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`[19]
`United States Patent
`5,871,618
`[11] Patent Number:
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`[45] Date of Patent: Feb. 16, 1999
`Lee et al.
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`U8005871618A
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`FOREIGN PATENT DOCUMENTS
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`C10VI 175/00
`3/1990 European Pat. Off.
`0 360 500
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`C10VI 175/00
`6/1990 European Pat. Off.
`0 372 276
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`10/1987 Germany ................... .. C10VI 175/02
`37 03 110 A1
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`9/1992 Germany
`..... .. C10G 9/42
`41 07 294 A1
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`4/1995 Germany
`C10G 55/06
`43 35 399 A1
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`8/1995 Germany
`C10G 15/08
`44 05 109 A1
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`2/1987
`C10VI 175/00
`62—36497
`Japan
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`1—268794
`Japan ......................... .. C10VI 175/00
`10/1989
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`2 274 850
`8/1994 United Kingdom ........... .. C10G 1/04
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`WO 92/22624 12/1992 WIPO ........................ .. C10VI 175/00
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`WO 92/22625
`C10VI 175/00
`12/1992
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`WO 94/07798
`C10VI 175/00
`4/1994
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`WO 95/14749
`6/1995 WIPO ............................. .. C10L 1/08
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`WO
`95/365356
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`12/1995 WIPO ........................ .. C10VI 175/00
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`Primary Examiner—Bekir L. Yildirim
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`Attorney, Agent, or Firm—Tilton, Fallon, Lungmus &
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`Chestnut
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`[57]
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`ABSTRACT
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`[54] APPARATUS FOR RECLAIMING FUEL OIL
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`FROM WASTE OIL
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`[76]
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`Inventors: Sung Rae Lee, 8-406 Kwang-Jang Apt,
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`28 Youido-Dong, Youngdeungpo-Ku,
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`Seoul, Rep. of Korea; Henry Kong,
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`1412-102 Avenue NW., Edmonton,
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`Alberta, Canada, T5K 0P9; Roy B.
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`Jefi'ries, Box 4, Site 5, RR. #1,
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`Cochrane, Alberta, Canada, TOL 0W0;
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`Norman L. Arrison; Wlodzimierz P.
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`Rzazewski, both of 11412-102 Avenue
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`NW., Edmonton, Alberta, Canada, T5K
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`0P9
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`[22]
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`[30]
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`[21] Appl. No.: 785,591
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`Filed:
`Jan. 16, 1997
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`Foreign Application Priority Data
`Aug. 28, 1996
`[KR]
`Rep. of Korea ................ .. 1996 35929
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`[51]
`Int. C1.6 ....................... .. C10M 175/00, C10G 57/00
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`[52] U.S. Cl.
`........................... .. 196/46.1; 196/46; 196/98;
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`202/84; 208/179
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`[58] Field of Search ............................. .. 196/46, 46.1, 98,
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`196/116, 139, 208/179, 181, 182, 184,
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`186; 202/84; 422/187
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`[56]
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`References Cited
`
`
`U.S. PATENT DOCUMENTS
`
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`
`4,073,719
`.................... .. 208/180
`2/1978 Whisman et a1.
`
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`
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`8/1992 Martin et a1.
`208/184
`5,141,628
`
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`
`
`7/1993 Brownawell
`.......................... .. 210/690
`5,225,081
`
`
`
`
`5,271,808 12/1993 Shurtleff .
`2/1994 Shurtleff .
`5,286,349
`
`
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`4/1994 Harrison et a1.
`5,306,419
`.
`
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`
`
`5,527,449
`6/1996 Brown et al.
`......................... .. 208/179
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`Disclosed is an apparatus and a process for reclaiming fuel
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`oil from waste oil. The apparatus comprises a thermal
`
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`cracking unit for cracking the high boiling hydrocarbon
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`material into lighter, lower boiling, material so as to separate
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`hydrocarbon vapor products from viscous materials; a
`
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`condenser/heat exchanger for condensing the hydrocarbon
`vapor products to the liquid state; a fuel stabilization unit for
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`chemically treating the condensates so as to give a oil
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`product and solid sediment; and a polishing unit for forming
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`a high quality fuel oil by physically removing solid con-
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`taminants. According to the present invention, high quality
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`fuel oil can be obtained together With an environmentally
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`innocuous solid ash cake, through a simple and efficient
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`process.
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`8 Claims, 14 Drawing Sheets
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`UTC-2007.001
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`GE v. UTC
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`Trial IPR2016-01301
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`UTC-2007.001
`
`GE v. UTC
`Trial IPR2016-01301
`
`

