Hot Water Separation of Bitumen from Alberta Bituminous Sand K. A. CLARKA N D D. S. PASTERNACK, Research
Council of Alberta, Edmonton, Alberta, Canada
HE work reported in this
the recovery of oil from oil sands A procedure is described for determining the by “flooding.” paper arose from the unyield of biturnen in laboratory-scale hot water expected behavior of the separation of bituminous sund. The procedure LABOHATORY S~PARATION PLANT separation procedure developed AND ITSOPERATION has been used for examining the qffect of acidity b y t h e R e s e a r c h Council of or alkalinity ‘and the presence of various salts, The l a b o r a t o r y Feparation Alberta when applied to some of plant used for o b t a i n i n g the the sand from the bituminous hydroxides, and clays iri bituminous sand on data p r e s e n t e d is illustrated sand quarry beside tlie Council’s the eQiciency of separation. It was found that by the diagrammatic drawing experimental separation plant in acidity in the bituminous sand must be neutralof Figure 1. The first part of the b i t u m i n o u s s a n d area of ized in a prelimiruzry treatment before washing the plant consistcd of a size 6 Northern A l b e r t a (Z-7). Alwith hot water is eflectize. Calcium and mags t eam- j a c k e t e d “Universal” t h o u g h most of the sand put mking and kneading machine. through tlie plant separated in a nesium hydroxides were found to be particularly The mixer could be d u m p e d n o r m a l , satisfactory manner, detrirrwerrlal. Clay afleded ficpurution adversely and its contents discharged into other sand froin certain scct.ions and is indicated as the most troublesome impurity a steam-jacketed h o p p e r s e t of the quarry acted badly. The in bituminous sand .from the slandpoint of over a screw-conveyor feeding recovery of bitumen was poor, s a n d t a i l i n g s were tarry; and cornnierckzl operations. device. Tlie feedinr! device was connected to the watermuch of the bitiimen dispersed in the plant water. It was found that the trouble was citculating systoni oE the remaining part of the plant. The rest of the p l a t consistcd of a number of containers associated with the presence in the sand of soluble salts carried into the bituminous beds from the overburden by for holding a large volume of water, and pipes and a pump ground water. The salts were sodium, calcium. magnesium, for setting u p a circulation of tbis water. The principal and ferrous sulfates. Ilydrolysis of fcrroirs sulfate inadc tlie container has been termed the “separation box.” A pipe bituminous Band distinctly acid. Clay from partings and connected the hopper bottom of the separation box witli a clay masses in the bituminous sand also seemed to be associated sand pump. The pump discharged into a settling cone. with the trouble. The influence of these various salts, The nverflou. of water from the settling cone passed into a acid, and clay on bituminous sand separation ljy hot water lieater where steam u%s blown int,o it to rcstore heat lost was studied in the laboratory. For this purpose a supply of during circulation. The overflow from this heater ran bituminous sand from three localities in the bitnminoufi down a vertical pipe past the connection with the screwsand area from beds that appeared to be fairly free from salts conveyor, tlirougli a device for arresting the flow of water and clay was secured. Acid, salts, and clay were added to and giving it a whirling, mixing motion, and then rc8ntered these sands and the effect on separation noted. The resnlts the separation box at. a level a little below the surface of the have considerably clarified the problem of separation of water in it A charge of about Alberta bituminous 17 poundsof bitumisand. They are nous sand was used probably applicable for a run. It was to the p r o b l e m of placed in the mixer water s e p a r a t i o n and left there for of o i l s a n d s i n afew minutes to genoral. warm and s o f t e n . The theories that The b l a d e s were have been advanced then set in motion. to account for the Next the r e a g e n t , d i s p l a c e m e n t of dissolved in 300 cc. bitumen or mineral of water, was added oil from silica sand to the bituminous h a v e b e e n well sand. Mixing was summarized b y c o n t i n u e d for 15 Rartell and Miller m i n u t e s . If a in their recent second reagent was paper reporting u s e d , it w a s then on their s t u d y of added i n a n o t h e r the d i s p l a c e m e n t 300 cc. of water and of oil from silica by mixing c o n t i n u e d a q u e o u 8 solutions for a n o t h e r 15 (2). T h e y give ~ I T U M l N O U S SAND QUARRY A N D EXPERIMENTAL SEPARATION 1 ) U N T OF minutes. Finally a references to exFEDEnaL DEPARTMENT OF MINES A N D RESEARCH COUNCIL OF ALBERTA q u a n t i t y of h o t ON CLEARWATER RIVER perimental work on
