US3846276A - Process for separating bitumen from tar sand recovered from deposits by mining - Google Patents

Process for separating bitumen from tar sand recovered from deposits by mining Download PDF

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Publication number
US3846276A
US3846276A US00371203A US37120373A US3846276A US 3846276 A US3846276 A US 3846276A US 00371203 A US00371203 A US 00371203A US 37120373 A US37120373 A US 37120373A US 3846276 A US3846276 A US 3846276A
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Prior art keywords
bitumen
tar sand
polyphosphate
sand
solution
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Expired - Lifetime
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US00371203A
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English (en)
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C Walker
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Texaco Inc
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Texaco Inc
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Priority to US00371203A priority Critical patent/US3846276A/en
Priority to DE2420556A priority patent/DE2420556A1/de
Priority to CA202,113A priority patent/CA1027889A/fr
Priority to BR490174A priority patent/BR7404901D0/pt
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Publication of US3846276A publication Critical patent/US3846276A/en
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
    • C10G1/04—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by extraction
    • C10G1/047—Hot water or cold water extraction processes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C3/00—Working-up pitch, asphalt, bitumen
    • C10C3/007—Working-up pitch, asphalt, bitumen winning and separation of asphalt from mixtures with aggregates, fillers and other products, e.g. winning from natural asphalt and regeneration of waste asphalt

