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WO2001003843A1 - Procede de traitement de fines particules de charbon - Google Patents

Procede de traitement de fines particules de charbon Download PDF

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Publication number
WO2001003843A1
WO2001003843A1 PCT/CA2000/000788 CA0000788W WO0103843A1 WO 2001003843 A1 WO2001003843 A1 WO 2001003843A1 CA 0000788 W CA0000788 W CA 0000788W WO 0103843 A1 WO0103843 A1 WO 0103843A1
Authority
WO
WIPO (PCT)
Prior art keywords
coal
oil
agent
aqueous phase
extraction
Prior art date
Application number
PCT/CA2000/000788
Other languages
English (en)
Inventor
Jaewon Choung
Jozef Szymanski
Zhenghe Xu
Original Assignee
The Governors Of The University Of Alberta
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 The Governors Of The University Of Alberta filed Critical The Governors Of The University Of Alberta
Priority to US10/019,667 priority Critical patent/US6767465B1/en
Priority to AU56691/00A priority patent/AU5669100A/en
Publication of WO2001003843A1 publication Critical patent/WO2001003843A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00—General arrangement of separating plant, e.g. flow sheets
    • B03B9/005—General arrangement of separating plant, e.g. flow sheets specially adapted for coal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D3/00—Differential sedimentation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D3/00—Differential sedimentation
    • B03D3/06—Flocculation
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L1/00—Liquid carbonaceous fuels
    • C10L1/32—Liquid carbonaceous fuels consisting of coal-oil suspensions or aqueous emulsions or oil emulsions
    • C10L1/322—Coal-oil suspensions

