WO2008106406A1 - Méthode de production d'huiles minérales - Google Patents

Méthode de production d'huiles minérales Download PDF

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Publication number
WO2008106406A1
WO2008106406A1 PCT/US2008/054910 US2008054910W WO2008106406A1 WO 2008106406 A1 WO2008106406 A1 WO 2008106406A1 US 2008054910 W US2008054910 W US 2008054910W WO 2008106406 A1 WO2008106406 A1 WO 2008106406A1
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WO
WIPO (PCT)
Prior art keywords
solvent
phase
water
purified
aromatic
Prior art date
Application number
PCT/US2008/054910
Other languages
English (en)
Inventor
Gabriel Farkas
Original Assignee
Gabriel Farkas
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
Application filed by Gabriel Farkas filed Critical Gabriel Farkas
Publication of WO2008106406A1 publication Critical patent/WO2008106406A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0426—Counter-current multistage extraction towers in a vertical or sloping position
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0446—Juxtaposition of mixers-settlers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0488—Flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B01D11/0492—Applications, solvents used
    • 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
    • C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
    • C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
    • C10G21/12—Organic compounds only
    • C10G21/27—Organic compounds not provided for in a single one of groups C10G21/14 - C10G21/26
    • 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
    • C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
    • C10G31/08—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by treating with water
    • 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
    • C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step

