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WO2025074039A1 - Procédé de purification de lipides - Google Patents

Procédé de purification de lipides Download PDF

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Publication number
WO2025074039A1
WO2025074039A1 PCT/FI2024/050525 FI2024050525W WO2025074039A1 WO 2025074039 A1 WO2025074039 A1 WO 2025074039A1 FI 2024050525 W FI2024050525 W FI 2024050525W WO 2025074039 A1 WO2025074039 A1 WO 2025074039A1
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WO
WIPO (PCT)
Prior art keywords
lipid feedstock
lipid
feedstock
mmol
treated
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.)
Pending
Application number
PCT/FI2024/050525
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English (en)
Inventor
Ronny WAHLSTRÖM
Petri Pulkkinen
Jonne HAKANPÄÄ
Annika Malm
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Neste Oyj
Original Assignee
Neste Oyj
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.)
Filing date
Publication date
Priority claimed from FI20236107A external-priority patent/FI131414B1/en
Priority claimed from FI20236108A external-priority patent/FI131419B1/en
Priority claimed from FI20245090A external-priority patent/FI131609B1/en
Priority claimed from FI20245163A external-priority patent/FI20245163A1/en
Application filed by Neste Oyj filed Critical Neste Oyj
Publication of WO2025074039A1 publication Critical patent/WO2025074039A1/fr
Pending legal-status Critical Current
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
    • C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
    • C10G3/50—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids in the presence of hydrogen, hydrogen donors or hydrogen generating compounds
    • 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
    • C11B11/00—Recovery or refining of other fatty substances, e.g. lanolin or waxes
    • 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
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases
    • 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
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1003—Waste materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1003—Waste materials
    • C10G2300/1007—Used oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10—Feedstock materials
    • C10G2300/1011—Biomass
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/202—Heteroatoms content, i.e. S, N, O, P
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/205—Metal content

Definitions

  • lipid materials such as oils and fats
  • impurities that need to be removed before catalytic processing as they are detrimental to the quality of the final product, and may cause plugging of the reactor, deactivation of the used catalyst, as well as fouling of the equipment.
  • the current methods may not be fully suitable for the most difficult oils and fats as despite sufficient removal of at least some of the impurities, they suffer from or even cause challenges in downstream unit operations such as filtering the purified products.
  • An objective of the present invention is thus to provide a method so as to overcome the above problems.
  • the objectives of the invention are achieved by a method which is characterized by what is stated in the independent claims.
  • the preferred embodiments of the invention are disclosed in the dependent claims.
  • lipid feedstocks may be successfully purified by a method combining adjusting the total net elementary charge of the lipid feedstock and optionally the free fatty acid content to a desirable level and removing of solid impurities from the lipid feedstock prior to further purification steps such as heat treatment followed by bleaching.
  • further purification steps such as heat treatment followed by bleaching.
  • Figure 1 illustrates the 1 st exemplary process flow of the present method
  • Figure 2 illustrates the 2nd exemplary process flow of the present method
  • Figure 3 illustrates the 3rd exemplary process flow of the present method
  • Figure 4 illustrates the 4th exemplary process flow of the present method
  • Figure 5 illustrates the 5th exemplary process flow of the present method
  • Figure 6 illustrates the 6th exemplary process flow of the present method.
  • the present invention further provides a process for providing renewable hydrocarbons, comprising x) purifying lipid feedstock by the method contemplated herein to obtain purified lipid material, and y) subjecting the purified lipid material to hydroprocessing to obtain at least one renewable hydrocarbon.
  • weight percentages are calculated based on the total weight of the material in question (typically a blend or a mixture). Any amounts defined as ppm (parts per million), are based on weight (i.e. mg/kg).
  • renewable in the context of renewable feed, renewable feedstock or renewable fuel or fuel component refers to one or more organic compounds derived from any renewable source (contrary to source of fossil origin).
  • renewable compounds or compositions are obtainable, obtained, derivable, derived, or originating from plants, animals and/or microbes, including compounds or compositions obtainable, obtained, derivable, derived, or originating from fungi and/or algae, in full or in part, whether these compounds or compositions are in their virgin, recycled or reclaimed form.