Definitions

  • the present invention relates to the recovery of coal fines as a valuable product and the clarification of water for recycling from coal tailings permitting the use of a single stage unit operation.
  • Oil agglomeration appears to be promising in recovering fine coals, as there is virtually no lower particle size limit and the ultimate floatability of coal is less affected by size compared to froth flotation (MEHROTRA, V.P., SASTRY, K.V.S. and MOREY, B.W., 1983. Review of Oil Agglomeration Techniques for Processing of Fine Coals, Int. J. Miner. Process. 11, p. 175-201.).
  • An attractive feature of oil agglomeration process is a product of low moisture content.
  • the recovered fine coals still need to be pelletized by adding an extra amount of heavy oil and screened to a few millimeters in diameter, to facilitate the storage and handling and to ensure an effective flame contact in combustion chambers.
  • a second stage treatment to remove fine particles from process effluent for water recycle is needed with the oil agglomeration process.
  • An object of the invention is to provide an economic process capable of recovering fine coals and cleaning up process water for recycle, preferably in an integrated, single stage operation.
  • the present invention related to extracting coal fines from an aqueous phase suspended coal fines and hydrophilic mineral matters comprising mixing an extraction oil with the coal fines suspended in said aqueous phase, the oil being added in an amount effective to extract the coal fines by hydrophobic extraction and form a nonqaueous phase containing said coal fines and said oil and a modified aqueous phase containing said hydrophilic mineral matters, adding at least one of a flocculating agent, a coagulating agent or a combination of said flocculating agent and said coagulating agent to said aqueous phase or said modified aqueous phase to facilitate the separation of said hydrophilic mineral matters from said aqueous phase to form a clarified aqueous phase and disposing of said mineral matters from clarified aqueous phase.
  • said mixing of said extraction oil for recovering fine coals and said addition of said at least one of said flocculating agent, said coagulating agent or said combination of the two for clarification of process water are integrated into a single stage.
  • said one stage includes removing the separated mineral matters from the aqueous phase to provide said a clarified aqueous phase for recycling.
  • said extraction oil will be added in the amount of between about 100 and 250 % based on the dry weight of the coal fines in the suspension.
  • said extraction oil will be selected from the group consisting of heavy crude, light mineral oils, fuel oils and landfill gas condensates.
  • said one comprises said flocculating agent, which is added to a concentration below 30 ppm
  • said flocculating agent is selected from the group comprising cationic or anionic flocculants.
  • said one comprises said coagulating agent is added to a concentration of up to about 1000 ppm
  • said coagulating agent is selected from the group comprising positively charged aluminum hydrosols and calcium, magnesium or other multivalent cations.
  • said one comprises said combination of said flocculating agent and said coagulating agent is used for separation of said hydrophilic mineral matters from said modified aqueous suspension.
  • said flocculating agent will be an anionic flocculant and said coagulating agent will be multivalent cations.
  • said flocculating agent and said coagulating agent are mixed in the ratio of between 1/10 and 1/100 of flocculating agent to coagulating agent.
  • Figure 1 is a graph showing the effect of oxidation temperature on coal surface hydrophobicity evaluated by thin film flotation (coal particles in - 417 + 208 ⁇ m size fractions were oxidized for 24 hours).
  • Figure 2 is a graph showing the effect of surface hydrophobicity on hydrophobic extraction as a function of oil/solid ratio (coal particles in - 417 + 208 ⁇ m size fractions were oxidized for 24 hours).
  • Figure 3 is a graph showing the effect of particle size on hydrophobic extraction at oil/solid ratio of 1.8.
  • Figure 4 is a graph showing the effect of order of flocculant addition on hydrophobic extraction at oil/solid ratio of 1.8 (coal particles in - 417 + 208 ⁇ m size fractions were oxidized for 24 hours).
  • Figure 5 is a graph showing the effect of anionic flocculants added prior to mineral oil on hydrophobic extraction at oil solid ratio of 1.8 (coal particles in - 417 + 208 ⁇ m size fractions were oxidized for 24 hours).
  • Figure 6 is a graph showing the effect of coagulant added prior to mineral oil on hydrophobic extraction at oil/solid ratio of 1.8 (coal particles, - 417 + 208 ⁇ m; solid symbols, with anionic flocculants; open symbols, no anionic flocculants).
  • Figure 7 is an illustration of hydrophobic extraction, flocculation and/or coagulation in a single stage process: a) hydrophobic extraction, b) a plus electrolytic coagulation, c) a plus flocculation, and d) all three mechanisms, i.e., a, b and c.
  • Figure 8 is a graph showing the clarity of processed water as a function of flocculants concentration
  • Figure 9 is a graph showing the role of hydrophobic coal on coalescence of oil droplets
  • Figure 10 is a graph showing schematically the concept of reactor/separator for the integrated technology Description of the Preferred Embodiments
  • the present invention comprises mixing an extraction oil with an aqueous suspension of fine coal particles containing other particles such as fine clay particles, as found for example in coal tailings, for a pe ⁇ od of time sufficient to form a coal ⁇ ch oil phase which floats I e the coal fines are extracted into the oil phase which phase-separates or floats on the aqueous phase to provide a non-aqueous phase that may be recovered using known techniques to provide a separated coal rich oil fraction
  • the coal rich oil fraction containing the coal fines forms a coal-in-oil mixture that may be used directly as a fuel product
