US3347775A - Separation of waxy hydrocarbons from oils by flotation - Google Patents

Separation of waxy hydrocarbons from oils by flotation Download PDF

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Publication number
US3347775A
US3347775A US432960A US43296065A US3347775A US 3347775 A US3347775 A US 3347775A US 432960 A US432960 A US 432960A US 43296065 A US43296065 A US 43296065A US 3347775 A US3347775 A US 3347775A
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US
United States
Prior art keywords
oil
flotation
fresh
waxy
flotation zone
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.)
Expired - Lifetime
Application number
US432960A
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English (en)
Inventor
Tritsmans Paul Albert
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.)
BELGE PETROLES SA
INDUSTRIELLE BELGE DES PETROLES S A Ste
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BELGE PETROLES SA
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 BELGE PETROLES SA filed Critical BELGE PETROLES SA
Application granted granted Critical
Publication of US3347775A publication Critical patent/US3347775A/en
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Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/14—Flotation machines
    • B03D1/1443—Feed or discharge mechanisms for flotation tanks
    • B03D1/1462—Discharge mechanisms for the froth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/14—Flotation machines
    • B03D1/1443—Feed or discharge mechanisms for flotation tanks
    • B03D1/1475—Flotation tanks having means for discharging the pulp, e.g. as a bleed stream
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/14—Flotation machines
    • B03D1/24—Pneumatic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/14—Flotation machines
    • B03D1/24—Pneumatic
    • B03D1/247—Mixing gas and slurry in a device separate from the flotation tank, i.e. reactor-separator type
    • 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
    • C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
    • 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
    • C10G73/00—Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/02—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils
    • C10G73/26—Recovery of petroleum waxes from hydrocarbon oils; Dewaxing of hydrocarbon oils by flotation
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/04—Wing frames not characterised by the manner of movement
    • E06B3/06—Single frames
    • E06B3/08—Constructions depending on the use of specified materials
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/04—Wing frames not characterised by the manner of movement
    • E06B3/06—Single frames
    • E06B3/08—Constructions depending on the use of specified materials
    • E06B3/12—Constructions depending on the use of specified materials of metal
    • E06B3/14—Constructions depending on the use of specified materials of metal of special cross-section
    • E06B3/16—Hollow frames of special construction, e.g. made of folded sheet metal or of two or more section parts connected together
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; Specified applications
    • B03D2203/005—Fine and commodity chemicals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; Specified applications
    • B03D2203/006—Oil well fluids, oil sands, bitumen

