EP3666863B1 - Procédé de nettoyage des graisses et des huiles de déchets contenant des particules en matière plastique - Google Patents

Procédé de nettoyage des graisses et des huiles de déchets contenant des particules en matière plastique Download PDF

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Publication number
EP3666863B1
EP3666863B1 EP18211748.1A EP18211748A EP3666863B1 EP 3666863 B1 EP3666863 B1 EP 3666863B1 EP 18211748 A EP18211748 A EP 18211748A EP 3666863 B1 EP3666863 B1 EP 3666863B1
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EP
European Patent Office
Prior art keywords
plastic particles
plastic
oils
waste
filter aid
Prior art date
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EP18211748.1A
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German (de)
English (en)
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EP3666863A1 (fr
Inventor
Martin Ernst
Robert RAUDNER
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BDI Holding GmbH
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BDI Holding GmbH
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    • 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
    • C11B3/02—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
    • 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
    • C11B3/16—Refining fats or fatty oils by mechanical means

Definitions

  • the invention relates to a method for cleaning waste fats and / or oils containing plastic particles, in particular animal fats.
  • Waste materials such as used cooking oils or animal fats have been increasingly used as raw materials for biodiesel production in recent years.
  • animal fat which comes from the recycling of residual and waste materials from the meat industry and subsequently comes from animal carcass recycling plants ("rendering")
  • a high proportion of plastic polyethylene (PE) and related substances
  • PET polyethylene
  • This plastic material mostly in the form of microparticles, comes from, among other things, packaging that has not been completely separated.
  • a starting material e.g. animal fat
  • a high plastic content > 50 mg / kg
  • the animal fat is adjusted to a temperature just above its solidification point and mixed with an organic solvent in which only the fat dissolves.
  • the undissolved plastic particles are then removed from the solution by means of filtration.
  • the U.S. 3,758,533 teaches a method for cleaning fats containing plastic particles, in which the temperature of the fat is set in such a way that it is above the melting point of the starting material but below 95 ° C so as not to dissolve the polyethylene impurities in the fat, so that they can then be removed by filtration or Centrifugation can be separated. Before the separation, 0.5-2% by weight of a particulate material, for example Celite or fuller's earth, can be added as a filter aid.
  • a particulate material for example Celite or fuller's earth
  • precoat filtration is also often used, which is associated with high investment and operating costs.
  • the one in the U.S. 4,159,992 The method described in turn requires an organic solvent, which must be removed from the animal fat at the end of the process by means of energy-consuming distillation.
  • the invention attempts to overcome the above-mentioned disadvantages of the prior art, and has the object of providing a method for cleaning waste fats and / or oils containing plastic particles, in particular animal fats, which reduces the content of plastic particles without or achieved with lower amounts of filter aid than the known methods.
  • the softening temperature of the plastic is the Vicat softening temperature (VST) measured according to method A according to ISO 306, which was introduced as a substitute for the melting point of thermoplastics. It denotes the temperature at which a circular indenter with a 1 mm 2 cross-section sinks exactly 1 mm into the test specimen under a standardized load of 10 N.
  • VST Vicat softening temperature
  • ASTM D 1525 ASTM D 1525
  • the method further comprises the step of adding filter aid to the waste fats and / or oils containing plastic particles, before or after the heating step, to produce a mixture of the waste fats and / or oils and the filter aid, wherein the filter aid is removed together with the plastic particles from the liquid waste fats and / or oils in the step of separation.
  • animal fat usually contains a proportion of solid impurities, namely the plastic particles that are to be removed or whose proportion is to be reduced by means of the method according to the invention, and other solid particles, such as bone fragments (in particular "bone meal"), protein residues , etc ..
  • the proportion of these solid particles that are not plastic particles depends on the origin and processing of the starting material and is usually about 0.03% by weight or more, based on the raw material. In the process according to the invention, these solid particles can achieve the same effect as a filter aid.
  • the plastic particles are deposited on solid particles that are not plastic particles, i.e. either those that are already present in the raw material or those of the admixed Filter aid, or both, deposited and fixed thereon by the subsequent step of cooling.
  • the solid particles with the plastic fixed on them can then easily be separated from the liquid waste fats and / or oils.
  • the step of admixing filter aids known to the person skilled in the art such as bleaching earth, for example bentonite, is provided. This step can be done before or after the heating step. It is advantageous to ensure thorough mixing, for example by stirring, of waste fats and / or oils and filter aids containing plastic particles.
  • the step of adding filter aid preferably comprises adding filter aid in an amount of 0.1-1.0% by weight, based on the amount of waste fat and / or oil, such as 0.2% by weight, 0, 3% by weight, 0.4% by weight, 0.5% by weight, 0.6% by weight, 0.7% by weight, 0.8% by weight or 0.9% by weight.
  • filter aid in comparison to conventional bleaching earth filtration, significantly smaller amounts of filter aid are advantageously required according to the invention.
