EP0728175B1 - Verfahren zur dechlorierung einer altölfraktion - Google Patents

Verfahren zur dechlorierung einer altölfraktion Download PDF

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Publication number
EP0728175B1
EP0728175B1 EP95930569A EP95930569A EP0728175B1 EP 0728175 B1 EP0728175 B1 EP 0728175B1 EP 95930569 A EP95930569 A EP 95930569A EP 95930569 A EP95930569 A EP 95930569A EP 0728175 B1 EP0728175 B1 EP 0728175B1
Authority
EP
European Patent Office
Prior art keywords
dechlorination
oil
used oil
chlorine
process according
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.)
Expired - Lifetime
Application number
EP95930569A
Other languages
English (en)
French (fr)
Other versions
EP0728175A1 (de
Inventor
Michel Laborde
Philippe Dolbecq
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TotalEnergies Marketing Services SA
Original Assignee
Total Raffinage Distribution SA
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 Total Raffinage Distribution SA filed Critical Total Raffinage Distribution SA
Publication of EP0728175A1 publication Critical patent/EP0728175A1/de
Application granted granted Critical
Publication of EP0728175B1 publication Critical patent/EP0728175B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
    • 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
    • C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/006—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents of waste oils, e.g. PCB's containing oils

Definitions

  • the present invention relates to a dechlorination process a fraction of used oil.
  • the present invention therefore aims to reduce the content of used oils chlorine at a rate compatible with recycling operations in refinery of these oils and she proposes, for this purpose, to use composite products solids, capable of fixing chlorinated ions, already known in the technical for other applications and under conditions different use.
  • chlorine traps based on alumina or metal oxides or metal hydroxides such as CaO, Na 2 O, K 2 O, MgO, as well as the corresponding hydroxides, for eliminating the chlorine present in the liquid or gaseous flows of process units, in particular in reforming or isomerization units.
  • compositions generally have a dimension particles of the order of 0.5 to 3 mm and they neutralize usually chlorine by adsorption. They are generally used at room temperature or order, at most 100 ° C and atmospheric pressure, and they usually retain about 15% of the chlorine present in the charges processed.
  • the Applicant has established that such chlorine traps are particularly well suited for an operation of partial dechlorination of used oils, upstream of any recycling operation in a refinery, in particular a vacuum distillation, and that, unexpectedly, their chlorine binding power increases significantly with the temperature of the treated oils, the chlorine trap can retain at least 40% of the chlorine present in the treated oil at a temperature between 300 and 400 ° C and at pressure atmospheric.
  • this amount of chlorine greater than 40% represents roughly the fraction of chlorine compounds that break down in a used oil recycling operation or which distill in a fractionation column under used oil vacuum, leading to acid formation hydrochloric, and the invention therefore proposes, in a simple manner, subjecting used oil to dechlorination upstream of any recycling operation.
  • the invention therefore relates to a method of dechlorination of a fraction of used lubricating oil, possibly mixed with another charge hydrocarbon, this process being characterized in that, in upstream of an oil refinery recycling operation used, the used oil is subjected to a dechlorination operation at least partial by passing over a bed of particles of an adsorption neutralizing composition containing, as active compound capable of fixing chlorine at least one oxide of a metal belonging to groups I and II of the Periodic classification and / or at least one hydroxide of a metal belonging to groups I and II of the Classification Periodic.
  • the active compound of the composition neutralizing will be an oxide of calcium, magnesium, sodium or potassium, or a calcium hydroxide, magnesium, sodium or potassium.
  • Calcium oxide and calcium hydroxide are active compounds even more preferred.
  • the dechlorination phase will be carried out under conditions such that at least 40% and, preferably, 60% of the amount of chlorine present in the used oil is retained by the neutralizing composition by adsorption.
  • These conditions are, for example, the following: a temperature of at least 150 ° C and, preferably, of the order of 400 ° C, an hourly space velocity of the used oil of 0.5 h -1 ( volume of used oil, per volume of adsorbent and per hour) and a pressure substantially equal to atmospheric pressure.