  • renewable compounds or compositions may comprise gene manipulated compounds or compositions.
  • the 14C-isotope content can be used as evidence of the renewable or biological origin of a feedstock or product.
  • Carbon atoms of renewable material comprise a higher number of unstable radiocarbon (14C) atoms compared to carbon atoms of fossil origin. Therefore, it is possible to distinguish between carbon compounds derived from biological sources, and carbon compounds derived from fossil sources by analyzing the ratio of 12C and 14C isotopes.
  • a particular ratio of said isotopes can be used to identify and quantify renewable carbon compounds and differentiate those from non-renewable i.e. fossil carbon compounds.
  • the isotope ratio does not change in the course of chemical reactions.
  • Example of a suitable method for analyzing the content of carbon from biological sources is ASTM D6866 (2020).
  • a renewable material such as a feedstock or product
  • pMC modern carbon
  • hydrocarbons refer to compounds consisting of carbon and hydrogen.
  • hydrocarbons include paraffins, including n-paraffins and i- paraffins, naphthenes, aromatics, and olefins (alkenes).
  • Oxygenated hydrocarbons refer herein to hydrocarbons comprising covalently bound oxygen. Examples of oxygenated hydrocarbons include tri-, di-, and monoglycerides, fatty acids and alkyl-esters of fatty acids (e.g. methyl- or ethyl-ester of fatty acids).
  • paraffins refer to non-cyclic alkanes, i.e., non-cyclic, open chain saturated hydrocarbons that are linear (normal paraffins, n-paraffins) or branched (isoparaffins, i-paraffins). In other words, paraffins refer herein to n-paraffins and/or i-paraffins.
  • olefins refer to unsaturated, linear, branched, or cyclic hydrocarbons, excluding aromatic compounds. In other words, olefins refer to hydrocarbons having at least one unsaturated bond, excluding unsaturated bonds in aromatic rings.
  • Nephthenes refer herein to cycloalkanes or cycloalkenes containing at least one cyclic structure, with or without side chains, including also compounds having one or more olefinic bonds in the cyclic structure and/or in a side chain, but excluding compounds with any aromatic ring structure(s).
  • “Aromatics” refers herein to hydrocarbons containing at least one aromatic ring structure, i.e. cyclic structure having delocalized, pi bonds satisfying the Huckel (4n + 2) rule.
  • Term “fuel” refers to both fuels usable as such and/or as fuel components, which fulfill the requirements of standards for the respective use.
  • gasoline is EN 228 (2017), for paraffinic diesel EN 15940 (2019), and for aviation turbine fuel containing synthesized hydrocarbons D7566 (2020).
  • the lipid feedstock contemplated herein comprises at least 15 mg/kg, such as 15 to 2000 mg/kg, dissolved phosphorus impurities, and at least 20 mg/kg, such as 20 to 3000 mg/kg, dissolved metal impurities, measured as elemental phosphorus and elemental metal(s).
  • the net elemental charge of the lipid feedstock contemplated herein based on phosphorus and the metal(s) contained in the lipid feedstock may be positive or negative, however the process is particularly beneficial for lipid feedstocks having negative net elementary charge Q1 , i.e., there are more negative charge from phosphorus impurities than positive charge from metal impurities.
  • the present method is particularly suitable for lipid feedstocks having net elementary charge Q1 below 0 mmol/kg, such as from -60 to -0.5 mmol/kg, in particular below -0.5 mmol/kg, such as from -30 to -1 mmol/kg.
  • Metal impurities may similarly be present in the lipid feedstock in various chemical forms in varying metal continuing compounds, inorganic or organic, in water soluble, oil soluble, or insoluble forms.