  • any suitable extraction oil may be used which includes anything from kerosene to vegetable oil, heavy crude, light mineral oils, fuel oils and landfill gas condensates, but preferably the oil will be selected from the group including heavy crude, light mineral oils, fuel oils and landfill gas condensates
  • the oil is mixed with the aqueous phase it is simultaneously mixed with either a flocculating agent, a coagulating agent or a combination of flocculating agent and coagulating agent ⁇ vhich promotes aggregation of other particles (rejects) that sink, leaving a clarified aqueous phase, which may be used for any suitable purpose, the most likely being recycled to the processing plants
  • the aqueous suspension of fine coal particles containing other particles may be first mixed with the oil to form a modified aqueous phase and then a flocculating agent, a coagulating agent or a combination of flocculating agent and coagulating agent may be mixed with the modified aqueous phase and the other particles permitted to sink to provide the
  • the initial suspension (tailings) will contain particles in the size range below 2mm. and will have a solids content in the lange of about 1 to 10 % by dry weight solids with the coal comp ⁇ sing about 20 to 70 % by weight of the solids
  • the extraction oil will be added in the amount of between about 100 and 250 % based on the dry weight of coal in the suspension
  • the flocculating agent will normally be added in the concentration below 30 ppm, and a coagulating agent in the concentration of up to about 1000 ppm, or a combination of the two in the ratio of between 1/10 and 1/100 of flocculants to coagulant
  • the preferred flocculants or flocculating agent for use in the present invention includes cationic or anionic flocculants and the preferred coagulant or coagulating agent includes positively charged aluminum hydrosols or multivalent cations, such as calcium or magnesiu
  • the preferred combination will contain an anionic flocculants and multivalent cations Examples
  • Sample 2 A fine coal tailings sample taken from the tailings stream of the 2 nd bank of flotation cells at Smoky River Coal Ltd. was tested. To simplify the test procedures, the solids in the stream were collected after filtration and dried at 105 °C. The fine solid samples with a top particle size of 500 ⁇ m contained 37.7% mineral matters. To study the effect of particle size on process performance, a portion of the sample was dry-screened to obtain -45 ⁇ m size fractions. The sample obtained as such contained 41.1% mineral matters.
  • Sample 3 A combined thickener underflow, i.e., total fine refuse from preparation plant, at OBED Coal Ltd. was tested. A portion of the samples were wet-screened to separate the - 45 :m size fractions which contain 83.6% mineral matters and used as clays. The remaining fractions containing 52% mineral matters and as-received tailings samples were tested with the current technology. Chemicals
  • Analytical grade light mineral oil was purchased from Anachemia, Canada.
  • the cationic (Magnifloc 591-C, MW of -200,000), anionic (Superfloc 218 Plus, MW of -10 6 ) and nonionic (Superfloc 127 Plus, MW of -10 6 ) flocculants were provided by Cytec Industries Inc., USA.
  • Analytical grade calcium chloride was purchased from Fisher Scientific, Canada All the chemicals were used as received. Unless otherwise stated, all the experiments were carried out at room temperature with de-ionized water prepared using an Elix-5, followed by the purification with a Millipore-UV unit (Millipore, Canada). Procedures The batch type experiments were conducted in a 400 mL glass beaker.
  • the coal slurry was prepared by adding 5.76 grams of dried sample into 200 mL of de-ionized water under mechanical agitation at 1300 rpm for 5 minutes (Caframo Lab. Stirrer 4405-10, Cole- Parmer). This resulted in a pulp of 2.8% solids, corresponding to the percent solids in the original coal tailings stream
  • the desired amount of mineral oil, flocculants and/or coagulant were added into the resultant coal slurry under mechanical agitation.
  • the slurry was poured as quickly as possible into a separatory cylinder. Following a 15-minute settling during which phase separation occurred, the rejects (aqueous phase) and floats (organic phase) were separated into a beaker and an aluminum pan, respectively.
  • the solids retained in the aqueous phase were filtered on a filter circle fixed on a funnel, washed with toluene, dried in the oven at 105 °C for 5 hours, and weighed.
  • the solids extracted in the oil phase were then determined from mass balance. The yield of solids retained in the oil phase was used to evaluate the extraction performance. Similar procedures were applied to the tailings sample.
  • the ash content of the feed and solids in the aqueous phase was determined in accordance with ASTM (D 3174).
  • the combustible recovery and ash content in organic phase were then calculated based on the solid mass of the feed and rejects, along with their ash contents.
  • the amount of suspended solids rernaining in the treated water was determined by a spectrophotometer (Spectronic 21, Spectronic Instruments, Inc.) after calibration.
  • the hydrophobic oil extraction featured in this process is conceptually different from the oil agglomeration process, in which case oil is used as a bridge to link particles.
  • the current process produces a liquid fuel in the form of coal-in-oil mixture (COM).
  • COM coal-in-oil mixture
  • the moisture content entrapped by fine coal in oil phase is minimal compared to the moisture in flotation froth product even after dewatering. Therefore, a higher thermal efficiency is anticipated from coal-in-oil fuel.
  • Another added advantage of the liquid fuel from coal tailings produced by the present invention is the easy handling and transportation of slurry product.
  • the COM is currently used in water-tube boilers originally designed for oil firing.
  • Hydrophobic extraction is effective for recovery of coals over a wide particle size range (up to 2 mm) as long as they are sufficiently hydrophobic

