GB2063906A - Coal liquefaction - Google Patents
Coal liquefaction Download PDFInfo
- Publication number
- GB2063906A GB2063906A GB8036343A GB8036343A GB2063906A GB 2063906 A GB2063906 A GB 2063906A GB 8036343 A GB8036343 A GB 8036343A GB 8036343 A GB8036343 A GB 8036343A GB 2063906 A GB2063906 A GB 2063906A
- Authority
- GB
- United Kingdom
- Prior art keywords
- coal
- extract
- atmospheres
- solvent
- proton
- 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.)
- Withdrawn
Links
- 239000003245 coal Substances 0.000 title claims abstract description 34
- 239000000284 extract Substances 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 7
- 239000011707 mineral Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 229910001872 inorganic gas Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 15
- 150000002894 organic compounds Chemical class 0.000 claims description 4
- 239000011343 solid material Substances 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 15
- 239000007792 gaseous phase Substances 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 abstract description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 150000001454 anthracenes Chemical class 0.000 abstract description 4
- 239000000571 coke Substances 0.000 abstract description 3
- 238000000638 solvent extraction Methods 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 1
- 239000002574 poison Substances 0.000 abstract 1
- 231100000614 poison Toxicity 0.000 abstract 1
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 10
- 238000000605 extraction Methods 0.000 description 9
- 238000000926 separation method Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000004517 catalytic hydrocracking Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000005984 hydrogenation reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- 239000002802 bituminous coal Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction 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
- C10G1/006—Combinations of processes provided in groups C10G1/02 - C10G1/08
-
- 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
- C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
- C10G1/045—Separation of insoluble materials
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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Coal liquefaction by solvent extraction at 1 with a proton-donating solvent (e.g. hydrogenated anthracene oil) results in an extract which is contaminated with mineral solids and unreacted coal solids which can poison catalysts used in subsequent processing. These solids are removed by treating the extracts at 2 under supercritical conditions with an organic vapour (e.g. toluene, hexane or crude coke benzol) or inorganic gas (e.g. carbon dioxide) having a critical temperature of greater then 31 DEG C and a critical pressure of less than 100 atmospheres so that the extract passes into the gaseous phase. By controlled expansion and cooling first to 100 to 350 DEG C and 25 to 75 atmospheres at 5 and then to 100 to 150 DEG C and 1 to 5 atmospheres at 7, first the coal liquid 11 and then the proton- donating solvent 13 may be separately recovered. A third expansion and cooling may recover the organic vapour or inorganic gas 12. The second and third recovered material may be recycled. <IMAGE>
Description
SPECIFICATION
Separation of coal extracts
The present invention relates to a method for the removal of mineral matter and nonreacted coal from extracts obtained from coal liquefaction by extraction with proton-donor solvents.
The extract obtained in the solvent extraction of coal is a high-boiling mixture of polyaromatic hydrocarbons of high molecular weight, which is subsequently processed by hydrogenation or hydrocracking.
The known process for coal liquefaction involves extraction of coal with proton-donor solvents, e.g.
tetralin or hydrogenated anthracene oil. Separation of mineral matter and nonreacted coal from the solvent extract is a difficult technical problem.
Filtration, as described in West German Patent No.
2 520 500, Belgian Patent No.823 129 and-Polish
Patent No. 72 912 is the most frequently used method of separation. However, filtration is highly complicated and therefore new types of filters and new improved filtration methods are constantly sought.
U.S. Patent No. 3748 254, for example, discloses that the product of solvent extraction of coal is introduced to a revolving drum, where the suspension undergoes agglomeration to yield course particles, which are easily filtered.
In the Bergius-Pier's process the extract and the solvent are distilled to remove them from the mineral matter and non-reacted coal. The unavoidable application of high temperature and, in consequence, high consumption of energy, the possibil ityofcoking, decomposition and degradation of the extract and the loss of the lightest fraction of the extract are examples of the disadvantages of this process.
An object of the present invention is to obviate or mitigate the aforesaid disadvantages.
According to the present invention there is provided a method for the removal of solid material, namely unreacted coal and mineral matter, from a solvent extract of coal obtained during a coal liquefaction process using a proton-donor solvent, comprising treating the said solvent extract under supercritical conditions with an organic compound vapour or an inorganic gas having a critical temperature greater than 31"C and a critical pressure of less than 100 atmospheres, and recovering the coal extract from the vapour phase.
