GB2154318A - Coal carbonisation test - Google Patents

Coal carbonisation test Download PDF

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Publication number
GB2154318A
GB2154318A GB08404222A GB8404222A GB2154318A GB 2154318 A GB2154318 A GB 2154318A GB 08404222 A GB08404222 A GB 08404222A GB 8404222 A GB8404222 A GB 8404222A GB 2154318 A GB2154318 A GB 2154318A
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United Kingdom
Prior art keywords
sample
coal
reactivity
test
test temperature
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GB08404222A
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GB2154318B (en
GB8404222D0 (en
Inventor
Joseph Goleczka
Edmund Peter Mills
Edward Keith Harrison
Roy Nichols
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Coal Industry Patents Ltd
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Coal Industry Patents Ltd
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Priority to GB08404222A priority Critical patent/GB2154318B/en
Publication of GB8404222D0 publication Critical patent/GB8404222D0/en
Publication of GB2154318A publication Critical patent/GB2154318A/en
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Publication of GB2154318B publication Critical patent/GB2154318B/en
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    • 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

Micro-reactivity of cokes can be estimated by carbonising a small sample of finely divided coal until constant weight at a desired test temperature, then passing carbon dioxide over the sample at the desired test temperature and measuring weight loss in a given time.

Description

SPECIFICATION Coal carbonisation test This invention concerns a coal carbonisation test, more especially it concerns a test which gives information on coke micro-reactivity.
Considerable attention is currntly being paid to the reactivity to carbon dioxide of carbonised coals or cokes. A favoured test for the reactivity of coke is the Nippon Steel Corporation (NSC) method (COMA Yearbook 1980, 87), involving determining the percentage weight loss of a 200 g sample of a closely sized lump coke (20 + 1 mm) in carbon dioxide at 1 100'C for 2 hours. A special standard apparatus has been devised for carrying out the NSC method; not only is the apparatus expensive but the method is time-consuming and labour-intensive. Thus to assess a coal or coal blend for commencial use, test cokes have to be prepared and this requires up to one day. Thereafter, the method itself requires skilled laboratory personnel.It would be of considerable assistance to coke oven plant operators if a simpler, quicker and cheaper test could be devised capable of being carried out by relatively unskilled personnel at the plant and enabling plant management to predict and monitor the likely performance of a coal feed or blend on the commercial scale before coke is actually made. It would be most advantageous if any test method could be found to bypass the need to make test cokes in a test or pilot oven. We believe that we have found a quick and simple method which avoids most if not all of the drawbacks of the NSC method, yet gives results which correlate very well with those of the NSC method.
Accordingly, the present invention provides a method for assessing the micro-reactivity of coke, which comprises taking a small representative sample of a finely divided coal or coak blend, carbonising it under an inert gas by heating until a constant weight is obtained at the desired reactivity test temperature, passing carbon dioxide over the carbonised sample at the desired test temperature and measuring the weight loss in a given time.
It can be seen at once that the starting material for the method of the invention is not a coke but a coal. We do not believe that this has previously been suggested although it offers particular advantages which will become clearer hereinafter. The coal or coal blend is preferably ground or crushed to a suitable size; for example in tests which are found to give good correlation with the NSC method a suitable size range is 72-120 BS sieve sizes (212-125 yam), which is within a size range frequently prepared in the UK industry for proximate analysis of the feed coal(s). The weight of the sample is not critical to the present invention, and successful tests have been carried out with as little as 1 50 mg of coal, although it is envisaged that a test method suitable for plant use would use about 10 g.However, it is important to ensure that the sample is representative, and known methods exist for sampling to give a statistically representative sample, normally involving a riffling procedure.
The coal or blend sample is heated to a preselected temperature under an inert gas, preferably under a stream of the gas which is conveniently nitrogen, although any inert gas may be used. The preselected temperature would normally be in the range 900 to 1 200 C, and in the NSC method is 1 1 00to.
The rate of heating is also conveniently that met with in conventional carbonisation in an oven, of the order of 5 C/min. It may be possible, if desired, to speed up the test by heating at a faster rate, especially in the postplastic phase above about 500"C, but because the method can operate with small samples the problems of bulk heating are avoided, and carbonisation times are of the order of 3 > hours instead of 17-20 hours in coke ovens. If the coal(s) being tested are strongly caking, it is desirable to physically separate the individual particles of coal to prevent agglomeration. Since the method of the invention is a micro-reactivity test and not intended to simulate or give information on coke bulk reactivity, it is necessary only to form a clear rather than a coke in which fusion has taken place.
The reaction of the carbonised sample with carbon dioxide is suitably carried out by passing a stream of CO2 over the sample. Preferably, the weight of the sample is constantly monitored against time, but the sample may be weighted before and after a known period of CO2 treatment. The NSC method specifies weight before and after passing CO2 for 2 hours; we have found that the CO2 treatment may be carried out until a 20% weight loss or for a fixed time since weight loss is linear with time, providing that the same procedure is used for comparisons.
Preferably, the method of the invention is carried out in a furnace in which the sample of coal or blend can be heated and exposed to, in turn, the inert gas and CO2, and in which the sample can be weighted continu ousiy or at the necessary points in the procedure.
We have also noted that there is a closely linear relationship between NSC reactivity results and post-reaction strengths (involving the tumbling of a coke which has undergone reaction with CO2, under standard conditions and measuring the breakage). Accordingly, we believe that the method of the present invention can be used to give useful information on post reaction strength as well as micro-reactivity.
The invention will now be described by way of example only.
EXAMPLE Representative samples of a variety of coals and coal blends were crushed and sieved to yield finely divided coal in the size range 212-125,um and 1 50 mg samples were carefully taken. The samples were placed in the sample holder of a commercial thermobalance and then heated under flowing nitrogen (400 ml/min) at 5'C/min to the temperature at which the reactivity measurements were to be made, 1100 C. The thermobalance provides a continuous reading of weight and when the temperature and weight of the sample had stabilised, the nitrogen was replaced by CO2 for 10 minutes.Each test could be completed within 4 hours, compared to at least one day normally required to carry out the NSC method by coking in a pilot oven then carrying out the NSC specified procedures.
For comparison purposes, the same coals and blends were coked in a 250 kg pilot oven by crushing the raw coal so that 85% passed through 3.35 mm screen and charging to the oven in the wet state (9% moisture). The pilot oven was gas heated, the flue side of the walls being maintained at 11 80"C. After 1 7 hours nominal carbonisation time, the charge was discharged and water quenched. The charge centre temperature was about 1030"C upon discharge. 200 g samples of the resulting cokes were tested in accordance with the NSC method.
The results of NSC reactivity and microreactivity according to the present invention are plotted in the accompanying Figure. The slope of the best straight line gives an equation: NSC reactivity = 1.152 MR + 9.050 where MR is the % weight loss after 10 minutes in the method of the invention as described above.
A correlation coefficient of 0.936 is found, and we believe that the method offers a valuable alternative to the NSC method.
While the method of the invention describes specifically an alternative to the NSC method, it is believed that the invention offers alternatives to many other reactivity tests carried out at local level to assess cokes and carbonised solid fuels of many types.