  • the present method may be used to purify any lipid feedstock, such as plant oils, plant fats, animal fats, animal oils, fish fats, fish oils, waste fats, waste oils, residue fats, residue oils, a fatty acid distillate, acidulated soapstock, mold oils, rapeseed oil, canola oil, colza oil, babassu oil, carinata oil, coconut butter, muscat butter oil, sesame oil, maize oil, poppy seed oil, cottonseed oil, soy oil, laurel seed oil, jatropha oil, palm kernel oil, camelina oil, tall oil, fraction of tall oil, crude tall oil, tall oil pitch, sunflower oil, corn oil, technical/distillers corn oil, soybean oil, hemp seed oil, olive oil, linseed oil, cottonseed oil, mustard oil, mustard seed oil, peanut oil, castor oil, coconut oil, palm oil, crude palm oil, palm seed oil, palm fatty acid distillate, a sludge originating from plant oil production, palm oil mill effl
  • Typical lipid feedstocks comprise waste and recycle oils, typically combinations thereof.
  • Such lipid materials typically initially contain high amounts of phosphorus, typically as phosphorus containing compounds, metals, and solid impurities.
  • lipid materials benefiting from the present purification method include soapstock acid oil (SAO), low quality animal fat (LQAF) grades such as choice white grease (CWG) and poultry fat (APF), used cooking oil (UCO), and palm oil mill effluent (POME), as well as mixtures thereof.
  • SAO soapstock acid oil
  • LQAF low quality animal fat
  • CWG choice white grease
  • API poultry fat
  • UEO used cooking oil
  • POME palm oil mill effluent
  • Soapstock acid oil is a by-product from the vegetable oil refining industry obtained by acidification of soapstock.
  • SAO comprises high amounts of phosphorus and metal impurities, such as at least 30 mg/kg, e.g. 50 to 700 mg/kg, phosphorus, at least 10 mg/kg, e.g. 10 to 3000 mg/kg, metals, and at least 0.1 wt%, e.g. 0.1 to 3 wt%, solids.
  • the net elementary charge of SAO is -13 mmol/kg, such as from -60 to -10 mmol/kg.
  • SAO comprises at least 10 wt%, such as 15 to 80 wt% FFA of the total weight of the composition.
  • LQAF Low quality animal fat
  • LQAF Low quality animal fat
  • LQAF comprises high amounts of phosphorus and metal impurities, such as at least 50 mg/kg, e.g. 100 to 700 mg/kg, phosphorus, at least 50 mg/kg, e.g. 50 to 1200 mg/kg, metals, and at least 0.01 wt%, e.g. 0.01 to 2.0 wt%, solids.
  • the net elementary charge of LQAF is -30 mmol/kg, such as from -50 to -5 mmol/kg.
  • LQAF comprises at least 2 wt%, such as 2 to 10 wt%, FFA of the total weight of the composition.
  • CWG choice white grease
  • CWG is an inedible low quality animal fat obtained from the rendering process of swine in the North American feedstock market.
  • CWG comprises high amounts of phosphorus and metal impurities, such as at least 300 mg/kg, e.g. 300 to 700 mg/kg, phosphorus, at least 600 mg/kg, e.g. 600 to 1200 mg/kg, metals, and at least 0.4 wt%, e.g. 0.4 to 2.0 wt%, solids.
  • the net elementary charge of CWG is -10 mmol/kg, such as from -30 to -5 mmol/kg.
  • Palm oil mill effluent is oil waste separated from wastewaters generated in palm oil milling.
  • POME comprises high amounts of phosphorus and metal impurities, such as at least 5 mg/kg, e.g. 5 to 150 mg/kg, phosphorus, at least 10 mg/kg, e.g. 10 to 4000 mg/kg, metals, and at least 0.01 wt%, e.g. 0.1 to 2.0 wt%, solids.
  • the net elementary charge of POME is 10 mmol/kg, such as from 0 to 70 mmol/kg.
  • POME comprises 50 wt%, such as 10 to 85 wt% FFA of the total weight of the composition.
  • the amount of phosphorus and metal impurities may be determined e.g. according to ASTM D5185-18 standard test method or as described herein in the experimental part, preferably as described herein.
  • CP is the concentration of dissolved phosphorus in the feedstock in mmol/kg of feedstock
  • QP is the elementary charge of dissolved phosphorus in the feedstock
  • QMi is the elementary charge of the dissolved metal i in the feedstock, and i is the number of dissolved metals taken into account, and i is 1 -n.