Definitions

  • the extraction solvent can be separated from the extract by addition of water (or other solvents or solvent mixtures) to the extract stream.
  • water or other solvents or solvent mixtures
  • the addition of water results in the formation of a biphasic system in which the water and extraction solvent form an aqueous phase, and the (partially purified) desired product or extract forms a second phase.
  • the aqueous phase can be distilled. Water can also be used to control the solubility of aromatic species in the solvent.
  • the present invention provides improved methods and systems for preparing highly purified mineral oils.
  • the inventive methods and systems are generally less expensive and more environmentally-friendly than previously-known methods.
  • PMB 348934.1 2 an extraction solvent; (b) separating a mineral oil phase from the extract phase;
  • the process further comprises the steps of: (h) contacting the aromatic phase of step (d) with regenerated water of step (e) to provide a purified aromatic phase and water with solvent traces; (i) contacting the wetted solvent phase of step (d) with the purified aromatic phase of step (h) to provide a partially purified wetted solvent and an aromatic phase; and (j) contacting the partially purified wetted solvent of step (i) with the light hydrocarbon feedstock to provide a purified wetted solvent and a modified feedstock (e.g., a feedstock enriched in saturates extracted from the solvent).
  • a modified feedstock e.g., a feedstock enriched in saturates extracted from the solvent.
  • the water with solvent traces from step (h) is purified with reverse osmosis to remove solvent traces prior to contacting the aromatic phase of step (d) and the mineral oil phase of step (b).
  • the purified wetted solvent of step (j) is further treated by nano-filtration.
  • Figure 1 is a flow diagram illustrating one embodiment of a purification process according to the invention.
  • Figure 2 is a flow diagram illustrating another embodiment of process for producing mineral oils.
  • the present invention relates generally to improved methods and systems for the production of mineral oils from light distillate feedstock.
  • the hydrocarbon feedstock which may be treated by the process of this invention is preferably a lighter boiling feedstock (such as a distillate, preferably a light distillate) from petroleum or synthetic sources.
  • the feedstock may be derived from a synthetic liquid such as shale oil, coal liquid, or mixtures thereof.
  • the contacting of the feedstock with the solvent is carried out, and/or the mixture is maintained, at a temperature of from about 5 to about 20 0 C, preferably from about 5° to 10 0 C, below the critical solution temperature of the mixture.
  • the critical solution temperature is the highest temperature at which the particular mixture of solvents and feedstock becomes miscible, i.e., the solvents form only one homogeneous phase.
  • the temperature to which the components of the mixture are exposed should maintain the solvent- feedstock system as a two-phase system. The exact temperatures which will be employed for this purpose depend on many factors such as the specific feedstock utilized and particular solvent
  • temperatures employed during the contacting must be sufficient to achieve relatively low phase viscosities in continuous countercurrent towers if such towers are employed to extract the solvents.
  • the extraction process of this invention is particularly suited for being conducted in a continuous mode with reference to the schematic diagram of FIG. 1.
  • a feedstock 30 from line 2 is contacted in a first contacting zone 4 with a solvent 32 via line 6.
  • First contacting zone 4 may be any apparatus suitable for obtaining an intimate mixture of hydrocarbon feedstock and solvents at temperatures up to and above 100 0 C, such as a contacting tower or a mixer-settler.
  • the mineral-oil containing phase 34 is drawn off, and the remaining phase 36 (containing the aromatics and the solvent 40) is transferred via line 8 through area 10 to second contacting zone 12.
  • Second contacting zone 12 may be any apparatus where mixing and separation of the liquid phases may take place, such as a settler where the aromatics-containing phase settles to the bottom.
  • Water 42 is added via line 20 to the mixture in second contacting zone 12; the aromatic-containing layer then separates and is removed from the second contacting zone 12 via line 14 as aromatics 44.
  • the remaining phase is transferred to separation zone 18, where the water is removed and recycled to second contacting zone 12 via line 20 and the solvent is recovered and returned via line 6 for further extraction procedures.
  • PMB 348934.1 5 When a mixer is required, many conventional mixers known in the art can be used.
  • static mixers include, for example, Multiflux, Sulzer, PMR, McHugh, Komax and Honeycomb, X, Ross-ISG and helical mixers.
  • water must be purified prior to use in the removal of remaining traces of solvent in the aromatics and in the aliphatics. While water can be purified by any technique known in the art, it is somewhat difficult to completely separate pure water from solvents such as NMP by distillation.
  • the water can be purified in two steps, e.g., by (i) contacting the water with the aromatic (to remove aromatics from the water and to remove traces of solvent from the aromatic) and (ii) purifying the water by reverse osmosis to remove traces of solvent from the water.
  • a reverse osmosis membrane which is resistant to NMP in this step; for example, polytetrafluoroethylene polymer membranes are relatively NMP resistant.
  • Emulsion formation is undesirable because it slows processing and increases the likelihood of contamination of the desired products.
  • the wetted solvent is mixed with the same aromatic produced in the process disclosed herein, but it is preferably cleaned of solvent traces.
  • the ratio of aromatics to solvent can be about 2:1; therefore a recirculation scheme must be used (the overall production of aromatics in the process does not generally approach a level required to sustain this ratio);
  • the wetted solvent is cleaned of aliphatics, by contacting the wetted solvent with the feedstock for the process. Aliphatics are a major cause of emulsions, specially the denser type which do not separate fast enough in the decanters.
  • the aromatics must be removed (see step (i)) and taken out of the process. If aliphatics are removed (e.g., by contacting with the raw material (feedstock), but aromatics remain to contaminate the wetted solvent, then some aromatics will go back into the process and potentially diminish the capacity of the process.
  • steps (i) and (ii) are not sufficient to provide clean wetted solvent, a nano-filtration step can be used to further reduce the hydrocarbon content in the wetted solvent.
