CA1215306A - Monitoring coal extraction - Google Patents

Monitoring coal extraction

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Publication number
CA1215306A
CA1215306A CA000440563A CA440563A CA1215306A CA 1215306 A CA1215306 A CA 1215306A CA 000440563 A CA000440563 A CA 000440563A CA 440563 A CA440563 A CA 440563A CA 1215306 A CA1215306 A CA 1215306A
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CA
Canada
Prior art keywords
solvent
extraction
coal
yield
test
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
Application number
CA000440563A
Other languages
French (fr)
Inventor
Geoffrey M. Kimber
James W. Clarke
Terry D. Rantell
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.)
Coal Industry Patents Ltd
Original Assignee
Coal Industry Patents Ltd
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 Coal Industry Patents Ltd filed Critical Coal Industry Patents Ltd
Application granted granted Critical
Publication of CA1215306A publication Critical patent/CA1215306A/en
Expired legal-status Critical Current

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/14Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22Fuels; Explosives
    • G01N33/222Solid fuels, e.g. coal

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Immunology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

Case 4525/CAN

ABSTRACT OF THE DISCLOSURE

"MONITORING COAL EXTRACTION"

The amount of donatable hydrogen in a liquid hydrogen donor solvent extraction of coal process may be assessed by diluting the solvent with an aromatic liquid diluent, carrying out a test extraction of the coal under standard conditions, determining the extraction yield and, preferably, comparing the yield with yields of calibration tests.
The method is reliable and quicker than known methods of characterising solvents, and may be used to control coal extraction processes.

Description

53~)6 "MONITOR~NG COAL EXTRACTION"
This invention concerns the monitoring of coal extraction, and more particularly concerns the monitoring of the condition of hydrogen donor solvents used in coal extraction.
In the liquid solvent extraction of coal, including bituminous coals and lignites, we have found that the highest yields of extracted coal substance are obtained using hydrogen donor solvents. Such a solvent is a high boiling partially hydrogenated aromatic oil which transfers hydrogen from itself to hydrocarbon radicals formed by thermal cleavage of molecules of coal substance, ehus stabilising the resulting moieties against recombination or polymerisation. The solvent itself becomes more aromatic in character, and less effective as a solvent, during the extraction process, and requires re-activation or replenishment by hydrogenation. However, it has proved difficult to monitor the amount of donatable hydrogen ln process solvents in continuous coal extraction plants, not least because such process solvents are not single compounds but are complex mixtures of a large number of compounds. Methods of characterisation of process solven~6 which have been proposed, such as adsorption chromatography, ~MR
spectro copy, gas chromatography and mass spectrometry are not only lZ153~6 very time consuming, thus making them unsuitable for proce6s control, but can be m~sleading or open to alternative interpretation. It i~ therefore an aim of the present invention to provide a method of monitoring the conditlon of hydrogen donor solvents ~hich is sufficiently quick to be relevant in process control and also is applicable to the extraction of lignites as well as bituminous coals.
The pre~ent invent~on provide~ a method of monito~ing the condition of a hydrogen donor solvent in a coal extraction process, comprising sampling the solvent, diluting the solvent with a pre-determined amount of an aromatic liquid diluent compatible with the~olvent, effecting a test extraction of the coal with the diluted solvent under standard condltions, and determining the extraction yield. The extraction yield i6 conveniently expressed in terms of the total yield of liquid and gas on a dry minersl matter free (DMMF) basis. The liquld yield may be readily determined using a known method based on quinoline insolubility (e.g. "Fuel", 1978,57, 147) and the gas yield tetermined by collecting and analysing the gas evolved during digestion.
Tests have shown that there is a sub6tantially linear relationship between the yield a~ determined in the method of the invention and the sctual amount of donor hydrogen present. It is thus posslble and, we believe, useful, to perform a number of cal~bration tests with the particular coal and solvent and to create a "~olvent di6solving index for the assessment of process ~olvents. Accordingly, the method of the invent~on enables the ` ~Z~S3Q6 amount of tonatable hydrogen, or the position of the solvent on a "solvent dissolving index , to be monitored. The dilution of the solveDt ln the test enables a prediction of a fall-off of performance to be made and enabling counter measures to be taken before a significant 1088 of yield is experienced with the ~ndiluted solvent. The method of the invention requlres only relatively simple equipment of the bomb type and may be carried out in a few hours under favourable conditions.
The invention also provides a method of controlling a liquid solvent extraction of coal process comprising the monitoring of the condition of a hydrogen donor solvent u~ed ~n the process accord~ng to the $nvention, and applying corrective measures when necessary to restore the conditlon of the solvent to a predetermined acceptable range of donatable hydrogen content.
In lntegrated coal solvent extraction plants utili6ing liquid hydrogen donor solvent, there has to be provision for the regeneration of the process solvent, and mere recycle of a cut from the straight product is not sufficient. The solvent cut may be hydrogenated, or as is more likely, the appropriate cut may be taken after the hydrogenation or hydrocracklng of all the liquid product. It i6 posslble that a hydrogenated recycle solvent contains more donatable hydrogen than is necessary to achieve maximum yield; the method of the invention enables this condition also to be monitored (unllke any straightforward test based on extraction yield) and permits optimisation of the amount of hydrogenated product recycle.
The aromatic diluen~ u6ed in the present invention is preferably a polynuclear ~romatic, which may be substituted by alkyl groups, and may be a 6ingle compound or a ~tandard mixture of compounds. The preferred diluent i8 naphthalene, although compoundæ such as anthracene or phenanthrene and mi~tures thereof may be used or any compound which i6 not reactive in the extraction process .
The standard conditions for the test extraction need not exactly replicate those of the main extraction process, but are preferably 6imilar to the nominal conditions of the main extraction process. The conditions of the main extraction process may be difficult to reproduce in test apparatus or the main process may be operated under non-constant conditions.
The invention will now be described by way of example only.

