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Rates of penetration of solvents into bituminous sand Tiedje, John Louis 1945

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RATES of PENETRATION of SOLVENTS into BITUMINOUS SAND  A T h e s i s submitted i n p a r t i a l f u l f i l l m e n t of the requirements f o r the Degree of Master of A p p l i e d Science i n the Department o f Chemical E n g i n e e r i n g  by John L o u i s T i e d j e  U n i v e r s i t y o f B r i t i s h Columbia October, 1945  The author wishes t o thank the men of the Dominion F o r e s t Products L a b o r a t o r y f o r t h e i r p a r t i n p r e s s i n g the sand samples used i n these measurements.  Contents  Introduction Experimental Apparatus Proceedure  ,...  P r o p e r t i e s of Sand . Results Conclusions .  •Figures Page 1.  Apparatus  3  2.  D e f l e c t i o n Curves  3.  Rates of P e n e t r a t i o n , Log-Log P l o t  12  4.  Rates of P e n e t r a t i o n  15  5.  Volumes P e n e t r a t e d  6.  L o n g t i t u d i n a l S e c t i o n s of Sand Permeated by Solvents  .  Tables  ...»  9  16  17  Page  1.  Sand A n a l y s i s  7  2.  Load vs D e f l e c t i o n  8  3.  Volumes of Solvents Added  11  4.  Rates of P e n e t r a t i o n  13  b.  Equations f o r Rates and Volumes of P e n e t r a t i o n  14  Rates of P e n e t r a t i o n of S o l v e n t s into Bituminous Sand  Introduction At p r e s e n t , the worlds l a r g e s t undeveloped r e s e r v e of • k  petroleum hydrocarbons i s the bituminous sand of n o r t h e r n A l b e r t a . These sands u n d e r l y an a r e a of thousands of square m i l e s i n an a p p a r e n t l y continuous bed of around 100 f e e t i n t h i c k n e s s . ( l ) Except where i t outcrops on r i v e r banks, t h i s d e p o s i t i s covered by up t o 600 f e e t of overburden.  A l l attempts a t commercial e x t r a c t i o n of the  bitumen t o date have i n v o l v e d e x c a v a t i n g the sand and p r o c e s s i n g i t e i t h e r by f l o t a t i o n o r s o l v e n t e x t r a c t i o n .  T h i s method can o n l y be  used where t h e r e i s l i t t l e o r no overburden and a s u i t a b l e d i s p o s a l ground f o r waste sand. excavate and t o handle.  The bituminous sand i s extremely d i f f i c u l t t o I t has been suggested (Dr. Seyer) t h a t i t may  be p o s s i b l e t o e x t r a c t the bitumen w i t h s o l v e n t s w i t h o u t d i s t u r b i n g the sand by methods s i m i l a r t o those used t o r e c o v e r s a l t from underground s a l t d e p o s i t s as a b r i n e s o l u t i o n .  T h i s t h e s i s i s a r e c o r d of some  p r e l i m i n a r y work done towards d e t e r m i n i n g the f e a s i b i l i t y of t h i s method of e x t r a c t i o n .  Experimental V a r i o u s s o l v e n t s were a l l o w e d t o flow r a d i a l l y i n t o u n i f o r m l y compacted c y l i n d e r s of bituminous sand.  The r a t e of p e n e t r a t i o n of the  s o l v e n t was measured under constant head. Apparatus The p r i n c i p a l p i e c e of equipment used v/as a 13 i n c h piece o f standard 4 i n c h s t e e l pipe w i t h a l o o s e l y f i t t e d a slightly  l o n g e r piece of 3 i n c h p i p e .  