  • the invention provides a process in which distilled
  • PMB 348934.1 6 water is freed of solvent and aromatics, and the recovered solvent is freed from aromatics and aliphatics. This can be accomplished without using additional inputs by careful recirculation and purification of the materials (water, solvent, feedstock) used in the process, e.g., as described below.
  • stage 100 the inputs into stage 100 are feedstock and solvent; outputs are solvent plus aromatics (extract) and an aliphatic phase retaining traces of solvent.
  • the aliphatic material is further purified by removal of remaining solvent.
  • the solvent so separated can be recovered and re-used, as described herein.
  • the aliphatic phase and purified water are mixed, e.g., in a static mixer, and then separated, e.g., by settling in a decanter.
  • stage 200 will include 1-2 countercurrent extraction stages, and that the water will be present at about 100%-200% by weight of the aliphatic.
  • An equivalent mass-transfer column can also be used.
  • the inputs into stage 200 are partially-purified aliphatic and water; outputs are water (with some solvent) and purified aliphatic phase.
  • stage 300 of FIG. 2 aromatic material is separated from solvent.
  • the solvent so separated can be recovered and re-used, as described herein, and the aromatic can be further purified so as to be sufficiently pure to be used or re-sold.
  • the solvent (extract) phase from stage 100 is mixed with water from stage 200, e.g., in a static mixer, and then separated, e.g., by settling in a decanter.
  • stage 300 will include one countercurrent extraction stage, and that the water will be present at about 80% by weight of the solvent phase (extract).
  • An equivalent mass-transfer column can also be used.
  • the inputs into stage 300 are solvent phase (extract) from stage 100 and water with solvent traces from stages 200 and 600; outputs are wetted solvent (with traces of
  • the aromatics recovered from the process according to this invention can have not more than 10% aliphatics, more preferably not more than 5% aliphatics after purification according to the disclosed process. More highly purified aromatics generally can be sold for a higher price than less-purified aromatics. In addition, a higher proportion of aliphatics are recovered from the raw material, increasing the overall efficiency of the process.
  • the water used in the extraction process has no more than 1% hydrocarbons after purification and before recirculation and re-use of the water. In certain embodiments, the water has no more than 0.5% or 0.1% hydrocarbons after purification and before recirculation and re-use.
  • the disclosed process is capable of providing an aliphatic
  • the solvent (NMP) used in the extraction process has no more than 1 % hydrocarbons after purification and before recirculation and re-use of the solvent.
  • the water has no more than 0.5% or 0.1% hydrocarbons after purification and before recirculation and re-use.
  • the present invention can use lower amounts of solvent and therefore lower amounts of energy to evaporate, and recover, the water, via a lower solvent-to-raw material ratio.
  • Figure 3 shows a schematic diagram of a system according to one embodiment of the present invention. Referring to Figure 3:
  • processor 300 the aqueous fraction from processor 200 is mixed with the
  • PMB 348934.1 10 aqueous fraction from processor 600 and with the extraction solvent phase from processor 100.
  • wetted solvent may be added from reverse osmosis unit 700 via conduit 7A, and additional recovered hydrocarbons may be added from mixer 900 via conduit 9A.
  • the phases are separated, and the aromatics-containing phase (at this point containing some traces of solvent) is drawn off via conduit 3A to processor 400.
  • the solvent-containing phase is transferred to processor 500 via conduit 3B.
  • processor 500 which is preferably capable of high volume recirculation of the aromatics phase from processor 400, the aromatics phase is mixed with the solvent-containing phase from processor 300, to recover traces of aromatics from the solvent-containing phase.
  • the aromatics phase (now having traces of extraction solvent) is transferred via conduit 5A to processor 600, while the solvent-containing phase (now having traces of aliphatics but with most of the aromatics removed) is drawn off to processor 800 via conduit 5B.
  • the aromatics phase from processor 500 is combined with water received via conduit 7C from reverse osmosis unit 700. After mixing and separation, the aromatics phase, now largely free of extraction solvent, is removed via conduit 6 A to be stored for further processing or sale.
  • extraction solvent present in the aqueous phase recovered from processor 400 is separated from the water by reverse osmosis.
  • the separated extraction solvent can be recycled, e.g., by transfer to processor 300 via conduit 7A.
  • the purified water is recycled, e.g., to processors 200 and 600 via conduits 7B and 7C.
  • the wetted solvent received from processor 500 via conduit 5B is mixed with the hydrocarbon feedstock. This mixing removes traces of hydrocarbons from the extraction solvent; after phase separation, these hydrocarbons are extracted into the feedstock and
  • PMB 348934.1 1 1 are transferred with the feedstock to processor 100 via conduit 8A.
  • the wetted solvent is removed via conduit 8B to processor 900.
  • the extraction solvent is treated by ultrafiltration to remove traces of hydrocarbons from the extraction solvent. These recovered hydrocarbons can be discarded or can be recycled, e.g., by transferring to processor 300 via conduit 9A.
  • the wetted solvent now largely tree of hydrocarbons, is recovered for recycling or reuse. For example, water can be removed from the wetted extraction solvent by distillation as described below.
  • the wetted solvent passes through a conduit to distillation unit 1000, where the wetted solvent is heated to cause vaporization and separation of the solvent from the remaining water.
  • the distillation process can be performed under reduced pressure to reduce the boiling point of the components and thereby minimize the damage to the solvent.
  • the distillate may be fractionated using distillation columns or other means to ensure separation of the components.
  • Some modern distillation technologies allow for very low operating costs, e.g., by recovery of heat (energy inputs). Technologies are known in the art for recovery of up to 95% of heat input in the recovery of sweet water from sea water, and such technologies can be used to reduce the energy costs.
  • the recovered solvent can be returned via a conduit 1OA to processor 100 for reuse; similarly, the recovered water can be returned via conduit lOBto processor 400 for reuse.