  • the used oil prior to the dechlorination operation, the used oil will be subjected to a distillation phase atmospheric at a temperature of 300 to 400 ° C in sight to remove the water and the light solvents it contains, and the dechlorination operation will be carried out on the used oil from this atmospheric distillation, possibly after reheating of this oil, by example by heat exchange, to increase the efficiency of dechlorination.
  • the used oil thus dechlorinated can then be subjected, for example, to vacuum distillation, preferably mixed with another filler, such as residue from atmospheric distillation, with a view to separating into particular vacuum diesel, vacuum distillate and a bituminous vacuum residue, without forming, as it is usual at this stage, hydrochloric acid responsible marked corrosion in the installations.
  • vacuum distillation preferably mixed with another filler, such as residue from atmospheric distillation, with a view to separating into particular vacuum diesel, vacuum distillate and a bituminous vacuum residue, without forming, as it is usual at this stage, hydrochloric acid responsible marked corrosion in the installations.
  • compositions of dechlorination used in the process of the invention are well known in the art and generally contain at least 25% by weight of active compound. They are marketed, for example, under the names TRAP'IT sales by Catalysts and Chemicals Europe, SELEXSORB HCl by ALCOA, and DISCOVERY ALUMINAS by the Dycat International Company.
  • the preferred composition for the implementation of the invention is that marketed under the name TRAP'IT, which contains, in% by weight, from 23.0 to 27.0% of CaO, constituting the active product, and from 43 to 53.0% of oxide of zinc, serving as a support, the complement to 100% being consisting of a binder.
  • TRAP'IT which contains, in% by weight, from 23.0 to 27.0% of CaO, constituting the active product, and from 43 to 53.0% of oxide of zinc, serving as a support, the complement to 100% being consisting of a binder.
  • This composition has, in general, an apparent specific mass of 0.720 to 0.800 cm 3 / g, a pore volume of 0.35 to 0.45 cm 3 / g and a specific surface of at least 22 m 2 / g. It is usually in the form of rods with a diameter of 1.2 to 1.8 mm and a length of about 4.0 to 12.0 mm.
  • the used oil to be treated arriving via the line 1, is first topped, by atmospheric distillation, in a column 2.
  • the water present in the used oil (4 to 10% by weight) is discharged at the top of the column via line 3, while the light solvents are evacuated via line 4.
  • the chlorine trap contained in the tank 6 retains about 60% of the chlorine present in the oil used, and the treated oil, which contains only about 200 ppm of chlorine, is evacuated by a line 8 towards a vacuum distillation column 9, in which it is introduced, for example, with a residue of atmospheric distillation arriving via line 10.
  • the chlorine content of the treated oil is compatible with the conditions of vacuum distillation, which is takes place without any particular risk of corrosion due to formation of hydrochloric acid in column 9.
  • Example 1 which follows relates to an application of the method according to the invention using the device of the figure 1, it being understood that other forms of implementation are within the scope of the invention.
  • Example 2 illustrates improved dechlorination of treated oil as the treatment temperature rises dechlorination.
  • TRAP'IT registered trademark
  • the oil leaving balloon 6 via line 8 does not contain more than 123 ppm by weight of chlorine and 62% of the chlorine present in the oil at the inlet of balloon 6 have therefore been fixed and retained by the TRAP'IT composition.
  • composition of TRAP'IT can be scrapped or regenerated.
  • This example aims to show the interest of driving the dechlorination operation at such a high temperature as possible.
  • a head of used oil containing 325 ppm of chlorine is treated in a flask containing 15m3 of the TRAP'IT composition, at an hourly space speed of 0.5 h -1 .
  • the treatment is carried out at various temperatures and the dechlorination rate is measured each time, that is to say the fraction, expressed in%, of chlorine of the charge retained by the dechlorination composition.
  • the composition of DYCAT 115, in% by weight, is given in Table II below.
  • the DYCAT 115 is in the form of spheres of approximately 3 to 5 mm in diameter.
  • COMPOUNDS % in weight Calcium oxide At least 60 Aluminum oxide 8 Manganese oxide 5 Sodium oxide 4.5 Silica 5.0 Lead ⁇ 0.1 As, Cd Traces