  • the metals include Na, K, Mg, Ca, Fe, Al, Cr, Pb, Mn, Zn, W, Ni and Cu, or any combinations thereof.
  • the elementary charge of a metal is the valence the metal typically has when forming a metal salt, such as metal phosphate.
  • a person skilled in the art may also use another method for this determination. Only the concentration of dissolved phosphorus and metal(s) (not solid impurities) are used in the net elementary charge calculation. In accordance with the present method, solids are removed from the feedstock to be treated by heat treatment and are thus not considered for determining the net elementary charge Q1 and/or total net elementary charge Qt.
  • the FFA concentration of the lipid feedstock is adjusted to at least 3 wt%, such as from 3 to 30 wt%, of the total weight of the resulting lipid feedstock, preferably to at least 4 wt%, such as from 4 to 20 wt%, of the total weight of the lipid feedstock, more preferably to 4 to 10 wt%, of the total weight of the resulting lipid feedstock.
  • concentrations of 2 wt% and below clogging of the filter may be observed and loss of charge balancing component. While there appears to be no upper limit for the FFA concentration of the lipid feedstock in regards to observation of the desired effect, it is not economically feasible to adjust the FFA concentration much above the lowest required limit.
  • step iv) the lipid feedstock is subjected to removing solid impurities, and optionally excess water, from the lipid feedstock (a).
  • Solid impurities removed in step iv) include e.g. salts, protein residues, bone meal, fibers, carbohydrates, and/or sand.
  • Step iv) and step ii) can be performed in any order in relation to each other.
  • removal of solid impurities in step iv) can be done before adjusting the net elementary charge of the lipid feedstock in step ii).
  • adjusting the net elementary charge of the lipid feedstock in step ii) is done before removal of the solid impurities in step iv).
  • step iii) is advantageously performed before removal of the solid impurities.
  • filter aid i.e. filter aid filtration
  • suitable filter aid materials include, but are not limited to, any material comprising or consisting of mineral, silicon, and/or cellulose based material, e.g. diatomaceous earth, diatomite, perlite, bentonite, palygorskite, kaolin, kaolinite, silica in various crystalline or amorphous configurations, sepiolite, magnesium silicate, silicon, aluminum oxide based materials, zinc oxide based materials, neutral bleaching earth, activated carbon, activated charcoal, cellulose fibers, or any combinations thereof.
  • the filter aid material may be activated by means known in the art.
  • the amount of insoluble impurities may be determined according to ISO 663:2017.
  • the heat treatment in step v) may be carried out at a pressure of 100 to 5100 kPa(a), preferably 150 to 2100 kPa(a), more preferably 200 to 600 kPa(a), most preferably 300 to 500 kPa(a).
  • a person skilled in the art will be competent to adjust the time to fit the intended purpose, appreciating that elevating the pressure minimizes losses of lipid material in the heat treatment step.
  • Solid impurities formed in the heat treatment step v) and/or further treatment step vi) as well as solid adsorbent material resulting from step vi) may be phase separated based on the lipid material forming a phase of its own, an oily phase, from which any impurities containing aqueous and/or solid reject may be removed by ordinary separation unit processes.
  • phase-separating refers both to liquid-liquid and liquid-solid phase separation. Suitable phase separation means include, but are not limited to, filtration, centrifugation, settling, and any combination thereof.
  • the heat-treated lipid feedstock (c) and/or further treated lipid feedstock (d), respectively may be subjected to drying, in particular evaporation, under conditions capable of removing water vapor from said lipid feedstock.
  • the evaporation conditions are controlled such that low-boiling components, such as low-boiling fatty acids of the lipid material are not lost.
  • the evaporation could be performed at temperature from 50 to 130 °C, and pressure from 1 to 100 kPa(a).
  • a combination of temperature of 105 °C and pressure of 8 kPa(a) could be applied to evaporation.
  • the thus rendered purified lipid feedstock typically comprises residual phosphorus and metals both below 30 mg/kg, preferably below 2.0 mg/kg, more typically close to 1 .0 mg/kg.
