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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 int o BITUMINOUS SAND A Thesis 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 Applied Science i n the Department of Chemical Engineering by John Louis Tiedje U n i v e r s i t y of B r i t i s h Columbia October, 1945 The author wishes to thank the men of the Dominion Forest Products Laboratory f o r t h e i r part i n pressing the sand samples used i n these measurements. Contents Introduction Experimental Apparatus Proceedure ,... Properties of Sand . Results Conclusions . •Figures Page 1. Apparatus 3 2. D e f l e c t i o n Curves . 9 3. Rates of Penetration, Log-Log P l o t 12 4. Rates of Penetration 15 5. Volumes Penetrated ...» 16 6. L o n g t i t u d i n a l Sections of Sand Permeated by Solvents 17 Tables Page 1. Sand Analysis 7 2. Load vs D e f l e c t i o n 8 3. Volumes of Solvents Added 11 4. Rates of Penetration 13 b. Equations f o r Rates and Volumes of Penetration 14 Rates of Penetration of Solvents i n t o Bituminous Sand Introduction At present, the worlds l a r g e s t undeveloped reserve of k • petroleum hydrocarbons i s the bituminous sand of northern A l b e r t a . These sands underly an area of thousands of square miles i n an apparently continuous bed of around 100 feet i n thick n e s s . ( l ) Except where i t outcrops on r i v e r banks, t h i s deposit i s covered by up to 600 feet of overburden. A l l attempts at commercial e x t r a c t i o n of the bitumen to date have involved excavating the sand and processing i t e i t h e r by f l o t a t i o n or solvent e x t r a c t i o n . This method can only be used where there i s l i t t l e or no overburden and a s u i t a b l e disposal ground f o r waste sand. The bituminous sand i s extremely d i f f i c u l t to excavate and to handle. I t has been suggested (Dr. Seyer) that i t may be possible to extract the bitumen with solvents without d i s t u r b i n g the sand by methods s i m i l a r to those used to recover s a l t from underground s a l t deposits as a brine s o l u t i o n . This t h e s i s i s a record of some preliminary work done towards determining 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 Various solvents were allowed to flow r a d i a l l y i n t o uniformly compacted c y l i n d e r s of bituminous sand. The rate of penetration of the solvent was measured under constant head. Apparatus The p r i n c i p a l piece of equipment used v/as a 13 inch piece of standard 4 inch s t e e l pipe with a l o o s e l y f i t t e d p i s t o n mounted on a s l i g h t l y longer piece of 3 inch pipe. Two sheet metal disks of the i n s i d e diameter of the pipe were placed one at each end to prevent the sand from s t i c k i n g to the p i s t o n or base when under pressure. The top dis k and p i s t o n had holes at t h e i r centres to accommodate a length of s t e e l rod 0.325 cm. i n diameter used to keep a c e n t r a l channel i n the sand open during compression. A lead 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 during the compression. The coarse threads 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 connection be-tween the glass feed tube and the sand. The feed tube (No. 6 pyrex) was sealed 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 night. This type of connection was found necessary to 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 leak between the bitumen and the glass tube. The solvent was maintained i n t h i s tube at a mark 30 cm. above the top of the sand. A large bulb blown i n the tube j u s t below t h i s mark permitted a considerable volume of solvent to flow i n t o the sand between additions without too great a l o s s of head. A 35 ohm heating c o i l wound on the i n s i d e of a 6 inch diameter sheet metal tube 12 inches long was used to heat the sand while under compression. To ex-trude the sand, the 4 inch pipe holding the sand was supported on a