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WO2001094497A1 - Procede et appareil de separation de solides d'une huile pyrolytique - Google Patents

Procede et appareil de separation de solides d'une huile pyrolytique Download PDF

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Publication number
WO2001094497A1
WO2001094497A1 PCT/FI2001/000536 FI0100536W WO0194497A1 WO 2001094497 A1 WO2001094497 A1 WO 2001094497A1 FI 0100536 W FI0100536 W FI 0100536W WO 0194497 A1 WO0194497 A1 WO 0194497A1
Authority
WO
WIPO (PCT)
Prior art keywords
pyrolysis
solid matter
liquid
pyrolysis liquid
separating
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.)
Ceased
Application number
PCT/FI2001/000536
Other languages
English (en)
Inventor
Yrjö SOLANTAUSTA
Anja Oasmaa
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.)
VTT Technical Research Centre of Finland Ltd
Original Assignee
VTT Technical Research Centre of Finland 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 VTT Technical Research Centre of Finland Ltd filed Critical VTT Technical Research Centre of Finland Ltd
Priority to AU2001274126A priority Critical patent/AU2001274126A1/en
Publication of WO2001094497A1 publication Critical patent/WO2001094497A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the present invention relates to a method as defined in the preamble of claim 1 and to an apparatus as defined in the preamble of claim 9 for the separation of solid matter from a pyrolysis liquid produced by flash pyrolysis of solid raw material by condensing the pyrolysis steam generated, .producing a pyrolysis liquid.
  • the solid raw material used in the pyrolysis process may consist of e.g. wood, bark, forest waste chips or a mixture of these, or peat or other solid biomass .
  • the pyrolysis steam and liquid produced con- ventionally contain solid matter, e.g. carbonization residue, sand and/or impurities or the like. Some of the solid matter can be removed during the flash pyrolysis process by using e.g. filters and cyclones, as described e.g. in patent applications FI 19992080 and FI 19992181. However, some of the solid matter may remain in the pyrolysis liquid product. This solid matter causes problems in the storage and use of the pyrolysis liquid product, e.g. when the pyrolysis liquid is used as a fuel in boilers and power plants. The solid matter tends to block filters and atomizers in such apparatus and it may also cause erosion. In addition, sediments accumulate on the bottom of containers during storage. Such sediments cannot be easily removed and they are difficult to treat using conven- tional fuel treatment apparatus. Moreover, solid matter in the fuel increases particle emissions from the combustion process.
  • solid matter e.g. carbonization residue, sand and/or impurities or the
  • the object of the invention is to eliminate the above-mentioned problems and to disclose a new and practicable method for separating solid matter from a pyrolysis liquid that is more effective than previously known methods.
  • a further object of the invention is to disclose a method that is easy to implement while allowing easy elimination of the problems caused by solid matter in connection with the use of pyroly- sis liquid.
  • the invention is based on separating solid matter from a pyrolysis liquid obtained via pyrolysis. Most of the solid matter contained in the pyrolysis liquid is separated from it in a separating device after a suitable delay by removing from the surface of the pyrolysis liquid a desired surface fraction having a high solid matter content.
  • the pyrolysis liquid is produced from solid raw material by generating pyrolysis steam via flash pyrolysis and condensing the steam into a liquid.
  • the surface fraction is separated from the pyrolysis liquid after condensation performed in a condenser, wh-ere the gas and liquid phases are effectively intermixed.
  • a gas e.g. pyrolysis vapor
  • the condenser As the liquid-gas mixture is cooling down, the gas is released and rises as gas bubbles toward the surface of the pyrolysis liquid. Solid matter particles adhere to the surface of the gas bubbles, rising with the bubbles to the surface portion of the pyrolysis liquid. In this way, a surface fraction having a high solid matter content is. formed. With time, however, the solid matter begins to settle back to the bottom.
  • the surface fraction separated constitutes 1 - 30 vol-%, preferably 1- 20 vol-% of the pyrolysis liquid.
  • the surface fraction is a substantially separate surface phase.
  • the formation of a separate surface phase depends on the raw material used and the processing conditions; phase separation does not always occur in the pyrolysis liquid.
  • a separate surface phase may also be formed in a situation where e.g. a scrubbing liquid in the condenser forms a multiphase oil with the pyrolysis liquid.
  • a suitable delay is 1 - 720 min, preferably 1 - 60 min.
  • the surface fraction is separated after a delay period, preferably within 1 h - 5 days, by which time possible phase separation from the pyrolysis liquid will substantially have taken place.
  • the surface fraction containing solid matter may be first separated from the pyrolysis liquid within a delay of 1 - 720 min, whereupon the separate surface phase is separated after phase separation has occurred. The phase separation may take place considerably more slowly than the rising of solid matter into the surface fraction of the pyroly- sis liquid.
