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PATENT OFFICE 2,159,312 PROCESS for BREAKING OL-N-WATER, TYPE PETROLEUM EMULSIONS Carles M

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PATENT OFFICE 2,159,312 PROCESS for BREAKING OL-N-WATER, TYPE PETROLEUM EMULSIONS Carles M Patented May 23, 1939 2,159,312 UNITED STATES PATENT OFFICE 2,159,312 PROCESS FOR BREAKING OL-N-WATER, TYPE PETROLEUM EMULSIONS Carles M. Blair, Jr., Webster Groves, Mo., assign or to fhe Tret-O-Lite Company, Webster Groves, Mc., a corporation of Missouri No orawing. Application December 13, 1937, Serial No. 179,471 1. Claims. (CI. 196-4) This invention relates to the treatment of a tive colioid or equivalent thereof. To this extent, certain peculiar kind of naturally occurring crude although not necessarily due to this factor alone, oil emulsion and has for its main object to provide these particular or peculiar oil field emulsions, a practicable process for separating the water ianiely, the naturally occurring oil-in-water ... and oil contained in said peculiar emulsion. emulsions having a significant proportion of dis 5 The vast majority of petroleum emulsions are of persed phase and a substantially complete absence the Water-in-oil type and comprise fine droplets Of a protective colloid or equivalent substance of naturally occurring waters or brines dispersed appear to be substantially a new type of emulsion in a more or less permanent state throughout the that requires a new method of treatment, in 10. oil, which constitutes the continuous phase of the order to separate them economically and rapidly O emulsion. They are obtained from producing into their component parts, and thus permit the wells and from the botton of oil storage tanks, recovery of dry or merchantable oil, and are commonly referred to as "cut oil', 'roily It is to be emphasized that the external phase oil', 'emulsified oil', and 'bottom settlings'. The o: continuous phase of these peculiar naturally 5 preSent invention is not concerned with the treat CCCurring petroleum emulsions consists of water 5 ment of such conventional water-in-oil type pe or a relatively dilute brine that apparently does troleum emulsions. not froth, that apparently has a normal surface In certain oil fields, there are produced crude tension, and which on evaporation, does not ap oil emulsions which, instead of being of the pear to yield a Substance having the character 20 Water-in-oil type, are of the oil-in-water type, istic properties of hydrophile protective colloids 20 and comprise fine droplets of naturally occurring or common emulsifying agents for the oil-in-water petroleum oil dispersed in a more or less perma type of emulsion. nent State throughout the water or relatively The copending application of Charles M. Blair, dilute brine, which constitutes the continuous Jr. and Charles Clinton Rogers, Jr., Serial No. phase of the emulsion. As far as I am aware, 179,472, filed December 13, 1937, discloses that 25 the expressions “cut oil', 'roily oil', etc. com these unusual emulsions may be separated into monly used to designate conventional water-in their component parts of oil and water by treat oil emulsions, are not used to designate or refer illent with a minimal concentration of a multi to the peculiar oil-in-Water petroleum emulsions poiar, substantially un-ionized hydrophile colloid. 30 which my improved process is capable of Success I have discovered that these unique emulsions 30 fully treating to recover the oil contained in having these peculiar characteristics can be Sae. treated more rapidly and at a lower temperature Although such peculiar emulsions are recog and with the separation of Somewhat clearer oil nized technically as being of the oil-in-water and water phases, if they are treated with a mix 35 type, their physical-chemical constitution is only ture containing a multipolar, Substantially un 35 partially understood. It is recognized that one ionized hydrophile colloid of the kind hereinafter may have emulsions of the oil-in-water type in described, and an electrolyte of the kind herein which the dispersed phase is present to the ex after described. tent of a few tenths of 1%, or less, in which the Effective hydrophile colloids which may be used stability of the emulsion appears to be predicated in the mixture employed as the treating agent or 40 On factors other than the presence of a sig dealsifying agent of my process, are those which nificant amount of a conventional emulsifier; give rise only to very small electrical effects when that is, factors such as particle size, electric adsorbed at interfaces. In general, they are charge, etc. It is also known that emulsions of either the weakly ionized, amphioteric, or un the oil-in-water type may exist in which the ionized hydrophile colloids, and are further char 45 - dispersed phase represents a significant propor acterized by the fact that they contain a multi tion of the total emulsion; for instance, from 3% plicity of polar groups, such