  • Impurity reduction for phosphorus is typically over 90% and for metals over 95% as compared to the lipid feedstock (a) factoring out any dilution of the lipid feedstock (a) due addition of charge balancing component(s) and/or FFA adjustment with lipid component(s).
  • the actual purification result is dependent on the quality of the initial feedstock.
  • step 11 with a FFA component 3 to obtain a FFA adjusted and charge balanced lipid feedstock 12 as discussed herein for step iii).
  • the FFA adjusted and charge balanced lipid feedstock 12 is then subjected to as step of removal 30 of solid impurities 39, preferably by filter aid filtration, as discussed herein for step iv) to obtain a conditioned lipid feedstock 13 having a total net elementary charge Qt above 0 mmol/kg, preferably 0.5 mmol/kg, such as from 0.5 to 3 mmol/kg.
  • a feed of lipid feedstock 1 is subjected to a step of adjusting the free fatty acid concentration 20 of the lipid feedstock 1 with a lipid component 3 to obtain a FFA adjusted lipid feedstock 14 as discussed herein for step iii).
  • the FFA adjusted lipid feedstock 14 is then subjected to a step of adjusting 10 the net elementary charge of the FFA adjusted lipid feedstock 14 with a charge balancing component 2 to obtain a FFA adjusted and charge-balanced lipid feedstock 12 as discussed herein for step ii).
  • the conditioned lipid feedstock 13 having a total net elementary charge Qt above 0 mmol/kg, preferably 0.5 mmol/kg, such as from 0.5 to 3 mmol/kg.
  • the conditioned lipid feedstock 13 is then subjected to a step of heating 40 the conditioned lipid feedstock 13, preferably in the presence of water, at a temperature from 180 to 325 °C as discussed herein for step v) to obtain a heat-treated lipid feedstock 41 .
  • the heat-treated lipid feedstock may then optionally be subjected to step of further treating 70 with an acid and/or absorbent material 71 , such as under bleaching conditions, to further purify the heat- treated lipid feedstock 41 as discussed herein for step vi) to obtain a further treated lipid feedstock 43.
  • a feed of lipid feedstock 1 is subjected to a step of adjusting 90 the free fatty acid concentration and the net elementary charge of the lipid feedstock 1 with second lipid feedstock 4 representing a FFA component and a charge balancing component as discussed herein for step ii) and iii) to obtain a FFA adjusted and charge-balanced lipid feedstock 14.
  • the FFA adjusted and charge balanced lipid feedstock 14 is then subjected to as step of removal 30 of solid impurities 39, preferably by filter aid filtration, as discussed herein for step iv) to obtain a conditioned lipid feedstock 13 having a total net elementary charge Qt above 0 mmol/kg, preferably 0.5 mmol/kg, such as from 0.5 to 3 mmol/kg.
  • the conditioned lipid feedstock 13 is then subjected to a step of heating 40 the conditioned lipid feedstock 13, preferably in the presence of water, at a temperature from 180 to 325 °C as discussed herein for step v) to obtain a heat-treated lipid feedstock 41 .
  • FIG 4 illustrates a fourth exemplary process flow of the present method.
  • the process flow exemplified in Figure 4 is particularly suitable for lipid feedstock having the net elementary charge Q1 of the lipid feedstock below 0 mmol/kg and free fatty acid concentration above 2 wt%.
  • a feed of lipid feedstock 1 is subjected to a step of adjusting 10 the net elementary charge of the lipid feedstock with a charge balancing component 2 to obtain a charge balanced feedstock 12 as discussed herein for step ii).
  • the charge balanced lipid feedstock 12 is then subjected to as step of removal 30 of solid impurities 39, preferably by filter aid filtration, as discussed herein for step iv) to obtain a conditioned lipid feedstock 13 having a total net elementary charge Qt above 0 mmol/kg, preferably 0.5 mmol/kg, such as from 0.5 to 3 mmol/kg.
  • the conditioned lipid feedstock 13 is then subjected to a step of heating 40 the conditioned lipid feedstock 13, preferably in the presence of water, at a temperature from 180 to 325 °C as discussed herein for step v) to obtain a heat-treated lipid feedstock 41.
