, the process can be used to improve the Deterioration of Bleachability Index (DOBI) of crude vegetable oil. Finally, the present process also reduces the amount of oil mill effluent.
  • DOBI Deterioration of Bleachability Index
  • the present invention also pertains to a treated vegetable oil that is obtained by the present process.
  • a first aspect of the invention relates to a process of treating crude vegetable oil, said process comprising the steps of.
  • biologically treated aqueous discharge from an oil milling process, said biologically treated aqueous discharge having a water content of at least 80 wt.% and a total alkalinity of at least 1 ,000 mg CaC0 3 per litre;
  • oil refers to glyceride oil that may be liquid, semi-solid or solid at ambient temperature (20°C).
  • glycolide oil refers to an oil that is composed of esters of glycerol and one or more fatty acids.
  • vegetable oil refers to an oil that has been isolated from a plant material.
  • the term "crude vegetable oil” as used herein refers to a vegetable oil that has not been bleached or deodorised.
  • the free fatty acid (FFA) content of a vegetable oil can suitably be determined by titration method with the use of potassium hydroxide (Ainie, K.et al. (2004) MPOB Test Methods - A Compendium of Test on Palm Oil Products, Palm Kernel Products, Fatty Acids, Food Related Products and Others.
  • the DOBI index of a vegetable oil is defined as the absorbance ratio ⁇ , ⁇ nm / A 26 g n m of around 0.1 g oil dissolved in 25 mL of hexane or 2,2,4Trimethylpentane (iso-octane).
  • the biological treatment employed may include aerobic and/or anaerobic biological treatment.
  • the present process is particularly suitable for treating crude vegetable oil having an FFA content of at least 0.5%, more preferably of 1-12%, even more preferably of 1.2-8% and most preferably of 1.3-6%.
  • the crude vegetable oil used in the present process typically has a DOBI index of at least 2, more preferably of a DOBI index of at least 2.5, and most preferably a DOBI index in the range of 3.0 to 4.0.
  • the crude vegetable oil that is treated in the present process preferably is a non-degummed vegetable oil.
  • the biologically treated aqueous discharge has undergone aerobic biological treatment. Aerobic treatment processes take place in the presence of air and utilize microorganisms (also called aerobes), which use molecular/free oxygen to assimilate organic impurities i.e. convert them into carbon dioxide, water and biomass.
  • the biologically treated aqueous discharge is preferably produced by subjecting aqueous discharge from an oil milling plant to aerobic biological treatment (optionally after anaerobic biological treatment), followed by removal of suspended solids from the aqueous discharge by static settling, filtration and/or centrifugation.
  • the treated aqueous discharge has undergone anaerobic biological treatment.
  • Anaerobic treatment processes take place in the absence of air (and thus molecular/free oxygen) by microorganisms (also called anaerobes) which do not require air
  • the biologically treated aqueous discharge is produced by subjecting aqueous discharge from an oil milling plant to an anaerobic biological treatment.
  • the treated aqueous discharge employed in the present process has undergone both aerobic and anaerobic biological treatment.
  • the treated aqueous discharge has first undergone anaerobic biological treatment, followed by aerobic biological treatment.
  • the biologically treated aqueous discharge that is employed in the present process is preferably obtained from a vegetable oil mill.
  • the treated aqueous discharge is obtained from an oil mill that produces one or more vegetable oils selected from palm oil, palm kernel oil, coconut oil and combinations thereof.
  • the treated aqueous discharge is obtained from an oil mill that produces palm oil and/or palm kernel, most preferably, it is obtained from a palm oil mill.
  • the biologically treated aqueous discharge typically contains at least 1 ,000 ppm of potassium ions (K + ). More preferably, the treated aqueous discharge contains 2,000-10,000 ppm of potassium ions, most preferably 2,500-8,000 ppm of potassium ions.
  • the biologically treated aqueous discharge has a pH at 25°C in the range of 7.5 to 10.0, more preferably in the range of 8.0 to 9.8 and most preferably of 8.5 to 9.5.
  • Total alkalinity of the biologically treated aqueous discharge typically is in the range of 1 ,000-10,000 mg CaC0 3 per litre. More preferably, total alkalinity is in the range of 2,000-6,000 mg CaC0 3 per litre and most preferably of 3,000-5,000 mg CaC0 3 per litre.
  • the biologically treated aqueous discharge preferably contains no more than limited amounts of dissolved solids, oil and other suspended material.
  • the biologically treated aqueous discharge typically contains at least 95 wt % water, most preferably 98.00-99.50 wt.% water.
  • the dry matter content of the biologically treated aqueous discharge preferably has been reduced to less than 5 g/l. More preferably, the biologically treated aqueous discharge has a dry matter content of 0.3-4 g /I and most preferably of 1-3 g/l.
  • the biologically treated aqueous discharge contains less than 5 g/l of suspended solids, more preferably less than 4g/l of suspended solids and most preferably less than 2 g/l of suspended solids.
  • the suspended solids content of the biologically treated aqueous discharge can suitable be reduced by subjecting the biologically treated aqueous discharge to e.g. static settling or filtration, before mixing it with the crude vegetable oil.
  • the biologically treated aqueous discharge employed in the present process advantageously has a biological oxygen demand (BOD) of less than 500 mg/l and a chemical oxygen demand (COD) of less than 5,000 mg/l. More preferably, the BOD of the biologically treated aqueous discharge is less than 300 mg/l, most preferably less than 200 mg/l.
  • the COD of the biological treated aqueous discharge is more preferably less than 3,000 mg/l, most preferably less than 2,000 mg/l.
  • vegetable oils that may be treated in the present process include palm oil, palm kernel oil, coconut oil, soybean oil, sunflower oil, rapeseed oil, cottonseed oil, maize oil, linseed oil and combinations thereof.
  • the crude vegetable oil that is treated in the present process is selected from palm oil, palm kernel oil, coconut oil and combinations thereof. Even more preferably, the vegetable oil is selected from palm oil, palm kernel oil and combinations thereof. Most preferably, the vegetable oil is palm oil.
  • the crude vegetable oil and the biologically treated aqueous discharge are typically mixed in a weight ratio of crude vegetable oil to biologically treated aqueous discharge in the range of 1 :10 to 10:1. More preferably, the latter ratio is in the range of 1 :3 to 3:1 , most preferably in the range of 1:2 to 2:1.
  • said crude vegetable oil and the biologically treated aqueous discharge are preferably mixed for at least 1 minute to maintain the neutralization mixture in the form of an oil-and-water emulsion, preferably an oil-in- water emulsion.
  • the neutralization mixture is preferably kept at a temperature of at least 50°C, more particularly of 50- 00 °C for at least 1 minute, more preferably for at least 2 minutes, most preferably for 3-180 minutes.
  • the soap-containing biological aqueous liquor that is obtained from the separation of the neutralization mixture typically contains at least 0.1 g/l soap. More preferably, the soap content of the aqueous liquor is at least 0.5 g/l, most preferably 1-10 g/l.
  • the neutralization mixture may suitably separated into treated vegetable oil and soap-containing aqueous liquor by means of centrifugation and/or decanting and/or static settling. Most preferably, this separation is done by means of centrifugation.
  • the present process typically yields a treated vegetable oil having an FFA content that is at least 5% lower than the FFA content of the crude vegetable oil. More preferably, the FFA content of the treated vegetable oil is at least 10% lower, even more preferably at least 20% lower, and most preferably at least 30% lower than the FFA content of the crude vegetable oil.
  • Another aspect of the present invention relates to treated vegetable oil obtained by a process as described herein. According to a particularly preferred embodiment, this treated vegetable oil is a treated palm oil, more particularly a non-bleached, non-deodorized palm oil. Typically, the non-bleached, non-deodorized palm oil obtained by the present process has an FFA content below 5%.
  • the DOBI index of said non-bleached, non-deodorized palm oil is preferably in the range of 3.3-4.8, more preferably in the range of 3.5-4.5 most preferably in the range of 3.6-4.2.
  • Raw effluent was subjected to anaerobic biological treatment, followed by aerobic biological treatment.
  • the biologically treated aqueous discharge was pre-treated (by filtration) to remove suspended solids.
  • the characteristics of treated effluent so obtained are described in Table 1.
  • the crude oil and the biological treated aqueous discharge were heated to 80 degree Celsius.
  • the hot crude oil was mixed with the hot biological treated aqueous discharge in different weight ratios and the mixture was stirred for 5 to 10 minutes whilst maintaining the temperature of the mixture at 80 degree Celsius.
  • Example 1 was repeated, again using biologically treated aqueous discharge from a palm oil mill's effluent treatment plant that had been subjected to anaerobic and aerobic biological treatment This time a crude palm oil having an FFA-content of below 3% was mixed in different weight ratios with the aforementioned biologically treated aqueous discharge to remove free fatty acids.
  • Example 1 was repeated, again using biologically treated aqueous discharge from a palm oil mill that had been subjected to anaerobic and aerobic biological treatment.
  • Example 1 was repeated, again using biologically treated aqueous discharge from a palm oil mill that had been subjected to anaerobic and aerobic biological treatment.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Fats And Perfumes (AREA)