longer piece of 5 inch pipe by a bushing f i t t i n g the two s i z e s of pipe while the p i s t o n forced the sand out. The press used to compress the sand and extrude i t from the pipe was a 200,000 pound Olsen Testing Machine i n the Forest Products Laboratory at the U n i v e r s i t y . This machine was also used to make the central channel i n 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 softened. I t was c a r e f u l l y broken up with a large spoon and small 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 at a time then tamped down with a short length of 1 1/2 inch wooden dowel to remove as much entrapped a i r as p o s s i b l e . One ampere flowing through the heater kept the pipe warm while being loaded. When the pipe was f i l l e d , the heater was disconnected and the sand allowed to cool overnight. The f o l l o w i n g day the pipe was put i n a lathe and a cone shaped hole bored i n the top of the sand to accommodate the lead f i t t i n g . This hole was bored with 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 lead f i t t i n g . The c e n t r a l channel was formed next by f o r c i n g a 3/8 inch rod ( F i g . 1) into the sand to a d i s -tance from the bottom of the pipe approximately equal to the pipe rad i u s . The rod was e a s i l y centred on the sand with,the a i d of the tapered hole already bored. The lead f i t t i n g , a f t e r being coated with t a r sand applied hot, was placed i n i t s hole. A s t e e l rod was put i n t o the c e n t r a l channel to keep i t open during compression. The top metal disk was put on and the p i s t o n put i n place. A pressure of 25,100 pounds (2,000 psi) was applied and the sand allowed to stand for 9 days. A pressure drop of 2 - 3,000 pounds occurred overnight f o r the f i r s t few days, decreasing to a few hundred pounds tov/ards the end of the 9 day period. The pressure on the sand was r a i s e d to 25,100 pounds once every 24 hours. 5. One ampere flowing through the heater maintained the sand at the centre of the pipe at about 60°C. A f t e r standing 9 days, the heater was d i s -connected and the sand allowed to cool overnight under pressure, then removed from the press. This treatment was found to be s u f f i c i e n t to bring the sand close to i t s e q u i l i b r i u m condition. The top disk 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. The c e n t r a l rod was removed a f t e r loosening i t by t w i s t i n g . The glass tube was then cemented to the lead f i t t i n g . The pipe f u l l of sand was placed i n a large glass j a r i n o a water bath (22 C.) to 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 temperature. Solvent was added up to the 30 cm. mark on the feed tube (measured from the top of the lead plug) from a 50 ml. burette. Add-i t i o n a l volumes necessary to r e t u r n the l e v e l to t h i s mark were measured from a & ml. burette at approximately logarithmic time i n t e r v a l s . The solvent l e v e l would drop as much as a centimeter i n the i n t e r v a l s be™ tween additions and hence the head was not absolutely constant. A 2 1/2 inch cap on the feed tube made from number 10 pyrex glass tubing, reduced evaporation l o s s e s . An evaporation c o r r e c t i o n was determined by measuring with a cathetoraeter the drop i n l e v e l i n a capped piece of tubing s i m i l a r to the feed tube. At the conclusion of the experiment, the sand was extruded from the pipe. A f o r c e of 7,000 pounds was found necessary to s t a r t the sand moving. About one quarter'of the length of the extruded sand was cut o f f each end with a hack saw blade that had been ground to a kni f e edge. The blade was heated during c u t t i n g by a gas flame to soften the bitumen i n the sand. The part of the sand i n t o which the solvent had penetrated was found to be very s o f t and e a s i l y scooped out with 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 possible with