T
1410
December, 1932
INDUSTRIAL AND ENGINEERING CHEMISTRY
water, varying from 500 to 1500 cc., the amount depending on the nature of the bituminous sand, was added to the contents of the mixer. Mixing was continued for 3 minutes. The purpose of adding the water was mainly to give the bituminous sand mixture a suitable consistency for feeding freely through the feed hopper and screw-conveyor. At the end of the final 3 minutes of mixing, the contents of the mixing machine were dumped into the hopper from where they were carried by the screw-conveyor into the stream of circulating water. Upon meeting the water stream and being mixed with it,, the bituminous sand sepa-
1411
off with the circulating stream to tlie separation box where it was collected as a secondary yield. The “total” yield was the sum of the initial and secondary yields. The difference between the initial and total yields indicated the extent of the tendency, under the experimental conditions imposed, for the bitumen to stay dispersed in the plant water. The charge of bituminous sand for a run was weighed. A 100-gram sample was taken from the mixer for analysis before any reagent solution had been added to it. The sample was analyzed for content of water and mineral matter (and bitumen by difference). Frequently a sieve analysis of the sand was made. The sum of the water and bitumen contents was determined by heating a weighed sample with kerosene until all the water was expelled, separating the solution of bitumen in kerosene from the sand by use of a Dulin Rotarex centrifuge, washing the sand with benzene while in the centrifuge, and then drying and weighing the sand, The water in the bituminous sand was determined by the A. S.T. M. distillation method for water in bituminous materials. The i n i t i a l y i e l d ,ooo of bitumen was col- Q 900 lected in a cylindrical t i n vessel with a 0 cone bottom and petcock. The tin was s e t inca h o t w a t e r bath maintained a t 75” to 80” C., for one ,t hour. It was t h e n 3 removed and w a t e r which h a d s e t t l e d 7 from the bitumen was 13 drained off t h r o u g h fi t h e p e t c o c k . The tin w i t h its content of b i t u m e n w a s w e i g h e d , t h e bi70 80 90 I O 0 /fO I20 130 14.0 tumen was mixed T€MP€/?AFUR€- OC. a FIGURE2. RELATIONSHIP BETWEEN samples of it takenfor VISCOSITYAND TEMPERATURE FOR analysis for content of BITUMENS CONTAINEDIN BITUMIwater a n d m i n e r a l NOUS SANDS 1, 2, AND 3 m a t t e r . T h e secondary yield was collected separately and weighed after settling and draining. It was assumed that the composition of the secondary yield was the same as that of the initial yield. Under good separation conditions, the secondary yield was too small for satisfactory samples for analysis. Analyses of large secondary yields under poor separation conditions indicated that the assumption was fairly correct. The “water” in the plant was a brine of common salt of from 20 to 25 per cent concentration. This brine is as good a separating medium as water. The reason for using it
2
*
FIQURE
OF LABORATORY BITUMINOUS SAND 1. DIAGRAM
SEPARATION PLAN‘P
rated and was swept into the separation box as dispersed bitumen and sand. The bitumen rose to the surface of the water and collected there as a froth. The sand sank and was carried by the circulating water through the sand pump into the settling cone. Clarified water overflowed the settling cone and returned to the separation box. The mixing machine raised the temperature of the bituminous sand to 85” C. The plant water was maintained a t 80” to 85” C. When separation proceeds satisfactorily, the bitumen comes out of its dispersion in the plant water promptly and collects on the surface of the separation box. However, there is always some that stays dispersed for some time and is carried around the plant in the circulation stream. It is as likely to appear, finally, on the surface of the water in the settling cone or water heater as in the separation box. When separation proceeds poorly, a larger proportion of the bitumen is carried out of the separation box. I n practical work this creates a troublesome condition. The bitumen accumulates on water surfaces all through the plant instead of remaining in the separation box where things are arranged for handling it. TaBLE BITUMINOUS
I.
