US20080299015A1 - Apparatus and method for top removal of granular material from a fluidized bed deposition reactor - Google Patents

Apparatus and method for top removal of granular material from a fluidized bed deposition reactor Download PDF

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Publication number
US20080299015A1
US20080299015A1 US11/810,422 US81042207A US2008299015A1 US 20080299015 A1 US20080299015 A1 US 20080299015A1 US 81042207 A US81042207 A US 81042207A US 2008299015 A1 US2008299015 A1 US 2008299015A1
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Prior art keywords
gas
product
bed
height
dust
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Abandoned
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US11/810,422
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English (en)
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Stephen Michael Lord
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Lord Ltd LP
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Individual
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Priority to US11/810,422 priority Critical patent/US20080299015A1/en
Priority to AU2008260467A priority patent/AU2008260467B2/en
Priority to EP08780156.9A priority patent/EP2167227B1/en
Priority to JP2010511225A priority patent/JP2011527625A/ja
Priority to KR1020107000046A priority patent/KR101534879B1/ko
Priority to PCT/US2008/008569 priority patent/WO2008150552A2/en
Priority to CN200880018753.8A priority patent/CN101743057B/zh
Priority to TW097143379A priority patent/TWI387484B/zh
Publication of US20080299015A1 publication Critical patent/US20080299015A1/en
Assigned to LORD LTD LP reassignment LORD LTD LP ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LORD, STEPHEN M
Priority to US12/647,283 priority patent/US8703087B2/en
Abandoned legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B15/00—Fluidised-bed furnaces; Other furnaces using or treating finely-divided materials in dispersion
    • F27B15/02—Details, accessories or equipment specially adapted for furnaces of these types
    • F27B15/09—Arrangements of devices for discharging
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
    • B01J8/0025—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor by an ascending fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005—Separating solid material from the gas/liquid stream
    • B01J8/0055—Separating solid material from the gas/liquid stream using cyclones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1809—Controlling processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836—Heating and cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B9/00—Combinations of apparatus for screening or sifting or for separating solids from solids using gas currents; General arrangement of plant, e.g. flow sheets
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D17/00—Arrangements for using waste heat; Arrangements for using, or disposing of, waste gases
    • F27D17/20—Arrangements for treatment or cleaning of waste gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/0061—Controlling the level
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00743—Feeding or discharging of solids
    • B01J2208/00761—Discharging

