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Solubility Studies on High Molecular Weight Paraffin Hydrocarbons

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Solubility Studies on High Molecular Weight Paraffin Hydrocarbons SOLUBILITY STUDIES on HIGH MOLECULAR WEIGHT PARAFFIN HYDROCARBONS OBTAINED from PETROLEUM ROD WAXES Downloaded from http://onepetro.org/trans/article-pdf/204/01/151/2176381/spe-485-g.pdf by guest on 26 September 2021 THE TEXAS CO. c. C. NATHAN BELLAIRE, TEX. T. P. 4122 ABSTRACT A few of the salient findings of his report are briefly as follows: Data are presented on the physical properties of five waxes obtained fr0111 fields in Texas and Louisiana in The term "paraffin" as used to describe this problem which "paraffin" troubles are being experi?nced. The refers to the deposit of carbonaceous material which crude paraffin was fractionated into three components. is not soluble or dispersible by the crude oil under the soluble in cold acetone, soluble in boiling acetone, and conditions where deposition occurs. The "paraffin" nor­ insoluble in boiling acetone. The acetone insoluble frac­ mally consists of high molecular weight paraffin hydro­ tion was found to consist essentially of straight chain carbons, both straight chain and branched, resins and paraffin hydrocarbons in the molecular weight range asphaltic materials of undetermined nature, occluded 525 to 700. oil and water, and possibly sand. In consistency, the deposit may vary from a soft, sticky material, to one Solubilities of the purified high molecular weight which is hard and brittle. Deposits are usually black, paraffins were determined in a number of solvents. It although lighter colors are sometimes observed. was found that in hydrocarbon solvents, including crude oil, solubilities could be calculated satisfactorily by use Under the conditions of temperature, pressure, and of ideal solubility relations. In chlorinated, and oxygen­ crude oil composition occurring in the underground ated solvents, large deviations from ideal behavior were reservoir, the paraffin is in suspension or solution in observed. These deviations could be partially corre­ the crude. As the oil flows to the surface, there is gen­ lated with the internal pressure of the solvent. erally a reduction of temperature, pressure, and the amount of dissolved gases contained in the oil. Reduc­ tion of temperature and gas break-out were shown by INTRODUCTION Reistle to be factors causing reduced solubility of the paraffin in the crude. Thus, as the crude containing A problem encountered in many producing oil fields paraffin rises to the surface and flows to storage tanks is that of "paraffin" deposition. The problem refers to at atmospheric temperature, the solubility of the par­ the deposition of material from the crude oil onto affin may be exceeded. Deposition will begin at the tubing, pumping rods, flow lines, or other material point in the system where the temperature of the sys­ contacted by the crude. This problem has been recog­ tem falls below its cloud point, and continue as long nized for nearly a hundred years, and numerous in­ as there is a further drop in the solution power of the vestigations have been reported on its causes and pre­ crude for the paraffin. The severity of the deposition vention or alleviation. One of the more comprehensive as well as the location of the bulk of the deposition, of such investigations was published by Reistle' in 1932. i.e., in subsurface or surface equipment, will depend on the amount of paraffin originally in the crude, the lReferences given at end of paper. Manuscript received in Petroleum Branch office on April 21, 1950. manner in which pressure and temperature of the crude VOL. 20~. 1955 SPE 485-G 151 .J.re reduced, and other properties of the crude and of combined and cooled at 100 C. Any material which the paraffin. precipitated on cooling of the acetone is described as As was shown by Reistle, the melting point of the "soft wax." The acetone, filtered of soft wax, was then paraffin is the principle factor influencing the solubility evaporated and the residue, soluble in cold acetone. i~ described as "oil." of a paraffin in a given solvent, the solubility decreas­ ing sharply with increased melting point, as would be Further purification of the hard waxes was effected by standard purification methods employing recrys­ expected. For hydrocarbon solvents, the main factor tallization from suitable solvents and by urea extractive which influenced solvent power was shown by Reistle crystallization."' The final products were white, flaky to be the API gravity of the solvent, solvents of high waxes of fairly sharp melting points. API gravity (or lower specific gravity) being superior Table 