COMPOSITIONS AND COMPOBITION Mineral matter Bitumen
s2
MECHANICAL ANALYBES OF BITUMINOUS SANDS USED I N PERCENTLGE RETlINED O N M E S H : 40 50 SO
7
INVESTIGATION
PAESINQ 200
BAND
Water
%
%
%
%
%
%
%
%
%
%
%
1 2 3
0 0.4-0.6 1.3-1.7
89.6-90.0 82.4-82.8 80.2-81.0
10.0-10.4 16.8-17.0 17.7-18.1
1.7-1.9
2.9-3.4
0.7-2.7
0.3-0.5
4.7-5.3 0.3-1.1 6.5-8.7
4.4-6.6 0.1-0.3 13-16
30-35 6.4-7.8 41-44
22-25 28-37 17-18
25-29 52-58 13-14
1.9-2.3 3.6-4.6 2.1-2.6
20
30
In the laboratory experiments, the bitumen floating on the separation box when the run had been completed was collected and termed the “initial” yield. During the following half hour or more during which preparations were proceeding for another run, bitumen separated from the plant water and appeared on the various water surfaces. Before making the next run, all this bitumen was loosened and sent
100
200
rather than water was to get a positive settling of the washing medium from the separated bitumen so that satisfactory samples for quantitative work could be secured. A surprising quantity of the washing medium becomes occluded in the bitumen as it collects in the plant. If the medium is water, it does not settle, and when the bitumen is stirred for sampling, so much free water appears that representative
INDUSTRIAL AND ENGINEERING CHEMISTRY
1412
sampling is impossible. This is because the specific gravity of the bitumen is practically the same as that of water. When concentrated brine is used, the heavy brine settles below the bitumen and can be removed. Although the bitumen still contains water and brine, this does not separate on stirring, and there is no difficulty in obtaining proper samples. Since the separated bitumen contained salt brine, part of the mineral matter found by analysis was salt. The salt content was found by extracting the total mineral matter with water, drying, and re-weighing. A determination of the acidity or alkalinity of the charge of bituminous sand at the end of the period of heating and mixing with reagent solution was made for each run. Just before the water was added to the charge in the mixer for the final 3 minutes of mixing, a 150-gram sample of the treated bituminous sand was removed. This sample was stirred with 200 cc. of hot distilled water. Some of the water was then filtered and a determination of its pH made, colorimetrically, by the indicator strips and color standards of F. & M. Lautenschlager, Munich. The ranges of analytical values for the various constituents of the three bituminous sands used in the investigation are given in Table I. The specific gravities of the bitumens in bituminous sands 1, 2, and 3, a t 25"/25" C. were 1.033, 1.027, and 1.008, respectively. The viscosities of the three bitumens over the temperature range of 80" to 135" C., expressed in Saybolt Furol seconds, are shown by Fiffure 2. The three sands contained 0.05, 0.04, and 0.02 per cent of watersoluble material, respectively. The mineral matter