Definitions

  • This invention relates generally to the field of deposition reactors and more specifically to an apparatus and method for top removal of granular material from a fluidized bed deposition reactor.
  • Fluidized bed reactors have a long tradition in the chemical industry where the bed usually consists of a finely divided valuable catalyst which makes it necessary to design the reactors to prevent catalyst losses. Thus was developed the practice of requiring a large disengaging height above the bed surface and of using cyclones to capture the fine dust and return it to the bed. A concept called total disengaging height, or TDH, was developed to estimate the height where all the particles that would settle out by gravity had settled out. Internal cyclones were provided at this height to capture the finer dust and return it to the bed. Whenever the catalyst was removed it was removed from the bottom by gravity. Other reactors called dilute phase or transport reactors entrained all the solids up through the reactor and out the top, but these reactors did not have a recognizable bed.
  • 6,827,786 provides a detailed description of a multistage deposition reactor which takes advantage of increased bed height to produce additional silicon by use of additional gas injection points along the side of the reactor.
  • the seed generation by grinding is spread out along the reactor because of the extra nozzles and some deposition occurs further from the inlet, but most of the grinding and deposition occurs in the bottom where the solid product is removed.
  • Lord discusses, Col3 line 25, the “De Beers” paper which showed the need for some residence time and temperature to fully crystallize the product and dehydrogenate the beads. He does this in the pulsed bead heater at high temperature and with short residence time.
  • Lord and his many references do not discuss energy recovery from the effluent gas although Lord in U.S. Pat. No. 5,798,137 and 6,451,277 discusses the use of the heat from the outgoing product to heat the incoming gas.
  • the primary object of the invention is to provide a shorter reactor with greater production.
  • Another object of the invention is to provide a passive method of level control.
  • Another object of the invention is to provide a better quality product.
  • a further object of the invention is to reduce the need for high temperature at the bottom of the reactor.
  • Yet another object of the invention is to reduce the risk of plugging.
  • Still yet another object of the invention is to reduce the thickness of wall deposits.
  • Another object of the invention is to reduce the pressure in the product removal system.
  • Another object of the invention is to recover energy.
  • an apparatus and method for top removal of granular material from a fluidized bed deposition reactor comprising: removal of the product from the top of the reactor together with the effluent gas, separation of the granular product from the effluent gas, simultaneous recovery of heat from the product and the gas and optional further dust and heat recovery.
  • FIG. 1 is a schematic diagram illustrating the operation of a fluidized bed deposition reactor of the prior art with bottom removal and a large disengaging space.
  • FIG. 2 a is the same diagram modified to show the benefits of the invention.
  • FIG. 2 b is a detailed schematic of the top of the reactor showing the granular particle removal mechanism.
  • FIG. 3 is a schematic of a product separator with integrated heat recovery.
  • FIG. 1 there is shown a schematic of a typical fluidized bed deposition reactor comprising a containment vessel or liner, 111 , of a height, 144 , a gas introduction means, 112 , an optional gas distribution means, 113 , a bottom product removal means, 114 , a bed heating means, 115 , a gas/dust mixture exit, 116 , a connecting means, 127 , a dust/gas separation means, 117 , a dust removal means, 118 , and a gas exit, 119 .
  • a typical fluidized bed deposition reactor comprising a containment vessel or liner, 111 , of a height, 144 , a gas introduction means, 112 , an optional gas distribution means, 113 , a bottom product removal means, 114 , a bed heating means, 115 , a gas/dust mixture exit, 116 , a connecting means, 127 , a dust/gas separation means, 117 , a dust removal means,
  • the containment vessel, 111 surrounds a bed of granules, 120 , fluidized by gas bubbles, 121 , and having an average top level, 122 , above which product granules, 123 , thrown up above the bed describe arcs as they rise from random impact within the bed then fall under gravity in a reduced disengaging space, 124 , while the small entrained dust particles, 125 , continue up and leave with the effluent gas, 126 , through the gas/dust mixture exit, 116 , through the connecting means, 127 , then enter the dust/gas separation means, 117 , where most of the dust, 125 , is removed from the gas, 126 , and then ultimately leaves the system via the dust removal means, 118 , while the gas, 126 , and residual dust leaves via an exit, 119 .
  • the differential pressure meter, 128 measures the difference in pressure between the bottom product removal means, 114 , and the gas exit, 119 . This measurement indicates the level, 122 , of the bed of granules, 120 .
  • the bottom removal means, 114 is used to control the top level, 122 , to maintain the disengaging space, 124 , so that the product granules, 123 , are returned to the bed of granules, 120 , and are thus removed by the bottom product removal means, 114 .
  • FIG. 2 a shows a schematic similar to FIG. 1 but modified to remove the granular product from the top via a gas/granular separator means, 230 , inserted before the effluent gas enters the gas/dust separation means, 217 .
  • a further modification is the removal of the differential pressure transmitter, 128 , shown in FIG. 1 , which is not required for bed level control.
  • the invention thus comprises a containment vessel or liner, 211 , of a height, 244 , a gas introduction means, 212 , an optional gas distribution means, 213 , an optional bottom product removal means, 214 , a bed heating means, 215 , a gas/dust/granular mixture exit, 216 , a first connecting means, 241 , a gas/granular separator means, 230 , with a granular removal means, 231 , an optional heat recovery means, 242 , a further connecting means, 229 , a gas/dust separation means, 217 , a further optional heat recovery means, 243 , a dust removal means, 218 , and a gas exit, 219 .
  • the containment vessel, 211 surrounds a bed of granules, 220 , fluidized by gas bubbles, 221 , and slugs, 240 , and having an average top level, 222 , above which some granules, 223 , thrown up above the bed describe arcs as they rise from random impact within the bed then fall under gravity in a reduced disengaging space, 224 , while some granules, 236 , and the small entrained dust particles, 225 , continue up and leave with the effluent gas, 233 , through the gas/dust/granular mixture exit, 216 , the connecting means, 241 , and into the gas/granular separator means, 230 , where the granules are removed via the granular removal means, 231 .