EXAMPLE
The coal being extracted on a continuous pilot plant was a lignite crushed to 80% less than 75um and vacuum dried to a moisture content less than 5~. A hydrogenated anthracene oil solvent which had been rigorously characterised by NMR spectroscopy was used, and calibration extrsctions with the solvent blended with naphthalene in concentrations from 0 to 100% were carried out using a 40% coal in ~olvent slurry. The test extractions were carried out by loading accurately weighed amounts of coal, solvent and naphthalene into a stirred bomb reactor, which was immersed in a lZ153~6 fluldised sand bath of 4300. After 67 ml~utes, the reactor was removed from the sand bath and water quenched. The gas evolved was collected and its volume measured. The li~uld product was thoroughly removed from the bomb, weighed and the qulnoline insolubles measured by a stsndard method. The total yields were determined and calculated on a DMMF basis.

The sample of hydrogenated anthracene oil had previously been e6tabli~hed to have a donatable hydrogen concentration of 2.lX.
Even in the absence of donatable hydrogen, le using 100%

naphthalene a6 solvent, approximately 45% of the coal was extracted. To achieve the maximum obtainable extraction yield of 95%, a minimum of 1.4% donatable hydrogen was requlred. A
calibration chart was prepared, giving a "solvent di~solving index"
value (SDI) of 0 to an extraction yield of 45%, equivalent to 0%
donatable hydrogen, and an SDI of 20 to an extraction yield of 9~%, corresponding to 1.4X donatable hydrogen. Thls chart is reproduced in the accompanying Figure.
For the assessment of process solvents, the solvent~as diluted with it6 own weight of naphthalene. Hence, the SDI for the hydrogenated anthracene oll was 15, and solvent6 having higher as well as lo~er concentrations of donatable hydrogen find a place on the SDI scale. The ~cale accurately predicted that process fiolvents having an SDI of 10 or above were capable of obtalning excellent extraction yields of the lignite, and solvents having an SDI below 10 showed dlminlshlng ylelds.

.` 12153~)6 The sensitivity of the SDI test is dependent upon the precislon of mea6urement of the yield of quinolineinsolubles, but dupllcatlon could be expected to give values of quinoline lnsolubles within +1%. For a high mlneral matter lignite, this ~s equivalent to + 3% on the measurement of extraction yield and +1.5 on the SDI value.

The above Example was repeated using, instead of lignite, a British high volatile bituminous coal. A different SDI calibration i6 u6ed, but accurate predictions were achleved of the extraction capability of test solvents.

Claims (4)

Case 4525/CAN
WE CLAIM:
1. A method of monitoring the donatable hydrogen content of a hydro-gen donor solvent in a coal extraction process using said solvent, comprising the steps of a) sampling the solvent, b) diluting the sol-vent sample with a predetermined amount of an aromatic liquid diluent compatible with the solvent, c) effecting a test extraction of the coal with the diluted solvent under standard conditions, and d) determining the extraction yield of said test extraction.
2. A method as claimed in claim 1, comprising the carrying out of preliminary calibration extractions with the coal and the solvent having different amounts of donatable hydrogen to establish calibration extrac-tion yields under said standard conditions, and comparing the test extraction yield with the calibration extraction yields.
3. A method as claimed in claim 1, wherein the aromatic liquid di-luent is selected from naphthalene, anthracene, phenanthrene and mixtures thereof.
4. A method of controlling a liquid solvent extraction of coal pro-cess using a hydrogen donor solvent, comprising the monitoring of the condition of the solvent used in the process by a method as claimed in claim 1, and applying corrective measures when necessary to restore the condition of the solvent to a predetermined acceptable range of donatable hydrogen content.
CA000440563A 1982-11-19 1983-11-07 Monitoring coal extraction Expired CA1215306A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB08233125A GB2130366B (en) 1982-11-19 1982-11-19 Monitoring coal extraction
GB82/33125 1982-11-19

Publications (1)

Publication Number Publication Date
CA1215306A true CA1215306A (en) 1986-12-16

Family

ID=10534387

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000440563A Expired CA1215306A (en) 1982-11-19 1983-11-07 Monitoring coal extraction

Country Status (6)

Country Link
JP (1) JPS59102983A (en)
AU (1) AU565697B2 (en)
CA (1) CA1215306A (en)
DE (1) DE3341346A1 (en)
FR (1) FR2536409B1 (en)
GB (1) GB2130366B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63270792A (en) * 1987-04-30 1988-11-08 Sumitomo Metal Ind Ltd Coal liquefaction method

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5313604A (en) * 1976-07-23 1978-02-07 Mitsui Cokes Kogyo Kk Method of liquefying coals
US4347117A (en) * 1979-12-20 1982-08-31 Exxon Research & Engineering Co. Donor solvent coal liquefaction with bottoms recycle at elevated pressure

Also Published As

Publication number Publication date
JPS59102983A (en) 1984-06-14
AU565697B2 (en) 1987-09-24
FR2536409B1 (en) 1986-02-28
AU2107483A (en) 1984-05-24
DE3341346A1 (en) 1984-05-24
FR2536409A1 (en) 1984-05-25
GB2130366A (en) 1984-05-31
DE3341346C2 (en) 1993-01-07
GB2130366B (en) 1986-02-05

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