  • the method according to the invention further comprises a step of holding the waste fats and / or oils containing plastic particles or the mixture of waste fats and / or oils and the filter aid, preferably for 10-25 min, at the temperature above the softening temperature of the plastic of the plastic particles before the step of cooling.
  • plasticized plastic particles This makes it easier for the plasticized plastic particles to contact the solid particles (particles or filter aids already present in the waste fats and / or oils) and to settle or deposit on them, so that plastic particles can be fixed on them during the cooling step.
  • the method according to the invention also comprises a step of holding the waste fats and / or oils containing plastic particles or the mixture of the waste fats and / or oils and the filter aid, preferably for 10-25 minutes, at the temperature below the softening temperature of the plastic of the plastic particles before the step of separating.
  • This step improves the adhesion of the plastic particles to the solids, as a result of which a higher proportion of plastic can be removed from the waste fats and / or oils.
  • the step of heating comprises heating to a temperature 130 ° C.
  • the step of cooling comprises cooling to a temperature ⁇ 100.degree. This is particularly beneficial because the plastic most commonly found as a contaminant in animal fats is polyethylene, which, depending on the type, has a softening temperature of about 110 ° C to about 135 ° C.
  • the plastic of the plastic particles preferably comprises polyethylene, in particular it consists of it.
  • Polyethylene-type polymers are defined according to analytical method ISO 6656 as impurities which are soluble in boiling perchlorethylene.
  • a preferred embodiment of the method is characterized in that the step of separation comprises centrifugation, in particular decanting centrifugation.
  • the type of fat preparation according to the invention not only cleans the waste fats and / or oils from plastic particles, but also removes substances that lead to phase separation difficulties in the further process.
  • the method advantageously further comprises the step of adding water or steam and acid after the step of cooling (or after the step of maintaining below the softening temperature), the acid preferably being selected from phosphoric acid, sulfuric acid, citric acid, methanesulfonic acid or any combination of these.
  • Unsaponifiable are understood as meaning, in particular, sterols, hydrocarbons, carotenoids and tocopherols. These fat components have a disruptive effect on biodiesel production and should therefore be removed from the raw material as much as possible.
  • the addition step preferably comprises the addition of water or steam in an amount of 5-15% by weight or the addition of acid in an amount of 0.2-1.5% by weight, based in each case on the amount of waste fat and / or oil.
  • the step of separation comprises separation by means of a 3-phase decanter, an oil, a water and a solid phase being obtained.
  • Animal fat for example for biodiesel production, is usually cleaned of solids and impurities by washing water at high temperature using a 3-phase decanter (three-phase separator).
  • the method according to the invention can advantageously be carried out by decanting centrifugation in a 3-phase decanter.
  • filter aid By adding and stirring in filter aid, if necessary, at temperatures above the softening point of the plastic of the plastic particles, these particles are brought onto the solid particles that are not plastic particles and / or the filter aid and are fixed on them by subsequent cooling below the softening temperature.
  • the solid particles and / or the filter aid are then separated off with the three-phase separator required for the raw washing. In this way, the plastic particles can be removed without complex filtration equipment in a simultaneous washing step with a 3-phase decanter required for fat processing.
  • Fig. 1 shows a block diagram of an embodiment of the method according to the invention.
  • waste fat and / or oil containing plastic particles referred to as oil phase 1
  • oil phase 1 waste fat and / or oil containing plastic particles
  • tank 2 the oil phase is heated to a temperature which is above the softening temperature of the plastic of the plastic particles.
  • a filter aid 3 for example bleaching earth, can be added to the oil phase 1 in order to produce a mixture of the oil phase 1 and the filter aid 3.
  • the heated oil phase 1 or the mixture of the oil phase 1 and the filter aid 3 is advantageously kept in the tank 2 for 10-25 minutes at the temperature above the softening temperature of the plastic of the plastic particles.
  • the oil phase 1 or the mixture of the oil phase 1 and the filter aid 3 is then conveyed into the tank 4, where it is cooled to a temperature below the softening temperature.
  • the cooled oil phase 1 or the cooled mixture of the oil phase 1 and the filter aid 3 is preferably left to rest for a period of time, for example 10-25 minutes, before water / steam 5 and acid 6 are added.
  • the mixture is then separated in a 3-phase decanter 7 into a purified oil phase 8, a water phase 9 and a solid phase 10 containing the plastic particles (optionally together with the filter aid) and other solid particles.
  • Example 1 and Example 2 show that the content of plastic particles by means of the method according to the invention is clear even without the aid of filter aids can be reduced.
  • the addition of filter aid leads to a further reduction, although a far smaller amount of filter aid is required for the end result compared to the known prior art.
  • An animal fat with 342 ppm PE (and 0.08% by weight of solid impurities that are not plastic, based on the animal fat) was mixed with 0.25% by weight of filter aid, based on the animal fat, heated to 130 ° C. and after different residence times (5, 10 and 20 minutes) cooled to 90 ° C. After a further residence time of 10 minutes, the mixture was mixed with 10% by weight of water and 0.5% by weight of phosphoric acid, each based on the fat, and the fat phase was then separated off using a three-phase decanter.
  • the fat phases obtained had the following PE content: 5 minutes dwell time: 80 ppm PE (77% reduction) 10 minutes dwell time: 66 ppm PE (81% reduction) 20 minutes dwell time: 35 ppm PE (90% reduction)