Definitions

  • the mined tar sand material is fed into a mixing container and contacted with a hot alkaline polyphosphate solution.
  • Bitumen separates from sand without formation of an emulsion or a froth.
  • the fluid used in conjunction with this separation technique is an aqueous solution of a polyphosphate wetting agent such as sodium acid pyrophosphate plus an alkalinity agent such as sodium hydroxide, heated to a temperature of from about 100 F. to about 200 F.
  • the portion of bituminous petroleum dispersed in the aqueous phase is separated from the phosphate solution by contacting the fluid with a hypdrocarbon fluid such as diesel oil.
  • This invention pertains to a method for separating and recovering bitumen from tar sand recovered from subterranean tar sand deposits.
  • strip mining requires 3,846,276 Patented Nov. 5, 1974 ice removal of the overburden by mechanical means and the mixture of bitumen and sand that constitutes the tar sand deposit is then similarly removed by mechanical means and transported to a surface processing plant for separation of bitumen and sand.
  • In situ separation processes make use of techniques for separating the bitumen from the sand within the tar sand deposit itself, so the bitumen in some modified form may be transported to the surface with the sand left in the tar sand deposit. Techniques presently employed for in situ separation may be classified as thermal or emulsification processes.
  • the thermal techniques include in situ combustion, (fire flooding), and steam flooding.
  • Emulsification processes also involve the use of steam plus some additional chemical to promote emulsification of the high viscosity bitumen so that it may be transported to the surface in the form of a low viscosity oil-in-water emulsion, where the emulsion is resolved into bitumen and Water.
  • Emulsion formation is almost spontaneous when bituminous petroleum contacts hot water containing an alkalinity agent such as sodium hydroxide. While formation of a stable oil-in-Water emulsion is useful in some in situ recovery processes, emulsions of both the oil-in-water and water-in-oil type are frequently formed as a by product of cold or hot water separation processes. In either case, the emulsion must be broken or resolved into its individual phases. Resolving emulsions involving bituminous petroleum is usually difficult for several reasons. Asphaltic substances are 'very effective emulsifying agents and form very stable emulsions. Furthermore, the specific gravity of bitumen is almost exactly equal to the specific gravity of water, which means there will be no gravity related forces due to density differences to aid in phase separation even if surface forces responsible for emulsification can be neutralized.
  • bitumen may be separated from tar sands by a technique wherein the tar sand is contacted by a hot, aqueous polyphosphate solution containing an alkaline substance such as caustic or sodium hydroxide.
  • the tar sand is fed continually into a mixing vat Where contact with the hot alkaline polyphosphate solution occurs.
  • the mixture is fed to a settling tank where separation into sand, bitumen and an aqueous phase having a minor amount of bituminous material contained therein occurs.
  • the mixture is contacted with a hydrocarbon treating fluid which solubilizes the bitumen and facilitates separation thereof.
  • Polyphosphate wetting agents suitable for use in my invention include sodium acid pyrophosphate, tetrasodium pyrophosphate, sodium trimetaphosphate and sodium tetrametaphosphate.
  • the heated alkaline aqueous polyphosphate solution mixes with tar sand in tank 3, where the mixture is agitated by mixer 4 and then pumped by pump 8 into separation tank 9.
  • a series of separation tanks may be used in parallel, with sequential routing of the fluid to the several tanks so the mixture can remain quiesent for a period of time sufiicient to facilitate settling of sand 10 in the bottom of the tank.
  • Most of the bitumen accumulates in a zone immediately above the sand layer.
  • An aqueous layer forms on top, which is comprised of the hot, alkaline polyphosphate solution having a small amount of bitumen dispersed therein.
  • Sand is removed from the lower zone in tank 9 by some means such as the screw conveyor 13 on a continuous or intermittent basis.
  • a hydrocarbon fluid from tank 14. is metered by pump 15 into the separation tank 9 at a predetermined flow rate.
  • the aqueous solution and hydrocarbon treating fluid are mixed in separation tank 9 by stirrer 16.
  • Bituminous material from the lower layer as well as from the aqueous suspension dissolves in the hydrocarbon treating fluid and forms layer 17.
  • the treating fluid with bitumen dissolved therein is transported via line 18 to a refinery. Presence of hydrocarbon treating fluid in the bitumen aids pumping same to the refinery process unit. Separation and recovery of hydrocarbon treating fluid may be accomplished in the refinery unit. Of course, hydrocarbon treating fluid recovery may be accomplished immediately after leaving separation unit 9 if desired.
  • the alkaline, aqueous polyphosphate solution 19 is pumped via line 20 and pump 21 through filter element 22 to tank 5 for recycling through the separation process equipment.
  • the fluid used in this process is an aqueous alkaline solution of a polyphosphate such as tetrasodium pyrophosphate Na P O sodium acid pyrophosphate Na 2H2P2 07 or pentasodium tripolyphosphate, plus an alkalinity agent such as caustic soda (sodium hydroxide, NaOH).
  • a polyphosphate such as tetrasodium pyrophosphate Na P O sodium acid pyrophosphate Na 2H2P2 07 or pentasodium tripolyphosphate
  • an alkalinity agent such as caustic soda (sodium hydroxide, NaOH).
  • Polyphosphates are inorganic salts whose anions contain P units linked by sharing oxygens with other tetrahedra.
  • the polyphosphates may be in chain form, e.g. [P 0 1 1 or [P 0 1 1 or in a ring form [P O and [P 0 1 1 triand tetra-metaphosphates respectively.
  • Polyphosphates are hydrophilic surface active agents as opposed to organic wetting agents which may be considered hydrophobic surface active agents. There are no oleophilic moieties present in inorganic polyphosphates so they are not surfactants in the sense of alkyl or alkylaryl sulfates, sulfonates or phosphates.
  • the prior art teaches the use of polyphosphates as builders in household detergents, and that polyphosphates function as deflocculants in drilling fluids and other suspensions, and for the purpose of forming soluble complexes.
  • any Water soluble salt of pyrophosphoric acid, H P O may be used in the process of my invention.
  • the sodium, potassium or lithium salt of pyrophosphoric acid may be used.
  • the sodium salts are tetrasodium pyrophosphate, 'Na P O trisodium hydrogen pyrophosphate, Na HP O disodium dihydrogen pyrophosphate (known commercially as sodium acid pyrophosphate) Na H P O and sodium trihydrogen pyrophosphate, NaHgPzoq.
  • sodium polyphosphates such as pentasodium tripolyphosphate, Na P O is also known and may be used in my process.
  • Ring polyphosphates such as sodium trimetaphosphate Na (PO and sodium tetrametaphosphate Na (PO may also be used.
  • the preferred materials are the water soluble salts of pyrophosphoric acid, and especially sodium acid pyrophosphate or tetrasodium pyrophosphate.
  • concentration of polyphosphate in the aqueous solution may be quite dilute, as low as 0.10-5.0 percent. Although concentrations greater than this may be used, there is no particular advantage in using larger concentrations, and while the cost of the material is low, economics of the process are optimized by using the lowest effective concentration.
  • an alkalinity agent will be added to the polyphosphate solution. Care should be taken to insure that the cation associated with the alkalinity agent does not form an insoluble salt with the particular polyphosphate being used.
  • sodium hydroxide is the preferred material, although other monovalent bases such as potassium hydroxide, lithium hydroxide or ammonium hydroxide may be used also. Polyvalent bases such as calcium hydroxide should not be used.
  • Suflicient alkalinity agent should be added to the solution to bring the pH thereof to a value above about 10 and preferably above 12. Generally 0.105.0 percent by weight will be suflicient.
  • One convenient means for maintaining the desired pH is to add approximately equal amounts of the alkalinity agent and the polyphosphate.
  • Heating the aqueous alkaline polyphosphate to a temperature in excess of F. will increase the effectiveness of this separation technique.
  • the preferred operating temperature is from about 100 F. to about 200 F.
  • Any hydrocarbon fluid which will dissolve a substantial amount of bitumen may be used.
  • Aliphatic hydrocarbons having from 4 to 20 carbon atoms such as naphtha or diesel oil may be used.
  • Aromatic hydrocarbons including benzene, toluene and xylene are also very effective materials for use in my invention.
  • bitumen is not emulsified and no froth is formed on being contacted with the hot aqueous alkaline polyphosphate solution. Bitumen is removed eflectively from the sand but remains in a separate phase which will form a discrete layer distinct from the aqueous solution if agitation is stopped. The bitumen may be pumped to the refining process unit, the polyphosphate solution being recycled through the separation equipment.
  • FIELD EXAMPLE A tar sand deposit having an overburden varying from 10 to 40 feet in thickness, said deposit having an average thickness of 65 feet, is exploited by means of open pit strip mining. After stripping away the overburden, tar sand is dug from the deposit using scrapers and transported by truck to the separation process equipment. The equipment is theoretically capable of removing the tar sand at a rate of 1500 tons per hour, although actual production rate is 1000 tons per hour. The bitumen content of the tar sand is 14 percent by weight.
  • Separation is accomplished by using a number of units, each with a capacity of 200 tons per hour.
  • the tar sand is fed by screw conveyor into a 5000 gallon mixing tank.
  • An aqueous solution of 0.30 percent by weight sodium acid pyrophosphate and 0.30 percent by weight sodium hydroxide is formulated in a 1000 gallon tank and fed into the 5000' gallon tank at a rate of 1000 gallons per hour.
  • the polyphosphate solution is heated to a temperature of 160 F. by passing through a gas fired heater prior to being added to the 5000 gallon tank.
  • Each separation tank has a volume of 3000 gallons.
  • a screw conveyor removes sand from the bottom of the separation tank.
  • Bituminous petroleum accumulates in a layer immediately above the sand layer, and an aqueous layer having a small amount of bitumen dispersed therein accumulates on top.
  • Diesel oil is added to the separation tank and mixed. Bitumen from the layer immediately above the sand as well as that dispersed in the aqueous phase, dissolves in the diesel oil. After mixing is stopped, a layer of diesel oil and bitumen forms on top, which is decanted and sent to the refinery.
  • the aqueous sodium pyrophosphate solution is passed through a sand pack filter and then back to the pyrophosphate make up tank for recycling through the unit.
  • Sand from the settling tank is placed in excavations formed in earlier stages of strip mining operations.
  • the separation technique elfectively removes approximately 90 percent of the bitumen from the tar sand.
  • a process for separating bitumen and sand from tar sand material recovered from subterranean deposits by mining comprising:
  • a method as recited in Claim 1 comprising the additional step of contacting the aqueous polyphosphate solution with a hydrocarbon fluid to promote separation of residual bitumen from the aqueous polyphosphate solution.
  • alkalinity agent is selected from the group consisting of sodium hydroxide, lithium hyrdoxide, potassium hydroxide and ammonium hydroxide.
  • a method for separating bitumen from tar sand material comprising:
  • a polyphosphate surface active agent selected from the group consisting of water soluble salts of pyrophosphoric acid, water soluble tripolyphosphate salts and water soluble ring polyphosphates
  • a method as recited in Claim 19 comprising the additional step of contacting said tar sand material and polyphosphate solution with a hydrocarbon fluid selected from the group consisting of paraflinic hydrocarbons having from 4 to 20 carbon atoms, naphtha, diesel oil, aromatic hydrocarbons, benzene, toluene and xylene, and mixtures thereof.
  • a hydrocarbon fluid selected from the group consisting of paraflinic hydrocarbons having from 4 to 20 carbon atoms, naphtha, diesel oil, aromatic hydrocarbons, benzene, toluene and xylene, and mixtures thereof.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Working-Up Tar And Pitch (AREA)
US00371203A 1973-06-18 1973-06-18 Process for separating bitumen from tar sand recovered from deposits by mining Expired - Lifetime US3846276A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US00371203A US3846276A (en) 1973-06-18 1973-06-18 Process for separating bitumen from tar sand recovered from deposits by mining
DE2420556A DE2420556A1 (de) 1973-06-18 1974-04-27 Verfahren zur abtrennung von bitumen aus teersand
CA202,113A CA1027889A (fr) 1973-06-18 1974-06-11 Procede pour l'extraction du bitume des sables asphaltiques recuperes de gisements par des methodes minieres
BR490174A BR7404901D0 (pt) 1973-06-18 1974-06-14 Processo para separar betume de areias alcatroadas