  • the average top level, 222 is very close to the gas/dust/granular mixture exit, 216 , and consequently some of the product granules, 236 , thrown up above the bed do not describe arcs as they rise then fall under gravity in the disengaging space, 224 , but continue with the entrained dust, 225 , out the gas/dust/granular mixture exit, 216 . Since the average bed level, 222 , is closer to the exit, 216 , the bed level, 222 , can be taller and/or the overall height, 244 , can be shorter compared to the prior art as shown in FIG. 1 .
  • FIG. 2 b there is shown in detail the various mechanisms which cause the product granules, 236 , to be carried out the gas exit, 216 .
  • the basic mechanism is the random ejection of product granules, 236 , from the top of the bed, 222 , and the pneumatic conveying of these granules out the gas/dust/granular exit, 216 .
  • the bed level oscillates up and down due to the formation of gas slugs, 240 , which lift sections of the bed up to the high level, 232 , until they break through and the bed level recedes to the low level, 234 . It is also possible for the bed to reach extra high levels, 235 , where the bed is above the exit briefly.
  • the exit tube, 241 can be attached to the exit, 216 , at 90° as shown or sloped above or below the horizontal. The angle chosen can be determined by the application of standard pneumatic conveying calculations using the gas velocity in the exit tube, 241 .
  • FIG. 3 there is shown a more detailed schematic of a product separator, 330 , with an integrated heat recovery system, 301 , suitable for high temperature and high purity applications.
  • the gas/dust/granular mixture, 333 enters the product separator, 330 , through an inlet, 357 , which goes through the heat recovery system, 301 , via a penetration, 358 ; the gas and dust, 356 , then separate to the top and exit via the exit tube, 329 , while the granules, 336 , separate to the bottom exit, 331 , where it is fluidized by a purge stream, 359 , and withdrawn as needed.
  • the heat recovery system, 301 is comprised of a heat transfer fluid, 360 , contained in a container, 351 , which is shaped to capture heat, 350 , from the wall of the product separator and has an inlet, 354 , and an outlet, 355 , for the heat transfer fluid, 360 .
  • the container can use various heat transfer fluids such as water or hot oil. It is usually advantageous for the container to be a pressure vessel to permit heat recovery at higher temperatures.
  • the heat may be transferred from the wall to the container by radiation, conduction or convection and well-known heat transfer techniques can be used to enhance the heat transfer from the gas and solids to the wall. Similarly, well-known gas-solids removal techniques, such as cyclones or filters, can be used to enhance the gas-solids separation.
  • the heat is transferred by radiation from the hot surface of the product separator to a pressurized container which has water, 352 , coming in through the inlet, 354 , and steam, 353 , leaving through the exit, 355 .
  • FIG. 2 An example using FIG. 2 would be as follows.
  • the diameter of the container is 300 mm
  • the overall height of the liner, 244 is 7 meters
  • the average bed level, 222 is 6 meters
  • the high level is about 6.6 meters
  • the low level is about 5.4 meters.
  • the gas superficial velocity at the top of the container is 4.7 ft/s (1.4 m/s).
  • the average particle size of the granules is 1 mm and the terminal velocity is 21.8 ft/s (6.56 m/s).
  • the particle terminal velocity is thus about 4 times the superficial gas velocity. This means that in order to carry the granules out of the reactor, the local velocity in areas just above the bed must have local surges where it is 4 times higher than average.
  • Velocity surges of this magnitude occur close to the top of the bed at about 20 cm above the bed.
  • the slug, 240 has a maximum length of about 1.2 meter, and so the periodic growth and bursting of the slug provides the variation in height of 1.2 meters between low and high level. As the slug bursts, it also accelerates the granular particles which are. then entrained out of the reactor. Thus the granular removal varies with the pulsing of the slugs, 240
  • the granules and gas at the bottom of the reactor are at 700° C., then are heated up and leave the reactor as stream, 233 , via exit, 216 , at a temperature of 800° C. They enter the cyclonic product separator, 230 , through a tangential inlet which forces the gas and solids to the wall of the vessel to improve gas to wall heat transfer.
  • the diameter of the cyclone is 10 inches (250 mm) and the length is 6 ft (1.8 m). This is longer than needed for solely the solids removal in order to provide sufficient surface area for heat transfer.
  • the gas and granules both leave at 600° C.
  • the dust/gas separator, 217 is of a similar size but only removes about half the heat because of the reduction in the temperature difference. The gas and dust then leave the dust/gas separator at 500° C. Both heat recovery systems recover the heat as 150 psig steam, which is a standard utility useful in the facility for a variety of purposes and thus always in demand.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
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  • Silicon Compounds (AREA)
US11/810,422 2007-06-04 2007-06-04 Apparatus and method for top removal of granular material from a fluidized bed deposition reactor Abandoned US20080299015A1 (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
US11/810,422 US20080299015A1 (en) 2007-06-04 2007-06-04 Apparatus and method for top removal of granular material from a fluidized bed deposition reactor
PCT/US2008/008569 WO2008150552A2 (en) 2007-06-04 2008-07-10 Apparatus and method for top removal of granular from a fluidized bed deposition reactor
EP08780156.9A EP2167227B1 (en) 2007-06-04 2008-07-10 Apparatus and method for top removal of granular from a fluidized bed deposition reactor
JP2010511225A JP2011527625A (ja) 2007-06-04 2008-07-10 流動床析出からの粒状微細物質の上方取り出しのための器械と方法
KR1020107000046A KR101534879B1 (ko) 2007-06-04 2008-07-10 유동층 증착 반응기로부터 과립상 및 미세 물질의 상부 제거를 위한 장치 및 방법
AU2008260467A AU2008260467B2 (en) 2007-06-04 2008-07-10 Apparatus and method for top removal of granular and fine material from a fluidized bed deposition reactor
CN200880018753.8A CN101743057B (zh) 2007-06-04 2008-07-10 从流化床沉积反应器顶部移除颗粒物质的装置和方法
TW097143379A TWI387484B (zh) 2007-06-04 2008-11-10 用於從流體化床沉積反應器上方移除顆粒材料之裝置及方法
US12/647,283 US8703087B2 (en) 2007-06-04 2009-12-24 Apparatus and method for top removal of granular material from a fluidized bed deposition reactor