a. centimeter scale. Properties of the Sand. The bituminous sand used was taken from the Abasand workings ea r l y i n 1944. I t had a bitumen content of and a density i n i t s n a t u r a l state of 1.989 grams per c.c. The density of the compressed sample was 1.925 grams per c.c. The extracted sand p a r t i c l e s were found to have a density of 2.659 grams per c.c. Taking the density of the bitumen as 1.022 (Seyer and Krieble)(2) The f r a c t i o n of u n f i l l e d voids may be c a l c u l a t e d as shown: In 1,000 grams bituminous sand there w i l l be: 183.6 grams of bitumen of volume 179.6 c.c. 816.4 grams of sand " n 307.0 c.c. Total 486.6 c.c. Volume of 1,000 grams of bituminous sand Natural Compressed 502.8 519.5 c.c. Volume of sand plus bitumen 486.6 486.6 Volume of u n f i l l e d voids: 16.2 32.9 F r a c t i o n voids of t o t a l volumes 3.2^ 6.3^ Mesh Retained Table I gives the a n a l y s i s of the 50 0 sand as percents retained on U.S. 60 0.1 standard screen s i z e s . Measuring 70 0.5 the d e f l e c t i o n s caused by various 100 42.9 loads on the compressed sand f o r 140 45.4 both increasing and decreasing loads 200 5.4 ' gives the r e s u l t s shown i n "fable I I Passing and Figure I I . The sample tested 200 5.7 was 11.9 inches long and 12.6 square Table I - Screen Analysis inches i n cross section. • For an increasing load the Modulus of e l a s t i c i t y , remained constant at 272,000 p s i . a f t e r the load reached 6,000 pounds (500 psi) B. = (19,000) (11.9) (0.066) (12.6) = 272,000 p s i . 8. • LOAD DEFLECTION (INCHES) (Pounds) Increasing Decreasing 0 0 0.003 1000 0.016 0.067 2000 O.030 0.081 3000 0.043 0.090 4000 " 0.053 0.097 1 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 I 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 , 0.132 24 0.129 0.133 25 0.133 0.133 Table I I . Load vs D e f l e c t i o n 10. Results. The r e s u l t s were obtained as a s e r i e s of volumes of solvent 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. These volumes were corrected f o r evaporation loss from the feed tube by subtracting the solvent loss from a s i m i l a r tube i n the same i n t e r v a l of time. Over long i n t e r v a l s of time when the glass cap was not removed, the evaporation losses 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 disulphide r e s p e c t i v e l y . When the cap was removed frequently to add solvent at the beginning of a run, the evap-o r a t i o n losses were s l i g h t l y higher but of l e s s consequence due to the much shorter i n t e r v a l s between solvent a d d i t i o n s . The r e s u l t s are shown i n t a b l e 3 to 25 hours corrected f o r evaporation l o s s e s . Readings were a c t u a l l y taken up to 300 hours as shown i n F i g . 3. CARBON TETRACHLORIDE BENZENE CARBON DISULPHIDS Time 0.0722 . 0.117 0.190 0.281 i 0.330 0.471 0.563 0.680 ; 0.850 ; 0.985 1.14 1.53 a.08 2.39 2.71 3.10 3.55 3.98 •I 4.87 5.88 7.05 8.17 i 9.13 11.82 14.80 19.10 24.08 Volume 0.45 0.15 0.10 0.08 0.06 0.09 0.03 0.09 0.10 0.06 0.11 0.12 0.20 0.10 0.10 0.12 0.17 0.10 0.27 0.23 0.33 0.41 0.28 .0.58 0.60 0.79 0.85 Table I I I , Time 0.0681 0.0945 0.138 0.167 0.236 0.282 0.350 0.442 0,592 0.825 0.985 1.34 1.83 2.50 2.78 3.30 2.83 4.32 5.10 5.99 6.83 7.83 8.83 11.38 12.78 14.60 Volume 0.32 0.15 0.12 0.06 0.10 0.03 .0.02 0.05 0.05 0.07 0.12 0.11 0.10 0.10 0.05 0.07 0.06 0.05 0.07 0.08 0.06 0.08 0.06 0.13 0.07 0.08 23.07 0.33 Volumes of Solvent Added. Time 0.302 0.373 0.454 0.536 0.636 0.732 0.807 0.889 0.983 1.17 1.38 1.65 2.08 2.51 2.99 3.55 4.41 5.20 5.58 6.16 7.04 8.19 8.87 16.20 16.53 20.64 23.62 Volume 0.27 0.35 0.29 0.30 0.27 0.21 0.18 0.20 0.31 0.28 0.23 0.43 0.37 0.36 0.36 0.36 0.50 0.43 0.20 0.'31 0.40 0. 