constituents of all three sands were composed almost entirely of silica particles. The three bituminous sands proved suitable for the purposes of the investigation. All were as free from soluble salts as could be hoped for and contained only small amounts of very fine mineral matter. On the other hand, they differed markedly in the consistency of their bitumen contents and in the grading of the sand particles. I n other words, they represented the range of variation of good grades of Alberta bituminous sand.
SEPARATION TESTS
Vol. 24, No. 12
to see whether all acted alike. The results are given in Table 11. TABLE11. EFFECTOF VARIATIONS OF ACIDITYAND ALKALINITY OF BITUMINOUS SAND ANALYEES OF SEPARATED BITUMEN Sand and silt YIELDOF TREATXEKT OF BITUMINOUS (brine- BITUMBN SAND Water Salt Sand free InitialReagents added p H content content and silt basis) total
%
%
1 2 . 8 3.1 14.3 3.4 13.4 2.3 14. l a 3.9" 11.3 2.4 10.3 2.0 12.4 1.9 17.0 1.9 19.6 1.2 22.0 1.3 21.7 1.7 15.8 3.1 1 8 . 6 3.8 13.8 2.5 18.4 2.8 16.1 3.2
%
%
17.6 4.4 3.8 12.4a 3.8 4.2 3.2 2.4 2.6 1.8 2.5 3.0 2.4 4.1 2.0 2.0
20.8 5.4 4.5 15.10 4.4 4.8 3.7 3.0 3.3 2.3 3.3 3.7 3.1 4.9 2.5 2.5
%
9s- 99 93-100 98-100 83- 97
6.7
18.1
3.9
2.1
2.7
93- 95
7.0 7.9 7.8
20.2 20.8 10.0
3.0 1.5 1.4
1.8 2.7 3.2
2.3 3.5 3.6
81- 98
3.1 3.0 2.6 2.0 4.2 3.8 6.aQ 3.6 3.2 3.3 2.2 2.6
3.7 3.3 3.2 2.4 5.2 4.5
BITUMINOUE BAND 1
0.026% HzSO4 0.013% &SO4 0.065% HzSO4 No reagent No reagent 0.013% NaOH 0.026% NaOH 0 . 0 4 0 7 NaOH 0.065% NaOH 0.078% NaOH 0 , 1 0 4 7 NaOH 0 . 0 6 0 d KOH 0.060% NazC03 NH4OH 0 . 1 6 5 7 NRsPOvlZHtO 0.23 NazHPOd. 12H2O 0.07 %, sil. of soda (calcd. t o solid) 0.04% 0.039% NaOH sil. of soda 0.065% NaOH technical 0.078% NazCO'?, technical
3.1 5.2 5.6 6.1 5.9 6.3 6.4 6.7 8.3 10.0 11.2 6.5 6.8 8.2 6.7 6.5
0 0 2 6 7 NaOH 0:045% NaOH 0.065% NaOH 0.072% NaOH 0.047 % HzSO4 0.023% HzSO4 No reaient No reagent
6.4 6.7 7.7 9.5 3.5 5.4 5.8 5.8 6.4 6.9 8.3 9.1
%
+
33- 48 32- 60
5 0 - 74
30- 55" 52- 75 85- 97 90- 9 8 91- 99 94-100 96-100 94-100
92- 95
94- 96 86- 94
BITUMINOUS BAND 2
12.7 8.6 15.8 15.8 14.3 12.9 11.9" 11.5 10.0 11.2 10.1 9.3
3.5 10 2.5 1.6 4.4 3.5 3.4" 3.0 2.7 1.5 1.0
0.8
a
BITUMINOUS BAND
0.023% HzSO4 No reagent No reagent 0.020 NaOH 0 . 0 3 9 p NaOH 0.052% NaOH ;:7;97 NaOH NaOH
5.3 6.3 6.3 6.5 6.7
8.8 9.1 11.3
15.5 20.55 15.9 18.3 8.0 15.2 15.4 18.8
8.05
4.2 3.7 3.8 2.5 2.9
84- 95 89- 99 95-100 93-100 47- 63 57- 74 65- 99s 50- 78 76- 99 92-100 93-100 91-100
4.7 5.95 4.2
16.2 5.1" 2.3
2.0 2.3 1.9 2.8
1.9 3.2 3.8 2.5
5.1
1.8
20.3 6.95 2.9 2.4 2.1 3.9 4.6 3.2
6880808678828388-
85 935 86 98 90 91 92 97
11.0 5.5 0.045% NanCOs 6.7 2.7 3.3 94-100 11.6 3.2 0.052 % NazC03 7.1 1.2 1.4 84- 95 10.3 3.0 0 . 0 9 1 7 NazCOa 8.1 2.1 2.4 85- 98 14.0 0.12 '$ NazCOs 9.1 3.3 3.8 4.6 88- 99 9.7 16.0 2.6 0.22 NanCOa 2.0 2.5 87-100 a Obtained when separation without addition of reagent was first tried; addition of 300 cc. of water and 15-minute mixing period omitted.
