CA1088445A - Tar sands bitumen recovery from aqueous effluent - Google Patents
Tar sands bitumen recovery from aqueous effluentInfo
- Publication number
- CA1088445A CA1088445A CA300,148A CA300148A CA1088445A CA 1088445 A CA1088445 A CA 1088445A CA 300148 A CA300148 A CA 300148A CA 1088445 A CA1088445 A CA 1088445A
- Authority
- CA
- Canada
- Prior art keywords
- tar sands
- effluent
- bitumen
- carbon
- aqueous
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
TITLE
TAR SANDS BITUMEN RECOVERY FROM AQUEOUS EFFLUENT
INVENTORS
Aurelio Frederick Sirianni John A. Ripmeester ABSTRACT OF THE DISCLOSURE
Tar sands bitumen is recovered concurrently from tar sands and from aqueous effluents from water-based pro-cesses for treating tar sands, by steps comprising:
(a) recycling the aqueous effluent containing waste bitumen and incorporating therewith i) hydrophobic carbon, and ii) tar sands, suitably in a pre-mixed form, (b) agitating with a shearing action the ternary mixture to intimately contact the carbon with the effluent and tar sands to cause the hydrophobic surfaces to scrub or-ganic material from the effluent, and continuing agitation until the carbon and effluent-bitumen form into a unitary organic phase with the bitumen from the tar sands;
(c) separating the unitary organic phase from the aqueous phase, and discharging aqueous effluent of reduced organic content;
and (d) recovering carbon and hydrocarbons from the organic phase.
TAR SANDS BITUMEN RECOVERY FROM AQUEOUS EFFLUENT
INVENTORS
Aurelio Frederick Sirianni John A. Ripmeester ABSTRACT OF THE DISCLOSURE
Tar sands bitumen is recovered concurrently from tar sands and from aqueous effluents from water-based pro-cesses for treating tar sands, by steps comprising:
(a) recycling the aqueous effluent containing waste bitumen and incorporating therewith i) hydrophobic carbon, and ii) tar sands, suitably in a pre-mixed form, (b) agitating with a shearing action the ternary mixture to intimately contact the carbon with the effluent and tar sands to cause the hydrophobic surfaces to scrub or-ganic material from the effluent, and continuing agitation until the carbon and effluent-bitumen form into a unitary organic phase with the bitumen from the tar sands;
(c) separating the unitary organic phase from the aqueous phase, and discharging aqueous effluent of reduced organic content;
and (d) recovering carbon and hydrocarbons from the organic phase.
Description
~ ~0~384~5 This inven-tion deals with the recovery of bitumen from aqueous effluents from tar sands separation processes utili7ing water media, particularly from the hot water pro-cess. The aqueous effluent containing bitumen is scrubbed ;
using hydrophobic carbon such as refinery coke, the coke being combined with the bitumen from added tar sands, to form a composite organic phase which is separated and recovered.
The hot water process is in use in Alberta to treat tar sands for recovery o bitumen. The tar sands are slurried with hot water a~d steam, the pulp is a~itated ana fed to a separation vessel. Entrained air causes the " . ~ .
bitumen to rise to the top of the vessel as a froth. The separated froth is usuall~ further treated as by centri~uge to remove addi~ional mineral solids. ~he aq~leous phase con-ta.in~ hydrophilic qolids and some bitumen. Much o~ the sand settles out from the aqueous phase bu-t very fine hydrophilic solids such as clays/ and entrained or emulsified bitumen material are very difficult to remove from the aqueous tai-lings. Even prolonged settling in ponds will not completely separate the clays etc. and the lost bitumen materia:Ls from the a~ueous phase.
Many e~forts have been made to separate the sus-pended solids rom the aqueous phase, and to re-use the tai-lings water. U.S. Patent 3,816,305, Schutte describes the , addition of acid to tailings and middlings water to accele-rate clariication. U.S. Patent 3,607,720, Paulson utilizes ~ ;
hot flue gases to treat pond water from tar sands processing.
` U.S. Patent 3,526,585, Camp adds a volatile organic fluid ;j immiscible with water to the pond water to form an inter-'1 30 face layer higher in clay content. U.S. Patent 3,487,003, Baillie et al treats the pond water with a flocculating agent, pH change and centrifuging.
. , : --1-- ~ .
, .
.. . . . . . . . . . . . ..
~08~445 .:
Canadian Patent 982,966, February 3, 1976, Maloney, describes recycling tar sands hot water process effluen-t to contact fresh tar sands in a kneading agglomerating zone, and recovering tar agglomerates, sand and an effluent stream of reduced clay, silt and bitumen con-tent. No amounts of bitumen recovered from the effluent are given.