Definitions

  • the present invention therefore, provides a simple alternative method of cooling the oil in a wax flotation process.
  • a process for the separation of waxy hydrocarbons from oil by flotation in which gas is passed upwardly through the oil cooled to a temperature below its cloud point is characterised in that fresh oil is fed to the flotation zone at a temperature above its cloud point, and that the fresh oil is cooled by withdrawing a stream of oil from the Zone, cooling this stream and recycling it to the zone, the ratio of recycled oil to fresh oil being at least 5:1, preferably :1.
  • coolers can be arranged in parallel, with means for feeding the oil to all or any of the coolers. In this way one or more coolers can be taken off stream for cleaning without shutting down the whole plant. Cleaning can be carried out simply and easily by warming the cooler with for example warm oil.
  • coolers for the recycle oil can be of any convenient type.
  • suitable coolers is tubular heat ex- 3,347,775 Patented Oct. 17, 1967 changers.
  • coolant is not critical; liquefied petroleum gases such as liquid propane or butane are convenient coolants.
  • the stream of recycle oil is withdrawn from the flotation zone at a point removed from the fresh oil inlet and preferably also it is withdrawn from the bottom of the zone.
  • the recycle oil may bereturned to the flotation zone via a separate line entering the bath preferably at a point close to the fresh oil inlet.
  • a single recycle and fresh oil line may be used provided this line is not too long, the recycle and fresh oil being then conveniently mixed in or near the'fresh oil and recycle pumps.
  • Dewaxed oil product must clearly be withdrawn in an amount suflicient to keep a constant liquid in the zone and this may conveniently be achieved by bleeding off the required amount from the recycle stream.
  • Wax which collects at the top of the zone is also withdrawn continuously or at intervals.
  • a particularly convenient way of removing the wax froth is by means of an arm extending across the length or breadth of the bath and which traverses along the top of the bath. This may be caused to traverse for example by attaching it to an endless belt. The arm pushes the wax over a weir into a collecting chamber, which may conveniently be thermally insulated from the zone and contain a heating coil. The warmed wax can then be readily withdrawn as a liquid.
  • Waxy hydrocarbons can cause in the kerosine, gas oil and wax to 650 C.
  • the cloud points of the oils being treated may vary over a fairly wide range and hence the flotation temperature may also vary. Likely temperatures will however be in the range 0 F. to F., especially 20 F. to 40 F.
  • the cloud point of the dewaxed oil will with efiicient operation be substantially equal to the temperature used.
  • the amount of gas used is not results have been obtained with a to oil feedstock of as low as 0.2 and with no indication that this is a limiting ratio. Higher rates are not detrimental although they add little further benefit and a suitable range is thus from 0.1 to 10.
  • Any convenient gas may be used, for example nitrogen, gases rich in nitrogen such as flue gas, hydrogen or normally gaseous hydrocarbons. Air is also suitable, but its use may be limited on a commercial scale by safety regulations regarding fire hazard.
  • the gas should naturally pass upwardly through the oil in the form of bubbles and if necessary it can be introduced into the bottom of the flotation bath through known bubblers and dispersers. It has been found, however, that the gas can be introduced quite simply and effectively by injecting it into the suction side of the pump feeding oil to the bath, taking care to obtain a pump discharge pressure between 2 and 10 kg./cm.
  • the rate of flow of the oil into and the withdrawal of dewaxed oil from the flotation zone should be adjusted to give a suitable residence time and these can readily be determined by experiment. In practice residence times of upwards of 7 hours have been found suitable.
  • the flotation zone is a rectangular tank 1 with an oil inlet 2 and outlet 3.
  • Fresh feed is fed into the system at 4 together with gas which is injected through line 5 into the suction side of pump 6.
  • the fresh feed is mixed with a recycle stream described in more detail below and passes via line 7 to the inlet 2.
  • a stream of oil is withdrawn through outlet 3 and line 8. A portion of this stream is bled off through line 9 as dewaxed oil product and the remainder is passed through a series of heat exchangers 10, 11, 12.
  • the oil can be fed to all or any of the exchangers.
  • the oil cooled in the exchangers goes via line 13 to join the fresh feed and flotation gas and hence back to the tank 1 via inlet 2. Pumps are placed in this recycle line as appropriate for example at 25 and 26.
  • the heat exchangers are supplied with coolant via line 14 which again may go to all or any of the exchangers and which is withdrawn via line 15.
  • pipe and valve work may be added to allow a cleaning fluid such as warm oil to pass through any exchanger which has been isolated from the system.
  • the level of oil in the tank is maintained constant by balancing the supply and withdrawal of oil at a level just below that of the weir 16.
  • An endess belt 17 driven by pulleys 18 and 19 has an arm 20 extending across the breadth of the bath.
  • a wax collecting chamber 21 At the end of the bath having the weir is a wax collecting chamber 21 with a heating coil 22 and outlet 23. The side of the bath against the collecting chamber has thermal insulation 24.
  • tank 1 which was 25 metres long, 12 metres broad and 1.5 metres deep was filled with oil at 70 F.
  • the oil was a catalytic cracker cycle oil of 320 to 370 C. boiling range and 50 centistokes viscosity at 32 F. diluted with straight run kerosine to give an oil of 13 centistokes viscosity at 32 F., 62 F. cloud point, 60 F. pour point and 170 to 370 C. boiling range.
  • the oil was then cooled to 30 F. by recycling it via line 8 through heat exchangers 10, 11, 12 and back to the tank via lines 13 and 7. At this initial cooling stage wax deposition in the exchangers may occur and exchangers may be isolated from the system as necessary and cleaned with a separate stream of warm oil.
  • initial start-up may be carried out by filling the settling vessel with kerosine, cooling the kerosine to the required temperature and only then introducing the feed oil.
  • Liquid propane at 20 F. is passed .41 through the other side of the exchangers via lines 14 and 15.
  • the fresh oil feed rate was 10 m. /h., the ratio of recycle oil to fresh oil was 20:1 and the temperature drop of the recycle oil through the exchangers was 2 F.
  • a continuous process for the flotation separation of waxy hydrocarbons from waxy oil to produce dewaxed oil having reduced cloud and pour points which comprises passes fresh waxy oil into a flotation zone at a temperature above its cloud point, withdrawing a portion of oil from said flotation zone at a point remote from the fresh oil inlet of the flotation zone, passing the withdrawn oil through heat exchanger means at a rate of flow to minimize any wax deposition thereon and to cool the withdrawn oil to a temperature at which when recycled for admixture with fresh oil, the resulting mixture will be at a temperature at which wax separation will occur, recycling the cooled oil back to the flotation zone at a point to the fresh oil inlet to cool the oil present therein to a temperature below the cloud point of the oil, the ratio of recycled cool oil to fresh oil into said flotation zone being at least 5:1, passing a flotation gas upwardly through the cooled waxy oil in said flotation zone to separate the mixture into a top waxy froth layer and a bottom dewaxed oil layer, and withdraw

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biotechnology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Lubricants (AREA)
US432960A 1964-08-21 1965-02-16 Separation of waxy hydrocarbons from oils by flotation Expired - Lifetime US3347775A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BE2043901 1964-08-21

Publications (1)

Publication Number Publication Date
US3347775A true US3347775A (en) 1967-10-17

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Application Number Title Priority Date Filing Date
US432960A Expired - Lifetime US3347775A (en) 1964-08-21 1965-02-16 Separation of waxy hydrocarbons from oils by flotation

Country Status (10)