  • the delay may be dependent on the condenser, e.g. a scrubber, on the velocity and/or volume of gas flow in it and the efficiency of the liquid-gas contact. Moreover, the delay may depend on circumstances like design of the solids separation device, the raw material, its particle size, the reaction conditions, the number of phases in the pyrolysis liquid and other physical properties of the solid matter and liquid. An appropriate selection of the delay can have a decisive effect on the efficiency of separation of solid matter. In an embodiment of the invention, solid matter is substantially removed from the surface fraction separated.
  • At least part of the surface fraction separated is passed to an energy production stage in the pyrolysis process, e.g. into a combustion boiler.
  • the solid matter removed from the surface fraction may also be taken into a combustion boiler.
  • the apparatus of the invention comprises at least one separating device for separating solid matter from the pyrolysis liquid obtained from a pyrolysis process by separating a desired surface fraction having a high solid matter content from the surface of the pyrolysis liquid, and at least one control device for setting a suitable delay and/or controlling the separation of a desired surface fraction.
  • the device is disposed substantially in conjunction with a flash pyrolysis apparatus comprising a pyrolyzer for generating pyrolysis steam and a condenser for condensing the pyrolysis steam into pyrolysis liquid.
  • the device is disposed in conjunction with the condenser, preferably a scrubber. In an embodiment, the device is disposed after the condenser.
  • the scrubbing fluid used may consist of any scrubbing fluid known in the art, e.g. the pyrolysis liquid or an external scrubbing fluid.
  • the method of the invention makes it possible to improve the quality of the pyrolysis liquid/oil produced in a pyrolysis process by reducing its solid matter content.
  • a lower solid matter content facilitates the storage and processing of the pyrolysis liq- uid while making the pyrolysis liquid more usable as a fuel in boilers and power plants.
  • the separation of solid matter from pyrolysis liquid can be per- formed more effectively than by prior-art methods.
  • the method and apparatus of the invention have the advantages of being easy and economical to use. Further, the apparatus of the invention can be easily combined with existing equipment and the method can be easily implemented in prior-art apparatus even after small investments.
  • the method and apparatus of the invention can be advantageously combined with the methods and apparatus presented in patent applications FI 19992080 and FI 19992081, the result being an effective pyrolysis process and a very good pyrolysis liquid product regarding its quality, e.g. stability.
  • Fig. 1 presents a diagram representing an embodiment of the apparatus of the invention
  • Fig. 2 - 5 illustrate the effect of the delay on the separation of solid matter and the distribution of solid matter particles between the surface fraction and the pyrolysis oil-
  • Fig. 1 presents an apparatus according to the invention for the separation of solid matter, in conjunction with a flash pyrolysis apparatus also pre- sented in the figure.
  • the flash pyrolysis apparatus in Fig. 1 comprises a pyrolyzer 1 for generating pyrolysis steam and a condenser 2, in the present embodiment a scrubber, for condensing the pyrolysis steam into a pyroly- sis liquid.
  • the flash pyrolysis apparatus may be any type of pyrolysis apparatus known in the art and it will not be described here in detail .
  • the apparatus of the invention comprises one separating device 3 for separating a surface fraction 6 containing solid matter from the surface of the pyrolysis liquid obtained from the pyrolysis process.
  • the apparatus comprises a control device 9 for setting a suitable delay and controlling the separation of a desired surface fraction and surface phase.
  • the control device may be a manually or automatically oper- ated device.
  • the separating device 3 used may be a simple separating device, such as a sedimentation basin, flotation apparatus or the like.
  • the separating device is a sedimentation basin 3.
  • the embodiment in Fig. 1 further comprises an extraction pipe 8 for bringing the pyrolysis liquid product, i.e. pyrolysis oil, out of the separating device 3.
  • the pyrolysis oil is passed via the extraction pipe 8 preferably into a product container 4.
  • the apparatus in Fig. 1 comprises an extraction pipe 10 for bringing the separated surface fraction 6 out of the separating device 3. Via this extraction pipe 10, the surface fraction can be passed into a separator device 5, in the pres- ent embodiment a filter 5, or to a direct utilization stage 12, e.g.
  • an energy production device such as a combustion boiler, for the pyrolysis process.
  • solid matter 7 is separated from the surface fraction 6, producing a surface fraction 11 with a low solid matter content.
  • the solid matter fraction 7 and/or the surface fraction 11 may be passed e.g. into a combustion boiler.