Two  p i s t o n mounted on  sheet metal d i s k s of the  i n s i d e diameter of the pipe were p l a c e d one a t each end to prevent  the  sand from s t i c k i n g t o the p i s t o n or base when under p r e s s u r e .  top  The  d i s k and p i s t o n had h o l e s a t t h e i r c e n t r e s to accommodate a l e n g t h of s t e e l rod 0.325 cm.  i n diameter used t o keep a c e n t r a l channel i n the  sand open d u r i n g compression.  A l e a d f i t t i n g as shown i n F i g . 1 was  pressed s o l i d l y i n t o the sand d u r i n g t h e compression. on t h i s f i t t i n g  (not shown i n F i g . 1) ensured a r i g i d c o n n e c t i o n  tween the g l a s s feed tube and the sand. was  The coarse  threads be-  The feed tube (No. 6 pyrex)  s e a l e d i n t o t h i s f i t t i n g by a p o r c e l a i n cement s e t t i n g over n i g h t .  T h i s type of c o n n e c t i o n was found necessary t o prevent s l i g h t j a r r i n g of the feed tube from s t a r t i n g a l e a k between the bitumen and the g l a s s tube.  The s o l v e n t was maintained  the top of the sand.  i n t h i s tube a t a mark 30 cm.  above  A l a r g e bulb blown i n the tube j u s t below t h i s  mark p e r m i t t e d a c o n s i d e r a b l e volume of s o l v e n t t o f l o w i n t o the sand between a d d i t i o n s without too g r e a t a l o s s of head. c o i l wound on the i n s i d e of a 6 i n c h diameter  A 35 ohm  heating  sheet metal tube 12  inches l o n g was used t o heat the sand w h i l e under compression. trude the sand, the 4 i n c h pipe h o l d i n g the sand was  To  ex-  supported on a  l o n g e r p i e c e of 5 i n c h pipe by a bushing f i t t i n g the two s i z e s o f pipe w h i l e the p i s t o n f o r c e d the sand out. The press used t o compress the sand and extrude i t from the pipe was a 200,000 pound Olsen T e s t i n g Machine i n the F o r e s t  Products  Laboratory at the U n i v e r s i t y . c e n t r a l channel i n the  T h i s machine was a l s o used to make the  sand.  Proeeedure The  sand to be loaded i n t o the t e s t pipe was heated on a  water bath u n t i l completely s o f t e n e d .  I t was c a r e f u l l y broken up w i t h  a l a r g e spoon and s m a l l lumps of non bituminous m a t e r i a l present were removed as completely as p o s s i b l e .  The sand was put i n t o the pipe a  few spoonfuls a t a time then tamped down w i t h a s h o r t l e n g t h of 1 i n c h wooden dowel t o remove as much entrapped a i r as p o s s i b l e .  1/2  One  ampere f l o w i n g through the h e a t e r kept the pipe warm w h i l e being loaded. When the pipe was f i l l e d , the h e a t e r was d i s c o n n e c t e d and the sand a l l o w e d to c o o l o v e r n i g h t . The f o l l o w i n g day the pipe was put i n a l a t h e and a cone shaped h o l e bored i n the top of the sand to accommodate the l e a d f i t t i n g . T h i s h o l e was bored w i t h a t r i a n g u l a r t o o l having the same shape as the l o n g t i t u d i n a l s e c t i o n of the l e a d f i t t i n g . formed next by f o r c i n g a 3/8  The c e n t r a l channel  was  i n c h rod ( F i g . 1) i n t o the sand t o a d i s -  tance from the bottom o f the pipe approximately equal t o the pipe radius.  