EP0265598B1 - Verfahren zur Entsalzung von Steinkohlenteeren und -pechen - Google Patents
Verfahren zur Entsalzung von Steinkohlenteeren und -pechen Download PDFInfo
- Publication number
- EP0265598B1 EP0265598B1 EP87110278A EP87110278A EP0265598B1 EP 0265598 B1 EP0265598 B1 EP 0265598B1 EP 87110278 A EP87110278 A EP 87110278A EP 87110278 A EP87110278 A EP 87110278A EP 0265598 B1 EP0265598 B1 EP 0265598B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- water
- pitches
- coal
- tar
- pitch
- 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
Links
- 238000000034 method Methods 0.000 title claims description 14
- 238000011033 desalting Methods 0.000 title claims 2
- 239000011294 coal tar pitch Substances 0.000 title description 3
- 239000011300 coal pitch Substances 0.000 title 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 22
- 239000011269 tar Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000011295 pitch Substances 0.000 claims description 16
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 12
- 239000001569 carbon dioxide Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- 239000003245 coal Substances 0.000 claims description 6
- 239000011299 tars and pitches Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 235000019270 ammonium chloride Nutrition 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 239000000571 coke Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000005083 Zinc sulfide Substances 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- WHRZCXAVMTUTDD-UHFFFAOYSA-N 1h-furo[2,3-d]pyrimidin-2-one Chemical compound N1C(=O)N=C2OC=CC2=C1 WHRZCXAVMTUTDD-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 235000006173 Larrea tridentata Nutrition 0.000 description 1
- 244000073231 Larrea tridentata Species 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229960002126 creosote Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011339 hard pitch Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000006253 pitch coke Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
Definitions
- the invention relates to a process for separating salts, in particular sodium and ammonium chloride and zinc sulfide, from coal tars and pitches.
- the ammonium chloride present in the raw tar causes severe corrosion damage in the distillation columns during the tar processing. Since the salt is water-soluble, the water contained in the raw tar is mechanically separated. However, up to 2% water remains in the tar (Franck / Collin: Coal tar, p. 27).
- An additional water wash can further reduce the ammonium chloride content.
- the water wash can also be carried out at elevated temperature under elevated pressure and in several stages (GB-A 849 987). However, this measure is too complex if the chloride content is to be reduced to such an extent that chloride corrosion no longer takes place. Therefore, the chloride is usually bound to a stronger base to prevent the ammonium chloride from going into the gas phase. This is generally done by metering in an amount of an aqueous NaOH or Na z COs solution adapted to the chloride content of the tar.
- the salts formed like all other ash formers, remain in the respective distillation residue during tar processing, that is to say in normal pitch, hard pitch or pitch coke.
- Metallic impurities are extremely undesirable, especially when using pitch as a binder or coke as a carbon material in the manufacture of anodes for aluminum electrolysis. Not only do they form additional slags, they also increase the burn-off of the anodes. This applies in particular to sodium, which acts as an oxidation catalyst (Light Metals, AIME 1981, 471-476).
- the object was therefore to develop a process with which salts can be selectively removed from coal tars and pitches.
- the object is achieved in that the coal tars or pitches with water and a gas containing carbon dioxide, optionally with the addition of a solvent or / and entrainer, in a pressure vessel at a temperature and a pressure near the critical point of the gas used washed and decanted, the liquid or dissolved tars or pitches and the water being drawn off separately and then being released.
- the object of the present invention is not achieved by the known method, since the tar is not selectively ashed. It is also not recommended to use supercritical carbon dioxide for water washing.
- the zinc present as insoluble zinc sulfide in the tar dissolves to a considerable extent in the aqueous phase, precipitates out after the pressure has been let down, and can be filtered off. It is thus possible to circulate the washing water freed from the zinc salt and to enrich the sodium or ammonium chloride content to the extent that this makes sense for technical reasons. Thereafter, the wash water must be at least partially processed or renewed.
- the system of pitch or tar, water and CO 2 -containing gas is preferably present in the supercritical state. If additional dragging or solvents are used, they can be separated from the pitch and reused by gradually releasing the pressure.
- All known pitch solvents come into question as solvents, that is to say pure aromatics, such as, for. B. toluene, or aromatic oils, such as. B. washing oil, or tar bases such as pyridine and quinoline, which can also be used as an entrainer.
- gases containing carbon dioxide are also mixtures, especially hydrocarbons containing 1 to 6 carbon atoms, such as propane, butane or liquid gas.
- the phases are separated and drained.
- the chlorine or chlorides are almost completely removed by a single-stage wash.