We have now found that improved recoveries of waste bitumen from tar sands process aqueous effluent can be achieved by incorporating hydrophobic carbon as scrub-: .
bing or nucleating agent toge~her with added tar sands and recycled effluent. The mixture must be subjected to agita-tion with shearing action and agitation continued until a unit.ary organic phase orms. This organic phase is readily separated by physical means.
The lnventi.on i.~ more particularly a method for 'l ~ recovering tar sand~ l~iturnen concurrently from tar salids and rom aqueous e1uents ~rcm water-based proces~es for ~ -treating tar sands, comprising: -(a) recycling aqueous e~fluent conta.Lnin~ waste bitumen and incorporating therewi~h i) hydropho~ic carbol in amounts of about 0.5 to 5% by wt. based on the tar sands, and ii) tar sand~s in amounts yielding a 1uid slurry;
~b) agïtating with shearing action the ternary mixture to contact intimately the carbon with the effluent and added tar sand to cause the hydrophobic surfaces to scrub organic material from the ef~luent, and continuins agitation until the carbon and bitumen from the e1uent orms into ... ,~ . ... .
i 30 a unitary organic phase with the bitumen from the -tar sands;
~ ~c) separating the unitary organic phase rom the . .
. . .
:! . . . , :
~ 88~45 :~
aqueous phase and from the bulk of the mineral solids, and discharging a~ueous effluent of reduced organic con-tent;
and (d) recovering carbon and hydrocarbons from ~he organic phase. -The hydrophobic carbon can be any solid ~orm of car-bon which is not wetted by water bu-t is we-tted by the bitumen phase. Hydrophobic forms of low grade coal, coke and carbon adsorbents may be used. A local refinery coke or '!delayed`' coke, particularly one prepared from tar sands bitumen has been found very satisfactory. It is possible to recover and re-cycle the initial carbon solids, e.g., b~ solvent washing and retorting of the organic phase. The amount of the ~,f.~.. ' .
hydrophobic carbon solids incorporated is suitabl~ about 0.5 t~ about 5~ by wt. based on the tar sands. ~he par~icle si2e o the carbon solids can vary widely. The larger the particle size, the easier to separate the organic phase as ~ ;
by screening. Usually the particle size will be less than about 0.3 mm diameter or passing a 50 mesh screen, to give an adequate surface area for contact with bitumen. -. .
The effluent containing waste bitumen can be ob-tained directly from a hot-water or similar ~ar sands sepa-ration process, or from ponds resulting from such processes.
The effluent can be from lower settled-out layers of such . .
effluent ponds including so-called sludge layers. Usuallyr the effluent will contain about 0.5 to 2% wt. or more bitu-men material. The settled pond layers or sludge will con- -;` tain up to 5~ or more of bitumen. The solids content of the effluent is usually within about 5 to 10% wt. in the form of a stabIe colloidal suspension.
The mixing may be carried out in two stages, e.g., the carbon and tar sands pre-mixed, and then incorporated with the major portion of effluent. The pre-mixing is 1~884~5 suitably at low water contents not more than about 15 - 20%
wt., and the effluent then added to raise -the water content . ..
to at leas-t about 30% wt. (based on total mixture), usually -to at least 50%. ~arge amounts of effluent can be scrubbed by the carbon and bitumen, e.g., amounts of about 200% wt.
or higher based on wt. of tar sands (see Example III).
The agitation may be carried out by any suitable . .
means but should be accompanied by a definite shearing action.
A milling action, as bekween hard solid surfaces urged to-gether, is preferred. This milling action is believed to expose hydrophilic surfaces of the mineral solids and faci-litate their transfer to the a~ueous phase, as well as aid the scrubbin~ ac~ion of the carbon solids on the a~ueous phase. It is preferred to carry out an initial milling action on a partial mi~ture of hyd~ophobic carbon and tar sands to aid disruption of the tar sands (see Examples).
The separation of the resulting unitary organic phase of carbon solids plus bitumen is readily achieved by screening or coarse filtration. Centrifugal action can also be used. It is desirable to wash the organic phase with water to help remove hydrophilic impurities. This washing . , .
can conveniently take place in the separation zone to faci-litate removal of the wash water. `~
The agitation and separation are suitably carried ; out at ambient temperatures. If the recycled effluent is -warm, say up to about 50C, the scrubbing action and uni-tary organic phase formation appear to proceed more quickly.
Some reduction in process time is also possible if the pH
is raised slightly, e.g., to pH 8-9 with alkali metal l 3Q hydroxide.
`~3 The separated organic phase is further processed , by conven-tional techniques to recover carbon ~olids and :
'" ' ',~."' .:
34~S
. ~ :
hydrocarbons. The orgniac phase can be retorted to sepa-rate gaseous and liquid products from the solid residue.