Country Link
US (1) US3347775A (fr)
BE (2) BE652106A (fr)
CH (1) CH478222A (fr)
DE (1) DE1545347A1 (fr)
DK (1) DK120854B (fr)
FR (2) FR1443921A (fr)
GB (1) GB1022430A (fr)
LU (1) LU53778A1 (fr)
NL (2) NL6502144A (fr)
NO (1) NO115407B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4447311A (en) * 1982-07-22 1984-05-08 Mobil Oil Corporation Dewaxing process
US20100236990A1 (en) * 2009-03-17 2010-09-23 James William Gleeson Bubble separation to remove haze and improve filterability of lube base stocks
WO2016083946A3 (fr) * 2014-11-26 2016-08-04 Sabic Global Technologies B.V. Systèmes et procédés pour séparer des produits de cire à partir de produits

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1994485A (en) * 1931-06-20 1935-03-19 Atlantic Refining Co Treatment of oil-wax mixtures
US2314994A (en) * 1940-06-01 1943-03-30 Phillips Petroleum Co Process for dewaxing lubricant stocks
US2370453A (en) * 1942-02-28 1945-02-27 Mid Continent Petroleum Corp Method of separating wax and oil
US2410483A (en) * 1944-11-13 1946-11-05 Mid Continent Petroleum Corp Processes of dewaxing oils
GB734123A (en) * 1951-07-26 1955-07-27 Bataafsche Petroleum Separating solid paraffin wax or a paraffln wax concentrate from oil
US2719817A (en) * 1951-07-26 1955-10-04 Shell Dev Process of dewaxing oils by flotation
US2813074A (en) * 1954-08-23 1957-11-12 Infilco Inc Clarifying apparatus and process
US2880159A (en) * 1955-07-20 1959-03-31 Exxon Research Engineering Co Solvent dewaxing of petroleum oil
US2904496A (en) * 1956-07-25 1959-09-15 Socony Mobil Oil Co Inc Process for separating wax from oils
US2961397A (en) * 1955-12-21 1960-11-22 Sun Oil Co Preventing deposition of wax on equipment during dewaxing by utilizing smooth surface equipment and a surface-active agent

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1994485A (en) * 1931-06-20 1935-03-19 Atlantic Refining Co Treatment of oil-wax mixtures
US2314994A (en) * 1940-06-01 1943-03-30 Phillips Petroleum Co Process for dewaxing lubricant stocks
US2370453A (en) * 1942-02-28 1945-02-27 Mid Continent Petroleum Corp Method of separating wax and oil
US2410483A (en) * 1944-11-13 1946-11-05 Mid Continent Petroleum Corp Processes of dewaxing oils
GB734123A (en) * 1951-07-26 1955-07-27 Bataafsche Petroleum Separating solid paraffin wax or a paraffln wax concentrate from oil
US2719817A (en) * 1951-07-26 1955-10-04 Shell Dev Process of dewaxing oils by flotation
US2813074A (en) * 1954-08-23 1957-11-12 Infilco Inc Clarifying apparatus and process
US2880159A (en) * 1955-07-20 1959-03-31 Exxon Research Engineering Co Solvent dewaxing of petroleum oil
US2961397A (en) * 1955-12-21 1960-11-22 Sun Oil Co Preventing deposition of wax on equipment during dewaxing by utilizing smooth surface equipment and a surface-active agent
US2904496A (en) * 1956-07-25 1959-09-15 Socony Mobil Oil Co Inc Process for separating wax from oils

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4447311A (en) * 1982-07-22 1984-05-08 Mobil Oil Corporation Dewaxing process
US20100236990A1 (en) * 2009-03-17 2010-09-23 James William Gleeson Bubble separation to remove haze and improve filterability of lube base stocks
US8216449B2 (en) * 2009-03-17 2012-07-10 Exxonmobil Research And Engineering Company Bubble separation to remove haze and improve filterability of lube base stocks
JP2012520919A (ja) * 2009-03-17 2012-09-10 エクソンモービル リサーチ アンド エンジニアリング カンパニー 潤滑基礎原料の曇りを除去し、濾過性を向上させる泡分離
WO2016083946A3 (fr) * 2014-11-26 2016-08-04 Sabic Global Technologies B.V. Systèmes et procédés pour séparer des produits de cire à partir de produits
CN107001944A (zh) * 2014-11-26 2017-08-01 赛贝克环球科技公司 与从费‑托产物中分离蜡产物有关的系统和方法

Also Published As

Publication number Publication date
FR1530070A (fr) 1968-06-21
FR1443921A (fr) 1966-07-01
BE652106A (fr) 1965-02-22
BE698743A (fr) 1967-11-03
NO115407B (fr) 1968-09-30
NL6708226A (fr) 1968-11-20
CH478222A (de) 1969-09-15
GB1022430A (en) 1966-03-16
LU53778A1 (fr) 1967-07-31
DK120854B (da) 1971-07-26
DE1545347A1 (de) 1970-02-26
NL6502144A (fr) 1966-02-22

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