  • the apparatus of the invention is disposed after the scrubber 2, the separation of solid matter being performed upon the lapse of a certain delay after the condensation 2.
  • the scrubber 2 used is a device in which the gas and liquid phases intermingle effectively, in other words, the gas and liquid phases have a good liquid-gas contact surface with respect to each other.
  • the pyrolysis liquid is used as a scrubbing fluid.
  • the apparatus of the invention may be disposed in conjunction with a scrubber 2 for separating solid matter from the condensed pyrolysis liquid after a certain delay.
  • the gas 13 released from the separation 3 of solid matter is passed back into the pyrolysis reactor 1 or into a combustion boiler used in the pyrolysis process while any scrubbing fluid 14 that may be separated is taken back into the scrubber 2.
  • any types of known separating devices, control devices, extraction pipes and separator devices which will not be described here in detail.
  • the apparatus comprises two separating devices 3.
  • a first separating device is arranged to separate a surface fraction containing solid matter from the surface of the pyrolysis liquid after a short delay, 1 - 720 min.
  • a second separating device is ar- ranged to separate after a longer delay, 1 h - 5 days, the entire surface phase that may have been formed in the surface portion of the pyrolysis liquid.
  • the apparatus may also comprise one or more control devices.
  • the pyrolysis liquid is preferably produced from a raw material which is pyrolyzed to produce a multiphase liquid.
  • the pyrolysis liquid was produced by condensing pyrolysis steam in a scrubber in which the gas and liquid phases intermingled effectively.
  • the separated surface fraction containing solid matter was passed into a combustion boiler disposed in conjunction with a flash pyrolysis apparatus, where it was burned to produce energy.
  • Substantially the entire separate surface phase was separated from the surface of the pyrolysis liquid after a period during which phase separation had occurred in the pyrolysis liquid. The period was 1 h - 5 days .
  • solid matter was substantially removed using a filter.
  • the solid matter was taken into a combustion boiler and the rest of the surface phase was recovered for later utilization, e.g. in the production of a chemical.
  • the surface phase can be utilized or burned as such without removal of solid matter.
  • a surface fraction containing solid matter was separated from the surface of the pyrolysis liquid after a short delay, 1 - 60 min. After this, phase separation was allowed to take place in the pyrolysis liquid, about 1 h - 5 days. After the phase separation, the entire surface phase was separated from the pyrolysis liquid. The surface phase contained only small amounts of solid matter.
  • the separation of solid matter was performed in a separating device at a low temperature, below 50 °C.
  • the surface phase was in a solid state while the oil at the bottom, i.e. the pyrolysis product, was in a fluid state.
  • the oil was removed from the separating device via a drain valve.
  • Fig. 2 shows the quantity of solid matter in the surface fraction and in the oil at the bottom, i.e. in the pyrolysis oil product, as a function of the delay in the separation of solid matter.
  • Fig. 3 illustrates the distribution of the total amount of solid matter in the pyrolysis liquid between the surface fraction and the bottom oil as a function of the delay. From Fig. 2 - 3, it can be seen that an advantageous delay for the separation of solid matter from a single-phase pyrolysis liquid is in the range of 10 min - 60 min, when the criterion is minimization of solid matter content in the bottom oil.
  • Fig. 3 further shows that, within the range of advantageous delay, 70 - 95 w-% of the total amount of solid matter originally contained in the pyrolysis liquid can be removed.
  • Fig. 4 shows the amount of solid matter in the surface phase and in the bottom oil, i.e. in the pyrolysis oil product, as a function of the delay in the separation of solid matter.
  • Fig. 5 shows the distribution of the total amount of solid matter in the pyrolysis liquid between the surface phase and the bottom oil as a function of the delay.
  • an ad- vantageous delay for the separation of a surface phase containing solid matter from a multiphase pyrolysis liquid is in the range of 30 min - 6000 min when the criterion is minimization of solid matter content in the bottom oil.
  • Fig. 5 further shows that, within the range of advantageous delay, 70 - 90 w-% of the total amount of solid matter originally contained in the pyrolysis liquid can be removed.
  • a pyrolysis liquid produced from peat is a multiphase liquid, so the entire separate surface phase was separated. From the separated surface phase, solid matter was further separated, whereupon the surface phase was fit to be used e.g. for the production of a lubricant, because the surface phase of a pyrolysis liquid produced from peat has a lower resin content than the surface phase of a pyrolysis liquid pro- prised from e.g. forest waste.
  • the method and apparatus of the invention in its various embodiments are applicable for the separation of any kind of solid matter from any kind of py- rolysis liquid.