Abstract

La présente invention concerne un procédé de traitement d'une huile végétale brute, ledit procédé comprenant les étapes consistant à : • fournir une huile végétale brute possédant une teneur en acides gras libres d'au moins 0,5 % ; • fournir des déchets aqueux traités biologiquement provenant du processus de pressage pour obtenir l'huile, lesdits déchets aqueux traités biologiquement possédant une teneur en eau d'au moins 80 % en poids et une alcalinité totale d'au moins 1000 mg de CaCO3 par litre ; • mélanger l'huile végétale brute avec les déchets aqueux traités biologiquement selon un rapport en poids de l'huile végétale brute aux déchets aqueux traités biologiquement situé dans la plage de 1:10 à 10:1 pour produire un mélange de neutralisation ; et • séparer le mélange de neutralisation en une huile végétale traitée et en une liqueur aqueuse savonneuse. Ce procédé offre l'avantage qu'il permet la préparation d'une huile végétale brute possédant une faible teneur en acides gras libres sans utiliser de produits chimiques tels que de la soude caustique. En outre, le procédé peut être utilisé pour améliorer la détérioration de l'indice de blanchiment (DOBI) de l'huile végétale brute. Enfin, le procédé permet également de réduire la quantité d'effluent du moulin à huile.
PCT/MY2016/000007 2015-04-16 2016-02-05 Procédé d'élimination d'acides gras libres d4une huile végétale brute Ceased WO2016167638A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
MYPI2015701211A MY175853A (en) 2015-04-16 2015-04-16 A process of removing free fatty acids from crude vegetable oil
MYPI2015701211 2015-04-16

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WO2016167638A1 true WO2016167638A1 (fr) 2016-10-20

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB257170A (en) * 1926-02-16 1926-08-26 Alfred Eisenstein Process for separating fatty acids from glycerides
US6111120A (en) * 1995-08-11 2000-08-29 Hyam Myers Consulting Pty. Limited Method of refining oils and fats
US20120040442A1 (en) 2010-08-12 2012-02-16 Ahmad Anwar Method for use in palm oil mill effluent (pome) treatment
WO2013169091A1 (fr) 2012-05-11 2013-11-14 Ronser Bio-Tech Sdn Bhd Système de traitement zéro déchet d'un effluent d'huilerie de palme (pome)
WO2014112703A1 (fr) * 2013-01-16 2014-07-24 Bae Hee Dong Appareil et procédé de traitement de l'effluent final et de sous-produits de palme rejetés par un processus de moulin à huile de palme

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB257170A (en) * 1926-02-16 1926-08-26 Alfred Eisenstein Process for separating fatty acids from glycerides
US6111120A (en) * 1995-08-11 2000-08-29 Hyam Myers Consulting Pty. Limited Method of refining oils and fats
US20120040442A1 (en) 2010-08-12 2012-02-16 Ahmad Anwar Method for use in palm oil mill effluent (pome) treatment
WO2013169091A1 (fr) 2012-05-11 2013-11-14 Ronser Bio-Tech Sdn Bhd Système de traitement zéro déchet d'un effluent d'huilerie de palme (pome)
WO2014112703A1 (fr) * 2013-01-16 2014-07-24 Bae Hee Dong Appareil et procédé de traitement de l'effluent final et de sous-produits de palme rejetés par un processus de moulin à huile de palme

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CHAN: "Optimization of palm oil mill effluent treatment in an integrated anaerobic-aerobic bioreactor", SUSTAIN. ENVIRON. RES., vol. 23, no. 3, 2013, pages 153 - 170
SARITA SHARMA ET AL: "ISSN: 2321-4902 Volume 2 Issue 3 Edible oil refinery waste water treatment by using effluent treatment plant Corresponding Author", INTERNATIONAL JOURNAL OF CHEMICAL STUDIES, 1 January 2014 (2014-01-01), pages 2014, XP055278916, Retrieved from the Internet <URL:http://www.chemijournal.com/vol2issue3/nov2014/19.1.pdf> [retrieved on 20160608] *

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