as -COOH,-COOR, to 5% of the emulsion, up to 60% to 70%, or R-O-R, -OH, -NH2, -NRH, NR2 -CO-NH-, etc., even more, provided that there is a protective where R is a univalent organic radical. It 50 colloid or conventional emulsifying agent present. may happen that all the polar groups which are 50 However, as far as I am aware, technologists have present in a hydrophile colloid are of the same not been confronted with a type of oil-in-Water kind, or they may be of substantially different emulsion in which there was dispersed a signifi kinds, or they may be of several varieties which cant portion of the oily phase in What appears to are generally related to each other. Such hydro SS be a substantially complete absence of a protec phile colloids are characterized by the fact that 55 2 2,159,312 the polar groups are not segregated at a particu loid of the kind previously described are: NaCl, lar point but are distributed more or leSS uni KC, HCl, H2SO4, HNO3, CaCl2, MgCl2, Ca(NO3)2, formly throughout the molecule, so that their FeCl3, Th(NO3)4, Ce(SO4)2, Mg(NO3)2, MgSO4, Solution or sol contains a body having what ap Al2(SO4)3, AlCl3, FeSO4, Fe(NO3)3, methylene pears to be a more or less uniformly hydrated Sur blue, fuchsin, many other basic dyes, perlargon face, although the chemical structure of the idin chloride, cetyl pyridinium bromide, toluidine molecule indicates that the hydrated Zones must hydrochloride, diphenyl guanidine hydrochlo be interrupted or alternated by non-hydrated ride, benzyl pyridinium chloride, many other Zones or groups of non-polar or hydrophobe char Water Soluble Salts of strong or relatively strong O acter. organic bases of moderately high molecular 0 This feature of distributed hydration along weight, etc. Because of their low cost and with the concomitant property of distributed availability, salts of alkaline earth metals and hydrophobe characteristics, distinguishes these of iron, such as CaCl2, MgCl2, MgSO4, BaCl2, and materials from other hydrophile colloids such as FeSO4, are usually employed. 5 soaps, the molecules of which are considered as The ratio of the hydrophile colloids to elec being made up of one definitely polar hydrated trolyte which should be added to a given emul 15 end, and one definitely non-polar, non-hydrated sion to give the optimum results, will depend end. Inasmuch as these hydrophile colloids Con Somewhat upon the emulsion, the hydrophile tain more than one polar group, they may be colloid, and the electrolyte employed. Some referred to as 'multipolar' and may be defined as times optimum results are obtained when ten 20 the multipolar, substantially un-ionized type of times as much hydrophila colloid is used as elec hydrophile colloid. The expression “substantial trolyte. In other cases, best results are obtained ly un-ionized' as herein used is intended to in when only one-tenth or one-twentieth or even clude the previously described hydrophile colloids one-hundredth as much hydrophile Colloid as 2 5 which give rise to minimal electrical effects. electrolyte is used. When the hydrophile colloid 25 The colloidal dispersions of these hydrophile used is glue and when the electrolyte used is colloids are relatively non-sensitive to electro CaCl2, it has been found that the mixture con lytes, and they often form gels or very viscous, taining one part of glue to four parts of CaCl2 aqueous dispersions. Materials such as Soaps, is effective on a number of emulsions. For the 30 highly ionized dyes, and other relatively strong treatment of any particular emulsion, the proper 30 coiloidal electrolytes, high molecular weight or proportions of hydrophile colloid and electrolyte ganic sulfates and Sulfonates, are not included to employ may be determined by a few simple in this classification. Examples of materials tests. Taking glue and calcium chloride as an having the properties which make them suitable example of a mixture to be tested, the test may for use as a demulsifying agent for breaking the be made as follows: 35. peculiar oil-in-water type emulsion previously Prepare five different solutions in water, all described are: glue, gelatin, casein, starch, albu containing the same total percentage Weight of min, tannin, dextrin, methyl cellulose, Water Sol material, but with one solution containing ten uble ethyl cellulose, Prosopis juliflord exudate, times as much glue as calcium chloride, another 40 gun arabic, many other water dispersible guns, containing five times as much glue as Calcium water dispersible urea-aldehyde resins, etc. In chloride, another containing equal Weights of 40, some instances, a mixture of two or more of Such glue and calcium chloride, one containing five materials or colloids may be more effective than times as much calcium, chloride as glue, and an one alone. It is recognized that Some of these other containing ten times as much calcium 45 products, such as starch, glue, or the like, pro chloride as glue.
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