EP0301172A2 - Procédé d'hydrogénation de charges contenant du carbone - Google Patents

Procédé d'hydrogénation de charges contenant du carbone Download PDF

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Publication number
EP0301172A2
EP0301172A2 EP88105773A EP88105773A EP0301172A2 EP 0301172 A2 EP0301172 A2 EP 0301172A2 EP 88105773 A EP88105773 A EP 88105773A EP 88105773 A EP88105773 A EP 88105773A EP 0301172 A2 EP0301172 A2 EP 0301172A2
Authority
EP
European Patent Office
Prior art keywords
cold
slop
fed
hydrogenation
phase reactor
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.)
Granted
Application number
EP88105773A
Other languages
German (de)
English (en)
Other versions
EP0301172B1 (fr
EP0301172A3 (en
Inventor
Eckard Dr. Wolowski
Frank Dr. Mirtsch
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.)
RAG AG
Original Assignee
Ruhrkohle AG
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 Ruhrkohle AG filed Critical Ruhrkohle AG
Publication of EP0301172A2 publication Critical patent/EP0301172A2/fr
Publication of EP0301172A3 publication Critical patent/EP0301172A3/de
Application granted granted Critical
Publication of EP0301172B1 publication Critical patent/EP0301172B1/fr
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Expired - Lifetime legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G1/00Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/004Inhibiting of corrosion

Definitions

  • the invention relates to the introduction of alkali donors, especially as a sodium compound, and cold slop in the common high pressure circuit of a bottom phase hydrogenation with integrated gas phase hydrogenation.
  • the feedstocks are also supplied with an alkali dispenser, especially as a sodium compound, so that the chlorine is chemically bound from the feedstocks and discharged from the process together with the hydrogenation residue. Otherwise chlorine corrosion and salt formation (e.g. ammonium chloride) can occur in the condensation path of the oil products.
  • an alkali dispenser especially as a sodium compound
  • the sodium is added to the liquid carbonaceous feedstocks as Na2S in solid form.
  • the Na2S dissolves well in aromatic oils - especially raw coal oils from the bottom phase hydrogenation.
  • the solubility for Na2S is very low.
  • the Na2S melts above 110 ° C and gradually releases its hydration water when heated further in the heating path. In cooler zones this can lead to recrystallization of the Na2S and thus blockages in pipes, fittings and containers.
  • soda Na2CO3
  • soda Na2CO3
  • Soda has the disadvantage compared to Na2S that soda has a specifically lower sodium content and the alkalinity compared to Na2S is reduced.
  • Na2S in solid or molten form has poor solubility in refined solvent. There are blockages in the area of mashing. If Na2S is fed into the heating path or into the bottom phase reactor in aqueous solution, these difficulties do not occur.
  • cold slop When operating the bottom phase hydrogenation with integrated gas phase hydrogenation, cold slop also falls - a mixture of partially unrefined product oils and phenolic water - on. This cold slop will not be worked up, as is customary in the bottom phase hydrogenation, in atmospheric distillation, in which the refined oil products and, if appropriate, the refined solvent are separated into boiling fractions.
  • Kaltslop contains unrefined oils and phenolic process water, which are not brought into contact with the refined oils in atmospheric distillation. According to the invention, the cold slop is run over the gas phase hydrogenation and refined.
  • the invention has for its object to feed the alkali dispenser - especially Na2S - while avoiding precipitation and clogging in the high pressure circuit and continue to perform cold slop processing without using an additional atmospheric distillation.
  • the object of the alkali dispenser supply is achieved according to the invention in that the alkali dispenser - especially Na2S - is fed as an aqueous solution into the heating path or upstream of the sump phase reactor or into the sump phase reactor where heating and evaporation of the aqueous Na2S solution takes place.
  • the Na2S is then in finely divided form in the reaction mixture.
  • the cold slop workup in the bottom phase hydrogenation with integrated gas phase hydrogenation is achieved according to the invention in that the cold slot is fed into the heating path or upstream of the bottom phase reactor or into the bottom phase reactor.
  • the cold slop is expediently added to the hot separator head product. In this way, the addition of cold slops also supports the temperature setting in the gas phase reactor.
  • FIG 1 shows an example of use from coal hydrogenation with an integrated refining stage.
  • the mash (1) consisting of ground coal, catalyst and oil, is mixed with a partial stream of the hydrogenation gas (2) in the mash heat exchangers (24), (25) by indirect heat exchange with the hot separator head product stream (9) and the gas phase product stream (10), warmed up.
  • Most of the hydrogenation gas consisting of cycle gas (15) and fresh hydrogen (17), is heated up as stream (5) in the gas heat exchangers (26), (28), (29) and the heating furnace (30) and together with the preheated one Mash fed to the bottom phase reactor (31).
  • the aqueous Na2S solution is passed alone or together with the cold slop as a stream (18) by means of a high pressure pump (37) in the bottom phase reactor.
  • the heating or evaporation of aqueous Na2S solution and cold slop in the bottom phase reactor (31) also serves to partially dissipate the heat of reaction and thus reduces the amount of quench gas (16) required to adjust the temperature in the bottom phase reactor.
  • the aqueous Na2S solution can also be fed with the cold slop as a stream (19) upstream of the bottom phase reactor (31) or as a stream (20) between the mash heat exchangers (24) and (25). If the amount of cold slop differs in time, the furnace (30) is used to set a constant temperature for the reactor insert (7).
  • the cold slop - alone or together with vacuum gas oil - is fed into the hot separator head product stream (9) by means of a high-pressure pump (38).
  • a high-pressure pump (38) Different feed rates as material flow (21) before or as material flow (22) after the mash heat exchanger (25) make it possible to compensate for different heat transfer rates of the heat exchanger (25). This facilitates a constant temperature setting in the gas phase reactor (33).
  • the chlorine is largely bound in the sludge (8). This prevents salt formation in the material flow (10) and in the gas heat exchanger (28). Water injection to avoid salt formation or to dissolve salts is not necessary in normal operation.
  • the injection of demineralized water (23) behind the intermediate separator (34) into the material flow (12) can be useful as a preventative measure if the dosage of the Na2S solution is not adjusted to fluctuations in the chlorine content due to time-dependent wake.
  • VE water injection also supports the leaching out of ammonia in the cycle gas, which has a desirable effect on the salt formation balance in the suppressive direction. Density differences then separate cold oil (13) and water (14) in the cold separator (35) in a manner known per se.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
EP88105773A 1987-07-31 1988-04-12 Procédé d'hydrogénation de charges contenant du carbone Expired - Lifetime EP0301172B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3725367 1987-07-31
DE3725367A DE3725367C1 (de) 1987-07-31 1987-07-31 Verfahren zur Hydrierung kohlenstoffhaltiger Einsatzstoffe