`

`US. Patent
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`Feb. 16, 1999
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`Sheet 1 0f 14
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`5,871,618
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`
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`o5
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`.52most
`_.#59“.
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`A.
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`on
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`on
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`UTC-2007.002
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`UTC-2007.002
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`

`

`US. Patent
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`Feb. 16, 1999
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`Sheet 2 0f 14
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`5,871,618
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`NNanci
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`UTC-2007.003
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`

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`US. Patent
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`Feb. 16, 1999
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`Sheet 3 0f 14
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`5,871,618
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`FIGURE3
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`UTC-2007.004
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`UTC-2007.004
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`

`

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`US. Patent
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`Feb. 16, 1999
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`Sheet 4 0f 14
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`5,871,618
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`HGUREAB
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`UTC-2007.005
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`UTC-2007.005
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`

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`US. Patent
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`Feb. 16, 1999
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`Sheet 5 0f 14
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`5,871,618
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`FIGURESB
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`US. Patent
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`Feb. 16, 1999
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`Sheet 6 0f 14
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`5,871,618
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`US. Patent
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`Feb. 16, 1999
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`Sheet 8 0f 14
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`5,871,618
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`UTC-2007.009
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`FIGURE8
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`US. Patent
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`Feb. 16, 1999
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`Sheet 9 0f 14
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`>4
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`FIGURE9
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`UTC-2007.010
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`UTC-2007.010
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`US. Patent
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`Feb. 16, 1999
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`Sheet 10 0f 14
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`5,871,618
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`FIGURE10
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`UTC-2007.011
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`US. Patent
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`Feb. 16, 1999
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`Sheet 11 0f 14
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`5,871,618
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`FIGURE11
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`UTC-2007.012
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`US. Patent
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`Feb. 16, 1999
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`Sheet 12 0f 14
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`5,871,618
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`US. Patent
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`Feb. 16, 1999
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`Sheet 13 0f 14
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`5,871,618
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`905
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`FIGURE13
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`US. Patent
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`Feb. 16, 1999
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`Sheet 14 0f 14
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`
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`5,871,618
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`1
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`APPARATUS FOR RECLAIMING FUEL OIL
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`FROM WASTE OIL
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`BACKGROUND OF THE INVENTION
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`invention relates to an apparatus and a
`The present
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`process for reclaiming fuel oil from waste oil, and more
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`particularly,
`to an apparatus and a process for turning
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`environmentally hazardous waste lubricating oil into a high
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`quality diesel engine fuel oil together with a relatively small
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`amount of environmentally innocuous solid petroleum coke.
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`Waste lubricating oils are defined here as any lubricating
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`oil such as engine oil, metal cutting oils and hydraulic oils.
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`Lubricating oil is usually produced from a certain boiling
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`range(typically 300 to 500 degrees Celsius) cut of conven-
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`tional crude oil. This material
`is usually called “Bright
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`stoc ” and accounts for about 70% to 80% of typical
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`lubricating oil. The remainder consists of various additives
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`and they tend to be polymeric in nature.
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`Lubricating oils, while performing their job, ultimately
`deteriorate in their ability to satisfactorily perform any
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`longer and have to be periodically changed out. While
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`performing their job they pick up dirt and heavy metals both
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`from the metal parts of the engine and from the fuels used
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`in the engines and a typical used oil may contain significant
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`quantities of chromium, cadmium, zinc, and lead. Break
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`down of the hydrocarbons making up the lubricating oil can
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`also result in lower boiling point material being present.
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`Handling of the used oil after removal from the engine can
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`result in light solvents being added to it along with signifi-
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`cant quantities of water.
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`Therefore, used lubricating oils are environmentally haz-
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`ardous and have to be treated accordingly.
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`The apparatus for reclaiming useful oil products from
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`waste oil is described in, for example, US. Pat. No. 5,286,
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`349 and US. Pat. No. 5,271,808. In the apparatus described
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`in the above patents, a similar means of using a conventional
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`kettle type boiler is used for recovering some of the material
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`being boiled in the pot.
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`FIG. 1 is a partial diagrammatic view showing a part of
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`the conventional apparatus for reclaiming a useful oil from
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`waste oil.
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`Referring to the FIG. 1, the conventional apparatus 70 for
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`reclaiming a useful oil product from a waste oil comprises
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`an evaporator 80 and a condenser or heat exchanger 80. The