  • the heat-treated feedstock may then optionally be subjected to step of further treating 70 with an acid and/or absorbent material 71 , such as under bleaching conditions, to further purify the heat-treated lipid feedstock 41 as discussed herein for step vi) to obtain a further treated lipid feedstock 43.
  • the heat-treated lipid feedstock 41 may be subjected to a step of phase-separation 60 to remove solid material 69 comprised in the heat-treated lipid feedstock 41 to obtain a solid-depleted heat-treated lipid feedstock 42 which is then subjected to further treatment 70 to obtain the further treated lipid feedstock 43.
  • the heat-treated lipid feedstock 41 and/or the further treated lipid feedstock 43 is subjected to a step of phase-separation, preferably filtering, 50 to obtain a purified lipid feedstock 51 .
  • a process for providing renewable hydrocarbons comprising x) purifying a lipid feedstock to obtain purified lipid feedstock as described in the foregoing, and y) subjecting the purified lipid feedstock to hydroprocessing, preferably catalytic hydroprocessing, to obtain at least one renewable hydrocarbon.
  • the lipid feedstock is the lipid feedstock as defined herein.
  • the lipid material may comprise streams known for their high phosphorous, metal and/or solid impurity content, such as SAO, AFP, and LQAF.
  • the hydroprocessing preferably catalytic hydroprocessing, may be any upgrading process employing hydrogen and where the lipid material may be used as the process feed, optionally with a co-feed.
  • the hydroprocessing may be an upgrading process to obtain liquid transportation fuel components, solvents, technical fluids, such as electrotechnical fluids, fatty alcohols, cracking feedstocks, such as feedstocks for thermal cracking and/or catalytic cracking, and/or base chemicals for different syntheses.
  • the hydroprocessing is catalytic hydroprocessing.
  • a co-feed of fossil origin is fed to catalytic hydroprocessing.
  • the catalytic hydroprocessing may occur in the presence of a catalyst selected from Pd, Pt, Ni, Co, Mo, Ru, Rh, W, or any combination of these, such as CoMo, NiMo, NiW, CoNiMo, NiMoW or together with SAPO-11 , SAPO-41 , ZSM-22, ZSM-23, ZSM-12, ZSM-48, ZSM-5, beta zeolites, ferrierite and mixtures thereof, such as Pt/SAPO-11/AI2O3, Pt/ZSM-22/ AI2O3, Pt/ZSM-23/AI2O3, Pt/SAPO-11/SiO2, optionally on a support, wherein the support comprises preferably alumina and/or silica.
  • a catalyst selected from Pd, Pt, Ni, Co, Mo, Ru, Rh, W, or any combination of these, such as CoMo, NiMo, NiW, CoNiMo, NiMoW or together with SAPO-11 , SAPO-41
  • Bleaching was performed by adding citric acid, water and bleaching earth adsorbent to the heat treated feedstock. Typically, for UCO, 800 mg/kg of citric acid (added as a 50 wt% aqueous solution) and 0.9 wt% of water was added to the oil, followed by mixing 8000 rpm at 85 °C for 2 min. Then, the bleaching earth (0.7 wt%) was added and 800 mbar pressure was applied and mixing was continued for 20 min. Next, the sample was dried by reducing the pressure to 80 mbar, increasing temperature to 105 °C, and continuing mixing for 10 min at the elevated temperature.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Wood Science & Technology (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Fats And Perfumes (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un procédé de purification de charge d'alimentation lipidique, comprenant i) la fourniture de la charge d'alimentation lipidique (a) ; ii) lorsque la charge élémentaire nette Q1 de la charge d'alimentation lipidique (a) est inférieure à 0 mmol/kg, l'ajustement de la charge élémentaire nette de la charge d'alimentation lipidique (a) à la charge élémentaire nette totale Qt d'au moins 0 mmol/kg, telle que de 0 à 10 mmol/kg, de préférence d'au moins 0,5 mmol/kg, telle que de 0,5 à 5 mmol/kg, plus préférablement d'au moins 1 mmol/kg, telle que de 1 à 3 mmol/kg, par mélange