Publications (3)

Publication Number Publication Date
EP0301172A2 true EP0301172A2 (fr) 1989-02-01
EP0301172A3 EP0301172A3 (en) 1989-07-26
EP0301172B1 EP0301172B1 (fr) 1990-12-19

Family

ID=6332766

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88105773A Expired - Lifetime EP0301172B1 (fr) 1987-07-31 1988-04-12 Procédé d'hydrogénation de charges contenant du carbone

Country Status (6)

Country Link
EP (1) EP0301172B1 (fr)
JP (1) JPS6436686A (fr)
AU (1) AU609153B2 (fr)
BR (1) BR8803775A (fr)
DE (2) DE3725367C1 (fr)
PL (1) PL151645B1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007059783A1 (fr) * 2005-11-24 2007-05-31 Scf Technologies A/S Procede et dispositif pour la conversion d’un materiau organique par excitation micro-onde
US7678163B2 (en) 2005-04-29 2010-03-16 Scf Technologies A/S Method and apparatus for converting organic material
US8299315B2 (en) 2005-04-29 2012-10-30 Altaca Insaat Ve Dis Ticaret A.S. Method and apparatus for converting organic material
CN104388118A (zh) * 2014-11-24 2015-03-04 湖南省馨盛能源开发有限责任公司 煤焦油制柴油的工艺流程

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE692631C (de) * 1934-09-26 1940-06-24 I G Farbenindustrie Akt Ges Verfahren zur Verhinderung der Korrosion bei der Waermebehandlung von Kohle, Teeren, Mineraloelen u. dgl.
DE3038309A1 (de) * 1980-10-10 1982-05-19 Ruhrkohle Ag, 4300 Essen Kohleverfluessigung

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE692631C (de) * 1934-09-26 1940-06-24 I G Farbenindustrie Akt Ges Verfahren zur Verhinderung der Korrosion bei der Waermebehandlung von Kohle, Teeren, Mineraloelen u. dgl.
DE3038309A1 (de) * 1980-10-10 1982-05-19 Ruhrkohle Ag, 4300 Essen Kohleverfluessigung

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7678163B2 (en) 2005-04-29 2010-03-16 Scf Technologies A/S Method and apparatus for converting organic material
US8299315B2 (en) 2005-04-29 2012-10-30 Altaca Insaat Ve Dis Ticaret A.S. Method and apparatus for converting organic material
US8771601B2 (en) 2005-04-29 2014-07-08 Altaca Insaat Ve Dis Ticaret A.S. Method and apparatus for converting organic material
WO2007059783A1 (fr) * 2005-11-24 2007-05-31 Scf Technologies A/S Procede et dispositif pour la conversion d’un materiau organique par excitation micro-onde
CN104388118A (zh) * 2014-11-24 2015-03-04 湖南省馨盛能源开发有限责任公司 煤焦油制柴油的工艺流程
CN104388118B (zh) * 2014-11-24 2017-01-04 湖南省馨盛能源开发有限责任公司 煤焦油制柴油的工艺流程

Also Published As

Publication number Publication date
PL273853A1 (en) 1989-04-03
PL151645B1 (en) 1990-09-28
BR8803775A (pt) 1989-02-21
AU1909688A (en) 1989-02-02
AU609153B2 (en) 1991-04-26
JPS6436686A (en) 1989-02-07
DE3861308D1 (de) 1991-01-31
DE3725367C1 (de) 1988-09-22
EP0301172B1 (fr) 1990-12-19
EP0301172A3 (en) 1989-07-26

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