2
The effect of acidity and alkalinity of the bituminous sand on the efficiency of separation was examined first. All three bituminous sands were slightly acid according to the test for pH used. Sulfuric acid was added to the sands to make them more acid. Sodium hydroxide or sodium carbonate was used to neutralize them or make them alkaline. A number of alkaline reagents were used with bituminous sand 1
The effect of the presence of various salts was next examined. Since the first series of tests had shown that the bituminous sand should be nearly neutral or alkaline for good separation, charges of material into which salts were
OF PRESEXCE OF MAGNESIUM COMPOUNDS IN BITUMINOUS SAND TABLE111. EFFECT
TREATMENT OF BITUMINOUS SAND Reagents added
++ ++ ++
M g C k . 6 H ~ 0 0 . 0 7 8 7 NaOH MgCh.6H10 0.07S$ NaOH 0.091 NaOH MgC116Hz0 MgSO4.7HzO 0 . 0 7 8 7 NaOH M g S 0 ~ 7 H 2 0 0.085'-? NaOH MgSOI.7Hz0 0.11 NaOH MgO 0.0914 N a O d 0.065% MgO 0.078% NaOH
+ +
0.0457 0.065 0.085f 0.104%
9
NaOH +++ 0.091% 0 . 0 9 7 7 NaOH 0.104% NaOH + 0.104% NaOH
MgCL.6HzO MgCh.6H~0 MgCh.6HzO MgClz.6HzO
PH
9.5 9.5 9.5 9.4 8.6
9.5 11.2 11.1
ANALYSESOF SEPARATED BITUMEN , S,and and silt Water content Salt content Sand and silt (brine-free basis)
YIELDOF
BITu M E N Initial-total
%
70
%
%
%
15.6 9.9 9.8 9.1 10.0 12.1 11.7 8.9
1.6 0.5 1.4
20.8
5.1 8.3
6.7 7.9 27.0 4.0 13.4
6.2 9.3 23.4 7.4 8.9 31.7 4.5 14.8
94-100 85- 96 29- 58 82-100 73- 91 25- 47 so-100 63- 98
4.8 6.8 16.5 37.9
5.4 7.7 18.7 42.3
97- 100 83- 91 80- 97 31- 58
2.8
3.1 3.1 4.1
7.0 7.6 8.3 31.7
8.2 9.0 10.2 39.6
so-
3.1
2.4
0.8
1.6
2.6
0.3 0.4
BITUMINOTS BAND 2
9.6 9.5 9.6 9.8
9.5 9.9
1.1
8.5
1.8
10.2
1.6 1.5
BITUMINOUS S A R D 3
9.2 9.5 9.5 9.5 8.9
12.3 12.5 15.3 15.8 11.2
2.8
74737045-
95 89 93 81 67
CHEMISTRY
IIIAL A N D ENGINEERING
Vecerr,Lrr, 1932
introduced were made distinctly alkaline during treatincut. I n this way an additiveeffect from acidity as well as from the presence of salts was avoided. Cliemieally pure grades of reagents were used. The results of these experiments are presented in Tables 111 to VI. Finally, the effect of clay in the biturninous sand vas examined. Bei1tonit.e was included among the clays tested because it has been proposed as a treating reagent for preparing bituminous sanil for separation ($1). The bentonite used was a product of the American Colloid Co., of Upton, Wyo. The other two clays came froin the bituminous saud quarry in Northern Ali.ii.rta a l r e a d y m e n t i o n e d . Clay 1came from the overburdell of the quarry. Clay 2 c a m e f r o m t.lie b i t u m i n o u s sand beds. ( A chemical analysis of clay 2 was
CLOSE \'IE;\S
1,113
OP SXA1.1, t < x c V A T I O N INTO BlTUMIXoUs S A x D
ExPOsuriE
Soluble salts and coarse particles were reEach was dispersed in water, thoroughly wa,shed by ntlmerous decantations, washed through a 100mesh sieve, de-watered centrifugally, and airdrierl. The results of the tests m-it11 tire clays :are given in Table VII. The data in Table I1 leave 110 doubt as to tire bearing of acidit,y in bituminous sand on efficiency of separation. The sand must be neiirly neutral or alkaliire to s c ~ ~ a r a satiste factorily. If it is soirirwliat acid, the yield of Iiitumen is poor and t i e bitumen is sandy. The more acid the bituminous sand the more pronounced are these deficiencies. Furt,her, wiren acid bituminous sand is separated, there is a decided tendency for the bitumen to stay dispersed in the plant water. This is indiC I m F S OF BITUMSNOUS SAND Wrrsl 200 FEET EXPOSED IYD UY~Enr.Yruc cated by the wide difference b e t w e e n t t l c DEVONIAN LXXES~~ONE A T WATER'SEDOB figures showing tire initial and total yields. On the other hand, as enougli alkali is sdded as hllu!vr, in per cent: SiO,, 69.6; AL03,16.9; Fe,O,, 2.3; to the bitunrinous sand during treatment. nearly to neutralineit MgO: 2.9; SOr, 0.4; alkalies: 1.8; and ignition loss, 6.1, .A or to make it alkaline, separationeffieiencyreaches amaldmum. ceranlist rq~ortedthat the clay was a yellow-ware or stone- Recovery of bitumen becomes practically complete, tliere mare clay. It smelled at 1300' C. and w&s fused at 1450" C.) is little tendency for it to remain dispersed in the plant water, iiioved from clays 1 tilid 2.