Solvent washing can be used -to aid separation of bitumen ma-terial from the carbon solids. A coking operation can be carried out on part or all of the organic phase to yield coke and volatile products. In the unitary organic phase some fine mineral solids may remain entrained, but these solids are believed to be beneficial in~coke prepared from ` `
this phase by improving coke combus~ion properties. A ;
cracking operation can be incorporated in these recovery techniques if desired. Whatever recovery scheme is used, --it is usually desirable to obtain some hydrophobic carbon for recycle.
The final aqueous phase or eE~luent will have a reduced organic content usually corresponding to a loss-on-ignition of about 5 to 10% (when starting with about 27%
L.O.I. hot-water process pond effluent sludge). The re-duction in organic content from feed effluent to final effluent is normally to 1/5 - 1/10 or less of the initial content. This final effluent is depleted in organic sub-stances responsible ~or the slow settling of clay etc. r~
~olids, and these solids will now settle out more rapidly yielding water which can be recycled or at least is more acceptable for discharge to the environment.
The following examples are illustrative The hydrophobic carbon (nucleating agent) was refinery coke which was wet ball-milled to -140 mesh and filtered. The moist ~ilter cake containing about 44% solids was used in -the process. The effluent used was hot-water process pond e~fluent. Loss on ignition is % of dry solids content.
' i . .
:` l . . ' ,, ,'.,.:, ~' . ',:
.`', ` .. ...
Example I
Part (1) Clay-type Tar Sand 200 g (bitumen content 5.9~) .
Moist ~efinery Coke 25 g (abou-t 10.9 g solids) These two were admixed by rotating in a quart-size porcelain jar containing 5 s-teel 1/2" diameter balls for 2 hours. About 200 ml of water eEfluent containing about 26.6% non-aqueous material (bitumen + inorganic mine- -rals) was added and the jar rotated for 20 hours. About 225 ml aqueous phase tl) was removed by screening.
Part (2) About 200 g clay-type -tar sand was added to the oil phase from (1) above, and rotated in the jar for 30 minutes. Then about 200 ml effluent as above was added and the suspension rotated in the jar for 10 hours. About 220 ml o~ aqueous phase (2) was .removed by screening.
Part (3) ~ further 200 g ~uantity of clay-type tar sand and 200 ml effluent were added and treated as in part t2).
i The aqueous tailings (3) were separated from the oil phase i by screening. The oi] ~hase was worked twice by rotating 15 minutes with 100 ml clear water each time and screened~
The results obtained are summarized below:
Separated Solids Loss on Bitumen Re-Tailings Content Ignition Covered from % ~ 600 ml E~fluent and tar sands Part .
1 51.4 5.83
using hydrophobic carbon such as refinery coke, the coke being combined with the bitumen from added tar sands, to form a composite organic phase which is separated and recovered.
The hot water process is in use in Alberta to treat tar sands for recovery o bitumen. The tar sands are slurried with hot water a~d steam, the pulp is a~itated ana fed to a separation vessel. Entrained air causes the " . ~ .
bitumen to rise to the top of the vessel as a froth. The separated froth is usuall~ further treated as by centri~uge to remove addi~ional mineral solids. ~he aq~leous phase con-ta.in~ hydrophilic qolids and some bitumen. Much o~ the sand settles out from the aqueous phase bu-t very fine hydrophilic solids such as clays/ and entrained or emulsified bitumen material are very difficult to remove from the aqueous tai-lings. Even prolonged settling in ponds will not completely separate the clays etc. and the lost bitumen materia:Ls from the a~ueous phase.
Many e~forts have been made to separate the sus-pended solids rom the aqueous phase, and to re-use the tai-lings water. U.S. Patent 3,816,305, Schutte describes the , addition of acid to tailings and middlings water to accele-rate clariication. U.S. Patent 3,607,720, Paulson utilizes ~ ;
hot flue gases to treat pond water from tar sands processing.
` U.S. Patent 3,526,585, Camp adds a volatile organic fluid ;j immiscible with water to the pond water to form an inter-'1 30 face layer higher in clay content. U.S. Patent 3,487,003, Baillie et al treats the pond water with a flocculating agent, pH change and centrifuging.
. , : --1-- ~ .
, .
.. . . . . . . . . . . . ..
~08~445 .:
Canadian Patent 982,966, February 3, 1976, Maloney, describes recycling tar sands hot water process effluen-t to contact fresh tar sands in a kneading agglomerating zone, and recovering tar agglomerates, sand and an effluent stream of reduced clay, silt and bitumen con-tent. No amounts of bitumen recovered from the effluent are given.
We have now found that improved recoveries of waste bitumen from tar sands process aqueous effluent can be achieved by incorporating hydrophobic carbon as scrub-: .
bing or nucleating agent toge~her with added tar sands and recycled effluent. The mixture must be subjected to agita-tion with shearing action and agitation continued until a unit.ary organic phase orms. This organic phase is readily separated by physical means.
The lnventi.on i.~ more particularly a method for 'l ~ recovering tar sand~ l~iturnen concurrently from tar salids and rom aqueous e1uents ~rcm water-based proces~es for ~ -treating tar sands, comprising: -(a) recycling aqueous e~fluent conta.Lnin~ waste bitumen and incorporating therewi~h i) hydropho~ic carbol in amounts of about 0.5 to 5% by wt. based on the tar sands, and ii) tar sand~s in amounts yielding a 1uid slurry;
~b) agïtating with shearing action the ternary mixture to contact intimately the carbon with the effluent and added tar sand to cause the hydrophobic surfaces to scrub organic material from the ef~luent, and continuins agitation until the carbon and bitumen from the e1uent orms into ... ,~ . ... .
i 30 a unitary organic phase with the bitumen from the -tar sands;
~ ~c) separating the unitary organic phase rom the . .
. . .
:! . . . , :
~ 88~45 :~
aqueous phase and from the bulk of the mineral solids, and discharging a~ueous effluent of reduced organic con-tent;
and (d) recovering carbon and hydrocarbons from ~he organic phase. -The hydrophobic carbon can be any solid ~orm of car-bon which is not wetted by water bu-t is we-tted by the bitumen phase. Hydrophobic forms of low grade coal, coke and carbon adsorbents may be used. A local refinery coke or '!delayed`' coke, particularly one prepared from tar sands bitumen has been found very satisfactory. It is possible to recover and re-cycle the initial carbon solids, e.g., b~ solvent washing and retorting of the organic phase. The amount of the ~,f.~.. ' .
hydrophobic carbon solids incorporated is suitabl~ about 0.5 t~ about 5~ by wt. based on the tar sands. ~he par~icle si2e o the carbon solids can vary widely. The larger the particle size, the easier to separate the organic phase as ~ ;
by screening. Usually the particle size will be less than about 0.3 mm diameter or passing a 50 mesh screen, to give an adequate surface area for contact with bitumen. -. .
The effluent containing waste bitumen can be ob-tained directly from a hot-water or similar ~ar sands sepa-ration process, or from ponds resulting from such processes.
The effluent can be from lower settled-out layers of such . .
effluent ponds including so-called sludge layers. Usuallyr the effluent will contain about 0.5 to 2% wt. or more bitu-men material. The settled pond layers or sludge will con- -;` tain up to 5~ or more of bitumen. The solids content of the effluent is usually within about 5 to 10% wt. in the form of a stabIe colloidal suspension.
The mixing may be carried out in two stages, e.g., the carbon and tar sands pre-mixed, and then incorporated with the major portion of effluent. The pre-mixing is 1~884~5 suitably at low water contents not more than about 15 - 20%
wt., and the effluent then added to raise -the water content . ..
to at leas-t about 30% wt. (based on total mixture), usually -to at least 50%. ~arge amounts of effluent can be scrubbed by the carbon and bitumen, e.g., amounts of about 200% wt.
or higher based on wt. of tar sands (see Example III).
The agitation may be carried out by any suitable . .
means but should be accompanied by a definite shearing action.
A milling action, as bekween hard solid surfaces urged to-gether, is preferred. This milling action is believed to expose hydrophilic surfaces of the mineral solids and faci-litate their transfer to the a~ueous phase, as well as aid the scrubbin~ ac~ion of the carbon solids on the a~ueous phase. It is preferred to carry out an initial milling action on a partial mi~ture of hyd~ophobic carbon and tar sands to aid disruption of the tar sands (see Examples).
The separation of the resulting unitary organic phase of carbon solids plus bitumen is readily achieved by screening or coarse filtration. Centrifugal action can also be used. It is desirable to wash the organic phase with water to help remove hydrophilic impurities. This washing . , .
can conveniently take place in the separation zone to faci-litate removal of the wash water. `~
The agitation and separation are suitably carried ; out at ambient temperatures. If the recycled effluent is -warm, say up to about 50C, the scrubbing action and uni-tary organic phase formation appear to proceed more quickly.
Some reduction in process time is also possible if the pH
is raised slightly, e.g., to pH 8-9 with alkali metal l 3Q hydroxide.
`~3 The separated organic phase is further processed , by conven-tional techniques to recover carbon ~olids and :
'" ' ',~."' .:
34~S
. ~ :
hydrocarbons. The orgniac phase can be retorted to sepa-rate gaseous and liquid products from the solid residue.
Solvent washing can be used -to aid separation of bitumen ma-terial from the carbon solids. A coking operation can be carried out on part or all of the organic phase to yield coke and volatile products. In the unitary organic phase some fine mineral solids may remain entrained, but these solids are believed to be beneficial in~coke prepared from ` `
this phase by improving coke combus~ion properties. A ;
cracking operation can be incorporated in these recovery techniques if desired. Whatever recovery scheme is used, --it is usually desirable to obtain some hydrophobic carbon for recycle.
The final aqueous phase or eE~luent will have a reduced organic content usually corresponding to a loss-on-ignition of about 5 to 10% (when starting with about 27%
L.O.I. hot-water process pond effluent sludge). The re-duction in organic content from feed effluent to final effluent is normally to 1/5 - 1/10 or less of the initial content. This final effluent is depleted in organic sub-stances responsible ~or the slow settling of clay etc. r~
~olids, and these solids will now settle out more rapidly yielding water which can be recycled or at least is more acceptable for discharge to the environment.
The following examples are illustrative The hydrophobic carbon (nucleating agent) was refinery coke which was wet ball-milled to -140 mesh and filtered. The moist ~ilter cake containing about 44% solids was used in -the process. The effluent used was hot-water process pond e~fluent. Loss on ignition is % of dry solids content.
' i . .
:` l . . ' ,, ,'.,.:, ~' . ',:
.`', ` .. ...
Example I
Part (1) Clay-type Tar Sand 200 g (bitumen content 5.9~) .
Moist ~efinery Coke 25 g (abou-t 10.9 g solids) These two were admixed by rotating in a quart-size porcelain jar containing 5 s-teel 1/2" diameter balls for 2 hours. About 200 ml of water eEfluent containing about 26.6% non-aqueous material (bitumen + inorganic mine- -rals) was added and the jar rotated for 20 hours. About 225 ml aqueous phase tl) was removed by screening.
Part (2) About 200 g clay-type -tar sand was added to the oil phase from (1) above, and rotated in the jar for 30 minutes. Then about 200 ml effluent as above was added and the suspension rotated in the jar for 10 hours. About 220 ml o~ aqueous phase (2) was .removed by screening.
Part (3) ~ further 200 g ~uantity of clay-type tar sand and 200 ml effluent were added and treated as in part t2).
i The aqueous tailings (3) were separated from the oil phase i by screening. The oi] ~hase was worked twice by rotating 15 minutes with 100 ml clear water each time and screened~
The results obtained are summarized below:
Separated Solids Loss on Bitumen Re-Tailings Content Ignition Covered from % ~ 600 ml E~fluent and tar sands Part .
1 51.4 5.83
2 43.6 6.47 - --
3 49.4 7.32 51~8 g Blank (Pond (hot water pro-30Effluent) 26.6 26.9 cess effluent) ;
) About 131.95 g oil phase was recovered containing 38.2~ solids (includes the refinery coke) and 23.6~ water.
. ' ',': ~ .
~' 6~
.:' '.
:
i ` 1(~1~38445 `
Judging from the loss on ignition (L.O.I.) as in-dicator, gooc1 bitumen separa-tion from effluent was achieved by this method.
Example IIa Control - No nucleatinq a~ent added Part (la) Clay-type Tar Sand 200 g (bitumen content 5.9%) ~-Hot-water process ~
effluent 200 ml ~26.6% non-aqueous material) -These materials were admixed in a quart-size por-celain jar by rotating 10 hou~s using 5 steel 1/2l' balls. -The oil appeared present in "islands". About 150 ml of aqueous suspension (la) was separated by screening.
Part (2a) About 200 g clay-t~pe tar sand as above was added ! '' .,' to this resulting oil phase and the system admixed b~ ro-tating 30 minutes. Then 200 ml hot-waker process eE~luent ` i was added and the system again rotated for 5 hours. About 100 ml aqueous phase (2a) was separated by screening. The oil phase was rinsed twice by rotating 15 minutes with S0 ml clear water each time (3a). The results obtained are summarized below:
Separated Solids Loss on Bitumen Re-Tailings Content Ignitioncoverecl from % ~ 400 ml EEEluent and tar sands Part la 54 2 5.62 2a 54.4 19.15 -3a 41.4 10.45 16.75 g .
About 33.6 g bitumen product was recovered contai- -ning 27.6% solids and 22.5% water.
; 30 Example IIb Same as Control Example IIa, except refinery coke added Part (Ib) About 200 g clay-type tar sand (5.9% bitumen) was _7_ :', ' ' ,', ', ' ., .,'':,' ''.