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CA (1) CA1027889A (fr)
DE (1) DE2420556A1 (fr)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4132639A (en) * 1976-08-24 1979-01-02 The United States Of America As Represented By The United States Department Of Energy Method for improving the sedimentation and filterability of coal-derived liquids
US4160718A (en) * 1976-08-07 1979-07-10 Rohrtil S. A. Solvent extraction process
US4374023A (en) * 1981-10-26 1983-02-15 Chevron Research Company Process for recovering hydrocarbons from a diatomite-type ore
US4392941A (en) * 1980-07-28 1983-07-12 Suncor, Inc. Recovery of bitumen from tar sands sludge using additional water
US4529496A (en) * 1979-08-15 1985-07-16 Jan Kruyer Method and apparatus for separating slurries and emulsions
US4545891A (en) * 1981-03-31 1985-10-08 Trw Inc. Extraction and upgrading of fossil fuels using fused caustic and acid solutions
US5059307A (en) * 1981-03-31 1991-10-22 Trw Inc. Process for upgrading coal
US5085764A (en) * 1981-03-31 1992-02-04 Trw Inc. Process for upgrading coal
US20080110805A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Continuous flow separation and aqueous solution treatment for recovery of crude oil from tar sands
US20080110803A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Settling vessel for extracting crude oil from tar sands
US20080111096A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Composition for extracting crude oil from tar sands
US20080110804A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Slurry transfer line
WO2008110486A1 (fr) * 2007-03-12 2008-09-18 Bloechlinger Oskar Procédé et dispositif pour la séparation de mélanges
US20090261021A1 (en) * 2008-04-16 2009-10-22 Bower David J Oil sands processing