' T n r r T M r N r "P
lleneents added
l3iT"Mln""a
.
.-
SAND
pH
Water content
++ 00.085% . 0 7 2 7 NhOH ~OH + 0.104% NNsOH $ + 0.143% NKOE 0.02B/o CaO + 0.0587 NaOH 0.065% C ~ O + o.i43% N ~ O H 0.026% CaCOn + 0 . 0 6 5 7 N s O K i .05 70 C ~ C O + , o.osa9 N ~ O I I 3 . 2 5 9 cncoj+ 0.0,5s7! N ~ O H 5 . 2 % C d T . + 0.068% NaOll 0.0357 C G I ~
0.0579 CnCh 0.10 CaCl,
%
%
%
%
+ + + + ++ + +
8
11.2 11.1
I1 2
9 9
11.(1 11.0
11.0
13.s 0.5 10.0 21.4 9.2 25.6
2.4 2.6
2.8 2.0 6 8 56.8
93.100 8 s 98 67- 00 3- 5
7.8 8.0
R.7 8.4
*lh_l)
,
1.6
1.1
1.9 8.8 1.6 8.2 0.5
1.8 1.7 1.5
6.0
3'1 .6 3 1
.
41.8
r e + 4.3 2.6 2.4
+
+
1.5,s 10.6~ 15.4"
+ 20.8"
3.5
63.3 2,s I 6" 4.2 11.7" 2.0 17.2" 2.7 23.l*
+ + + +
Initial-tutai
56- 85 5 ~ -i n
82- 93 75- 93 48- 70 31- 45
IIIIuYlnocx BIND 2
0.036 CxCln 0.085 NnOIf 0 . ici$ NaOii 0.10 CnClz 0.14 NaOH 0 . 0 2 6 % ChO 0.10 '7 NsOH 0.039% ChO 0.11 NaOI5 u . 0 2 6 ~C ~ C O , 0.065% N ~ O H 1.05 CbCOs 0.062% NnOIX 3.9 % CrCOa 0 . 0 5 2 % NilOIi
o . o 5 4 CA,
11.2
Ii,TG\r&N
%
IIITONIXUVJ
9 0 11.2
YlXL" O F
Sand and ailt
% 0 . 0 1 4 % ChCb
Gand and si1L (brine-free bsaia)
Salt content
%
11 I
11.1 11.1 11 1 11.1 Y.7
9.5
9.4
7.1 8.2 8.0 10.1 18.4 22.4 21.4
1 .B 4.1 2.4 5.5 1nrumcient yicid I/,*IRinpiel 1.5 5.6 2.6 4.7 2.4 3 7 i-1 1 1 4.0 2 0 6.6' 3.8 2.9 15.2*
+ +
4.5 6.2
8sim 80- 98
6 2
88- 97 72- 94 91-100 93- 99
5.4
+ I 4'X 3 . 5 + 9 0' 3 . 0 + 20.3'. 4 7
88- 95
.. 0 , 1 4 7 FeS0.1-7Hs0
+ NaOII + 0.11% 0.15% NeOlI
FeSO.-7lirO FeSOc7140 i -9 . 2 1 0.570 E'cSO1.7llnO 0.26 1.0 E'eso..7nio 0.88 0 . 2 4 % PeCII-6lbC 0.18% NaOH 0 . 4 2 7 FsClaGli~O 0.25% NsOIf 0.558 ~ e c i ~ ~o.vz% i i ~ N ~~O E I
:::id, 4
++ ++ +
+ + + ." 0.55% FeChBHnO + 0.29 e NaOH 0.81% FeCb-6lhO + 0.48% NaOH
0 . 2 4 7 PeCiAH*O 0.17% NsOH 0 . 4 2 $ F ~ C I ~ G H ~0O .26% N ~ O H 0.55& BeCII-6H*0 0.34% .. NaOH
BLT"Y*NO"R
s.s
14.7
8.1
10.4 9.3 14.5 12.6 14.0 16.4
9.6 11.2 11.1 11.2 9.2 9.0
6.9
0.7
0.6 0.8
0.6
3.2
0.7
1.1 1.6
&*NU
2.6 2.5 3.6 2.4 3.0 2.6 2.4 2.9
3.1 2.7 4.0 2.7
3.5
91-100 92-100 89- 99 84- 96 37- 70 83-100 80- 95 46- 77
s .7
8.0 2.8
i!
