EP0257260B2 - Procédé de traitement par hydrogénation des huiles minérales contaminées avec les chlorobiphényles - Google Patents

Procédé de traitement par hydrogénation des huiles minérales contaminées avec les chlorobiphényles Download PDF

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Publication number
EP0257260B2
EP0257260B2 EP87109958A EP87109958A EP0257260B2 EP 0257260 B2 EP0257260 B2 EP 0257260B2 EP 87109958 A EP87109958 A EP 87109958A EP 87109958 A EP87109958 A EP 87109958A EP 0257260 B2 EP0257260 B2 EP 0257260B2
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EP
European Patent Office
Prior art keywords
weight
process according
oil
hydrogenation
phase
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
EP87109958A
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German (de)
English (en)
Other versions
EP0257260B1 (fr
EP0257260A1 (fr
Inventor
Werner Dr. Döhler
Rolf Dr. Holighaus
Klaus Dr. Niemann
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Veba Oel Technologie und Automatisierung GmbH
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Veba Oel Technologie und Automatisierung GmbH
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Application filed by Veba Oel Technologie und Automatisierung GmbH filed Critical Veba Oel Technologie und Automatisierung GmbH
Priority to AT87109958T priority Critical patent/ATE68099T1/de
Publication of EP0257260A1 publication Critical patent/EP0257260A1/fr
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Publication of EP0257260B1 publication Critical patent/EP0257260B1/fr
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Classifications

    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
    • A62D3/37—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by reduction, e.g. hydrogenation
    • 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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • A—HUMAN NECESSITIES
    • A62—LIFE-SAVING; FIRE-FIGHTING
    • A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
    • A62D2101/20—Organic substances
    • A62D2101/22—Organic substances containing halogen
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S210/00—Liquid purification or separation
    • Y10S210/902—Materials removed
    • Y10S210/908—Organic
    • Y10S210/909—Aromatic compound, e.g. pcb, phenol

Definitions

  • the invention relates to a process for the hydrogenating treatment of mineral oils contaminated with multiply chlorinated biphenyls (PCBs), and to distillation residues of such mineral oils.
  • PCBs multiply chlorinated biphenyls
  • PCB-containing liquids or PCB-containing liquids mixed with oil residues after their use are to be regarded as hazardous waste, which must be recorded, properly handled and disposed of or safely disposed of.
  • thermal incineration processes therefore require extensive precautions to control and possibly treat the resulting exhaust gases and, if necessary, also to treat and landfill any solid residues that may occur. Still, thermal combustion processes are the most developed and widely used. The rest of the processes are only partially developed on a laboratory scale or on a semi-industrial scale.
  • EP-0 178 001 A describes a further process for working up by refining and / or eliminating halogen, nitrogen and / or sulfur-containing compounds which are difficult to biodegrade in hydrocarbon feed streams.
  • the feed stream is first passed together with hydrogen gas over a pre-column filled with an absorbent and then over a fixed bed contact preferably made of nickel or cobalt plus molybdenum on a support.
  • the object of the invention is to provide a further process which can be used on an industrial scale for working up PCB-containing waste oils.
  • This process enables multi-chlorinated biphenyls to be broken down to values of up to 1 ppm and below.
  • the mineral base oils contained as the main component can be reused without being lost, for example, by incineration or other mining processes.
  • this object is achieved in that the above-mentioned feed hydrogen pressurization under the typical conditions of a sump phase hydrogenation or a combined sump / gas phase hydrogenation at hydrogen pressures of 20 to 325 bar. Temperatures from 250 to 500 ° C and gas-oil ratios of 100 to 3000 Nm 3 t are subjected to, wherein 0.5 to 5 wt .-% of a hollow surface-containing suspended solid are used in the bottom phase hydrogenation.
  • This method is particularly suitable for waste oils containing PCB or with drilling oils, cutting oils, transformer oils, hydraulic oils and the like. Work up mixed used oils in a sump or combined sump / gas phase hydrogenation.
  • the feed oils are preferably used as such or in a mixture with residual oils, heavy oils or finely ground coal in the bottom phase hydrogenation, with the use of coal providing a step for preparing the mixture of finely ground coal and the oil components. It is advantageous to add 30 to 95% by weight, preferably 50 to 95% by weight of residual oil or heavy oil to the bottoms hydrogenation.
  • additive a finely divided carbon-containing surface-rich suspended material
  • the feed mixture then goes through a compression stage and is charged with hydrogen-containing cycle gas and fresh hydrogen.
  • heat exchangers in which heat is exchanged with product streams to heat the feed mixture, the mixture passes through a so-called preheater and enters the bottom phase reactor from below. They are generally vertical tubular reactors without internals.
  • the hydrogenation reaction takes place at elevated pressure, at hydrogen pressures between 20 and 325 bar, and at elevated temperature, between 250 and 500 ° C and at gas-oil ratios of 100 to 3,000 Nm 3 / t, with the gas is the hydrogen-containing hydrogenation gas.
  • the desired degree of conversion and the required limit for the degradation of the chlorobiphenyls determine the flow rate of the feed products. Typical values are 0.4 to 1.0 t / m 3 h.
  • the reaction products are expediently passed over a hot separator operated at reaction pressure and at a temperature which is preferably 20 to 50 ° C. lower than the reaction temperature.
  • the uncondensed hydrocarbons are removed overhead and the bottom products containing residues at the bottom.
  • Distillable heavy oil components can be separated in a downstream stripper and can be further processed by combining with the top product of the hot separator.
  • the residue behind the stripper can be used to generate hydrogen or energy.
  • a gas phase hydrogenation for further processing of the uncondensed reaction products, which have been drawn off at the top of the hot separator, can be directly coupled to the previously described bottom phase hydrogenation without reheating or depressurization.
  • the further hydrogenation, stabilization and removal in the gas phase hydrogenation, for example of heteroatoms such as sulfur or nitrogen, to obtain feedstocks with reformer feed specification or middle distillate takes place on fixed bed catalysts using commercially available catalysts.
  • the product streams After passing through the gas phase hydrogenation, the product streams are condensed and cooled by intensive heat exchange and separated into a liquid phase and a gas phase in a high-pressure cold separator. After the liquid phase has been let down, it is usually fed to a stabilizing column in order to remove the C 4 products and to obtain a stabilized syncrude.
  • the gaseous products pass through a gas scrubber to remove, among other things, H 2 S and NH 3 .
  • Part of the purified hydrogen-rich gas is recycled as cycle gas into the bottom phase hydrogenation.
  • the separation is then carried out in an atmospheric distillation, depending on the determination of the boiling cuts in naphtha, middle distillate and vacuum gas oil. If coal and feed oil are used together, the ratio is preferably 1:20 to 1: 1, in particular 1: 5 to 4: 5.
  • a cold separator stage with subsequent expansion and separation of the liquid products into an aqueous phase and a mineral oil-containing phase and atmospheric distillation of the oil-containing phase can also directly follow the bottom phase hydrogenation.
  • the suspended lignite coke from shaft and hearth furnaces, lignite coarse, soot from the gasification of heavy oil, hard coal are additives.
  • Lignite or hydrogenation residues and activated coke, petroleum coke and dusts from the Winkler gasification and high-temperature Winkler gasification of coal, ie materials with a large inner surface and with a pore structure for demetallization and deasphalting and for taking up coke precursors when carrying out the phase-phase hydrogenation are suitable .
  • Red masses, Bavarian masses, iron oxides and electrostatic filter dust and cyclone dust from metal / ore processing can also be used with advantage.
  • the proportion of these additives is preferably 0.5 to 5% by weight and, if carbon-containing additives are used, these can be mixed with salts of metals from subgroups 1 to 8 and 4.
  • Main group of the periodic system of the elements preferably iron, cobalt, nickel, vanadium, molybdenum, for example Fe (II) sulfate.
  • Alkaline earth compounds can also be used to neutralize the hydrogen halide and form water-soluble salts.
  • the sodium compounds for example sodium sulfide, are preferred.
  • a used motor oil with 1 100 ppm polychlorobiphenyl (PCB) is contacted in a continuous hydrogenation system at 430 ° C and a pressure of 280 bar with 1500 Nm 3 t hydrogen.
  • PCB polychlorobiphenyl
  • 1% by weight of Fe-containing (Fe 2 O 3 ) dust from iron ore processing and 0.2% by weight of Na 2 S are added to the oil.
  • the PCBs are broken down below the analytical detection limit of 1 ppm, while the waste oil undergoes a shift in the boiling point according to the following tables.
  • Waste oil Raffinate IBP start of boiling
  • ° C 256 98 ⁇ 100 ° C% by weight - - 100 - 300 ° C% by weight 2nd 24th 300 - 500 ° C% by weight 76 70 > 500 ° C% by weight 22 5
  • FBP end of boiling point
  • the lubricating oil fraction in the raffinate (Frakt. 300 -500 ° C) has a viscosity index of 120, it is therefore a base oil component for the production of a quality motor oil.
  • the proposed process is therefore much more economical than the thermal combustion process for waste oils containing PCBs, which is also carried out on an industrial scale, and it also avoids the problems associated with combustion of the formation of non-harmless secondary products of the combustion of chlorinated hydrocarbons or Oils containing chlorobiphenyls.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Business, Economics & Management (AREA)
  • Emergency Management (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Fire-Extinguishing Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Processing Of Solid Wastes (AREA)

Claims (10)

  1. Procédé pour le traitement par hydrogénation d'huiles minérales contaminées par des biphényles, plusieurs fois chlorés (PEBs) ainsi que par des résidus de distillation de telles huiles minérales, en vue de la dégradation des biphényles plusieurs fois chlorés (PCBs) à des valeurs jusqu'à 1 ppm et en-dessous,
    caractérisé en ce que
    l'on soumet les substances de charge précitées à une hydrogénation sous pression dans les conditions caractéristiques d'une hydrogénation en phase liquide ou d'une hydrogénation en phase gazeuse/phase liquide combinées, sous des pressions d'hydrogène de 20 à 325 bars, à des températures de 250 à 500°C et à des rapports gaz/huile de 100 à 3 000 m3 normaux/t, en utilisant dans l'hydrogénation en phase liquide de 0,5 à 5 % en poids d'une matière solide carbonée en suspension, à grande superficie.
  2. Procédé selon la revendication 1,
    caractérisé en ce que
    l'hydrogénation en phase liquide est effectuée avec de l'huile résiduelle, de l'huile lourde ou du charbon finement broyé.
  3. Procédé selon la revendication 2,
    caractérisé en ce que
    l'on ajoute de 30 à 95 % en poids, de préférence de 50 à 95 % en poids, d'huile résiduelle ou d'huile lourde.
  4. Procédé selon la revendication 2,
    caractérisé en ce que
    l'on utilise du charbon et de l'huile de charge dans le rapport pondéral de 1:20 à 1:1, de préférence de 1:5 à 4:5.
  5. Procédé selon la revendication 1,
    caractérisé en ce que
    on utilise du coke de lignite provenant de fours verticaux et de fours à sole, des noirs de carbone provenant de la gazéification d'huile lourde, de houilles, de résidus d'hydrogénation, de lignite et les cokes actifs produits à partir de celle-ci, du coke de pétrole, des poussières provenant de la gazéification Winkler du charbon.
  6. Procédé selon la revendication 5,
    caractérisé en ce que
    les additifs carbonés utilisés sont imprégnés avec un sel métallique d'éléments des sous-groupes 1 à 8, ainsi que du groupe principal (4) du système périodique des éléments, de préférence le fer, le cobalt, le nickel, le vanadium, le molybdène.
  7. Procédé selon la revendication 1,
    caractérisé en ce que
    l'on utilise de 0,5 à 5 % en poids de matières rouges, oxydes de fer, poussières d'électrofiltres et poussières de cyclone provenant du traitement de métaux/minerais.
  8. Procédé selon la revendication 1,
    caractérisé en ce que
    l'on ajoute aux produits de charge de 0,01 à 5 % en poids d'un composé qui forme des sels par neutralisation avec un halogène hydrogène ou libère des ions hydroxyde en solution aqueuse.
  9. Procédé selon la revendication 8,
    caractérisé en ce que
    l'on ajoute de 0,01 à 5 % en poids d'un hydroxyde alcalin, carbonate alcalin, acétate alcalin, alcoolate alcalin, sulfure alcalin, de composés d'ammonium correspondants, dans la mesure où ils existent tels quels ou en solution aqueuse, ou de mélanges des composés précités.
  10. Procédé selon la revendication 8 ou 9,
    caractérisé en ce que
    l'on injecte dans l'effluent du réacteur à phase liquide le composé à ajouter, conjointement avec de l'eau.
EP87109958A 1986-07-11 1987-07-10 Procédé de traitement par hydrogénation des huiles minérales contaminées avec les chlorobiphényles Expired - Lifetime EP0257260B2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87109958T ATE68099T1 (de) 1986-07-11 1987-07-10 Verfahren zur hydrierenden behandlung von mit chlorbiphenylen u. dgl. kontaminierten mineraloelen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3623430 1986-07-11
DE19863623430 DE3623430A1 (de) 1986-07-11 1986-07-11 Verfahren zur hydrierenden behandlung von mit chlorbiphenylen u. dgl. kontaminierten mineraloelen

Publications (3)

Publication Number Publication Date
EP0257260A1 EP0257260A1 (fr) 1988-03-02
EP0257260B1 EP0257260B1 (fr) 1991-10-09
EP0257260B2 true EP0257260B2 (fr) 1996-08-07

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EP87109958A Expired - Lifetime EP0257260B2 (fr) 1986-07-11 1987-07-10 Procédé de traitement par hydrogénation des huiles minérales contaminées avec les chlorobiphényles

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Country Link
US (1) US4810365A (fr)
EP (1) EP0257260B2 (fr)
JP (1) JP2544391B2 (fr)
AT (1) ATE68099T1 (fr)
CA (1) CA1297063C (fr)
DE (2) DE3623430A1 (fr)
ES (1) ES2025597T5 (fr)
GR (2) GR3002876T3 (fr)

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Also Published As

Publication number Publication date
US4810365A (en) 1989-03-07
JPS6323989A (ja) 1988-02-01
GR3002876T3 (en) 1993-01-25
DE3623430A1 (de) 1988-01-28
CA1297063C (fr) 1992-03-10
EP0257260B1 (fr) 1991-10-09
ES2025597T5 (es) 1996-11-01
JP2544391B2 (ja) 1996-10-16
EP0257260A1 (fr) 1988-03-02
DE3773586D1 (de) 1991-11-14
GR3021219T3 (en) 1997-01-31
DE3623430C2 (fr) 1989-02-23
ATE68099T1 (de) 1991-10-15
ES2025597T3 (es) 1992-04-01

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