Preferably the vapour phase, containing the coal extract and free of solids, is sequentially condensed, first at a temperature of from 100 to 3500C and a pressure of from 25 to 75 atmospheres to yield the coal extract, then at a temperature of from 100 to 1500C and a pressure of from 1 to 5 atmospheres to yield the proton-donor solvent, and, optionally, then recovering the said organic compound or inorganic gas.
The gaseous phase may be triple-stage expanded and cooled to effect the condensation. At the first stage at a temperature of 100 to 350"C and under pressure of 25 to 75 atmospheres the heaviest compounds dissolved in "supercritical" gas, containing the product of the liquid extraction of coal, are recovered. At the second stage, at a temperature of 100 to 150"C and under pressure of 1 to 5 atmospheres, the solvent used for the liquid extraction is condensed and recycled to the process. The vapours of the "supercritical" solvent after the second stage of expansion may also be condensed in a third stage and recycled.
Since the extract separated at the first-stage of expansion is, as in the known process using no supercritical solvent, a high-boiling mixture of polyaromatic hydrocarbons of high molecular weight, it would normally be processed further e.g.
by hydrogenation or by hydrocracking. The residue from supercritical extraction is a porous semi-coke, which can be utilized either as a high-quality fuel or gasified to give a synthesis gas, which may be subsequently processed to yield a substitute of natural gas or hydrogen.
The method for separation of the liquid extraction product from mineral matter and nonreacted coal according to the invention is advantageous in that it eliminates troublesome filtration and also distillation of a high-boiling solvent. The extract obtained by this invention is substantially free of ash and particles of nonreacted coal and thus the method effectively prolongs the life of hydrogenation or hydrocracking catalysts.
The invention will now be described, by way of illustration, in the following Examples, with reference to the accompanying flow diagram.
Example 1
Coal is mixed with a hydrogenated anthracene oil and extracted in a conventional matter in a tank 1.
The mixture is piped with a pump 3 to an extractor 2, where it is treated under supercritical conditions with toluene vapour at 400 C and under 100 atmospheres. The anthracene oil and the extract together with toluene leave the extractor 2 as a gaseous phase, whereas a solid containing residue is passed as a stream 10 to a subsequent processing. The gaseous phase is cooled in a heat exchanger 4 and directed to a tank 5, where it is expanded to a pressure of 50 atmospheres and temperature 350"C.
Under these conditions the heaviest components boiling at a temperature higher than 400"C are condensed, i.e. the extract obtained from extraction of coal with anthracene oil, which is then directed in a stream 11 to a subsequent processing. The gaseous phase is then cooled in a heat-exchanger 6 and passed to a tank 7 where it is expanded to a pressure of 1 atmosphere and a temperature of 1500C. Under these conditions anthracene oil is condensed, which is recycled in a stream 13 to the tank 1. Toluene vapour is cooled in a heat-exchanger 8 and is condensed in a tank 9 at 20 C and 1 atmosphere and is recycled in a stream 12 to the extractor 2.
It was found that 88.7% by weight of the extract obtained from liquid extraction of coal was transferred to the gaseous phase. After separation at the first stage of expansion it was directed to hydrogenation or hydrocracking process.
Example 2
Bituminous coal was extracted with a liquid hyrogenated anthracene oil, and the crude extract was re-extracted with hexane under supercritical conditions, i.e. at 250"C and under pressure of 100 atmospheres in the manner described in Example 1.
The first stage of expansion was carried out at 2400C and at 50 atmospheres and the second stage at 1500Cand 1 atmosphere. It was found that 71 % by weight of the extract was transferred to the gaseous phase.
Example 3
Hard coal was extracted with a liquid hydrogenated anthracene oil and the extract was re-extracted under super-critical conditions of 130"C and 100 atmospheres with compressed gaseous carbon dioxide in the manner described in Example 1. The first stage of expansion was carried out at 1000C and 75 atmospheres and the second stage at 1000C and 1 atmosphere. It was found that 67% by weight of the extract was transferred to the supercritical gaseous phase.
