EP0068231B1 - Verfahren zur Hydrierung von Kohle, Schweröl, Bitumen und dergl. - Google Patents
Verfahren zur Hydrierung von Kohle, Schweröl, Bitumen und dergl. Download PDFInfo
- Publication number
- EP0068231B1 EP0068231B1 EP82105119A EP82105119A EP0068231B1 EP 0068231 B1 EP0068231 B1 EP 0068231B1 EP 82105119 A EP82105119 A EP 82105119A EP 82105119 A EP82105119 A EP 82105119A EP 0068231 B1 EP0068231 B1 EP 0068231B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- bar
- process according
- hydrogenation
- pressure
- hot
- 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
Links
- 238000000034 method Methods 0.000 title claims description 22
- 238000005984 hydrogenation reaction Methods 0.000 title claims description 15
- 239000003245 coal Substances 0.000 title claims description 8
- 239000000295 fuel oil Substances 0.000 title claims description 6
- 239000010426 asphalt Substances 0.000 title claims description 5
- 239000007789 gas Substances 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 16
- 239000010802 sludge Substances 0.000 claims description 13
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical class CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 4
- 235000013844 butane Nutrition 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical class CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 description 8
- 239000012263 liquid product Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 239000000571 coke Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000005292 vacuum distillation Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- 238000005360 mashing Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004449 solid propellant Substances 0.000 description 2
- NGCDGPPKVSZGRR-UHFFFAOYSA-J 1,4,6,9-tetraoxa-5-stannaspiro[4.4]nonane-2,3,7,8-tetrone Chemical compound [Sn+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O NGCDGPPKVSZGRR-UHFFFAOYSA-J 0.000 description 1
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- HOWJQLVNDUGZBI-UHFFFAOYSA-N butane;propane Chemical compound CCC.CCCC HOWJQLVNDUGZBI-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006392 deoxygenation reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/06—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by destructive hydrogenation
- C10G1/065—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by destructive hydrogenation in the presence of a solvent
Definitions
- the invention relates to the separation of liquid products from the hot separator residues of the bottom or combined bottom and gas phase hydrogenation of coal, heavy oil, bitumen and similar starting products, such as residues from top or vacuum distillation of crude oil.
- coal, heavy oils, bitumen and other residues can be converted into low-boiling hydrocarbon mixtures by hydrogenation and catalyst, optionally also mixed with a mashing oil originating from the product and this mixture heated at a pressure of 50-700 bar, preferably 100-325 bar in a heater to 200-500 ° C, preferably 350-450 ° C.
- the mixture After passing through a preheater, the mixture is passed from below through a reactor system in which hydrocracking reactions take place at temperatures between 250 and 550 ° C, preferably 380-480 ° C, which lead to the cleavage of large molecules and their partial desulfurization, denitrification and deoxygenation .
- Disposable catalysts are preferably used as catalysts.
- these are, for example, molybdic acid, tin oxalate / ammonium chloride, Bayer mass and lux mass.
- catalysts are used which contain catalytically active metal compounds, for example tungsten, molybdenum, lead, tin, chromium, cobalt and nickel, in particular iron, on a carrier such as active carbon or in particular coke.
- the catalysts are used in amounts of up to 10% by weight, in particular 1 to 6% by weight, based on the starting product.
- the reaction mixture passes into a hot separator, from the top of which gaseous and vaporous reaction products, which contain the major part of the liquid product yield, from the base of which unreacted feed, asphaltenes, catalyst and a certain amount of heavy and medium oil are drawn off as hot sludge.
- the hot separator which can also consist of a system of several separators connected in series, is operated at temperatures which are up to 100 ° C., preferably 20 to 40 ° C., below the reactor temperature.
- FR-A-23 74401 describes, in a process for converting a solid fuel into a liquid fuel, in which a mixture of solid fuel particles and solvent is produced, heating the mixture at elevated pressure and elevated temperature and the liquid part of the effluent from the heating zone to enter in a stripping zone.
- a gas containing hydrogen gas is used as a stripping agent in countercurrent contact with the entire liquid reaction product.
- the gaseous or vaporous products drawn off at the top of the hot separator are either regulated in a cold relaxation system and fed to further processing, or are passed under reaction pressure from a short distance from above into a system of reactors in which the gaseous or vaporous products are carried by fixed bed catalysts desulphurized, denitrified, deoxygenated and split (cf. W. Urban “Petroleum processing in the Scholvener 300 at combi hydrogenation chamber" in Petroleum and Coal, 8 (1955), pp. 780 - 782).
- the products of this "combi-hydrogenation" are regulated by a cold separator system and sent for further processing.