de la charge d'alimentation lipidique (a) avec un composant d'équilibrage de charge comprenant, ou incluant, un composé métallique ; iii) éventuellement l'ajustement de la concentration d'acide gras libre (FFA) de la charge d'alimenattion lipidique (a) à plus de 2 % en poids, par exemple de 2,5 à 40 % en poids, de préférence d'au moins 3 % en poids, par exemple de 3 à 30 % en poids, plus préférablement d'au moins 4 % en poids, par exemple de 4 à 20 % en poids, encore plus préférablement de 4 à 10 % en poids, du poids total de la charge d'alimentation lipidique résultante ; iv) l'élimination des impuretés solides, et éventuellement l'eau en excès, de la charge d'alimentation lipidique (a), pour obtenir une charge d'alimentation lipidique conditionnée (b) présentant une charge élémentaire nette totale Qt dans les valeurs définies à l'étape ii) ; v) le chauffage de la charge d'alimentation lipidique conditionnée (b), de préférence en présence d'eau, à une température de 180 à 325 °C pour obtenir une charge d'alimentation lipidique traitée thermiquement (c) ; vi) éventuellement le traitement supplémentaire de la charge lipidique traitée thermiquement (c) avec un matériau acide et/ou adsorbant, de préférence dans des conditions de blanchiment, pour obtenir une autre charge d'alimentation lipidique traitée (d) ; et vii) la récupération de la charge d'alimentation lipidique traitée thermiquement (c) et/ou l'autre charge d'alimentation lipidique traitée (d) par séparation de phase pour obtenir une charge d'alimentation lipidique purifiée (e). L'invention concerne en outre un procédé de fourniture d'hydrocarbures renouvelables, comprenant x) la purification d'une charge d'alimentation lipidique à l'aide dudit procédé fourni pour obtenir un matériau lipidique purifié, et y) la soumission du matériau lipidique purifié à un hydrotraitement pour obtenir au moins un hydrocarbure renouvelable.
PCT/FI2024/050525 2023-10-06 2024-10-04 Procédé de purification de lipides Pending WO2025074039A1 (fr)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
FI20236107A FI131414B1 (en) 2023-10-06 2023-10-06 Lipid material purification process
FI20236108 2023-10-06
FI20236107 2023-10-06
FI20236108A FI131419B1 (en) 2023-10-06 2023-10-06 Method for purification of lipids
FI20245090A FI131609B1 (en) 2024-01-31 2024-01-31 A method of pretreating a renewable feedstock
FI20245090 2024-01-31
FI20245163 2024-02-14
FI20245163A FI20245163A1 (en) 2024-02-14 2024-02-14 Method for treating low quality lipid feedstocks

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PCT/FI2024/050524 Pending WO2025074038A1 (fr) 2023-10-06 2024-10-04 Procédé de purification de matériel lipidique
PCT/FI2024/050525 Pending WO2025074039A1 (fr) 2023-10-06 2024-10-04 Procédé de purification de lipides

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PCT/FI2024/050524 Pending WO2025074038A1 (fr) 2023-10-06 2024-10-04 Procédé de purification de matériel lipidique

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US11466230B1 (en) * 2021-05-20 2022-10-11 Chevron U.S.A. Inc. Removing organic chlorides from glyceride oils
WO2023126563A1 (fr) * 2021-12-27 2023-07-06 Neste Oyj Procédé de production d'hydrocarbures en c3-c8 renouvelables

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CN101319169B (zh) * 2008-07-17 2011-01-05 四川大学 酯化/酯交换反应生物柴油清洁生产工艺
FI128069B2 (en) * 2018-07-20 2024-04-24 Neste Oyj Purification of recycled and renewable organic material

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US20200040278A1 (en) * 2016-09-30 2020-02-06 Neste Oyj Oil purification process
US20220073840A1 (en) * 2018-12-28 2022-03-10 Neste Oyj A method for treating lipid materials
US11466230B1 (en) * 2021-05-20 2022-10-11 Chevron U.S.A. Inc. Removing organic chlorides from glyceride oils
WO2023126563A1 (fr) * 2021-12-27 2023-07-06 Neste Oyj Procédé de production d'hydrocarbures en c3-c8 renouvelables

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