Landscapes

  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)
  • Fats And Perfumes (AREA)

Claims (7)

  1. Verfahren zum Entchloren einer Fraktion von altem Schmieröl, gegebenenfalls in Mischung mit einer weiteren teerhaltigen Fracht, dadurch gekennzeichnet, daß vorgeschaltet vor einem Arbeitsgang zum raffinerietechnischen Recycling des Altöls das Altöl einem Arbeitsgang zur zumindest teilweisen Entchlorung unter Überführung über ein Bett aus Teilchen einer durch Adsorption neutralisierenden Zusammensetzung unterzogen wird, welche als den zur Fixierung des Chlors geeigneten Wirkstoff mindestens ein Oxid eines Metalls aus der Gruppe I und II des Periodensystems und/oder mindestens ein Hydroxid eines Metalls aus der Gruppe I und II des Periodensystems enthält.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Entchlorungsschritt unter Bedingungen stattfindet, bei denen beispielsweise mindestens 40 % und vorzugsweise etwa 60 % des in dem verarbeiteten Altöl vorhandenen Chlors durch die adsorbierende Zusammensetzung zurückgehalten werden.
  3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß der Entchlorungsschritt bei einer Temperatur von mindestens 150 °C und vorzugsweise in der Größenordnung von 400 °C stattfindet, und daß die räumliche Geschwindigkeit pro Stunde der Altölfracht etwa 0,5 h-1 beträgt.
  4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß vor dem Schritt der Entchlorung das Altöl einem Schritt zur Destillation unter atmosphärischem Druck bei einer Temperatur von 300 bis 400 °C unterzogen wird, womit das Wasser und die darin enthaltenen leichten Lösungsmittel entzogen werden sollen, und daß der Schritt zur Entchlorung mit dem aus dieser Destillation unter atmosphärischem Druck kommenden Altöl, gegebenenfalls nach erneuter Erwärmung dieses Öls, durchgeführt wird.
  5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß der Wirkstoff in der durch Adsorption neutralisierenden Zusammensetzung ein Kalziumoxid, ein Magnesiumoxid, ein Natriumoxid oder ein Kaliumoxid und vorzugsweise ein Kalziumoxid ist.
  6. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß der Wirkstoff in der durch Adsorption neutralisierenden Zusammensetzung ein Kalziumhydroxid oder Magnesiumhydroxid oder Kaliumhydroxid und vorzugsweise ein Kalziumhydroxid ist.
  7. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß im Anschluß an den Entchlorungsvorgang das entchlorte Altöl einer Destillation im Vakuum unterzogen wird.
EP95930569A 1994-09-13 1995-09-11 Verfahren zur dechlorierung einer altölfraktion Expired - Lifetime EP0728175B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9410899 1994-09-13
FR9410899A FR2724391A1 (fr) 1994-09-13 1994-09-13 Traitement de dechloration d'une fraction d'huile usee
PCT/FR1995/001162 WO1996008546A1 (fr) 1994-09-13 1995-09-11 Procede de dechloration d'une fraction d'huile usee

Publications (2)

Publication Number Publication Date
EP0728175A1 EP0728175A1 (de) 1996-08-28
EP0728175B1 true EP0728175B1 (de) 1999-11-10

Family

ID=9466887

Family Applications (1)

Application Number Title Priority Date Filing Date
EP95930569A Expired - Lifetime EP0728175B1 (de) 1994-09-13 1995-09-11 Verfahren zur dechlorierung einer altölfraktion

Country Status (8)