- the content of zinc and other ash formers can be reduced even further by washing in several stages with more thorough mixing. It is advantageous that. To run wash water in countercurrent and to filter off the insoluble salts that occur during relaxation.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
- Epoxy Compounds (AREA)
- Epoxy Resins (AREA)
- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19863636560 DE3636560A1 (de) | 1986-10-28 | 1986-10-28 | Verfahren zur entsalzung von steinkohlenteeren und -pechen |
DE3636560 | 1986-10-28 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0265598A1 EP0265598A1 (de) | 1988-05-04 |
EP0265598B1 true EP0265598B1 (de) | 1990-09-19 |
Family
ID=6312587
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP87110278A Expired - Lifetime EP0265598B1 (de) | 1986-10-28 | 1987-07-16 | Verfahren zur Entsalzung von Steinkohlenteeren und -pechen |
Country Status (13)
Country | Link |
---|---|
US (2) | US4831101A (es) |
EP (1) | EP0265598B1 (es) |
JP (1) | JPS63122786A (es) |
AU (1) | AU593399B2 (es) |
CA (1) | CA1285897C (es) |
CS (1) | CS264297B2 (es) |
DE (2) | DE3636560A1 (es) |
DK (1) | DK561287A (es) |
ES (1) | ES2002257B3 (es) |
IN (1) | IN170362B (es) |
PL (1) | PL151418B1 (es) |
SU (1) | SU1512486A3 (es) |
ZA (1) | ZA876675B (es) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5274160A (en) * | 1991-08-22 | 1993-12-28 | Syracuse University | Method and apparatus for synthesis of highly isomerically pure stereoisomers of glycidol derivatives |
US5194637A (en) * | 1991-08-22 | 1993-03-16 | Syracuse University | Method and apparatus for synthesis of highly isomerically pure stereoisomers of glycidol derivatives |
US5576362A (en) * | 1992-04-20 | 1996-11-19 | Denki Kagaku Kogyo Kabushiki Kaisha | Insulating material and a circuit substrate in use thereof |
US5578740A (en) * | 1994-12-23 | 1996-11-26 | The Dow Chemical Company | Process for preparation of epoxy compounds essentially free of organic halides |
TW593401B (en) * | 1998-05-29 | 2004-06-21 | Sumitomo Chemical Co | Highly purified epoxy resin having glycidylamino group and the process thereof |
JP5245274B2 (ja) * | 2007-04-02 | 2013-07-24 | 三菱化学株式会社 | タール又はタールエマルジョンからの水除去方法、タールエマルジョンのタール化方法、及びタール中の含水率低減方法 |
CN104910944B (zh) * | 2015-06-10 | 2018-03-20 | 山东宝塔新能源有限公司 | 煤焦油脱盐工艺 |
CN106701157B (zh) * | 2015-11-12 | 2018-04-10 | 中国石油化工股份有限公司 | 一种高温煤焦油脱金属方法 |
Family Cites Families (27)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US32120A (en) * | 1861-04-23 | Floor-clamp | ||
US2572583A (en) * | 1948-12-21 | 1951-10-23 | Phillips Petroleum Co | Improved liquid-liquid contacting process using di(beta-cyanoethyl)-amine |
FR1038775A (fr) * | 1950-06-20 | 1953-10-01 | Collin F J Ag | Perfectionnements apportés aux procédés et dispositifs d'épuration du goudron etdes produits goudronneux |
GB849987A (en) * | 1957-12-02 | 1960-09-28 | Allied Chem | Process for treating coke oven tar |
US3202605A (en) * | 1962-06-06 | 1965-08-24 | Badger Co | Propane deaspihalting process |
GB1482690A (en) * | 1974-12-19 | 1977-08-10 | Coal Ind | Hydrogenation of coal |
US4101416A (en) * | 1976-06-25 | 1978-07-18 | Occidental Petroleum Corporation | Process for hydrogenation of hydrocarbon tars |
JPS6041111B2 (ja) * | 1976-11-26 | 1985-09-13 | 新日鐵化学株式会社 | コ−クス製造原料の調整方法 |
US4208267A (en) * | 1977-07-08 | 1980-06-17 | Exxon Research & Engineering Co. | Forming optically anisotropic pitches |
DE2810332C2 (de) * | 1978-03-10 | 1982-08-05 | Rütgerswerke AG, 6000 Frankfurt | Verfahren zur Abtrennung von chinolinunlöslichen Bestandteilen aus Steinkohlenteerpech |
US4219404A (en) * | 1979-06-14 | 1980-08-26 | Exxon Research & Engineering Co. | Vacuum or steam stripping aromatic oils from petroleum pitch |
DE3017876A1 (de) * | 1980-05-09 | 1982-05-19 | Peter, Siegfried, Prof.Dr., 8520 Erlangen | Verfahren zur abtrennung von feststoffen aus oelen |
