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High Density Brines for Use in Wellbore Fluids

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High Density Brines for Use in Wellbore Fluids (19) TZZ ¥ _T (11) EP 2 325 277 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.: of the grant of the patent: C09K 8/06 (2006.01) C09K 8/36 (2006.01) 13.05.2015 Bulletin 2015/20 (21) Application number: 11157578.3 (22) Date of filing: 14.12.2005 (54) High density brines for use in wellbore fluids SALZLÖSUNGEN HOHER DICHTE ZUR VERWENDUNG IN BOHRLOCHFLÜSSIGKEITEN SAUMURES HAUTE DENSITE EMPLOYEES DANS DES FLUIDES DE FORAGES (84) Designated Contracting States: (72) Inventors: AT BE BG CH CY CZ DE DK EE ES FI FR GB GR • Zhang, Hui HU IE IS IT LI LT LU LV MC NL PL PT RO SE SI Sugar Land, TX 77478 (US) SK TR • Horton, Robert, L. Sugar Land, TX 77479 (US) (30) Priority: 14.12.2004 US 635858 P • Prasek, Bethicia, B. The Woodlands, TX 77380 (US) (43) Date of publication of application: • Dimataris, Mary, L.K. 25.05.2011 Bulletin 2011/21 Houston, TX 77077 (US) (62) Document number(s) of the earlier application(s) in (74) Representative: Gill, Stephen Charles et al accordance with Art. 76 EPC: Mewburn Ellis LLP 05854181.4 / 1 833 941 33 Gutter Lane London EC2V 8AS (GB) (73) Proprietor: M-I L.L.C. Houston, (56) References cited: TX 77072 (US) WO-A1-93/19849 US-A- 4 381 241 US-A1- 2003 114 318 US-B1- 6 620 341 Note: Within nine months of the publication of the mention of the grant of the European patent in the European Patent Bulletin, any person may give notice to the European Patent Office of opposition to that patent, in accordance with the Implementing Regulations. Notice of opposition shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). EP 2 325 277 B1 Printed by Jouve, 75001 PARIS (FR) EP 2 325 277 B1 Description [0001] The use of sodium, potassium, and cesium tungstates in brine solutions are disclosed in U. S. utility patent application, No. 20030114318, to make dense solutions; but at the higher concentrations the brines are caustic due to 5 the manufacturing techniques. These brines are not stable when exposed to CO2 or other acidic materials, forming water insoluble compounds such as tungstic acid, W03, or polytungstic acids. [0002] As a consequence, we created the idea of making a Lewis salt of tungstate and some Lewis base. The Lewis definition of acids and bases is the broadest definition, so any acid or base by less general definition is also a Lewis acid or base. Some conventional bases like sodium, potassium, and cesium hydroxide are also Lewis bases. The sodium, 10 potassium, and cesium salts of phosphoric and silicic acids and triethanolamine, and the like are, also Lewis bases. [0003] Our idea is to react the Lewis acids, sodium, potassium, or cesium tungstate with a Lewis base to obtain a Lewis salt that will make a dense brine with a pH that is 7 or higher so that additives will be more stable in the brines. The Lewis salt of the Lewis acid sodium tungstate and the Lewis base disodium hydrogen phosphate is already known and is termed a phosphotungstate compound. Similarly, the Lewis salt of the Lewis acid sodium tungstate and the Lewis 15 base sodium hydrogen silicate is already known and is termed a silicotungstate compound. The phosphotungstates and silicotungstates make dense brines, and we think that other such Lewis salts will also make dense brines. The phos- photungstates and silicotungstates are sometimes termed, respectively, tungstophosphates and tungstosilicates. The addition of a complexing agent to these systems is optional. [0004] Fluids, such as completion or drilling fluids, containing at least one alkali metal salt of a transition metal oxy- 20 anion or polyoxy-anion, such as, for example, an alkali metal polytungstate are described. Methods of preparing a dense or heavy liquid comprising an aqueous solution of transition metal salts, such as, for example, polytungstate are also n+ x- described, wherein the aqueous solution contains anionic moieties having the formula [A BmOk] , where (A) is selected from group IV elements, group V elements, transition metal elements and rare earth elements; (B) is one or more transition metal elements having an atomic weight between 50 and 201 inclusive, O is oxygen, m is an integer between 25 6 and 18 inclusive, k is an integer between 24 and 62 inclusive, and x is a small integer, typically between 1 and 10 depending on the selections of A, B, m, and k, said dense liquid also comprising in said aqueous solution cationic moieties capable of forming salts of said anionic moieties. The cation values may be lithium, sodium, potassium, cesium, or a mixture thereof, with a small amount of hydrogen cations provided by free acid anionic moieties. The most preferred 4- anionic moiety is [SiW12O40] . The atom designated (B) alternatively may be molybdenum, vanadium, niobium or 30 tantalum. A