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

Claims (15)

  1. Procédé pour nettoyer des graisses et/ou des huiles de déchets contenant des particules de matière plastique, en particulier des graisses animales, caractérisé en ce qu'il comprend les étapes suivantes :
    - chauffer les graisses et/ou les huiles de déchets contenant des particules de matière plastique à une température supérieure à la température de ramollissement de la matière plastique des particules de matière plastique,
    - refroidir les graisses et/ou les huiles de déchets à une température inférieure à la température de ramollissement de la matière plastique des particules de matière plastique, et
    - séparer les particules de matière plastique des graisses et/ou des huiles de déchets liquides.
  2. Procédé selon la revendication 1, caractérisé en ce qu'il comprend en outre l'étape qui consiste à ajouter et à mélanger un adjuvant de filtration aux graisses et/ou aux huiles de déchets contenant des particules de matière plastique, avant ou après l'étape du chauffage, de manière à former un mélange composé des graisses et/ou des huiles de déchets et de l'adjuvant de filtration, dans lequel l'adjuvant de filtration est éliminé des graisses et/ou des huiles de déchets liquides conjointement avec les particules de matière plastique lors de l'étape de la séparation.
  3. Procédé selon la revendication 2, caractérisé en ce que l'étape d'ajout et de mélange d'un adjuvant de filtration comprend l'ajout et le mélange d'un adjuvant de filtration en une quantité qui est comprise entre 0,1 % en poids et 1,0 % en poids, par rapport à la quantité de graisses et/ou d'huiles de déchets.
  4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce qu'il comprend en outre une étape qui consiste à maintenir les graisses et/ou les huiles de déchets contenant des particules de matière plastique ou le mélange des graisses et/ou des huiles de déchets et de l'adjuvant de filtration, de préférence pendant 10 à 25 minutes, à la température supérieure à la température de ramollissement de la matière plastique des particules de matière plastique avant l'étape de refroidissement.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'il comprend en outre une étape qui consiste à maintenir les graisses et/ou les huiles de déchets contenant des particules de matière plastique ou le mélange des graisses et/ou des huiles de déchets et de l'adjuvant de filtration, de préférence pendant 10 à 25 minutes, à la température inférieure à la température de ramollissement de la matière plastique des particules de matière plastique avant l'étape de séparation.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que l'étape de chauffage comprend le chauffage à une température ≥ 130 °C.
  7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que l'étape de refroidissement comprend le refroidissement à une température < 100 °C.
  8. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que la matière plastique des particules de matière plastique comprend du polyéthylène.
  9. Procédé selon la revendication 8, caractérisé en ce que la matière plastique des particules de matière plastique est constituée de polyéthylène.
  10. Procédé selon l'une quelconque des revendications 1 à 9, caractérisé en ce que l'étape de séparation comprend une centrifugation, de préférence une centrifugation de décantation.
  11. Procédé selon l'une quelconque des revendications 1 à 10, caractérisé en ce qu'il comprend en outre l'étape qui consiste à ajouter de l'eau ou de la vapeur ainsi que de l'acide après l'étape de refroidissement.
  12. Procédé selon la revendication 11, caractérisé en ce que l'acide est sélectionné parmi l'acide phosphorique, l'acide sulfurique, l'acide citrique, l'acide méthanesulfonique ou une combinaison quelconque de ceux-ci.
  13. Procédé selon la revendication 11 ou 12, caractérisé en ce que l'étape d'addition comprend l'ajout d'eau ou de vapeur en une quantité qui est comprise entre 5 % en poids et 15 % en poids, par rapport à la quantité de graisses et/ou d'huiles de déchets.
  14. Procédé selon l'une quelconque des revendications 11 à 13, caractérisé en ce que l'étape d'addition comprend l'ajout d'acide en une quantité qui est comprise entre 0,2 % en poids et 1,5 % en poids, par rapport à la quantité de graisses et/ou d'huiles de déchets.
  15. Procédé selon l'une quelconque des revendications 11 à 14, caractérisé en ce que l'étape de séparation comprend la séparation à l'aide d'un décanteur trois phases de manière à obtenir une phase huileuse, une phase aqueuse et une phase solide.
EP18211748.1A 2018-12-11 2018-12-11 Procédé de nettoyage des graisses et des huiles de déchets contenant des particules en matière plastique Active EP3666863B1 (fr)