The rod was e a s i l y centred on the sand w i t h , t h e a i d of the  tapered h o l e a l r e a d y bored. tar  The l e a d f i t t i n g , a f t e r being coated w i t h  sand a p p l i e d hot, was placed i n i t s h o l e .  A s t e e l rod was  i n t o the c e n t r a l channel t o keep i t open d u r i n g compression. metal d i s k was  put on and the p i s t o n put i n p l a c e .  put The  top  A pressure of 25,100  pounds (2,000 p s i ) was a p p l i e d and the sand a l l o w e d t o stand f o r 9 days.  A p r e s s u r e drop of 2 - 3,000 pounds o c c u r r e d o v e r n i g h t f o r the  f i r s t few days, d e c r e a s i n g t o a few hundred pounds tov/ards the end of the 9 day p e r i o d .  The p r e s s u r e on the sand was r a i s e d t o 25,100 pounds  once every 24 hours.  5. One ampere f l o w i n g through the h e a t e r maintained the sand a t the centre of the pipe a t about 60°C. A f t e r standing 9 days, the h e a t e r was  dis-  connected and the sand a l l o w e d t o c o o l o v e r n i g h t under pressure, t h e n removed from the p r e s s .  T h i s treatment was found t o be s u f f i c i e n t t o  b r i n g the sand c l o s e t o i t s e q u i l i b r i u m c o n d i t i o n . The top d i s k was e a s i l y removed without d i s t u r b i n g the sand a f t e r warming i t with a bunsen burner. l o o s e n i n g i t by t w i s t i n g . lead f i t t i n g .  The c e n t r a l rod was removed a f t e r  The g l a s s tube was then cemented t o the  The pipe f u l l of sand was p l a c e d i n a l a r g e g l a s s j a r i n o  a water bath (22 temperature.  C.) t o minimize the e f f e c t s of f l u c t u a t i o n s i n room  S o l v e n t was added up t o the 30 cm. mark on the feed tube  (measured from the top of the l e a d plug) from a 50 ml. b u r e t t e .  Add-  i t i o n a l volumes necessary t o r e t u r n the l e v e l t o t h i s mark were measured from a & ml. b u r e t t e a t a p p r o x i m a t e l y l o g a r i t h m i c time i n t e r v a l s .  The  s o l v e n t l e v e l would drop as much as a c e n t i m e t e r i n the i n t e r v a l s be™ tween a d d i t i o n s and hence the head was not a b s o l u t e l y c o n s t a n t . A 2 1/2 i n c h cap on the feed tube made from number 10 pyrex g l a s s t u b i n g , reduced e v a p o r a t i o n l o s s e s .  An e v a p o r a t i o n c o r r e c t i o n  was determined by measuring w i t h a cathetoraeter the drop i n l e v e l i n a capped piece of t u b i n g s i m i l a r t o the f e e d tube. At the c o n c l u s i o n of the experiment, t h e sand was extruded from the p i p e . the sand moving.  A f o r c e of 7,000 pounds was found necessary t o s t a r t About one q u a r t e r ' o f the l e n g t h of the extruded sand  was cut o f f each end w i t h a hack saw blade t h a t had been ground t o a k n i f e edge.  The blade was heated d u r i n g c u t t i n g by a gas flame t o  s o f t e n the bitumen i n the sand.  The p a r t of the sand i n t o which the  s o l v e n t had p e n e t r a t e d was found t o be v e r y s o f t and e a s i l y scooped  out  w i t h a spoon without d i s t u r b i n g the remainder of the sand.  The  volume of the c a v i t i e s so formed was measured as c a r e f u l l y as p o s s i b l e w i t h a. c e n t i m e t e r s c a l e . P r o p e r t i e s of t h e Sand. The bituminous sand used was taken from the Abasand workings e a r l y i n 1944.  I t had a bitumen content of  and a d e n s i t y i n i t s  n a t u r a l s t a t e of 1.989 grams per c.c. The d e n s i t y of the compressed sample was 1.925 grams per c.c. The e x t r a c t e d sand p a r t i c l e s were found t o have a d e n s i t y of 2.659 grams per c.c. Taking the d e n s i t y of the  bitumen as 1.022 (Seyer and K r i e b l e ) ( 2 ) The f r a c t i o n of u n f i l l e d  v o i d s may be c a l c u l a t e d as shown: In  1,000 grams bituminous sand t h e r e w i l l be: 183.6 grams of bitumen of volume  179.6 c.c.  816.4 grams of sand  307.0 c.c.  "  n  Total  486.6 c.c.  Volume of 1,000 grams of bituminous sand Natural  Compressed  502.8  519.5  Volume of sand p l u s bitumen 486.6  486.6  Volume o f u n f i l l e d v o i d s :  16.2  F r a c t i o n v o i d s of t o t a l volumes  32.9 3.2^  6.3^  c.c.  Mesh  Retained  Table I g i v e s the a n a l y s i s of the  50  0  sand as percents r e t a i n e d on  60  0.1  standard screen s i z e s .  70  0.5  the d e f l e c t i o n s caused by v a r i o u s  100  42.9  loads on the compressed sand f o r  140  45.4  both i n c r e a s i n g and decreasing  200  5.4  Passing 200  '  U.S.  Measuring  loads  g i v e s the r e s u l t s shown i n "fable I I and F i g u r e I I . The sample t e s t e d  5.7 was 11.9  inches l o n g and 12.6  square  Table I - Screen A n a l y s i s inches i n c r o s s s e c t i o n . •• For an i n c r e a s i n g l o a d the Modulus of e l a s t i c i t y , remained constant a t 272,000 p s i . a f t e r the l o a d reached 6,000 pounds (500 p s i )  B.  =  =  (19,000) (11.9) (0.066) (12.6) 272,000 p s i .  8. • LOAD (Pounds) 0  DEFLECTION  (INCHES)  Increasing  Decreasing  0  0.003  1000  0.016  0.067  2000  O.030  0.081  3000  0.043  0.090  4000  " 0.053  0.097  5000  0.061  0.104  6000  0.067  0.108  7  0.072  0.112  8  0.077  0.115  :9  0.080  0.118  10  0.084  0.1195  11  0.087  0.121  12  0&090C  0.1225  13  0.094  0.124  14  0.097 ,  0.125  ; 15  0.100  0.126  16  0.103  0.127  17  0.106  0.128  •: 18  0.;109  0.128  : 19  0.112  0.129  ;• 20  0.115  0.130  21  0W11S  0.131  22  0.122  0.132  23  0.126  24  0.129  0.133  25  0.133  0.133  1  I  Table I I . Load vs D e f l e c t i o n  ,  0.132  10. Results. The  r e s u l t s were obtained  as a s e r i e s of volumes of  added at d e f i n i t e times a f t e r the s t a r t of the experiment. were c o r r e c t e d f o r evaporation  solvent  These volumes  l o s s from the feed tube by s u b t r a c t i n g  the s o l v e n t l o s s from a s i m i l a r tube i n the same i n t e r v a l of time. long i n t e r v a l s of time when the g l a s s cap was  not removed, the  Over  evaporation  l o s s e s were 0.0029, 0.0019, and 0.0031 c.c. per hour f o r carbon t e t r a c h l o r i d e , benzene and carbon d i s u l p h i d e r e s p e c t i v e l y . removed f r e q u e n t l y to add s o l v e n t a t the beginning  When the cap  was  of a run, the evap-  o r a t i o n l o s s e s were s l i g h t l y higher but of l e s s consequence due to the much s h o r t e r i n t e r v a l s between s o l v e n t a d d i t i o n s . i n t a b l e 3 t o 25 hours c o r r e c t e d f o r e v a p o r a t i o n  The  r e s u l t s are shown  l o s s e s . Readings were  a c t u a l l y taken up t o 300 hours as shown i n F i g . 