~ 88~5 admixed with 25 g moist xefinery coke ground to 140 mesh (10.9g solid) by rotating in a quart-size porcelain ~ar containing 5 steel 1/2" balls for 1 hour. The total solids were in the form of spherical bodies. Abou-t 200 ml hot-water process effluent (26.6% non-aqueous solids) was added and the jar rotated for 10 hours. The oil phase was sub-stantially in one mass. About 160 ml aqueous suspension was separated by screening (lb).
Part (2b) About 200 g clay-type tar sand was added -to oil phase from (lb) and admixed by rotating 30 minutes, then 200 ml hot-water process effluent containing about 26.6%
non-aqueous solids (bitumen ~ inorganics) was adcled and the entire system rotated for 5 hours. About 185 ml aqueous suspension (2b) was separated b~ screening. The oil phase was rinsed twice by rotating for 15 minutes with 50 ml of clear water each time and screened. The washings were com-bined as tailings (3b). The results from example IIb are su~lmarized below:
Separated Solids Loss onBitumen Re-20 Tailings Content IgnitionCovered from % % 400 ml Effluent and tar sands Part lb 57.1 5.93 2b 58.4 3b 38.7 6.33 41.6 g About B8.0 g bitumen product was recovexed containing about 23.9% water and 28.2% solids which included the refi- -nery coke.
Example III -~ 30 About 200 g clay-type tar sand (5.9% bitumen) was ! admixed with 15 g moist refinery coke as in example IIb, but rotating for 30 minutes. The entlre system pelletized.
` ' ' ' ' .
: .................................................................. ' , About 400 ml effluent from the hot-water process tailings - pond was added and the suspension admixed by rotating 10 hours. About 380 ml aqueous suspension was screened off (-).
The oil phase was rinsed twice by rotating for 15 minutes with 50 ml clear water each time. The results are summarized below:
Separated Solids Loss of Bi-tu~en Re- -~
Tailings Content Ignition Covered from % 400 ml effluent and tar sands 1 46 6.18 41.1 g : .
About 74.6 g bitumen product was recovered contai-ning about 23.7P6 water and 21.2% solids (including the re-finery coke).
~xample IV
About 400 g clay-type tar sand (5.9% bitumen) was admixed with 10 g moist reinery coke as in example IIb by rotating 1 hour. Then 400 ml effluent from the hot-water process tailings pond containing about 26.6% non-aqueous solids was added and the suspension rotated for 10 hours.
A~out 300 ml aqueous tailings (1) was separated by screening. - :
The oil phase was rinsed twice by rotating for 15 minutes wi.th 100 ml and 75 ml clear water respectively. About 140 ml aqueous tailings (2) were separated from the oil phase.
The results obtained are summarized below: :~
Separated Solids Loss on Bitumen Re- ~:
Tailings Content Ignition Covered from -P6 400 ml effluent and tar sands :~ . .:
' 1 57.5 3 35 ~, 2 37.9 7.45 37.7 g ; -., - - ,.' .. .
~ 30About 68.15 g crude bitumen were separated contai- ;
.. :
,, ning 23.7% water and 21.2% solids (including refinery coke).
:, :
:..
_9_ ,' '' ~ ''.
.
. . , .' ' .
: ,.
SUMMARY OF RESULTS
Example Refinery Coke Ml Effluent l~t. Tar Bitumen Re-Nucleating Added Sand Added covered from Agent Effluent and tar sands I 10.9 g 600 600 g 5108 g IIanone (control) 400 400 g 16.75 g IIb 10.9 400 400 g 41.6 g III 6.55 400 200 g 41.1 g ~-IV 4.36 400 400 g 37.7 g By using more vigorous agitation-mixing to increase ~ .
inter-phase contacts, the processing time in the Examples could be decreased considerably.
Optionally liquid hydrocarbon fractions such as naphtha or kerosene could be added in small amounts (e.g.
1 - 2% wt. of the tar sand) to the tar sand as softening ., agent at an initial stage before contact with the effluent :.
(to accelerate the unitary organic phase formation). : - .
The method of this invention can be operated as .:. .
a side loop in a hot-water type of tar sands process, or ::
as an initial upgrading for feed to another process. :.
.,, ' ' ' .
~'. .',: ,' , , ' .,', .
':1 ' : '' ' , . .
~ '', ,,~ -10-,;
) About 131.95 g oil phase was recovered containing 38.2~ solids (includes the refinery coke) and 23.6~ water.
. ' ',': ~ .
~' 6~
.:' '.
:
i ` 1(~1~38445 `
Judging from the loss on ignition (L.O.I.) as in-dicator, gooc1 bitumen separa-tion from effluent was achieved by this method.