drilling fluid or mud is also described wherein the drilling fluid contains at least one alkali metal polytungstate . The drilling fluid may be brine-based (also referred to as water-based) or may preferably further contain at least one emulsifier or surfactant and at least one hydrocarbon-based fluid. The various fluids of the present invention can contain other conventional ingredients such as, for example, viscosifiers, eomplexing agents, fluid loss control additives, pH buffers, corrosion inhibitors, and oxygen scavengers. The present invention permits the completion fluids to be essentially 35 free of suspended solids due to the use of the soluble alkali metal polytungstate or heteropolytungkate, and permits the drilling fluids to be quite low in suspended solids because they derive most of their density from the dissolved alkali metal polytungstate or heteropolytungstate. [0005] Unlike the teachings of the prior art, the present invention teaches the use of these aqueous solutions of n+ x- transition metal salts, wherein the aqueous solution contains anionic moieties having the formula [A BmOk] , where 40 the cations may be lithium, sodium, potassium, cesium, or a mixture thereof, or with a small amount of hydrogen cations provided by free acid anionic moieties, and especially where said salts are a major component of the solution and not merely an additive thereto. The present invention teaches, in particular, the sodium, potassium, and cesium salts of the heteropolytungstates and the blends of these salts with the heteropolytungstic acids. It has been observed that these salts are not readily water soluble, but surprisingly, we have developed methods to make brine containing potassium, 45 sodium, and cesium salts of the heteropoly anions. The aqueous solutions in accordance with the present invention may further include optional halide salts as additives, such as, for example, LiCl, LiBr, LiI, NaCl, NaBr, Nal, KCl, KBr, KI, RbCl, RbBr, RbI, CsCl, CsBr, CsI, MgCl2, MgBr2, CaCl2, CaBr2, ScCl2, SrBr2, ZnCl2, ZnBr2, and mixtures thereof, and similar compounds which should be well known to those of skill in the art. In addition to developing methods to make said brines, we have further developed methods to adjust the true crystallization temperature (TCT) and water activity 50 of said brines, to make the brines stable in the pH range 3-10. The TCT is also referred to as the Thermodynamic Crystallization Temperature to distinguish it from any phase transition producing a metastable solid rather than the thermodynamic equilibrium phase. By stating that the brines are stable, it should be noted that we have tested the ambient temperature and high temperature stability to 177 °C (350°F) and have found the brines to be stable; and expect further high temperature stability, although higher temperatures have not yet been tested. We have found that these 55 brines appear to be less toxic than zinc brines such as 2045 kg/m3 (20.5 lbm/gal) ZnHr2 or 1916 kg/m3 (19.2 lbm/gal) ZnBr2/CaBr2 brines, and possess a relatively favorable environmental, health and safety profile. We find that we can offer these products in a variety of colors, therefore they may have use as an optical tracer or to make themselves useful for readily making displacement efficiency visible and apparent. 2 EP 2 325 277 B1 [0006] We have observed that these brines display high temperature stability to 177 °C (350°F) and perhaps beyond, corrosion inhibition, complete compatibility with monovalent brines and magnesium chloride brines and some compat- ibility with calcium and zinc brines, the ability to buoyantly suspend solids, for example to prevent barite packing off, the ability to dissolve scale, the ability to deliver fluids of density up to 2494 kg/m3 (25m lb/gal), giving the potential for 5 shipping the brines as extremely heavy brine concentrates and later diluting on location to the density needed. [0007] We have observed that these brines can provide 1896 kg/m3 (19-lb m/gal) brines having surprisingly high water activities as compared to zinc brines or cesium formate brines of comparable density, making the brines in accordance with the present invention more useful than conventional brines as a base brine for brine-based drilling fluids (also known as water-based drilling fluids) and more useful than conventional brines as an internal phase in invert emulsion drilling 10 fluids including oil-based drilling fluids and synthetic-based drilling fluids and ester-based drilling fluids. [0008] ’WARP Fluids Technology’, which is a commercialized system of M-I, L.L.C., is a system of water based and oil based drilling and completion fluids that are weighted up with a high density weighting agent. The WARP particles impart a high density to the fluid and may be barite or other weighting agents that have been subjected to a proprietary process.
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