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`evaporator 80 has an evaporation chamber 82 including an
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`inlet for the waste oil, and an outlet for vaporized oil.
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`In the aforementioned patents, the lighter boiling compo-
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`nents are distilled off and condensed. In the process, a
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`significant amount of heavy material is carried over and
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`requires a second independent distillation in an apparatus
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`that is protected under US. Pat. No. 5,271,808. All of these
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`patents are quite specific to the design details of the specific
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`piece of machinery. They include fine detail on the con-
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`struction of the equipment and control strategy. The vessel
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`used for the cracking pot is rectangular in shape and does not
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`have the ability to expand and contract without permanent
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`deformation and does not produce a high quality product.
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`Nor does it have the capability of controlling the boiling
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`range of the product. As produced the fuel is not acceptable
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`to a typical diesel engine,
`it requires significant refining
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`before it can be so.
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`SUMMARY OF THE INVENTION
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`To solve the above problems, it is a first object of the
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`present invention to provide an apparatus and for reclaiming
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`10
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`15
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`20
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`25
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`30
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`35
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`45
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`50
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`55
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`60
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`65
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`2
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`fuel oil from waste oil which allows the production of a high
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`quality diesel
`type fuel oil from waste lubricating oils,
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`through a simple and efficient way.
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`It is a second object of the present invention to provide a
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`process for reclaiming environmentally innocuous fuel oil
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`from waste oil by using the above apparatus for reclaiming
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`fuel oil from waste oil.
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`To achieve the first object, there is provided an apparatus
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`for reclaiming fuel oil from waste oil, comprising: a thermal
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`cracking unit for cracking the high boiling hydrocarbon
`material into lighter, lower boiling, material so as to separate
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`hydrocarbon vapor products from viscous materials; a
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`condenser/heat exchanger for condensing the hydrocarbon
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`vapor products to the liquid state; a fuel stabilization unit for
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`chemically treating the condensates so as to give a oil
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`product and solid sediment; and a polishing unit for forming
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`a high quality fuel oil by physically removing solid con-
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`taminants.
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`It is preferred in the present invention that the thermal
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`cracking unit
`includes a cracking vessel having a “U”
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`shaped vertical section.
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`It is preferred in the present invention that the thermal
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`cracking unit includes a dephlegmator for controlling the
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`boiling range of the cracked material.
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`It is preferred in the present invention that the apparatus
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`for reclaiming fuel oil from waste oil according to the
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`present invention further comprises a flare system for burn-
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`ing gases and noncondensable vapors taken from said
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`condenser/heat exchanger.
`the fuel
`invention that
`is preferred in the present
`It
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`stabilization unit has a settling tank for separating said solid
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`sediment.
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`It is preferred in the present invention that the polishing
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`unit has a centrifugation unit for removing solid contami-
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`nants and water remaining in oil, and a filtration unit for
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`filtering the centrifuged oil to form a high quality fuel.
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`It is preferred in the present invention that the filtration
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`unit is filled with the attapulgite clay.
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`It is preferred in the present invention that the apparatus
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`for reclaiming fuel oil from waste oil according to the
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`present invention further comprises a distillation unit for
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`controlling the boiling range of said high quality fuel.
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`It is preferred in the present invention that the apparatus
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`for reclaiming fuel oil from waste oil according to the
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`present invention further comprises a cocking unit for form-
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`ing an ash cake by thermally treating the viscous materials
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`obtained from said thermal cracking unit.
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`To achieve the second object, there is also provided a
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`process for reclaiming fuel oil from waste oil, comprising
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`the steps of: thermally cracking waste oil in the range of 380
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`to 420 degrees Celsius to separate hydrocarbon vapor prod-
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`ucts from viscous materials; forming a liquid condensates by
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`condensing the hydrocarbon vapor products; chemically
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`treating the liquid condensates to give a oil product and solid
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`sediment; and forming a fuel oil by physically removing
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`solid contaminants from the oil product.
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`It is preferred that the step of thermally cracking waste oil
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`comprises the step of controlling the boiling range of the
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`hydrocarbon vapor products obtained by cracking, by using
`a dephlegmator.
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`It is preferred that the step of controlling the boiling range
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`of the hydrocarbon vapor products comprises the step of
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`controlling the outlet temperature from the dephlegmator in
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`the range of 250 to 280 degrees Celsius.
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`It is preferred that the step of forming a liquid condensates
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`comprises the step of condensing the hydrocarbon vapor
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`products by using an air cooled condensing heat exchanger.
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`UTC-2007.016
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`UTC-2007.016
`
`