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1278178C (fr) * 1989-01-04 1990-12-27 Sylvia K. Pachla Traitement antiboues
CA2263014C (fr) 1999-02-25 2007-04-17 Bj Services Company, U.S.A. Compositions et methodes pour accroitre par catalyse la vitesse de reduction du fer lors du traitement acide de puits

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4160718A (en) * 1976-08-07 1979-07-10 Rohrtil S. A. Solvent extraction process
US4132639A (en) * 1976-08-24 1979-01-02 The United States Of America As Represented By The United States Department Of Energy Method for improving the sedimentation and filterability of coal-derived liquids
US4529496A (en) * 1979-08-15 1985-07-16 Jan Kruyer Method and apparatus for separating slurries and emulsions
US4392941A (en) * 1980-07-28 1983-07-12 Suncor, Inc. Recovery of bitumen from tar sands sludge using additional water
US5059307A (en) * 1981-03-31 1991-10-22 Trw Inc. Process for upgrading coal
US4545891A (en) * 1981-03-31 1985-10-08 Trw Inc. Extraction and upgrading of fossil fuels using fused caustic and acid solutions
US5085764A (en) * 1981-03-31 1992-02-04 Trw Inc. Process for upgrading coal
US4374023A (en) * 1981-10-26 1983-02-15 Chevron Research Company Process for recovering hydrocarbons from a diatomite-type ore
US20080110805A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Continuous flow separation and aqueous solution treatment for recovery of crude oil from tar sands
US20080110803A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Settling vessel for extracting crude oil from tar sands
US20080111096A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Composition for extracting crude oil from tar sands
US20080110804A1 (en) * 2006-11-10 2008-05-15 Veltri Fred J Slurry transfer line
US7694829B2 (en) 2006-11-10 2010-04-13 Veltri Fred J Settling vessel for extracting crude oil from tar sands
WO2008110486A1 (fr) * 2007-03-12 2008-09-18 Bloechlinger Oskar Procédé et dispositif pour la séparation de mélanges
US20090261021A1 (en) * 2008-04-16 2009-10-22 Bower David J Oil sands processing

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DE2420556A1 (de) 1975-01-09
CA1027889A (fr) 1978-03-14

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