US4402824A (en) * | 1981-03-25 | 1983-09-06 | Sumitomo Metal Industries, Limited | Process for refining coal-based heavy oils |
USRE32120E (en) | 1981-04-01 | 1986-04-22 | Phillips Petroleum Company | Hydrotreating supercritical solvent extracts in the presence of alkane extractants |
DE3135368A1 (de) * | 1981-09-07 | 1983-03-31 | Siemens AG, 1000 Berlin und 8000 München | Verfahren und anordnung zur funktionspruefung einer programmierbare logikanordnung |
US4482453A (en) * | 1982-08-17 | 1984-11-13 | Phillips Petroleum Company | Supercritical extraction process |
JPS5941387A (ja) * | 1982-08-30 | 1984-03-07 | Osaka Gas Co Ltd | ピッチの製造方法 |
US4503026A (en) * | 1983-03-14 | 1985-03-05 | E. I. Du Pont De Nemours And Company | Spinnable precursors from petroleum pitch, fibers spun therefrom and method of preparation thereof |
US4502943A (en) * | 1983-03-28 | 1985-03-05 | E. I. Du Pont De Nemours And Company | Post-treatment of spinnable precursors from petroleum pitch |
US4447598A (en) * | 1983-04-07 | 1984-05-08 | The Dow Chemical Company | Method of preparing epoxy resins having low hydrolyzable chloride contents |
DE3335316A1 (de) * | 1983-09-29 | 1985-04-11 | Rütgerswerke AG, 6000 Frankfurt | Verfahren zur abtrennung harzartiger stoffe aus kohlestaemmigen schweroelen und verwendung der gewonnenen fraktion |
US4485221A (en) * | 1983-11-03 | 1984-11-27 | Ciba-Geigy Corporation | Process for making epoxy novolac resins with low hydrolyzable chlorine and low ionic chloride content |
US4604184A (en) * | 1983-11-16 | 1986-08-05 | Domtar Inc. | Modified coal-tar pitch |
JPS60200816A (ja) * | 1984-03-26 | 1985-10-11 | Kawasaki Steel Corp | 炭素材料の製造方法 |
US4575412A (en) * | 1984-08-28 | 1986-03-11 | Kawasaki Steel Corporation | Method for producing a precursor pitch for carbon fiber |
US4578177A (en) * | 1984-08-28 | 1986-03-25 | Kawasaki Steel Corporation | Method for producing a precursor pitch for carbon fiber |
DE3539432A1 (de) * | 1984-11-09 | 1986-06-05 | Instytut Chemii Przemysłowej, Warschau/Warszawa | Verfahren zur trennung von kohlenteeren |
-
1986
- 1986-10-28 DE DE19863636560 patent/DE3636560A1/de not_active Withdrawn
-
1987
- 1987-07-16 ES ES87110278T patent/ES2002257B3/es not_active Expired - Lifetime
- 1987-07-16 DE DE8787110278T patent/DE3765079D1/de not_active Expired - Fee Related
- 1987-07-16 EP EP87110278A patent/EP0265598B1/de not_active Expired - Lifetime
- 1987-08-26 CA CA000545431A patent/CA1285897C/en not_active Expired - Fee Related
- 1987-09-02 IN IN634/MAS/87A patent/IN170362B/en unknown
- 1987-09-03 CS CS876424A patent/CS264297B2/cs unknown
- 1987-09-07 ZA ZA876675A patent/ZA876675B/xx unknown
- 1987-09-23 SU SU874203340A patent/SU1512486A3/ru active
- 1987-09-24 US US07/100,471 patent/US4831101A/en not_active Expired - Lifetime
- 1987-10-26 JP JP62268387A patent/JPS63122786A/ja active Pending
- 1987-10-27 PL PL1987268457A patent/PL151418B1/pl unknown
- 1987-10-27 AU AU80174/87A patent/AU593399B2/en not_active Ceased
- 1987-10-27 DK DK561287A patent/DK561287A/da not_active Application Discontinuation
-
1989
- 1989-03-30 US US07/331,592 patent/US4871443A/en not_active Expired - Fee Related
Non-Patent Citations (1)
Title |
---|
Erdöl und Kohle, Erdgas; Bd. 34, Heft 7, Juli 1981, Seiten 296-300 * |
Also Published As
Publication number | Publication date |
---|---|
PL268457A1 (en) | 1988-11-24 |
SU1512486A3 (ru) | 1989-09-30 |
US4871443A (en) | 1989-10-03 |
DE3636560A1 (de) | 1988-05-05 |
DE3765079D1 (de) | 1990-10-25 |
PL151418B1 (en) | 1990-08-31 |
AU8017487A (en) | 1988-05-05 |
ZA876675B (en) | 1988-03-16 |
DK561287A (da) | 1988-04-29 |
CS264297B2 (en) | 1989-06-13 |
CS642487A2 (en) | 1988-09-16 |
CA1285897C (en) | 1991-07-09 |
EP0265598A1 (de) | 1988-05-04 |
US4831101A (en) | 1989-05-16 |
DK561287D0 (da) | 1987-10-27 |
ES2002257B3 (es) | 1991-04-01 |
IN170362B (es) | 1992-03-21 |
ES2002257A4 (es) | 1988-08-01 |
JPS63122786A (ja) | 1988-05-26 |
AU593399B2 (en) | 1990-02-08 |
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