Example IIa Control - No nucleatinq a~ent added Part (la) Clay-type Tar Sand 200 g (bitumen content 5.9%) ~-Hot-water process ~
effluent 200 ml ~26.6% non-aqueous material) -These materials were admixed in a quart-size por-celain jar by rotating 10 hou~s using 5 steel 1/2l' balls. -The oil appeared present in "islands". About 150 ml of aqueous suspension (la) was separated by screening.
Part (2a) About 200 g clay-t~pe tar sand as above was added ! '' .,' to this resulting oil phase and the system admixed b~ ro-tating 30 minutes. Then 200 ml hot-waker process eE~luent ` i was added and the system again rotated for 5 hours. About 100 ml aqueous phase (2a) was separated by screening. The oil phase was rinsed twice by rotating 15 minutes with S0 ml clear water each time (3a). The results obtained are summarized below:
Separated Solids Loss on Bitumen Re-Tailings Content Ignitioncoverecl from % ~ 400 ml EEEluent and tar sands Part la 54 2 5.62 2a 54.4 19.15 -3a 41.4 10.45 16.75 g .
About 33.6 g bitumen product was recovered contai- -ning 27.6% solids and 22.5% water.
; 30 Example IIb Same as Control Example IIa, except refinery coke added Part (Ib) About 200 g clay-type tar sand (5.9% bitumen) was _7_ :', ' ' ,', ', ' ., .,'':,' ''.
~ 88~5 admixed with 25 g moist xefinery coke ground to 140 mesh (10.9g solid) by rotating in a quart-size porcelain ~ar containing 5 steel 1/2" balls for 1 hour. The total solids were in the form of spherical bodies. Abou-t 200 ml hot-water process effluent (26.6% non-aqueous solids) was added and the jar rotated for 10 hours. The oil phase was sub-stantially in one mass. About 160 ml aqueous suspension was separated by screening (lb).
Part (2b) About 200 g clay-type tar sand was added -to oil phase from (lb) and admixed by rotating 30 minutes, then 200 ml hot-water process effluent containing about 26.6%
non-aqueous solids (bitumen ~ inorganics) was adcled and the entire system rotated for 5 hours. About 185 ml aqueous suspension (2b) was separated b~ screening. The oil phase was rinsed twice by rotating for 15 minutes with 50 ml of clear water each time and screened. The washings were com-bined as tailings (3b). The results from example IIb are su~lmarized below:
Separated Solids Loss onBitumen Re-20 Tailings Content IgnitionCovered from % % 400 ml Effluent and tar sands Part lb 57.1 5.93 2b 58.4 3b 38.7 6.33 41.6 g About B8.0 g bitumen product was recovexed containing about 23.9% water and 28.2% solids which included the refi- -nery coke.
Example III -~ 30 About 200 g clay-type tar sand (5.9% bitumen) was ! admixed with 15 g moist refinery coke as in example IIb, but rotating for 30 minutes. The entlre system pelletized.
` ' ' ' ' .
: .................................................................. ' , About 400 ml effluent from the hot-water process tailings - pond was added and the suspension admixed by rotating 10 hours. About 380 ml aqueous suspension was screened off (-).
The oil phase was rinsed twice by rotating for 15 minutes with 50 ml clear water each time. The results are summarized below:
Separated Solids Loss of Bi-tu~en Re- -~
Tailings Content Ignition Covered from % 400 ml effluent and tar sands 1 46 6.18 41.1 g : .
About 74.6 g bitumen product was recovered contai-ning about 23.7P6 water and 21.2% solids (including the re-finery coke).
~xample IV
About 400 g clay-type tar sand (5.9% bitumen) was admixed with 10 g moist reinery coke as in example IIb by rotating 1 hour. Then 400 ml effluent from the hot-water process tailings pond containing about 26.6% non-aqueous solids was added and the suspension rotated for 10 hours.
A~out 300 ml aqueous tailings (1) was separated by screening. - :
The oil phase was rinsed twice by rotating for 15 minutes wi.th 100 ml and 75 ml clear water respectively. About 140 ml aqueous tailings (2) were separated from the oil phase.
The results obtained are summarized below: :~
Separated Solids Loss on Bitumen Re- ~:
Tailings Content Ignition Covered from -P6 400 ml effluent and tar sands :~ . .:
' 1 57.5 3 35 ~, 2 37.9 7.45 37.7 g ; -., - - ,.' .. .
~ 30About 68.15 g crude bitumen were separated contai- ;
.. :
,, ning 23.7% water and 21.2% solids (including refinery coke).
:, :
:..
_9_ ,' '' ~ ''.
.
. . , .' ' .
: ,.