`

`
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`5,871,618
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`
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`3
`It is preferred that the step of forming a liquid condensates
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`comprises the step of controlling the flash point temperature
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`in the heat exchanger to recover separated liquid conden-
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`sates according to their boiling point.
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`It is preferred that the step of chemically treating the
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`liquid condensates comprises the step of diluting the liquid
`condensates with an antioxidant to form a mixture having a
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`predetermined concentration of the antioxidant, and settling
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`solids contained in the mixture by holding up the mixture for
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`a predetermined period.
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`It is preferred that the anti oxidant is dimethyl formamid,
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`and the concentration of the antioxidant is between 0.025
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`and 0.035 percent on an volume basis.
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`It is preferred that the step of forming a fuel oil by
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`physically removing solid contaminants from the oil product
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`comprises the step of removing solid contaminants and
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`water remaining in the oil by centrifuging the oil, and
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`filtering the centrifuged oil by using a filtration medium.
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`It is preferred that the filtration medium is an attapulgite
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`clay of 50 to 60 mesh particle size.
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`It is preferred that the process according to the present
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`invention further comprises the step of controlling the
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`boiling range of the fuel oil by distillating the fuel oil, after
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`the step of forming the fuel oil.
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`It is preferred that the step of thermally cracking waste oil
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`comprises the step of forming an ash cake by thermally
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`treating the viscous materials.
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`BRIEF DESCRIPTION OF THE DRAWINGS
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`The above objects and advantages of the present invention
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`will become more apparent by describing in detail a pre-
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`ferred embodiment thereof with reference to the attached
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`drawings in which:
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`FIG. 1 is a partial diagrammatic view showing a part of
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`the conventional apparatus for reclaiming a useful oil from
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`waste oil.
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`FIG. 2 is a simplified flowsheet of the process to produce
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`a high quality diesel engine fuel according to the preferred
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`embodiment of the present invention.
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`FIG. 3 is a schematic configuration of the thermal crack-
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`ing unit of the present invention.
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`FIGS. 4A and 4B are cross sectional views of a cracking
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`vessel which can be employed in the present invention.
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`FIGS. 5A and 5B are cross sectional views of another
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`cracking vessel which can be employed in the present
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`invention.
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`FIGS. 6A and 6B are simplified drawings of the dephleg-
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`mator.
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`FIG. 7 is a simplified drawing of the air cooled condenser/
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`heat exchanger of the present invention, including the means
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`to split the diesel and light fuels.
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`FIG. 8 is a flowsheet of the enclosed flare system which
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`can be employed in the present invention.
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`FIG. 9 is simplified flowsheets for the fuel stabilization
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`system of the present invention, which includes two tanks
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`for stabilization for short term storage.
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`FIG. 10 is simplified flowsheets for the fuel stabilization
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`system of the present invention, which includes two tanks
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`for stabilization for long term storage.
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`FIG. 11 is a schematic view of the final filtration unit of
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`the present invention.
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`FIG. 12 is a schematic view of the optional final distil-
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`lation system which can be employed in the present inven-
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`tion.
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`10
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`15
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`20
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`25
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`30
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`35
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`40
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`45
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`50
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`55