Claims (7)

1. A method for assessing the micro-reactivity of coke, which comprises taking a small representative sample of a finely divided coal or coal blend, carbonising said sample under an inert gas by heating until a constant weight is obtained at the desired reactivity test temperature, passing carbon dioxide over the carbonised sample at the desired test temperature and measuring the weight loss in a given time.
2. A method according to claim 1, wherein the coal or coal blend sample is of a particle size in the range 212-125 jum.
3. A method according to claim 1 or 2, wherein the test temperature is in the range 900 to 1200'C.
4. A method according to claim 1, 2, or 3, wherein the sample is heated at a rate of approximately 5 C/min.
5. A method according to any one of the preceding claims, wherein the sample is weighed continuously in the heating and the caron dioxide treatment steps.
6. A method according to claim 5, carried out in a thermobalance.
7. A method according to claim 1, substantially as hereinbefore described.
GB08404222A 1984-02-17 1984-02-17 Coal carbonisation test Expired GB2154318B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
GB08404222A GB2154318B (en) 1984-02-17 1984-02-17 Coal carbonisation test

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB08404222A GB2154318B (en) 1984-02-17 1984-02-17 Coal carbonisation test

Publications (3)

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GB8404222D0 GB8404222D0 (en) 1984-03-21
GB2154318A true GB2154318A (en) 1985-09-04
GB2154318B GB2154318B (en) 1987-08-05

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0558131A2 (en) * 1992-02-28 1993-09-01 Norsk Hydro A.S. Method for deciding the reactivity and soot index of carbon products and equipment therefor
EP0558130A2 (en) * 1992-02-28 1993-09-01 Norsk Hydro A.S. Apparatus for analysing carbon products
CN113252840A (en) * 2021-05-19 2021-08-13 重庆大学 Testing arrangement of simulation coal spontaneous combustion and process of putting out a fire

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0558131A2 (en) * 1992-02-28 1993-09-01 Norsk Hydro A.S. Method for deciding the reactivity and soot index of carbon products and equipment therefor
EP0558130A2 (en) * 1992-02-28 1993-09-01 Norsk Hydro A.S. Apparatus for analysing carbon products
EP0558130A3 (en) * 1992-02-28 1994-08-03 Norsk Hydro Technology
EP0558131A3 (en) * 1992-02-28 1994-08-03 Norsk Hydro Technology
CN113252840A (en) * 2021-05-19 2021-08-13 重庆大学 Testing arrangement of simulation coal spontaneous combustion and process of putting out a fire
CN113252840B (en) * 2021-05-19 2022-05-13 重庆大学 Testing arrangement of simulation coal spontaneous combustion and process of putting out a fire

Also Published As

Publication number Publication date
GB2154318B (en) 1987-08-05
GB8404222D0 (en) 1984-03-21

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PCNP Patent ceased through non-payment of renewal fee

Effective date: 19930217