11.1
0.7
11.1 14.0
1.0 1.0
3.4 3.8 4.0
3.9 4.3 4.1
85-100 83-100 63- 92
4.2 3.3
5.8
7.4
'76- 88 7s- 92
,n-PVldlNO"Y
6.5 0.7
t
14.9
Bii."MiiiOVB
ii n 11.2
.. ZIN"
17.0 15.1
QAN" i
4.6
5.6
It will be noted that, again, sodium hydroxide w&s used and it becomes comparatively free from retained nrineral matter. All of the alkaline cornpounds of sodium, potassium, in all eases but one to make the bituminous sand alkaline. and ammonium tried appear to serve about equally well as The result of this procedure was that the magnesium or calcium compound present after treatment, and when the neutralizing reagents. Each of the bituminous sands gave an acid test, and coli- treated sand was waslied to cause separation, was magnesium or calcium hydroxide. So it would appear that it was the siderable alkali had to be added to make them neutral. It will be noted that there were two tests for each hitu- hydroxides that affected separation adversely. If sodium minous sand in which no reagent was added. The second carbonate had been used, instead of sodium hydroxide, the of each pair fitted into the series, but the first did not. Fur- final compoimd present would have been magnesium or calcium carbonate. and since calcium carbonate was not ther mention of this will be made. found detrimental in small The effect of adding mag quantity, it is l i e l y that no n e s i u m compounds t o t h e marked bad effect of magbituminous sand (Table 111) n e s i u m or c a l c i u m comwaa striking. The presence p o u n d s would have been of a few hundredths of a per noted. The two experiments cent of the chloride, sulfate, in which s o d i u m carbonate or oxide resulted in increased was used support this idea. mineral matter content of the Bituminous sand containing separated b i t u m e n and in0.78 per cent of magnesium creased secondary yields with chloride and made alkalin? sands 1 and 2. Sand 3 was with sodium carbonate gave not very susceptible to ma,ga clean separated b i t u m e n nesium chloride, but its inbut a poor yield oE it. When fluence WRS adverse to good 0.13 per cent of calcium oxide s e p a r a t i o n . It sliould be nas present and sodium carnoted that sodium hydroxide bonate used, hot,li the yield was used in a11 cases but one and cleanliness of the sepato make the bituminous sand rated bitumen were good. alkaline. The data in Table V show The e f f e c t of calL' 'ium that iron salts are not very chloride and calcium oxide bad in their efiect on separawas s i m i l a r to that of the tion. One-half per cent of magnesium compounds Serrous sulfate increased the (Table IV). Small amounts tendency for the bitumen to of them spoiled the separastay in t h e p l a n t urater. tion of all three bituminous One per cent caused decided sands. The effect of Lalcium decrease in yield as well as c a r b o n a t e , h o w e v e r , was niore pronounced dispersion rather different. Amountsof of b i t n m e n . The effect of it, Nhicli in the case of the ferric chloride was much the soluble salts or oxide were same. r u i n o u s , caused no harm. Sodium sulfate (Table VI) Several per cent of calcium caused increased dispersion of carbonate caused little dethe hiturnen and a decrease crease in recovery of bitumen of yield when present to the with sands 2 and 3, but wit11 extent of one per cent or more. sands 1 and 2 a large proporIt did not affect the cleanlition of the calcium carbonate ness of the separation. Soadded was retained by the dium c h l o r i d e , h o w e v e r , separated bitumen. The excaused retention of mineral planation for its not being rematter by tbe bitumen ss well tained by the bitumen from ONE Humam FEET(IF BITUMINOUEI SANDST~ATA ON aa increased dirrpersion. TBIB~TARY OF ATHAHASKA RIVER sand 3 would be interesting. ~~
~
December, 1932
1ND U S T R I
i\
1.