1 lists the properties of the five waxes in­ paraffin solvents. vestigated. The melting points of the crude paraffins were determined from cooling curves of the molten OBJECTIVE OF THE PRESENT WORK paraffins. It will be observed that the melting points of the crude paraffins vary over a rather wide range, as do the melting points of the pure paraffins prepared It was thought that the various factors described from them. The crude paraffins all contain about the above could be embodied in a single relation on a same proportion of oil (23 to 36 per cent). The per­ quantitative basis, thus making it possible to predict centage of soft wax generally falls and the percentage Downloaded from http://onepetro.org/trans/article-pdf/204/01/151/2176381/spe-485-g.pdf by guest on 26 September 2021 the solubility of any paraffin in any crude or solvent of hard wax rises with the melting point of the crude at any temperature. If it can be assumed that the sys­ paraffin. The proportion of normal paraffins in the hard tem, paraffin-crude oil (or other solvent) is an ideal wax is uniformly high at 70 per cent or greater, while solution, then the familiar relation can be used:' the proportion of hard wax in the crude paraffin is 50 per cent or more. Thus, the proportion of high molec­ 6Hf In N, = - ~ (lIT - llTm) (l) ular weight normal paraffin hydrocarbons in the crude paraffin is about 40 to 60 per cent, and this fraction w 21M. has a melting point range of only 2 a C. alsoN" = - (2) - w,IM, w,/M, , , + w IM TABLE 1 ( since for dilute solutions w,IM, « wl /M,' Paraffin A D Combining Equations I and 2 and converting to com­ M.P. of Crude Paraffin, °F. __ 152 153 176 176 184 mon logarithms, we obtain '( 66.5 67 80 80 84.5 -6H, Per Cent Oil 24 30 30 36 23 log W, = 2.303 R (lIT - 11Tm) + log M, + Per Cent Soft Wax 26 17 7.5 13 2.5 Per Cent Hard Wax_._ -- ----- ------ 49 52.5 62 51.5 74.5 M.P. of Hard Wax, °C ___ .. ~~73.5·77 80.5·81.5 89·91 88·91 85.5-89 log W , - log M t (3) Yield of n-Paraffins from Hard Wax, % _______ 85 71.5 91.5 95 78 The last equation may be verified by determining 'field of n-Paraffins from Crude Wax, %", 42 38 57 48 58 cloud points of solutions of known weights of paraffin M.P. of Pure Wax, °C _____ .76·78 79.5·82 89.5·90 89-90 90-92 in solvents of known molecular weight. If the melting S. G. of Pure Wax, 77° F.. ..... 0.961 0.965 0.949 0.974 point and heat of fusion of the paraffin are known, it is In the calculation of the solubilities of the natural then possible to calculate the amount of paraffin which paraffins in their associated crudes, the hard wax puri­ would be in solution at the measured cloud point. The fied fraction has been considered to be the key frac­ equation then may be verified by comparing the ob­ tion, since its solubility is the least of the three frac­ served and calculated values of the paraffin solubility tions prepared. Furthermore, there can be little error at the cloud point temperature. introduced by this assumption, since the hard wax fraction is in every case 50 per cent or more of the total paraffin deposit. VERIFICATION OF THE EQUATION The average molecular weight of the purified hydro­ carbon can be determined as a function of its melting DETERMINATION OF Tn" M" AND 6H, point using the data of Van Nes and Van Westen', which function is reproduced in Fig. 1 as a plot of As stated previously, the paraffins obtained from field the number of carbon atoms, n, vs the melting point deposits are complex mixtures of hydrocarbons and of the normal paraffin. The latent heat of fusion was other materials. These materials have a wide range of determined by measuring the solubilities of the purified melting points, solubilities, etc. It was decided to at­ waxes in heptane at several temperatures. Equation I tempt a partial separation and purification of the sam­ may be written: ples received. Each sample of paraffin was separated DHr DHr InN, =.------ (4) into three fractions, by successive treatments with hot R Tm R T acetone. One hundred gm of the paraffin was melted A plot of In N, vs liT gives a straight line whose and poured into 300 ml of acetone, and refluxed for slope is - DHdR and whose intercept at N, = 1.000 one hour. equals IlL,. Fig. 2 gives the solubilities of the five The boiling acetone solution was then decanted from waxes in heptane, as well as the solubility of dotria­ the undissolved paraffin. The undissolved fraction was contane for comparison. It is unfortunate that the extra­ again treated with acetone, as many times as were polations had to be extended so far from lower tem­ necessary to remove all material soluble in boiling peratures because of insufficient quantities of wax to acetone.
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