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United States Patent 19 (11) 3,766,983 Chiu [45] Oct

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United States Patent 19 (11) 3,766,983 Chiu [45] Oct F I 7 - 2 3 &n f 99 ci United States Patent 19 (11) 3,766,983 Chiu [45] Oct. 23, 1973 54 STABILIZED NON ONIC 3,648,770 3/1972 Dreher et al........................ 166/275 POLYSACCHARIDE THICKENED WATER OTHER PUBLICATIONS (75) Inventor: Ying-Chech Chiu, Houston, Tex. Allene Jeanes, “Composition and Properties of a 73 Assignee: Heteropolysaccharide Produced from Glucose by Shell Oil Company, Houston, Tex. Xanthomonas Campestris', Abstract of Papers, 136th 22 Filed: May 15, 1972 Meeting American Chemical Society, Sept. 13-18, 21) Appl. No.: 253,420 1959, page 7D. Primary Examiner-Marvin A. Champion (52) U.S. Cl.................. 1661274, 166/270, 166/275, Assistant Examiner-Jack E. Ebel 166/305 R Attorney-H. W. Coryell et al. 51 Int. Cl............................................. E21b 43/16 58 Field of Search................ 166/244 D, 270, 274, 57 ABSTRACT 166/275, 300, 304 A reservoir oil displacing fluid that is relatively stable 56) References Cited toward multivalent metal ions comprises an aqueous liquid solution of a viscosity enhancing amount of a UNITED STATES PATENTS water soluble nonionic polysaccharide and an effec 3,371,710 311968 Harvey et al....................... 166/274 3,508,612 4/1970 Reisberg et al... ... 166/275 tive amount of a water soluble metal salt adapted to 3,532,166 10/1970 Williams........... clarify a calcium ion induced turbidity in that solution. ..., 166/275 3,581,824 6, 1971 Hurd.......... a - - 166/270 4 Claims, No Drawings 3,766,983 1. 2 STABILIZED NONIONIC POLYSACCHARIDE solution that contains a viscosity enhancing amount of THICKENED WATER a water soluble nonionic polysaccharide, has a rela tively low calcium ion concentration, preferably one of BACKGROUND OF THE INVENTION less than about 360 parts per million, and contains an This invention relates to a well treating process or oil 5 effective amount of a water soluble metal salt capable recovery process in which a relatively viscous aqueous of clarifying a calcium ion induced turbidity in an aque liquid is injected into a subterranean reservoir to dis ous solution of that polysaccharide, and (3) displacing place oil within the reservoir. More particularly, the in the viscosity enhanced aqueous solution through the vention relates to a nonionic polysaccharide (or biopol reservoir to displace the oil. ymer) thickened water which is stabilized against the 10 In certain situations, some or all of the above fluid in viscosity altering effects of the multivalent metal ion jecting steps can be accomplished by injecting a single containing waters that are apt to be encountered in fluid. For example, where the calcium ion concentra such reservoirs. tion of the reservoir water is not excessive and/or the Prior well treating processes or oil recovery pro distance by which the oil is to be displaced is too short cesses have used various natural or synthetic ionic 15 to cause a significant increase in the calcium ion con polymers as water thickeners or viscosity enhancing tent of an aqueous liquid being displaced through the agents. The natural ionic polymers are typified by the reservoir for that distance, no fluid need be injected in polysaccharide B-1459, produced by fermenting a order to effect the step 1 adjustment of the reservoir sugar with a bacteria of the Xanthomonas campestris water calcium ion concentration. The calcium ion con NRRL B-1459. Such an ionic polysaccharide contains 20 centration of the portion of the reservoir through which dextroglucose, detromannose and dextroglucuronic the oil is to be displaced is preferably kept below about acid groups along with a significant proportion of ace 1,000 parts per million. Where the distance by which tic acid (in the form of acetyl groups) and pyruvic acid the reservoir oil is to be displaced is relatively short (for (attached through ketal linkages). example, in a well treatment operation for removing a Although the previously used natural ionic polysac 25 water injectivity-impeding concentration of residual oil charide water thickeners are advantageous relative to from around an injection well) the step 3 displacement synthetic ionic polymer water thickeners (in having a of the viscosity enhanced aqueous solution can be ef relatively high thickening efficiency, being relatively fected by simply injecting more of that solution. Thus, stable under reservoir conditions, and being producible in certain situations, all 3 stpes can be effected by sim at lower cost) they tend to agglomerate and form reser 30 ply injecting the specified viscosity enhanced aqueous voir plugging materials when they are mixed with aque solution until the oil has been displaced. ous liquids containing multivalent ions (such as the al Nonionic polysaccharides suitable for use in this in kaline earth metal ions that are commonly present in vention comprise those characterized by a multiplicity waters encountered in subterranean reservoirs). For of D-glucose units