3.  CARBON TETRACHLORIDE  BENZENE  CARBON DISULPHIDS  Time  Volume  Time  Volume  Time  Volume  0.0722  0.45  0.0681  0.32  0.302  0.27  . 0.117  0.15  0.0945  0.15  0.373  0.35  0.190  0.10  0.138  0.12  0.454  0.29  0.281  0.08  0.167  0.06  0.536  0.30  i 0.330  0.06  0.236  0.10  0.636  0.27  0.471  0.09  0.282  0.03  0.732  0.21  0.563  0.03  0.350  .0.02  0.807  0.18  0.680  0.09  0.442  0.05  0.889  0.20  ; 0.850  0.10  0,592  0.05  0.983  0.31  0.985  0.06  0.825  0.07  1.17  0.28  1.14  0.11  0.985  0.12  1.38  0.23  1.53  0.12  1.34  0.11  1.65  0.43  a.08  0.20  1.83  0.10  2.08  0.37  2.39  0.10  2.50  0.10  2.51  0.36  2.71  0.10  2.78  0.05  2.99  0.36  3.10  0.12  3.30  0.07  3.55  0.36  3.55  0.17  2.83  0.06  4.41  0.50  3.98  0.10  4.32  0.05  5.20  0.43  •I 4.87  0.27  5.10  0.07  5.58  0.20  5.88  0.23  5.99  0.08  6.16  0.'31  7.05  0.33  6.83  0.06  7.04  0.40  8.17  0.41  7.83  0.08  8.19  0. 51  9.13  0.28  8.83  0.06  8.87  0.30  11.82  .0.58  11.38  0.13  16.20  3.01  14.80  0.60  12.78  0.07  16.53  0.16  19.10  0.79  14.60  0.08  20.64  1.50  0.85 23.07 0.33 23.62 Table I I I , Volumes o f Solvent Added.  1.08  ;  i  24.08  13. CARBON TETRACHLORIDE Time  Av/At  BENZENE Time  CARBON DISULPHIDE Time  Av/At  0.0426  0.332  0.0601  0.188  0.276  0.264  0.0925  0.142  0.0813  0.089  0.338  0.244  0.154  0.0596  0.116  0.103  0.414  0.211  0.236  0.0382  0.152  0.075  0.495  0.183  0.307  0.0502  0.202  0.536  0.586  0.153  0.402  0.0283  0.259  0.241  0.686  0.143  0.517  0.0142  0.316  0.109  0.771  0.142  :0.623  0.0326  0.391  0.201  0.848  0.114  0.766  0.0259  0.517  0.0123  0.936  0.108  0.918  0.0193  0.709  0.0111  1.076  0.0869  il.06  0.0280  0.905  0.0074  1.272  0.0702  1.33  0.0102  1.164  0.0113  1.515  0.0613  1.80  0.0126  1.598  0.0074  1.86  0.0526  2.08  0.0112  2.17  0.00566  2.29  0.0442  2.55  0.0107  2.64  0.00706  2.75  0.0385  2.91  0.0100  3.04  0.00522  3.27  0.0328  3,33  0.0135  3.57  0.00403  3.98  0.0306  3.77  0.00709  4.08  0.00377  4.81  0.0278  4.43  0.00978  4.71  0.0036  5.39  0.0272  5.38  0.00687  5.55  0.00342  5.87  0.0272  6.47  0.00891  6.42  0.00252  6.60  0.0239  7.61  0.0128  7.33  0.00284  7.61  0.0227  8.65  0.00952  8.33  0.00229  8.53  0.0239  10.48  0.0048.7  10.11  0.00185  12.54  0.0213  13.31  0.00570  12.08  0.0U174  16.37  0.0254  16.95  0.00496  13.69  0.00153  18.58  0.0189  21.59  22.13 0.00443 19.15 0.00143 Table IV, Rates of P e n e t r a t i o n  0.0187  '  '  .  • 14.  By d i v i d i n g the volume of s o l v e n t added at any time by the time elapsed t o the preceeding a d d i t i o n , an average r a t e of p e n e t r a t i o n i s obtained over t h i s p e r i o d .  By d i v i d i n g t h i s f i g u r e by the s u r f a c e area  of the c e n t r a l channel, the r a t e i s found per square c e n t i m e t e r ( t a b l e 4 ) . These were p l o t t e d as the instantaneous r a t e s a t the mean of the two times. The graphs of these p o i n t s on l o g - l o g paper were found t o be s t r a i g h t l i n e s .  