SUMMARY OF RESULTS
Example Refinery Coke Ml Effluent l~t. Tar Bitumen Re-Nucleating Added Sand Added covered from Agent Effluent and tar sands I 10.9 g 600 600 g 5108 g IIanone (control) 400 400 g 16.75 g IIb 10.9 400 400 g 41.6 g III 6.55 400 200 g 41.1 g ~-IV 4.36 400 400 g 37.7 g By using more vigorous agitation-mixing to increase ~ .
inter-phase contacts, the processing time in the Examples could be decreased considerably.
Optionally liquid hydrocarbon fractions such as naphtha or kerosene could be added in small amounts (e.g.
1 - 2% wt. of the tar sand) to the tar sand as softening ., agent at an initial stage before contact with the effluent :.
(to accelerate the unitary organic phase formation). : - .
The method of this invention can be operated as .:. .
a side loop in a hot-water type of tar sands process, or ::
as an initial upgrading for feed to another process. :.
.,, ' ' ' .
~'. .',: ,' , , ' .,', .
':1 ' : '' ' , . .
~ '', ,,~ -10-,;
Claims (10)
1. A method for recovering tar sands bitumen con-currently from tar sands and from aqueous effluents from water-based processes for treating tar sands, comprising:
(a) recycling aqueous effluent containing waste bitumen and incorporating therewith i) hydrophobic carbon in amounts of about 0.5 to 5% by wt. based on the tar sands, and ii) tar sands in amounts yielding a fluid slurry;
(b) agitating with shearing action the ternary mixture to contact intimately the carbon with the effluent and added tar sand to cause the hydrophobic surfaces to scrub organic material from the effluent, and continuing agitation until the carbon and bitumen from the effluent forms into a unitary organic phase with the bitumen from the tar sands;
(c) separating the unitary organic phase from the aqueous phase and from the bulk of the mineral solids, and discharging aqueous effluent of reduced organic content;
and (d) recovering carbon and hydrocarbons from the organic phase.
(a) recycling aqueous effluent containing waste bitumen and incorporating therewith i) hydrophobic carbon in amounts of about 0.5 to 5% by wt. based on the tar sands, and ii) tar sands in amounts yielding a fluid slurry;
(b) agitating with shearing action the ternary mixture to contact intimately the carbon with the effluent and added tar sand to cause the hydrophobic surfaces to scrub organic material from the effluent, and continuing agitation until the carbon and bitumen from the effluent forms into a unitary organic phase with the bitumen from the tar sands;
(c) separating the unitary organic phase from the aqueous phase and from the bulk of the mineral solids, and discharging aqueous effluent of reduced organic content;
and (d) recovering carbon and hydrocarbons from the organic phase.
2. The method of claim 1 wherein the recycled effluent in (a) includes sludge phase from settled tailing ponds.
3. The method of claim 1 wherein clay-containing tar sands are included in (a) ii).
4. The method of claims 1, 2 or 3 wherein a milling action is included with the shearing action in (b).
5. The method of claims 1, 2 or 3 wherein the hydro-phobic carbon is a local refinery coke or "delayed" coke.
CLAIMS (Cont.)
CLAIMS (Cont.)
6. The method of claims 1, 2 or 3 wherein the sepa-rated organic phase from (c) is washed with aqueous liquid to remove occluded hydrophilic materials.
7. The method of claims 1, 2 or 3 operated as a side loop in the hot-water tar sands process.
8. The method of claims 1, 2 or 3 wherein the total effluent added is up to about 200% wt. or higher based on the tar sands.
9. The method of claims 1, 2 or 3 wherein the sepa-ration in (c) is carried out by screening or coarse filtra-tion.
10. The method of claims 1, 2 or 3 wherein the hydro-phobic carbon and tar sands are pre-mixed at low water con-tents before incorporating the major portion of effluent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA300,148A CA1088445A (en) | 1978-03-31 | 1978-03-31 | Tar sands bitumen recovery from aqueous effluent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA300,148A CA1088445A (en) | 1978-03-31 | 1978-03-31 | Tar sands bitumen recovery from aqueous effluent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1088445A true CA1088445A (en) | 1980-10-28 |
Family
ID=4111122
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA300,148A Expired CA1088445A (en) | 1978-03-31 | 1978-03-31 | Tar sands bitumen recovery from aqueous effluent |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1088445A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2490104A1 (en) * | 1980-09-15 | 1982-03-19 | Petrolite Corp | RECOVERY OF HYDROCARBONS FROM AQUEOUS TAIL RESIDUES |
-
1978
- 1978-03-31 CA CA300,148A patent/CA1088445A/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2490104A1 (en) * | 1980-09-15 | 1982-03-19 | Petrolite Corp | RECOVERY OF HYDROCARBONS FROM AQUEOUS TAIL RESIDUES |
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