- the liquid product yield of the bottom or combined bottom and gas phase hydrogenation is increased in that part of the liquid constituents are separated from the base product of the hot separator with the aid of process gases and stripped.
- the process gas is passed through the product at temperatures between 20 and 300 ° C., preferably 50 to 200 ° C. and a pressure between 10 and 300 bar, preferably 50 to 200 bar.
- Any gas obtained in the process preferably a fraction enriched by washing from the process gas and containing methane, ethane, propane, butanes and pentanes, in particular high contents of propane, butene and / or pentane, can be used as stripping gas.
- the treatment of the hot sludge with the process gases expediently takes place continuously in that a pressure vessel coupled to the hot separator system is charged from above with the hot sludge and from below with the process gases.
- the weight ratio hot blowdown: process gas is 1:10, preferably 1: 3, the throughput 0.2 to 2.0 m 3 , preferably 0.3 to 0.6 m 3 blowdown per m 3 pressure vessel volume and per hour.
- the stripping gas can be from the entrained components of the hydrogenation residue by reducing the pressure to 100 to 1 bar, preferably 70 to 30 bar or increasing the temperature by 20 to 150 ° C, preferably 50 to 100 0 C or a combination of both measures, for example increasing the temperature by 20 up to 70 ° C with a pressure reduction to 100 to 50 bar.
- the liquid products are refined or split in the gas phase reactor; in the case of coal hydrogenation, they serve as asphaltene-free mashing oil components.
- the stripping gas can be used again for separation after pressure increase by means of a compressor or a fan or after cooling.
- the solid-containing residue, enriched in metals and asphaltenes, from the treatment of hot sludge with the process gases is removed from the process by the gas pressure via a lock system and can be fed to gasification, in order to cover the hydrogen requirement of the hydrogenation process.
- This hot sludge was placed in a downstream 5 l container with fittings for gas and liquid distribution at 200 bar and 150 ° C with 4.8 kg / h of a propane-butane mixture (propane: butane weight ratio 3: 2). treated.
- the gaseous product was let down to 40 bar, 0.9 kg / h of a liquid product with a boiling end of 520 ° C. separating.
- the product was free of asphaltenes and metals, its H / C ratio was 1.3; the sulfur content was 1.5% by weight.
- the solids in the residue were enriched to 28% by weight; the residue contained all metals which had been introduced into the process with the oil and the single-use catalyst.
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)
- Compositions Of Macromolecular Compounds (AREA)
- Working-Up Tar And Pitch (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19813123535 DE3123535A1 (de) | 1981-06-13 | 1981-06-13 | Verfahren zur hydrierung von kohle, schweroel, bitumen und dergl. |
DE3123535 | 1981-06-13 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0068231A2 EP0068231A2 (de) | 1983-01-05 |
EP0068231A3 EP0068231A3 (en) | 1984-09-12 |
EP0068231B1 true EP0068231B1 (de) | 1987-04-08 |
Family
ID=6134663
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP82105119A Expired EP0068231B1 (de) | 1981-06-13 | 1982-06-11 | Verfahren zur Hydrierung von Kohle, Schweröl, Bitumen und dergl. |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP0068231B1 (no) |
CA (1) | CA1171013A (no) |
DE (2) | DE3123535A1 (no) |
NO (1) | NO162864C (no) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3914057A1 (de) * | 1989-04-28 | 1990-10-31 | Ruhrkohle Ag | Strippung von rueckstaenden |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB892113A (en) * | 1957-05-08 | 1962-03-21 | Apv Co Ltd | Separation of low boiling point impurities from hydrocarbons |
GB1527570A (en) * | 1976-12-15 | 1978-10-04 | Texaco Development Corp | Coal liquefaction |
-
1981
- 1981-06-13 DE DE19813123535 patent/DE3123535A1/de not_active Withdrawn
-
1982
- 1982-06-03 NO NO821844A patent/NO162864C/no unknown
- 1982-06-11 DE DE8282105119T patent/DE3276003D1/de not_active Expired
- 1982-06-11 CA CA000405046A patent/CA1171013A/en not_active Expired
- 1982-06-11 EP EP82105119A patent/EP0068231B1/de not_active Expired
Also Published As
Publication number | Publication date |
---|---|
NO162864B (no) | 1989-11-20 |
DE3123535A1 (de) | 1982-12-30 |
CA1171013A (en) | 1984-07-17 |
DE3276003D1 (en) | 1987-05-14 |
EP0068231A3 (en) | 1984-09-12 |
EP0068231A2 (de) | 1983-01-05 |
NO821844L (no) | 1982-12-14 |
NO162864C (no) | 1990-02-28 |
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