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

Un procédé de récupération de fines particules de charbon et de clarification d'eau destinées à un recyclage comprend trois mécanismes distincts: extraction hydrophobe, coagulation électrolytique et floculation macromoléculaire, lesquels, si désirés, peuvent être intégrés en une seule phase. L'extraction hydrophobe est accomplie à l'aide d'huile pour former un mélange de charbon en huile. L'eau de traitement est clarifiée à l'aide de floculants, de préférence une combinaison d'un coagulant et de floculants anioniques. Avec un plan d'addition de réactifs bien défini, ce procédé permet une récupération de combustible supérieure à 88 % pour une teneur en cendres inférieure à 11 %, tout en produisant une eau propre contenant moins de 20 ppm de solides en suspension à partir d'un flux de résidus. Le mélange de charbon en huile peut être utilisé en tant que combustible par exemple dans des chaudières à charbon et des générateurs d'électricité.
PCT/CA2000/000788 1999-07-08 2000-07-04 Procede de traitement de fines particules de charbon WO2001003843A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US10/019,667 US6767465B1 (en) 1999-07-08 2000-07-04 Process for treating fine coal particles
AU56691/00A AU5669100A (en) 1999-07-08 2000-07-04 Process for treating fine coal particles

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US14277999P 1999-07-08 1999-07-08
US60/142,779 1999-07-08

Publications (1)

Publication Number Publication Date
WO2001003843A1 true WO2001003843A1 (fr) 2001-01-18

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WO (1) WO2001003843A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470583A (zh) * 2020-04-13 2020-07-31 华电电力科学研究院有限公司 一种选煤厂煤泥水智能加药系统与加药方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1507601A (en) * 1975-01-13 1978-04-19 American Minechem Corp Method of reclaiming water and coal from coal-treatment underflow by two-stage separation of solids
GB1584673A (en) * 1976-08-16 1981-02-18 Dow Chemical Co Method of separating coal from its accompanying gangue
JPS57170998A (en) * 1981-04-15 1982-10-21 Hitachi Ltd Removal of ash from coal and its device
JPS59105090A (ja) * 1982-12-09 1984-06-18 Ube Ind Ltd 石炭の灰分除去方法
US4456528A (en) * 1980-11-18 1984-06-26 Hitachi, Ltd. Process for removing ash from coal

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1507601A (en) * 1975-01-13 1978-04-19 American Minechem Corp Method of reclaiming water and coal from coal-treatment underflow by two-stage separation of solids
GB1584673A (en) * 1976-08-16 1981-02-18 Dow Chemical Co Method of separating coal from its accompanying gangue
US4456528A (en) * 1980-11-18 1984-06-26 Hitachi, Ltd. Process for removing ash from coal
JPS57170998A (en) * 1981-04-15 1982-10-21 Hitachi Ltd Removal of ash from coal and its device
JPS59105090A (ja) * 1982-12-09 1984-06-18 Ube Ind Ltd 石炭の灰分除去方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
C. DUONG ET AL.: "A novel process for recovering clean coal and water from coal tailings", MINERALS ENGINEERING, vol. 13, no. 2, February 2000 (2000-02-01), pages 173 - 181, XP000952142 *
PATENT ABSTRACTS OF JAPAN vol. 007, no. 014 (C - 146) 20 January 1983 (1983-01-20) *
PATENT ABSTRACTS OF JAPAN vol. 008, no. 222 (C - 246) 9 October 1984 (1984-10-09) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470583A (zh) * 2020-04-13 2020-07-31 华电电力科学研究院有限公司 一种选煤厂煤泥水智能加药系统与加药方法

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