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  • 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)

Abstract

L'invention concerne un procédé de séparation de matière solide d'un liquide pyrolytique produit à partir d'une matière brute solide par pyrolyse éclair, par condensation de la valeur de pyrolyse obtenue en un liquide pyrolytique. Selon l'invention, la plupart de la matière solide contenue dans le liquide pyrolytique obtenu par le processus de pyrolyse, est séparée dudit liquide dans un dispositif de séparation après un délai adéquat, par la séparation de la surface du liquide pyrolytique d'une fraction de surface souhaitée présentant une teneur élevée en matière solide. L'appareil comprend au moins un dispositif de séparation (3) permettant la séparation de matière solide, et au moins un dispositif de commande (9) permettant d'établir un délai adéquat et/ou de commander la séparation d'une fraction de surface souhaitée. L'appareil est placé en liaison avec un appareil de pyrolyse éclair (1, 2).
PCT/FI2001/000536 2000-06-08 2001-06-06 Procede et appareil de separation de solides d'une huile pyrolytique Ceased WO2001094497A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001274126A AU2001274126A1 (en) 2000-06-08 2001-06-06 Method and apparatus for separating solids from pyrolysis liquid

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20001371A FI108462B (fi) 2000-06-08 2000-06-08 Menetelmõ ja laite kiintoaineen erottamiseksi pyrolyysinesteestõ
FI20001371 2000-06-08

Publications (1)

Publication Number Publication Date
WO2001094497A1 true WO2001094497A1 (fr) 2001-12-13

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PCT/FI2001/000536 Ceased WO2001094497A1 (fr) 2000-06-08 2001-06-06 Procede et appareil de separation de solides d'une huile pyrolytique

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AU (1) AU2001274126A1 (fr)
FI (1) FI108462B (fr)
WO (1) WO2001094497A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE219919C1 (sv) * 1962-02-02 1968-04-09 Oil Shale Corp Förfarande och apparat för utvinning av i huvudsak slamfri olja ur fast kolhaltigt material
US4247367A (en) * 1979-11-16 1981-01-27 Reilly Bertram B Apparatus for solid waste pyrolysis
US4260473A (en) * 1979-05-03 1981-04-07 Occidental Research Corporation Removal of particulates from pyrolytic oil
GB2118856A (en) * 1982-03-16 1983-11-09 Safinco Nv Process for separating solids from oils

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE219919C1 (sv) * 1962-02-02 1968-04-09 Oil Shale Corp Förfarande och apparat för utvinning av i huvudsak slamfri olja ur fast kolhaltigt material
US4260473A (en) * 1979-05-03 1981-04-07 Occidental Research Corporation Removal of particulates from pyrolytic oil
US4247367A (en) * 1979-11-16 1981-01-27 Reilly Bertram B Apparatus for solid waste pyrolysis
GB2118856A (en) * 1982-03-16 1983-11-09 Safinco Nv Process for separating solids from oils

Also Published As

Publication number Publication date
FI108462B (fi) 2002-01-31
FI20001371A0 (fi) 2000-06-08
AU2001274126A1 (en) 2001-12-17

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