Country Link
US (1) US5783068A (de)
EP (1) EP0728175B1 (de)
JP (1) JP4027417B2 (de)
AT (1) ATE186563T1 (de)
CA (1) CA2176210C (de)
DE (1) DE69513277T2 (de)
FR (1) FR2724391A1 (de)
WO (1) WO1996008546A1 (de)

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US6196458B1 (en) * 1997-12-01 2001-03-06 Walker Digital, Llc Method and apparatus for printing a billing statement to provide supplementary product sales
US6026368A (en) * 1995-07-17 2000-02-15 24/7 Media, Inc. On-line interactive system and method for providing content and advertising information to a targeted set of viewers
FR2757873B1 (fr) * 1996-12-31 1999-03-19 Total Raffinage Distribution Procede de regeneration d'une fraction d'huile lubrifiante usee
US6106699A (en) * 1997-04-29 2000-08-22 Probex Process for de-chlorinating and de-fouling oil
US8838574B2 (en) * 2006-06-09 2014-09-16 International Business Machines Corporation Autonomic index creation, modification and deletion
US20080027252A1 (en) * 2006-07-27 2008-01-31 Burkholder Kermit L Oil dehalogenation method
US20120325724A1 (en) * 2011-06-27 2012-12-27 Driver Michael S Recovery of alkyl chloride adsorbtion capacity by basic solution treatment of spent adsorbent
US10829696B2 (en) 2016-08-01 2020-11-10 Sabic Global Technologies B.V. Dechlorination of mixed plastics pyrolysis oils using devolatilization extrusion and chloride scavengers
CN107892990B (zh) * 2017-11-14 2020-11-13 新疆聚力环保科技有限公司 一种废矿物油全氢型再生生产高档润滑油基础油的方法
CN108587765B (zh) * 2018-06-06 2021-02-26 武汉科林化工集团有限公司 一种废润滑油再生优质基础油的预处理工艺
CN108587766B (zh) * 2018-06-06 2021-03-19 武汉科林化工集团有限公司 一种无污染的废润滑油连续再生预处理工艺
CN110548479A (zh) * 2019-10-03 2019-12-10 武汉禾谷环保有限公司 一种高强度液相脱氯剂及其制备方法和应用

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US2481300A (en) * 1943-08-10 1949-09-06 Shell Dev Process for purifying hydrocarbons
AT262479B (de) * 1965-10-21 1968-06-10 Oemv Ag Verfahren zur Aufarbeitung von gebrauchten Schmierölen
US3761534A (en) * 1971-12-29 1973-09-25 Dow Chemical Co Removal of acidic contaminants from process streams
DE2508713C3 (de) * 1975-02-28 1979-04-12 Adolf Schmids Erben Ag, Bern Verfahren zur Aufarbeitung von gebrauchtem Mineralöl
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US4612404A (en) * 1982-05-24 1986-09-16 Thyagarajan Budalur S Process for treatment of fluids contaminated with polychlorinated biphenyls
DE3443722A1 (de) * 1984-11-30 1986-06-12 Foerster Guenther Verfahren zur thermischen beseitigung von halogenverbindungen, insbesondere dioxine, phosgen und polychlorierte biphenyle bildende chlorverbindungen enthaltenden abfaellen sowie wirbelschicht-reaktor zu seiner durchfuehrung
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CA2068905C (en) * 1992-05-19 1997-07-22 Terry A. Wilson Waste lubricating oil pretreatment process

Also Published As

Publication number Publication date
FR2724391B1 (de) 1997-02-21
EP0728175A1 (de) 1996-08-28
ATE186563T1 (de) 1999-11-15
JP4027417B2 (ja) 2007-12-26
FR2724391A1 (fr) 1996-03-15
DE69513277D1 (de) 1999-12-16
CA2176210C (fr) 2007-11-13
JPH09507878A (ja) 1997-08-12
WO1996008546A1 (fr) 1996-03-21
DE69513277T2 (de) 2000-05-11
US5783068A (en) 1998-07-21
CA2176210A1 (fr) 1996-03-21

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