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

Abstract

L'invention concerne une méthode de production d'un produit aliphatique purifié à partir d'une matière première contenant des aromates, par une méthode améliorée d'extraction liquide-liquide. L'huile minérale ainsi obtenue est hautement purifiée, contient une faible teneur en aromates, et est produite par une méthode abordable et écologique.
PCT/US2008/054910 2007-02-26 2008-02-25 Méthode de production d'huiles minérales WO2008106406A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US90376307P 2007-02-26 2007-02-26
US60/903,763 2007-02-26
US91020707P 2007-04-04 2007-04-04
US60/910,207 2007-04-04

Publications (1)

Publication Number Publication Date
WO2008106406A1 true WO2008106406A1 (fr) 2008-09-04

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PCT/US2008/054912 WO2008106407A1 (fr) 2007-02-26 2008-02-25 Méthode de production d'huiles minérales
PCT/US2008/054910 WO2008106406A1 (fr) 2007-02-26 2008-02-25 Méthode de production d'huiles minérales

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US (1) US20090200208A1 (fr)
WO (2) WO2008106407A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITRA20110036A1 (it) * 2011-12-30 2013-07-01 Dard Srl Estrazione di composti organici clorurati e composti aromatici da soluzioni liquide per mezzo di oli

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI656115B (zh) * 2014-01-24 2019-04-11 美商Ｇｔｃ科技美國有限責任公司 用於移除重烴之方法及系統
WO2016162887A1 (fr) 2015-04-09 2016-10-13 Bharat Petroleum Corporation Limited Solvant exempt de composés aromatiques et procédé de préparation associé à partir d'un flux de pétrole
EP3380583A4 (fr) * 2015-11-23 2019-07-17 Integrated Green Energy Solutions Ltd Production de combustibles hydrocarbonés à partir de plastiques
JP2023545518A (ja) * 2020-10-16 2023-10-30 シエル・インターナシヨナル・リサーチ・マートスハツペイ・ベー・ヴエー 脂肪族炭化水素の回収
US20230374400A1 (en) * 2020-10-16 2023-11-23 Shell Oil Company Recovery of aliphatic hydrocarbons
WO2022079012A1 (fr) * 2020-10-16 2022-04-21 Shell Internationale Research Maatschappij B.V. Récupération d'hydrocarbures aliphatiques
WO2022079059A1 (fr) * 2020-10-16 2022-04-21 Shell Internationale Research Maatschappij B.V. Récupération d'hydrocarbures aliphatiques
WO2022079046A1 (fr) * 2020-10-16 2022-04-21 Shell Internationale Research Maatschappij B.V. Récupération d'hydrocarbures aliphatiques
EP4229153A1 (fr) * 2020-10-16 2023-08-23 Shell Internationale Research Maatschappij B.V. Récupération d'hydrocarbures aliphatiques
WO2022079057A1 (fr) * 2020-10-16 2022-04-21 Shell Internationale Research Maatschappij B.V. Récupération d'hydrocarbures aliphatiques
WO2022101392A1 (fr) * 2020-11-13 2022-05-19 Shell Internationale Research Maatschappij B.V. Récupération d'hydrocarbures aliphatiques

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US3567791A (en) * 1969-05-12 1971-03-02 Exxon Research Engineering Co Extraction process
US5039399A (en) * 1989-11-20 1991-08-13 Texaco Inc. Solvent extraction of lubricating oils
US5041227A (en) * 1990-10-09 1991-08-20 Bend Research, Inc. Selective aqueous extraction of organics coupled with trapping by membrane separation

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US2246297A (en) * 1938-12-10 1941-06-17 Standard Oil Dev Co Solvent extraction process
US2837585A (en) * 1954-02-23 1958-06-03 Union Carbide Corp Separation of aromatics and aliphatics using alkylene carbonate
FR1326487A (fr) * 1962-03-27 1963-05-10 Raffinage Cie Francaise Procédé d'extraction d'hydrocarbures naphtaléniques
US3227632A (en) * 1962-10-22 1966-01-04 Koppers Co Inc Recovery of aromatic hydrocarbon by extractive distillation with anhydrous liquid propylene carbonate

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
US3567791A (en) * 1969-05-12 1971-03-02 Exxon Research Engineering Co Extraction process
US5039399A (en) * 1989-11-20 1991-08-13 Texaco Inc. Solvent extraction of lubricating oils
US5041227A (en) * 1990-10-09 1991-08-20 Bend Research, Inc. Selective aqueous extraction of organics coupled with trapping by membrane separation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITRA20110036A1 (it) * 2011-12-30 2013-07-01 Dard Srl Estrazione di composti organici clorurati e composti aromatici da soluzioni liquide per mezzo di oli

Also Published As

Publication number Publication date
US20090200208A1 (en) 2009-08-13
WO2008106407A1 (fr) 2008-09-04

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