51 0.30 3.01 0.16 1.50 1.08 CARBON TETRACHLORIDE BENZENE 13. CARBON DISULPHIDE Time 0.0426 0.0925 0.154 0.236 0.307 0.402 0.517 :0.623 0.766 0.918 il.06 1.33 1.80 2.08 2.55 2.91 3,33 3.77 4.43 5.38 6.47 7.61 8.65 10.48 13.31 16.95 21.59 Av/At 0.332 0.142 0.0596 0.0382 0.0502 0.0283 0.0142 0.0326 0.0259 0.0193 0.0280 0.0102 0.0126 0.0112 0.0107 0.0100 0.0135 0.00709 0.00978 0.00687 0.00891 0.0128 0.00952 0.0048.7 0.00570 0.00496 0.00443 Table Time 0.0601 0.188 0.0813 0.089 0.116 0.103 0.152 0.075 0.202 0.536 0.259 0.241 0.316 0.109 0.391 0.201 0.517 0.0123 0.709 0.0111 0.905 0.0074 1.164 0.0113 1.598 0.0074 2.17 2.64 3.04 3.57 4.08 4.71 5.55 6.42 7.33 8.33 0.00566 0.00706 0.00522 0.00403 0.00377 0.0036 0.00342 0.00252 0.00284 0.00229 10.11 0.00185 12.08 0.0U174 13.69 0.00153 19.15 0.00143 IV, Rates of Penetration Time 0.276 0.338 0.414 0.495 0.586 0.686 0.771 0.848 0.936 1.076 1.272 1.515 1.86 2.29 2.75 3.27 3.98 4.81 5.39 5.87 6.60 7.61 8.53 12.54 16.37 18.58 22.13 Av/At 0.264 0.244 0.211 0.183 0.153 0.143 0.142 0.114 0.108 0.0869 0.0702 0.0613 0.0526 0.0442 0.0385 0.0328 0.0306 0.0278 0.0272 0.0272 0.0239 0.0227 0.0239 0.0213 0.0254 0.0189 0.0187 ' ' . • 14. By d i v i d i n g the volume of solvent added at any time by the time elapsed to the preceeding a d d i t i o n , an average rate of penetration i s obtained over t h i s period. By d i v i d i n g t h i s f i g u r e by the surface area of the c e n t r a l channel, the rate i s found per square centimeter (table 4). These were p l o t t e d as the instantaneous rates at the mean of the two times. The graphs of these points on log- l o g paper were found to be s t r a i g h t l i n e s . By applying the method of l e a s t squares, the r e l a t i o n s between the rates and time were found. Integrating these expressions gives the volumes of solvent that w i l l penetrate the sand per square cm. i n a given time. These equations are given i n Table 5 and the corres-ponding graphs are shown i n f i g u r e s 4 and 5. Carbon Tetrachloride -0.522 dv - 0.0199t • dt f0.478 v = 0.0416V Benzene dv = 0.00903t dt -0.615 0.385 v = 0.0235t Carbon Disulphide -0.339 dv = 0.0484t dt 0.661 0.0732t Table 5, liquations At the conclusion of the experiments l o n g t i t u d i n a l sections of the volumes of sand permeated by the solvents were found to be as i n F i g . 6. 17. Carbon Tetrachloride Benzene Carbon Disulphide F i g . 6 L o n g t i t u d i n a l Sections of Sand Permeated by Solvents. These volumes, c a l c u l a t e d from the above dimensions allowing 2 cc. f o r the c e n t r a l channels were found to be: 132 c.c. 108 c.c. 465 c.c. The solvents penetrated i n t o these volumes i n 385 hours 292 hours 101 hours Applying the equations i n Table 5, the volumes of solvent which pene-t 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 surface 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 solvents 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 solvents had penetrated, these volumes were: 12.5% 5.2£ &.6% Tne l a s t two fi g u r e s ( f or benzene and carbon disulphide) are close to the f r a c t i o n of u n f i l l e d voids 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 twice t h i s f i g u r e . Conclusions The rates of penetration of carbon t e t r a c h l o r i d e , benzene, and carbon disulphide r a d i a l l y i n t o bituminous sand were measured under constant head. The rates were found to be i n i t i a l l y high, 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 very low f i g u r e s . The volumes of solvent which penetrated the sand were found to be roughly equal to the volumes of u n f i l l e d voids i n the sand with the ex-ception of carbon t e t r a c h l o r i d e . In t h i s case the solvent volume was twice that of the u n f i l l e d voids. There was no evidence of swelling with any of the three solvents used. Bibliography 1. E l l s , S. C. Bituminous sands of Northern A l b e r t a , Canadian Depart-ment 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 the Asphalt i n the ta r Sands of Northern A l b e r t a , Journal of American Chemical Society, V ol. 53, page 1337 (1921). 


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