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`60
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`65
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`4
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`FIG. 13 is a schematic view of the conventional coking
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`system.
`FIG. 14 is a typical time versus temperature curve for a
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`production cycle.
`DETAILED DESCRIPTION OF THE
`
`
`INVENTION
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`The apparatus for reclaiming fuel oil from waste oil
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`according to the present invention is designed to process a
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`feedstock of any used lubricating oil such as motor oil,
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`cutting oil or hydraulic oil into automotive fuels such as
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`gasoline and diesel fuel. The prime product being a high
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`quality diesel fuel that can be directly used in on-road or
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`industrial diesel engines. The process using the present
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`apparatus essentially consists of the following three parts:
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`(a) a semi-continuous thermal cracking process; (b) a sta-
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`bilization process of the product oil including stabilization
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`for short term storage and stabilization for long term storage;
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`and (c) the final polishing process. As an additive process,
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`(d) the final distillation process and (e) the external coking
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`process may be included.
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`The semi-continuous thermal cracking process according
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`to the present invention, the used lubricating oils are ther-
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`mally cracked into lighter material at elevated temperature
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`on a continuous basis until the build up of solid-like material
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`in the cracking vessel reaches a critical point. The vaporized
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`lighter fractions are condensed and stored at conditions
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`which are chosen to be optimum for the second part of the
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`process. The remaining heavy material that would not crack
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`and vaporize during the continuous portion of the process is
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`treated in a batchwise manner where it is heated to a much
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`higher temperature and turned into a coke-like material that
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`contains excess carbon, the solid residues, and the heavy
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`metals that were present in the original used oil. The coke is
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`removed from the cracking vessel and can be safety land-
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`filled. The coke has shown to be innocuous to the environ-
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`ment inasmuch as the tendency to leach the heavy metals
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`from the structure is very low. Provision is also made in the
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`thermal cracking vessel to extract this very high boiling
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`material such that it can be cocked in an external apparatus
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`thus making the operation of the thermal cracking process
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`much closer to a continuous operation. It is this external
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`coking apparatus that have been defined as the fifth part of
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`the present process. The offgas produced during the cracking
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`process is combusted in a flare system that is included in the
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`design. The combusted offgas has been shown to be accept-
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`able by meeting typical environmental standards.
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`According to the second feature of the present invention,
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`the second part of the process stabilizes the cracked products
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`from the first part of the process by chemically treating them
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`such that olefinic materials are polymerized or alternatively
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`treated such that the polymerization reaction is temporarily
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`relayed. The choice of whether to perform one or the other
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`of these processes is a function of whether or not the fuel
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`will be used quickly after being treated. Some of this
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`material is solid in nature and is separated out in this part of
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`the process. This second part of the process is batchwise in
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`nature.
`
`The third part of the process consists of a filtration
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`technique that takes advantage of the surface active prop-
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`erties of an activated attapulgite clay. The activated clay is
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`used to remove the very small amount of tar-like material
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`that is carried over from the thermal cracking vessel together
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`with any remaining solid material that precipitated during
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`the chemical treatment from part two of this oil treating
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`process. Attapulgite clays have been used for many years in
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`
`UTC-2007.017
`
`UTC-2007.017
`
`