h ND
E N G I N E E I< 1 N G C t i E 21 1 S T R Y
1415
The presence of bentonite in the bituminous sand affected and, as has just been stated, its obvious function is to render separation adversely (Table VU). Ealf of one per cent of the bituminous sand neutral or alkaline. Other conditions it decreased the yield of bitumen and increased the tendency which might be expected to be important have little effect. for the bitumen to stay in the plant water. One to two Tests have shown that it does not matter much whether the per cent caused marked loss of yield and dispersion of bitumen sand is mixed with alkaline reagent solution at a, high or as well as increased content of mineral matter. The two moderate temperatiire, or whether the treated sand is hot other clays had much the same influence as bentonite on or only warm when it is finally washed. It does not matter the separation, but they had to be present in the bituminous much whether the plant water is at a temperature of 85' or sand in much larger 50" C., whether it is quantities for a n acid or alkaline, equal effect. w h e t h e r it is plain Attention h a s alwater or brine of any ready been drawn to concentration, nr the two sets of figures whether it is clean or loaded with snsin Table IT for separat i o n o f bituminous pended clay and silt. sand to which no reIf t h e b i t u m i n o u s agent w a s a d d e d . sand is first treated to make it neutral or The first set was obalkaline, the rest of tained when separe tire p r o c e d u r e will tion without addition of reagent was first cause no trouble. tried, and it was obNeutral or alkaline served that the figures c o n d i t i o n s are a p did n o t f i t i n w i t h parently the c o n d i those resulting from tions u n d e r which tesks in wliicli acid or thines arranee them&ali had been added F I ~ I N BARRELS G WITW HOT, SEPARATED BITUMEN AT EXPERIMENTAL selves favorably for to the b i t u m i n o u s SSPAkMnON h & N T separation, or it may sand. There seemed turn out that they are the conditions under which things-arrange themselves favor110 good reason why they sliould not have fitted. On checking over the experimental procedure, it was found that there was a ably quickly enough for good separation by the procedure used difference in t,he case of these runs. Since no reaEent was in this investieation or in nractical bituminoussandseDaration. added, tilo addition of the 300 ec. of water and the 15-minute The fact t b z the bituminous sand has to he mi,& with period of mixing had been omitted. When the bituminous water for a longer time than 3 minutes at pH 5.8 to 6.3 is sand had reached the proper temperature, the final addition of significant and gives an obvious lead for furtber work. A 500 to 1500 ec. of watcr had been made, mixing had been test showed that 3 minutes of mixing with water are sufficient continued for 3 minutcs, and tbe chargc then dumped for at pIl 9.5. separation. On repeating the experiments but adding 300 cc. of water and mixing for 15 minutes, the second sot of the pairs of figures was oht,ained. These fitted into the table properly. ~~
TABLE
~
VI. EFFECT OF SODlUX SULFATE AND SODIUM CHLoilIDE IN B~TWMINOUS SAND
.~. . . . . .
silt OP Water Salt Sand (brio- BI?D,XIM.N T n a ~ n i m OF s ~ Urrii~rroosS A N D coo- o m - and free InitialReaiienis sdded pH tent tent silt baais) total
% nnd
Y1m.o
5dCisyl+0.13%~ON
7.5% Clay 1
+ 0.17Y
+
NaOU
104 Clay 1 0 . 2 1 9 NnOH 5 9 C l ~ y Z+0.11$ NaOH 1 0 % ~ 1+ ~ o ~ .2 ~ ~ % N
%
%
%
~
9.3 9.3 9.6 9.5 o9 . H 5
20.4 1 . 6 25.2 6 . 5 1 2 . 0 5.4 11.9 0 . 2
2 . 1 2.7 4 . 0 5.9 4 . 9 6.0
17.2
3.7 1.8 2.8
16.4
11.5 14.1
2.2 2 . 5
0.4 4.1 0.3
0.3 0.8
4.9 4.4 2.0 3.3
62- 91 27- 67 SO- 78
82-91 73- 83 6%- 78 74- 85 67- so
BITUMINYOB B I N D I
." r,lTObllNODB BIND t
1 . 3 % NaCl 2 . 6 % NaCl
%
HLTUIIIIOOB S h N D 1
0 . 5 % U a i * t v e j ~ e + O . O 5 9 Y NeOH 8 . 0 1.07 Hontonlte+O 0 4 9 q N a O l Z 7 + 2 . 0 0 I k n t o n i t a C O 059 aNnOlf 7 +
..
-
Y
++ 0.0654 NaO1I O.(IS2& NaOH
9.5 6.9
U.7 7.3
2.2 2.0
10.0
IP.5
11.4 74- 94 13.8 74-100
I'l3ACTICAL ~ I T i l M I N O U ESAND SEPARATlON
0 . 5 4 Renton?te+0.0599' NsOH 7.0 1 , 0 ~ R e n t o n ! t e + O . O S Y ~ N a O H6 . 7 2.0% Ilenlonite+0.!X5%NaOH 7 . 0 3 7