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US12/647,283 Expired - Fee Related US8703087B2 (en) 2007-06-04 2009-12-24 Apparatus and method for top removal of granular material from a fluidized bed deposition reactor

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EP (1) EP2167227B1 (enExample)
JP (1) JP2011527625A (enExample)
KR (1) KR101534879B1 (enExample)
CN (1) CN101743057B (enExample)
AU (1) AU2008260467B2 (enExample)
TW (1) TWI387484B (enExample)
WO (1) WO2008150552A2 (enExample)

Cited By (3)

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US20110117729A1 (en) * 2009-11-18 2011-05-19 Rec Silicon Inc Fluid bed reactor
US8535614B2 (en) 2008-09-16 2013-09-17 Sunnyside Technologies, Inc. Reactor and method for producing high-purity granular silicon
US8875728B2 (en) 2012-07-12 2014-11-04 Siliken Chemicals, S.L. Cooled gas distribution plate, thermal bridge breaking system, and related methods

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JP2014205145A (ja) * 2014-06-23 2014-10-30 ロード・リミテッド・エルピー 流動床析出からの粒状微細物質の上方取り出しのための器械と方法
US9404177B2 (en) * 2014-08-18 2016-08-02 Rec Silicon Inc Obstructing member for a fluidized bed reactor

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US20070040056A1 (en) * 2005-08-18 2007-02-22 Wacker Chemie Ag Process and apparatus for comminuting silicon

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US4642227A (en) * 1982-08-20 1987-02-10 California Institute Of Technology Reactor for producing large particles of materials from gases
US5876793A (en) * 1996-02-21 1999-03-02 Ultramet Fine powders and method for manufacturing
US20070040056A1 (en) * 2005-08-18 2007-02-22 Wacker Chemie Ag Process and apparatus for comminuting silicon
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Publication number Priority date Publication date Assignee Title
US8535614B2 (en) 2008-09-16 2013-09-17 Sunnyside Technologies, Inc. Reactor and method for producing high-purity granular silicon
US10576438B2 (en) 2008-09-16 2020-03-03 Xi Chu System for producing high-purity granular silicon
US20110117729A1 (en) * 2009-11-18 2011-05-19 Rec Silicon Inc Fluid bed reactor
US8075692B2 (en) 2009-11-18 2011-12-13 Rec Silicon Inc Fluid bed reactor
US9023425B2 (en) 2009-11-18 2015-05-05 Rec Silicon Inc Fluid bed reactor
US8875728B2 (en) 2012-07-12 2014-11-04 Siliken Chemicals, S.L. Cooled gas distribution plate, thermal bridge breaking system, and related methods

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AU2008260467B2 (en) 2012-07-19
JP2011527625A (ja) 2011-11-04
AU2008260467A1 (en) 2008-12-11
KR20110031270A (ko) 2011-03-25
EP2167227A2 (en) 2010-03-31
TW201018526A (en) 2010-05-16
WO2008150552A3 (en) 2009-03-12
US8703087B2 (en) 2014-04-22
CN101743057A (zh) 2010-06-16
EP2167227B1 (en) 2016-03-02
EP2167227A4 (en) 2012-10-10
KR101534879B1 (ko) 2015-07-07
WO2008150552A8 (en) 2010-01-14
US20100098850A1 (en) 2010-04-22
TWI387484B (zh) 2013-03-01
CN101743057B (zh) 2014-01-01
WO2008150552A2 (en) 2008-12-11

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