`

`5,871,618
`
`
`
`5
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`the fuel oil improving the color of diesel fuels and have the
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`
`
`property of removing the larger molecules from the liquid
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`passed through it. Hence, the removal of the tar and reacted
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`olefinic material.
`
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`The fourth part of the process is a standard distillation that
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`separates the product from the previous treatment into the
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`correct boiling ranges required for use as motor gasoline and
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`fuel. The heavier material
`that falls outside the
`diesel
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`maximum for the diesel fuel
`is returned to the original
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`cracking vessel where it is treated again. However, this part
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`of the process is only necessary if a very strict control on the
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`boiling range of the product
`is necessary. The primary
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`thermal cracking process is capable of some significant
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`degree of control of the quality of the product fuel without
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`the need to use a separate distillation step. This control is
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`done by limiting the maximum temperature of the produced
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`fluids from the cracking vessel and by separating the light
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`and heavier fuels within the product condenser.
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`The products from this process, then, are diesel fuel that
`
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`can be directly used as fuel in a diesel engine amounting to
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`about 90% of the original feed, about 10% material falling
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`in the gasoline boiling range that can be added to a typical
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`refinery gasoline pool or used to fuel the cracking vessel
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`burners, a small amount of gasified material which is com-
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`busted in the flare system, and a solid coke-like material that
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`can readily be landfilled. Because the process is based upon
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`the thermal cracking of heavy hydrocarbons into lighter
`ones, there is an actual increase in the volume of the liquid
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`products compared to the feed, although, of course,
`the
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`weight of the product fractions equal the weight of the feed
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`material.
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`The configuration of the apparatus for reclaiming fuel oil
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`from waste oil according to the preferred embodiment of the
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`present
`invention will now be described in detail with
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`reference to the drawings.
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`FIG. 2 shows a flowsheet of the units that make up the
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`process required for this invention to produce a high quality
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`diesel fuel oil from waste lubricating oil. In FIG. 2,
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`reference number “1” is a thermal cracking unit, the refer-
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`ence number “2” is a dephlegmator which is mounted
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`directly on top of the cracking vessel 101. The vapors from
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`the dephlegmator 2 pass to a condenser/heat exchanger 3.
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`Non-condensable gases and vapors flow to a enclosed flare
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`system 4. The product fuel flows from the heat exchanger 3
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`to a stabilization system 5. The final polishing operation is
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`accomplished by a centrifuge 6 and a filtration unit 7. an
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`optional final distillation system 8 and an optional external
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`coking system 9 may be included in the apparatus according
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`to the present invention.
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`FIG. 3 shows the schematic configuration of the thermal
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`cracking unit 1 of the present apparatus for reclaiming fuel
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`oil from waste oil. Referring to FIG. 3, a cracking vessel 101
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`is fabricated from either 316L or 321L stainless steel or the
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`equivalent specification. These materials are chosen because
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`they give the best weldability and because they produce a
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`minimum expansion. The bottom 102 and the side walls 105
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`of the vessel 101 are all butt welded for maximum strength
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`and flexibility. The vessel bottom 102 can be either 16 or 18
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`mm thick and has a very shallow dished surrounding portion
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`103 and the central flat surface 104. Thus,
`the cracking
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`vessel 101 has a generally “U” shaped vertical section.
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`FIGS. 4A and 4B show an example of the cracking vessel
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`that can be employed in the present apparatus. FIG. 4A is the
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`vertical sectional view and FIG. 4B is the horizontal sec-
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`tional view.
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`As shown in FIGS. 4A and 4B, in case of the 5,000 ton
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`per year unit, the bottom 102 of the cracking vessel 101Ahas
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`10
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`a generally elliptical shape, and is 5,000 mm long by 2,600
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`mm wide and 2,250 mm high. The vertical side walls 105 of
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`the cracking vessel 105 are welded to the bottom 102 by
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`means of butt welds, thus forming a deep bathtub or “U”
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`shape. The side walls 105 are 12 to 14 mm thick. The lid 106
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`is placed on the top of the cracking vessel 101A and welded
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`in place by fillet welds.
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`FIGS. 5A and 5B show another example of the cracking
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`vessel that can be employed in the present apparatus. FIG.
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`5A is the vertical sectional view and FIG. 5B is the hori-
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`zontal sectional view.
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`As sown in FIGS. 5A and 5B, in case of the special case
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`such as the smaller 2,500 ton per year unit, the bottom 102
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`of the cracking vessel 101B is circular in shape, and is
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`fabricated from a single shallow dished end also 16 or 18
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`mm thick and 2,800 mm diameter.
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`In either case, each of the cracking vessels 101, 101A,
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`101B is contained within a combustion chamber 108 of
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`height 1,000 mm containing plurality of burners. For
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`example, in case of FIGS. 4A and 4B, 6 burners 109 are
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`contained (only 2 burners are shown), and in case of FIGS.
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`5A and 5B, 3 burners 110 are contained (only 2 burners are
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`shown). Each of the burners 109 or 110 has a heat generating
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`capacity of 350,000 kJ per hour and can be fired with either
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`natural gas or fuel oil. There are also an equivalent number
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`of thermocouples T1 permanently installed in the combus-
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`tion chamber 108 which are used to assist in the control of
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`the burner firing sequence.
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`In FIGS. 3, 4A, 4B, 5A and 5B, the exhaust gases from the
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`combustion chamber 108 are led from the chamber along a
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`series of stainless steel ducts 112 that are an integral part of
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`the cracking vessel
`to the exhaust chimney 113 that
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`mounted on top of a housing 114 containing the cracking
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`vessel 101. The housing 114 is fabricated in two parts such
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`that the top portion can be removed with ease to perform
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`maintenance on the stainless steel cracking vessel 101
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`contained within. The vessels 101, 101A or 101B can be
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`lifted out of the bottom portion of the housing 114 that
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`contains the combustion chamber 108 for maintenance.
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`The cracking vessel 101 has inlet pipes(nor shown) for the
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`feed oil 115, for the level transmit