By a p p l y i n g the method of l e a s t squares, the r e l a t i o n s  between the r a t e s and time were found.  I n t e g r a t i n g these e x p r e s s i o n s  g i v e s the volumes of s o l v e n t t h a t w i l l penetrate the sand per square i n a g i v e n time.  cm.  These equations are g i v e n i n Table 5 and the c o r r e s -  ponding graphs are shown i n f i g u r e s 4 and 5.  Carbon T e t r a c h l o r i d e -0.522 dv - 0.0199t • dt  Benzene dv = 0.00903t dt  f0.478 v = 0.0416V  v = 0.0235t  -0.615  Carbon D i s u l p h i d e -0.339 dv = 0.0484t dt 0.661  0.385 0.0732t  Table 5, liquations At the c o n c l u s i o n of the experiments l o n g t i t u d i n a l s e c t i o n s of the volumes of sand permeated by the s o l v e n t s were found to be as i n Fig.  6.  17.  Carbon T e t r a c h l o r i d e Fig. 6  Benzene  Carbon D i s u l p h i d e  L o n g t i t u d i n a l S e c t i o n s of Sand Permeated by S o l v e n t s .  These volumes, c a l c u l a t e d from the above dimensions a l l o w i n g 2 c c . f o r the c e n t r a l channels were found t o be: 132 c.c.  108 c.c.  465 c.c.  The s o l v e n t s p e n e t r a t e d i n t o these volumes i n 385 hours  292 hours  101 hours  A p p l y i n g the equations i n Table 5, the volumes of s o l v e n t which penet r a t e d the sand per sq. cm. i n these times was, 0.715  c.c.  0.209 c.c.  1.57 c.c.  18. The s u r f a c e areas of the c e n t r a l channels were: .23.08 cm  2  27.07 cm  2  19.28 cm  2  and hence the t o t a l volumes of s o l v e n t s penetrated were: 16.5 c.c.  5.7 c.c.  30.3 c.c.  Expressed as f r a c t i o n s of the volumes of sand i n t o which the s o l v e n t s had p e n e t r a t e d , these volumes were: 12.5%  5.2£  &.6%  Tne l a s t two f i g u r e s ( f o r benzene and carbon d i s u l p h i d e ) are c l o s e t o the f r a c t i o n of u n f i l l e d v o i d s i n the sand ( 6 . 3 ^ ) , the f i r s t ( f o r carbon t e t r a c h l o r i d e ) i s roughly t w i c e t h i s  figure.  Conclusions The r a t e s of p e n e t r a t i o n o f carbon t e t r a c h l o r i d e ,  benzene,  and carbon d i s u l p h i d e r a d i a l l y i n t o bituminous sand were measured under constant head.  The r a t e s were found t o be i n i t i a l l y h i g h , f a l l i n g o f f  r a p i d l y with time.  A f t e r a few hours, they became s u b s t a n t i a l l y constant  at v e r y low f i g u r e s . The volumes of s o l v e n t which penetrated t h e sand were found t o be roughly equal t o the volumes of u n f i l l e d v o i d s i n the sand w i t h t h e exc e p t i o n of carbon t e t r a c h l o r i d e . t w i c e t h a t of the u n f i l l e d v o i d s .  I n t h i s case the s o l v e n t volume was There was no evidence of s w e l l i n g w i t h  any of the t h r e e s o l v e n t s used. Bibliography 1.  E l l s , S. C.  Bituminous sands of Northern A l b e r t a , Canadian Department of Mines, Mines Branch P u b l i c a t i o n Number 632.  2.  K r i e b l e and Seyer,  A chemical I n v e s t i g a t i o n of t h e Asphalt i n the t a r Sands of Northern A l b e r t a , J o u r n a l of American Chemical S o c i e t y , V o l . 53, page 1337 (1921).  

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