attached together in a straight chain example, in U.S. Pat. No. 3,581,824, the agglomerating 35 through beta-1,3 linkages. Such polysaccharides are tendency of an ionic polysaccharide, such as the poly produced when the appropriate molds are incubated in saccharide B-1459, is utilized to selectively plug the a medium containing carbohydrate source materials. most permeable zones in a reservoir being water Suitable polysaccharides and method for their produc flooded. The plugging is effected by preceding an injec tion are described in U. S. Pat. No. 3,301,848. Suitable tion of an aqueous solution of such a polysaccharide by 40 nonionic polysaccharides are commercially available an injection of an aqueous liquid having a relatively under the trade name Polytran from the Pillsbury Com high concentration of divalention. pany. A particularly suitable material comprises Poly tran-FS in the form of a water solution containing SUMMARY OF THE INVENTION about 0.3 to 0.4 percent by weight of the polysaccha This invention relates to a reservoir oil displacing 45 ride. fluid that is relatively stable toward multivalent metal The nonionic polysaccharides are chemically distinct ions and a use of such a fluid to displace oil within a from the ionic polysaccharides (particularly because of subterranean reservoir. The present oil displacing fluid the absence of any anionic carboxyl groups). In gen comprises an aqueous liquid solution containing a vis eral, the nonionic polysaccharide solutions tend to be cosity enhancing amount of a water soluble nonionic 50 strongly pseudoplastic and have viscosities which are polysaccharide and an effective amount of a water sol relatively free of fatigue or hysterisis when subjected to uble metal salt that is capable of clarifying a calcium varying degrees of shear. They also have viscosities ion induced turbidity in that solution (i.e. the specified which are relatively pH and salt insensitive and un aqueous solution of the specified poly-saccharide). dergo no apparent viscosity decrease with temperature The oil displacing process of this invention comprises 55 up to about 400°F. the steps of: (1) injecting an aqueous liquid of low cal In general, in displacing an oil within a subterranean cium ion content, preferably one containing less than reservoir formation by injecting a viscosity enhanced about 360 parts per million calcium ion, into a portion aqueous solution, the effective viscosity (or reciprocal of the reservoir through which oil is to be displaced, of the mobility within the reservoir) should be at least with said injection being continued to the extent re 60 substantially equal to and perferably greater than that quired to reduce the calcium ion concentration of the of the reservoir oil and/or any oil displacing liquid aqueous liquid in that portion of the reservoir to less (such as an aqueous or oil external sur-factant system) than one which could impart a significantly high cal that is injected ahead of the viscosity enhanced solu cium ion concentration, e.g. one greater than about 65 tion. In the present process, the concentration of the 1,000 parts per million, to slug of water which is dis nonionic polysaccharide should be in the order of from placed through that portion of the reservoir, (2) inject about 100 to 1,000 parts by weight of polysaccharide ing into the same portion of the reservoir an aqueous per million parts by weight of solution. Such a concen 3,766,983 3 4. tration provides viscosities in the order of from about Table 1 2 to 50 centipoises at room temperature in water con EFFECT OF ADDING SALT ON POLY TRAN-FS taining about 4,000 ppm total solid. Such viscosities are SOLUTION usually sufficient to provide effective displacements of 5 a reservoir oil. Wiscos- Ge. Although an aqueous solution of a nonionic polysac Total ity, cp Formation Amount (6 pm, Turbidity (after charide is generally salt insensitive, it tends to become of Salt too pH (Visual aging ppm temp.) Obser- OW turbid when mixed with more than about 20 parts per vation night) million of calcium ion. Such a turbidity can be removed 10 by filtration, for example, through a 5 micron millipore O 69.5 4. O O 250 ZnCl, 4.3 2.4 O 8 filter. However, such a filtration requires additional 250 MgCl, 42.6 2.5 O time and expense and causes the viscosity of the aque 50 CaCl, 43.2 2.9 turbid $8 250 FeSO, 44.0 2.2 0 & ous solution to be descreased, particularly when the 250 BaCl, 47.6 4.2 0 salt concentration of the solution is relatively high. 15 12,000 NaCl - 0 The nonionic polysaccharides are uniquely affected * After the addition of salt solution, the total volume increased by 25 by calcium ions. Although ionic polysaccharide solu percent. tions (e.g., Kelzan-M; a form of polysaccharide B-1459 that is commercially available from the Kelco Com The data in Table 2 shows the calcium induced tur pany) are generally more reactive with multivalent 20 bidity reducing effects of adding various metals to a so metal ions, the turbidity of a nonionic polysaccharide lution of about 900 parts per million Polytran-FS and solution (e.g.
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