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EP18211748.1A EP3666863B1 (fr) 2018-12-11 2018-12-11 Procédé de nettoyage des graisses et des huiles de déchets contenant des particules en matière plastique

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EP18211748.1A EP3666863B1 (fr) 2018-12-11 2018-12-11 Procédé de nettoyage des graisses et des huiles de déchets contenant des particules en matière plastique

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EP3666863B1 true EP3666863B1 (fr) 2021-07-14

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3758533A (en) 1970-06-04 1973-09-11 Colgate Palmolive Co Treatment of tallow and like fatty materials
WO2014202979A1 (fr) 2013-06-19 2014-12-24 Argent Energy Group Limited Procédé et appareil pour purifier un mélange gras et des produits apparentés comprenant les carburants

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4159992A (en) 1978-07-03 1979-07-03 The Badger Company, Inc. Removal of plastic polymer fines from tallow
FI128404B (en) * 2016-09-30 2020-04-30 Neste Oyj A new method for removing plastics

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3758533A (en) 1970-06-04 1973-09-11 Colgate Palmolive Co Treatment of tallow and like fatty materials
WO2014202979A1 (fr) 2013-06-19 2014-12-24 Argent Energy Group Limited Procédé et appareil pour purifier un mélange gras et des produits apparentés comprenant les carburants

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
"Oxford Dictionary of Chemistry, 6th ed.", 1 January 2008, pages: 410 - 411, 421, XP055917419
ANONYMOUS: "Animal and vegetable fats and oils — Determination of polyethylene-type polymers", INTERNATIONAL STANDARD ISO 6656 (2ND EDITION), 15 April 2002 (2002-04-15), XP093145913, [retrieved on 20240326]
BOEHME WERNER R.: "Removal of Polyethylene from Tallow in the Rendering Plant", DIRECTORS DIGEST, no. 113, 1 November 1973 (1973-11-01), pages 1 - 3, XP055917384
MITTELBACH ET AL.: "Biodiesel - The Comprehensive Handbook", 1 January 2004, article "I. Current technologies in biodiesel production", pages: 1 - 108, XP055917423
O'NEIL ET AL.: "The Merck Index - an Encyclopedia of Chemicals, Drugs and Biologicals,14th Edition", 1 January 2006, article ""Fuller's Earth'', ''Polyethylene'' and ''Tallow"", pages: viii - xii, 4286, 7565, 9043, XP055917394

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