Example 4
Bituminous coal was extracted with a liquid hyrogenated anthracene oil and the extract was re-extracted with a fraction obtained from the petrochemical industry, i.e. a crude coke benzol which is a mixture of aromatic hydrocarbons, mainly of benzene, toluene and zylenes. The extraction was carried out in the manner described in Example 1, under the same conditions for supercritical extraction and at corresponding expansion stages. It was found that 87.4% by weight of the extract from liquid extraction of coal was transferred to the supercritical gaseous phase.
Claims (3)
1. Amethodforthe removal of solid material, namely unreacted coal and mineral matter, from a solvent extract of coal obtained during a coal liquefaction process using a proton-donor solvent, comprising treating the said solvent extract under supercritical conditions with an organic compound vapour or an inorganic gas having a critical temperature greater than 310C and a critical pressure of less than 100 atmospheres, and recovering the coal extract from the vapour phase.
2. A method according to claim 1, in which the vapour phase, containing the coal extract and free of solids, is sequentially condensed, first at a temperature of from 100 to 350"C and a pressure of from 25 to 75 atmospheres to yield the coal extract, then at a temperature of from 100 to 1 50"C and a pressure of from 1 to 5 atmospheres to yield the proton-donor solvent, and, optionally, then recovering the said organic compound or inorganic gas.
3. A method or removing solid matter from a coal extract, according to claim 1, substantially as hereinbefore described.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PL21973479A PL122657B1 (en) | 1979-11-20 | 1979-11-20 | Method of separation of the extract from mineral substance and unreacted coal in the process of coal liquefaction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB2063906A true GB2063906A (en) | 1981-06-10 |
Family
ID=19999516
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8036343A Withdrawn GB2063906A (en) | 1979-11-20 | 1980-11-11 | Coal liquefaction |
Country Status (3)
| Country | Link |
|---|---|
| DE (1) | DE3043769A1 (en) |
| GB (1) | GB2063906A (en) |
| PL (1) | PL122657B1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2132223A (en) * | 1982-12-20 | 1984-07-04 | Exxon Research Engineering Co | The extraction of coal liquefaction bottoms |
| US4502940A (en) * | 1982-11-19 | 1985-03-05 | Coal Industry (Patents) Limited | Method for extracting caking coals |
| WO2009059369A1 (en) * | 2007-11-06 | 2009-05-14 | Advanced Biofuels Ltd | Liquefaction process |
| CN103589443A (en) * | 2013-10-31 | 2014-02-19 | 吴国存 | Pollution-free purifying and efficient using method for inferior organic wastes |
| CN111847564A (en) * | 2019-04-28 | 2020-10-30 | 华南理工大学 | Semi-coke wastewater extraction dephenolization and negative pressure type extractant recovery method and device |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3215102A1 (en) * | 1982-04-23 | 1983-10-27 | Joachim A. Dr.-Ing. 6636 Schwalbach Wilhelm | Process for liquefying coal |
-
1979
- 1979-11-20 PL PL21973479A patent/PL122657B1/en unknown
-
1980
- 1980-11-11 GB GB8036343A patent/GB2063906A/en not_active Withdrawn
- 1980-11-20 DE DE19803043769 patent/DE3043769A1/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4502940A (en) * | 1982-11-19 | 1985-03-05 | Coal Industry (Patents) Limited | Method for extracting caking coals |
| GB2132223A (en) * | 1982-12-20 | 1984-07-04 | Exxon Research Engineering Co | The extraction of coal liquefaction bottoms |
| WO2009059369A1 (en) * | 2007-11-06 | 2009-05-14 | Advanced Biofuels Ltd | Liquefaction process |
| CN103589443A (en) * | 2013-10-31 | 2014-02-19 | 吴国存 | Pollution-free purifying and efficient using method for inferior organic wastes |
| CN103589443B (en) * | 2013-10-31 | 2015-09-09 | 唐山山岛石油化学有限公司 | The nuisanceless purification of organic waste inferior and Efficient utilization method |
| CN111847564A (en) * | 2019-04-28 | 2020-10-30 | 华南理工大学 | Semi-coke wastewater extraction dephenolization and negative pressure type extractant recovery method and device |
Also Published As
| Publication number | Publication date |
|---|---|
| PL219734A1 (en) | 1981-06-19 |
| PL122657B1 (en) | 1982-08-31 |
| DE3043769A1 (en) | 1981-08-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |