Abstract:
A method is given for reducing fluid loss in downhole operations such as drilling and completion. A composition containing a fusing solid is injected into the fluid loss flow path; the fusing solid fuses at formation temperature when the injection pressure is released and the formation matrix surfaces forming the flow path close on the composition. The fusing solid is gilsonite, or a similar material, or resin coated particles. The composition may optionally contain one or more of fibers, flakes, an activator, and a dispersant.

Description:
CROSS-REFERENCE TO RELATED APPLICATION 
     This application claims the benefit of U.S. Provisional Patent Application No. 60/998,491, filed on Oct. 11, 2007, now expired. 
    
    
     BACKGROUND OF THE INVENTION 
     The invention relates to slurries of materials that fuse under pressure to act as lost circulation prevention materials, fluid loss agents, or cementacious materials in oil and gas wells. In particular, it relates to such slurries containing fibers and materials that fuse together under pressure. 
     In drilling and completion operations in the oilfield, fluids such as drilling muds are sometimes lost to the surrounding formation through natural fractures, cracks, fissures, or vugs, or through fractures and the like created during treatments or through fractures and the like created by prior treatments. Lost circulation is reduced, or total, loss of fluid flow up the annulus when fluid is pumped down through a drillstring. Substances called loss control agents or lost-circulation control agents are added to drilling fluids and the like when fluids are being lost to the formation downhole. Commonly used lost-circulation materials include fibrous (cedar bark, shredded cane stalks, mineral fiber and hair), flaky (mica flakes and pieces of plastic or cellophane sheeting) or granular (ground and sized limestone or marble, wood, nut hulls, FORMICA™, corncobs and cotton hulls). 
     Granules, fibers and flakes in loss control agents are known (see for example U.S. Patent Application No. 2005/0269080), including all three in one slurry; see for example U.S. Pat. No. 4,579,668. Gilsonite has been used in drilling muds as an extender and as a lost circulation material on a regular basis. 
     SUMMARY OF THE INVENTION 
     One embodiment of the Invention is a method for reducing fluid loss in downhole operations. The method involves injecting a composition containing a fusing solid into the fluid loss flow path in a formation matrix and allowing the fusing solid to fuse at formation temperature when the injection pressure is released, and the formation matrix surfaces, that form the fluid loss flow path, close on the composition. The fusing solid may be gilsonite, asphalt, asphaltite, uintaite, uintahite, bitumen, wurzilite, glance pitch, grahamite, asphaltum, or mixtures of these materials. In a particularly preferred embodiment, the fusing solid is gilsonite. The composition may also contain fibers. The fibers may be selected from ceramics, glass, organic polymers, polyethlene terphthalate, aramids, novoloids, nylon, metals, aluminum, steel and mixtures of these materials. In a preferred embodiment, the fibers are glass or novoloid. The composition may also contain flakes. The flakes may be selected from mica, calcium carbonate, cellophane or mixtures of these materials. Mica is preferred. The composition may also contain a dispersant. The dispersant may be selected from lignosulfonates, lignites, humic acids, sulfonated styrene maleic anhydride copolymers, sulfonated naphthalene formaldehyde copolymers, polyacrylates, polyphosphates, modified tannins, zirconium citrate, dextrins, and mixtures of these materials. 
     In another embodiment, the fusing solid is selected from resin coated sand, resin coated bauxite, resin coated synthetic proppant, resin coated polymer beads, resin coated walnut shells, and mixtures of these materials. A preferred fusing solid of this type resin coated sand. The composition of this embodiment may also contain fibers, flakes, and/or a dispersant as described above. The composition of this embodiment may also contain an activator. The activator may be selected from the group consisting of an alcohol; an ester, an ether, an amide, a ketone, benzene sulfonic acid, sulfuric acid, methane sulfonic acid, trichloroacetic acid, hydrochloric acid, hydrofluoric acid, ferric chloride, toluene sulfonic acid, chlorobenzene sulfonic acid, nitric acid, perchloric acid, a water soluble multivalent metal salt catalyst comprising at least one multivalent ion of either manganese, zinc, cadmium, magnesium, cobalt, nickel, copper, tin, iron, lead, or calcium, and combinations of these. 
     In any of the above embodiments, the composition may also contain one or more than one of an antisettling agent, a fluid loss additive, and an antifoam agent. In any of the previous embodiments, the composition may also contain a weighting agent. The weighting agent may be selected from silica sand, barite, fly ash, calcium carbonate, hematite and mixtures of these materials. A preferred weighting agent is calcium carbonate. In any of the previous embodiments, the composition may contain an agent that lowers the fluid specific gravity rather than a weighting agent. 
     Another embodiment of the Invention is a composition, containing a fusing solid, for reducing fluid loss in downhole operations. The fusing solid may be gilsonite, asphalt, asphaltite, uintaite, uintahite, bitumen, wurzilite, glance pitch, grahamite, asphaltum, or mixtures of these materials. In a particularly preferred embodiment, the fusing solid is gilsonite. The composition may also contain fibers. The fibers may be selected from ceramics, glass, organic polymers, polyethlene terphthalate, aramids, novoloids, nylon, metals, aluminum, steel and mixtures of these materials. In a preferred embodiment, the fibers are glass or novoloid. The composition may also contain flakes. The flakes may be selected from mica, calcium carbonate, cellophane or mixtures of these materials. Mica is preferred. The composition may also contain a dispersant. The dispersant may be selected from lignosulfonates, lignites, humic acids, sulfonated styrene maleic anhydride copolymers, sulfonated naphthalene formaldehyde copolymers, polyacrylates, polyphosphates, modified tannins, zirconium citrate, dextrins, and mixtures of these materials. 
     In another embodiment, the fusing solid of the composition is selected from resin coated sand, resin coated bauxite, resin coated synthetic proppant, resin coated polymer beads, resin coated walnut shells, and mixtures of these materials. A preferred fusing solid of this type resin coated sand. The composition of this embodiment may also contain fibers, flakes, and/or a dispersant as described above. The composition of this embodiment may also contain an activator. The activator may be selected from the group consisting of an alcohol; an ester, an ether, an amide, a ketone, benzene sulfonic acid, sulfuric acid, methane sulfonic acid, trichloroacetic acid, hydrochloric acid, hydrofluoric acid, ferric chloride, toluene sulfonic acid, chlorobenzene sulfonic acid, nitric acid, perchloric acid, a water soluble multivalent metal salt catalyst comprising at least one multivalent ion of either manganese, zinc, cadmium, magnesium, cobalt, nickel, copper, tin, iron, lead, or calcium, and combinations of these. 
    
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         FIG. 1  shows a modified fluid loss cell fitted with a slot. 
         FIG. 2  shows a slot plugged by a lost circulation pill of Fluid C (left) compared to a slot prior to testing (right). 
         FIG. 3  shows the appearance of Fluid C as prepared. 
         FIG. 4  shows Fluid C compacted and fused above and below the spacer ring above the slot after pressure had been applied in the slot test. 
         FIG. 5  shows compacted Fluid A material retrieved from the cell after the slot test. 
         FIG. 6  shows compacted Fluid D material after curing for 2 hours in fluid loss cell at 6.90 MPa (1000 psi) and 76.7° C. (170° F.). 
         FIG. 7  shows Fluid G plugging off above the ⅛ inch (0.318 cm) slot. 
     
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
     The Invention will be described in terms of treatment of vertical wells, but is equally applicable to wells of any orientation. The Invention will be described for hydrocarbon production wells, but it is to be understood that the Invention may be used for wells for production of other fluids, such as water or carbon dioxide, or, for example, for injection or storage wells. It should also be understood that throughout this specification, when a concentration or amount or other parameter range is described as being useful, or suitable, or the like, it is intended that any and every concentration or amount or other parameter within the range, including the end points, is to be considered as having been stated. Furthermore, each numerical value should be read once as modified by the term “about” (unless already expressly so modified) and then read again as not to be so modified unless otherwise stated in context. For example, “a range of from 1 to 10” is to be read as indicating each and every possible number along the continuum between about 1 and about 10. In other words, when a certain range is expressed, even if only a few specific data points are explicitly identified or referred to within the range, or even when no data points are referred to within the range, it is to be understood that the inventors appreciate and understand that any and all data points within the range are to be considered to have been specified, and that the inventors have possession of the entire range and all points within the range. 
     Although much of the following discussion emphasizes alleviation of lost circulation in drilling, the compositions and methods of the Invention may also be used in fluid loss control in other oilfield operations such as completion, cementing, remediation, and stimulation. The compositions and methods of the Invention may also be used to plug hydraulic fractures growing into regions in which they are not desired. The composition and methods of the Invention may also be used to plug hydraulic fractures in water bearing zones or to plug fractures in zones of water intrusion. 
     The invention is a wellbore control fluid that contains particles that can plug fissures or fractures efficiently to reinforce formation strength. The wellbore control fluid forms a solid mass when subjected to squeeze pressure. If the leak to be plugged is a new fracture (or a newly re-opened or further-opened fracture) that will close when pressure is released, the fluid remains in the fracture when the fracture is closing after the release of the squeeze pressure because the fluid is a slurry that solidifies or hardens inside the fracture because of the closure. The fluid does not set inside the wellbore and can be pumped through the drilling bottom hole assembly. The fluid is a slurry that contains particles that bridge in the fracture, preferably before the fracture closes, but necessarily after the fracture has closed. An important feature of the composition of the Invention is fusing particles of a solid that compact and harden into an impermeable mass when pressed together. Suitable materials may be illustrated by the following two types of materials. The first type is gilsonite or a similar material, for example natural asphalt, asphaltite, uintaite, uintahite, bitumen, wurzilite, glance pitch, grahamite, and asphaltum; the slurry preferably also contains a dispersant, flakes, and a fiber, and most preferably contains a dispersant and a fiber. The second such fusing solid is a resin coated sand, or similar material for example resin coated bauxite, resin coated synthetic proppant, resin coated polymer beads, and resin coated walnut shells, and, preferably, an activator. Any size range may be used, depending upon the surface equipment and the width of the fracture. Any curable, or partially cured, resin may be used, for example those commonly used for resin coated proppants, for example phenolic resins, furfuryl alcohol resins, novolac polymers, resole polymers, furan resins, phenolic-furan resins, phenolic-furan-formaldehyde terpolymers, and mixtures of these. The resin may be in multiple coats, for example a phenolic resin coat and a curable phenolic resin overcoat. The activator depends upon the nature of the resin and the temperature, but examples include an alcohol; an ester; an ether; an amide; a ketone; benzene sulfonic acid; sulfuric acid; methane sulfonic acid; trichloroacetic acid; hydrochloric acid; hydrofluoric acid; ferric chloride; toluene sulfonic acid; chlorobenzene sulfonic acid; nitric acid; perchloric acid; a water soluble multivalent metal salt catalyst comprising at least one multivalent ion of either manganese, zinc, cadmium, magnesium, cobalt, nickel, copper, tin, iron, lead, or calcium; and combinations of these. Of course, temperature may also be used to activate resin curing. 
     A pill containing a slurry of the fusing particles, and other necessary components, depending upon the choice of fusing particles, is injected across the loss or fractured zone and squeezed into the fractures. Once the squeeze pressure is released (bled off), the fracture closes on the fusing particles, and the closing pressure causes the fusing particles to bind to each other into a compact mass. As the fusing particles are compacted and fused, they are not expelled from the fracture into the wellbore upon pressure release and the mass stays inside the fracture. 
     Note that the second type of slurry, containing resin coated particles and an activator, may also be used to plug pre-existing fractures or voids by relying solely on the chemical reaction initiated by the activator, and not making use of squeeze or closure pressure. Care must be taken that none of the slurry of the second type is in a region that is not intended to be blocked, such as the wellbore. Testing of the resin and activator (chemistry and concentrations) should be done to ensure that a suitable plug is formed at the downhole temperature. 
     The present invention can be understood further from the following examples. 
     Example 1 
     Experimental fluids were evaluated for fracture plugging, nozzle plugging, mixability, and durability. A modified Fluid Loss cell was fitted with either a slot or a drill bit nozzle. The cell fitted with the slot is shown in  FIG. 1 . The cell is fitted with a high-pressure valve [ 2 ] connected to a test fluid chamber [ 4 ] containing a piston [ 6 ]; a gas inlet [ 8 ] is at the bottom. The slot [ 10 ] was ⅛ inch (3.18 mm) wide and ½ inch (1.27 cm) long and was used to evaluate the ability of a fluid to plug a fracture. (Other slots were available and are shown at the bottom of the figure.) The nozzle was the smallest drill bit nozzle available in the industry ( 8/32 inch) and was used to evaluate the ability of a fluid to flow through a drill bit. Only one nozzle was used as a restriction, instead of the three found in a normal drill bit; therefore, the flow area chosen in the test was very conservative. Each fluid tested was poured into the cell having either a nozzle or a slot and squeezed against the opening in steps from 100 to 500 psi. Mixability was evaluated by examining fluids for sedimentation or for abnormally high viscosity. Durability was evaluated by holding the fluid in the modified fluid loss cell after the slot (fracture) test at 13.8 MPa (2000 psi) and 62.8° C. (145° F.) for about 12 to 15 hours to simulate fracture closure after the end of a squeeze. The mass above the slot was then removed and examined for any compaction, solidification, or hardening. A fluid passed all tests if it plugged the slot but not the nozzle, was pumpable as mixed, and fused into a firm solid after squeezing. 
     Three fluids were prepared in the laboratory; each had a Solid Volume Fraction of 0.60; the fluids are shown in table I. 
     
       
         
               
             
               
               
               
               
             
               
             
               
               
               
               
             
               
             
               
               
               
               
             
               
             
               
               
               
               
             
               
             
               
               
               
               
             
           
               
                 TABLE I 
               
               
                   
               
             
             
               
                 Fluid A - Density 8.71 ppg (1.045 kg/L) 
               
             
          
           
               
                 Antisettling agent 
                 3.000 
                 lb/bbl (8.56 kg/m 3 ) 
                 BW/V Water 
               
               
                 Fiber 
                 2.000 
                 lb/bbl (5.71 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Fine Flakes 
                 4.000 
                 lb/bbl (11.41 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Medium Flakes 
                 4.000 
                 lb/bbl (11.41 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Gilsonite 
                 144.30 
                 lb/bbl (411.69 kg/m 3 ) 
                 BW/V Total Fluid 
               
             
          
           
               
                 Fluid B - Density 8.60 ppg (1.032 kg/L) 
               
             
          
           
               
                 Antisettling Agent 
                 3.000 
                 lb/bbl (8.56 kg/m 3 ) 
                 BW/V Water 
               
               
                 Fiber 
                 2.000 
                 lb/bbl (5.71 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Gilsonite 
                 147.72 
                 lb/bbl (421.44 kg/m 3 ) 
                 BW/V Total Fluid 
               
             
          
           
               
                 Fluid C - Density 8.74 ppg (1.049 kg/L) 
               
             
          
           
               
                 Antifoam 
                 0.050 
                 gal/bbl (1.23 l/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Antisettling Agent 
                 3.000 
                 lb/bbl (8.56 kg/m 3 ) 
                 BW/V Water 
               
               
                 Dispersant 
                 3.000 
                 lb/bbl (8.56 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 FLA 
                 3.000 
                 lb/bbl (8.56 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Gilsonite 
                 139.63 
                 lb/bbl (398.36 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Fiber 
                 2.000 
                 lb/bbl (5.71 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Fine Flakes 
                 4.000 
                 lb/bbl (11.41 kg/L) 
                 BW/V Total Fluid 
               
               
                 Medium Flakes 
                 4.000 
                 lb/bbl (11.41 kg/L) 
                 BW/V Total Fluid 
               
             
          
           
               
                 Fluid D - Density 10.48 ppg (1.258 kg/L) 
               
             
          
           
               
                 Antisettling Agent/ 
                 1.500 
                 lb/bbl (4.28 kg/m 3 ) 
                 BW/V Water 
               
               
                 FLA 
               
               
                 Dispersant 
                 0.500 
                 lb/bbl (1.43 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Gilsonite 
                 131.3 
                 lb/bbl (374.60 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Calcium Carbonate 
                 131.0 
                 lb/bbl (373.74 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Fiber 
                 2.000 
                 lb/bbl (5.71 kg/m 3 ) 
                 BW/V Total Fluid 
               
             
          
           
               
                 Fluid E - Density 11.19 ppg (1.343.kg/L) 
               
             
          
           
               
                 Antisettling Agent/ 
                 1.500 
                 lb/bbl (4.28 kg/m 3 ) 
                 BW/V Water 
               
               
                 FLA 
               
               
                 Dispersant 
                 0.500 
                 lb/bbl (1.43 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Gilsonite 
                 112.0 
                 lb/bbl (319.54 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Calcium Carbonate 
                 180.1 
                 lb/bbl (513.83 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                 Fiber 
                 1.000 
                 lb/bbl (2.85 kg/m 3 ) 
                 BW/V Total Fluid 
               
               
                   
               
               
                 BW/V Water means percentage weight by volume of water in the fluid 
               
               
                 BW/V Total Fluid means percentage weight by volume of the total fluid 
               
             
          
         
       
     
     A summary of the test results is shown below in table II: 
     
       
         
               
               
               
               
               
             
           
               
                 TABLE II 
               
               
                   
               
               
                   
                   
                   
                   
                 Gilsonite 
               
               
                   
                   
                   
                   
                 fusing after 
               
               
                 Fluid 
                 Slot Test 
                 Nozzle Test 
                 Mixability 
                 the test 
               
               
                   
               
             
             
               
                 Fluid A 
                 Plugged slot 
                 Plugged 
                 Pumpable - 
                 Solid - 
               
               
                   
                   
                 Nozzle 
                 Very thick 
                 Crumbly (See 
               
               
                   
                   
                   
                   
                 FIG. 5) 
               
               
                 Fluid B 
                 Plugged slot 
                 Plugged 
                 Pumpable - 
                 Not Tested 
               
               
                   
                   
                 Nozzle 
                 Thick 
               
               
                 Fluid C 
                 Plugged slot 
                 Nozzle not 
                 Pumpable - 
                 Solid - Set (See 
               
               
                   
                 (See FIG. 2) 
                 plugged* 
                 Thick 
                 FIG. 4) 
               
               
                   
                   
                   
                 (See FIG. 3) 
               
               
                 Fluid D 
                 Plugged slot 
                 Nozzle not 
                 Pumpable 
                 Solid Set 
               
               
                   
                   
                 plugged 
                   
                 (See FIG. 6) 
               
               
                 Fluid E 
                 Plugged slot 
                 Nozzle not 
                 Pumpable 
                 Solid Set 
               
               
                   
                   
                 plugged 
               
               
                   
               
               
                 *Some wet gilsonite and loss control material (fiber and flakes) was left inside the cell above the nozzle. 
               
             
          
         
       
     
     
       
         
               
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
               
             
           
               
                   
                 TABLE III 
               
               
                   
                   
               
               
                   
                 Test 1 
                 Test 2 
                 Test 3 
                 Test 4 
                 Test 5 
                 Test 6 
                 Test 7 
                 Test 8 
               
               
                   
                 Fluid A 
                 Fluid A 
                 Fluid B 
                 Fluid C 
                 Fluid C 
                 Fluid A 
                 Fluid D 
                 Fluid E 
               
               
                   
                   
               
             
             
               
                   
               
             
          
           
               
                 Nozzle or 
                 Slot 
                 Nozzle 
                 Nozzle 
                 Nozzle 
                 Slot 
                 Slot 
                 Slot 
                 Slot 
               
               
                 Slot 
               
               
                 0.689 
                 130 cc - 60 sec 
                  50 cc - 60 sec 
                  0 cc - 60 sec 
                 225 cc - 60 sec 
                 200 cc - 60 sec 
                 130 cc - 60 sec 
                 10 cc - 60 sec 
                 20 cc - 60 sec 
               
               
                 MPa 
               
               
                 (100 psi) 
               
               
                 1.379 
                 150 cc - 60 sec 
                  75 cc - 60 sec 
                 175 cc - 60 sec 
                 230 cc - 60 sec 
                 200 cc - 60 sec 
                 150 cc - 60 sec 
                 20 cc - 60 sec 
                 50 cc - 60 sec 
               
               
                 MPa 
               
               
                 (200 psi) 
               
               
                 2.068 
                 160 cc - 60 sec 
                 110 cc - 60 sec 
                 200 cc - 60 sec 
                 235 cc - 60 sec 
                 200 cc - 60 sec 
                 160 cc - 60 sec 
                 20 cc - 60 sec 
                 50 cc - 60 sec 
               
               
                 MPa 
               
               
                 (300 psi) 
               
               
                 2.758 
                 175 cc - 60 sec 
                 125 cc - 60 sec 
                 205 cc - 60 sec 
                 240 cc - 60 sec 
                 200 cc - 60 sec 
                 175 cc - 60 sec 
                 20 cc - 60 sec 
                 50 cc - 60 sec 
               
               
                 MPa 
               
               
                 (400 psi) 
               
               
                 3.447 
                 180 cc - 60 sec 
                 135 cc - 60 sec 
                 205 cc - 60 sec 
                 250 cc - 60 sec 
                 200 cc - 60 sec 
                 180 cc - 60 sec 
                 20 cc - 60 sec 
                 50 cc - 60 sec 
               
               
                 MPa 
                   
                   
                 (75 g left in cell) 
               
               
                 (500 psi) 
               
               
                 FLAC 
                 No 
                 No 
                 No 
                 Yes 
                 Yes 
                 No 
                 No 
                 No 
               
               
                 ° C. (° F.) 
                 26.7 (80) 
                 62.8 (145) 
                 62.8 (145) 
                 62.8 (145) 
                 62.8 (145) 
                 37.8 (100) 
                 26.7 (80) 
                 26.7 (80) 
               
               
                 Curing 
                   
                   
                   
                   
                 8.274 MPa 
                 8.274 MPa 
                 6.90 MPa 
                 6.90 MPa 
               
               
                 Condi- 
                   
                   
                   
                   
                 (1200 psi) -  
                 (1200 psi) -  
                 (1000 psi) 
                 (1000 psi) 
               
               
                 tions: 
                   
                   
                   
                   
                 12 hrs 
                 12 hrs 
                 2 hrs 
                 2 hrs 
               
               
                   
                   
                   
                   
                   
                 62.8 C (145 F) 
                 37.8 C (100 F) 
                 76.7 C (170 F) 
                 76.7 C (170 F) 
               
               
                   
                   
                   
                   
                   
                 Solid - Set 
                 Solid - Crumbly 
                 Solid 
                 Solid 
               
               
                 CS MPa 
                   
                   
                   
                   
                   
                   
                 0.448 (65) 
                 1.172 (170) 
               
               
                 (psi) 
               
               
                   
               
               
                 Notes: 
               
               
                 The total fluid used was 300 to 325 cc. 
               
               
                 The test started with 0.689 MPa (100 psi) pressure; if the fluid was stopped, the pressure was increased to 3.447 MPa (500 psi) for 60 seconds. 
               
             
          
         
       
     
     The details of selected tests were as shown in Table III, which gives the amount of total fluid passed through a given geometry (nozzle or slot) as a function of pressure. The flakes used in all of these fluids were mica; the fibers were fiberglass. The antisettling agent was a blend of a sulfonated organic polymer and a polysaccharide (D-glucopyranuronate with mannose and glucose). The FLAC was the ammonium salt of an acrylamido-methyl-propane sulfonate/acrylamide copolymer. The antifoam agent was polypropylene glycol, and the dispersant was sodium polynaphthalene sulfonate. 
     Fluid A was the most efficient when it came to plugging the slot, because it contained both fiber and flakes and dehydrated quickly through the slot, making it very efficient. However, Fluid A did not pass the “nozzle test” and plugged the bit nozzle. It was very thick, and the fused solid after the tests was crumbly.  FIG. 5  shows portions of compacted Fluid A material retrieved from the cell after a slot test. 
     Fluid B did not plug the slot as quickly as Fluid A and was not as thick, but eventually it also plugged both the slot and the nozzle. The material was not examined after the tests. 
     Fluid C plugged the slot (although not as quickly as Fluids A and B); however, Fluid C also passed through the nozzle without plugging it, and was less thick than Fluid A and Fluid B, so it was pumpable. The addition of a fluid loss control agent and dispersant provided a more stable fluid that did not dehydrate as quickly through a small restriction.  FIG. 2  shows a slot plugged by a lost circulation pill of Fluid C on the left compared to a slot before testing shown on the right.  FIG. 3  shows Fluid C as prepared [ 12 ] (a portion put into a beaker [ 14 ]).  FIG. 4  shows Fluid C compacted and fused [ 16 ] above and below the spacer ring [ 18 ] above the slot after pressure had been applied in the slot test. 
     Fluids D and E plugged the slot (more quickly than Fluids A, B, and C). Fluids D and E also passed through the nozzle without plugging it, and were less thick than Fluid C, they were pumpable. The addition of an antisettling agent/fluid loss additive provided fluid stability; therefore, the fluids did not dehydrate quickly through a small restriction. The calcium carbonate was used as a weighting agent and to increase the solid volume fraction; it may also have helped in the compaction, as the compressive strength was good. Fluids D and E passed all tests and are robust gilsonite systems for plugging fractures or fissures initiated during squeezing.  FIG. 6  shows compacted Fluid D material after curing for 2 hours in the fluid loss cell at 6.90 MPa (1000 psi) and 76.7° C. (170° F.). 
     Any antisettling agent may be used; typical materials are organoclays, laponite, xanthans, welan gums, and celluloses, for example HEC (hydroxyethyl cellulose). The concentration may range from about 8.56 to about 85.6 kg/m 3  (about 3 to about 30 lb/bbl), with lower concentrations preferred. Any fiber may be used, especially those used in oilfield fluids; examples include ceramics, for example glass, organic polymers, for example polyethlene terphthalate, aramids, and nylon, and metals, for example aluminum and steel; glass is preferred. The fiber must be insoluble and must not interact chemically with other components of the system. The concentration may be from about 1.43 to about 14.27 kg/m 3  (about 0.5 to about 5 lb/bbl), with about 5.71 kg/m 3  (about 2 lb/bbl) preferred. The fiber preferably has a length up to about 2 mm and a diameter of from about 6 to about 100 microns, although other sizes may be used. The fine and medium flakes may be made of any material (again provided that they are insoluble and do not interact chemically with other components of the fluid); preferred materials include those used for fluid loss control in oilfield fluids, for example mica, calcium carbonate, and cellophane; a preferred example is mica. They are optional but preferred and may be used at concentrations of from 0 to about 57.08 kg/m 3  (about 20 lb/bbl). The gilsonite used had a size range of from about 100 to about 600 microns; any size range may be used; the preferred range for lost circulation is from about 100 to about 500 microns. The concentration used is selected so that the total solids fraction ranges from about 40 to about 60% for gilsonite-containing slurries and about 35 to about 60% for resin-coated sand containing slurries. Higher concentrations may be used if the slurry is pumpable. For gilsonite, that is about 285.4 to about 713.5 kg/m 3  (about 100 to about 250 lb/bbl). Gilsonite is a natural antifoaming agent, although an additional antifoaming agent or defoaming agent may be used. Any such agent may be used (provided that it is compatible with all the other components); the concentration may range from 0 to about 12.3 l/m 3  (about 0.5 gal/bbl). Suitable antifoam agents include polypropylene glycol, polydimethylsilanes, silicones, and mixtures of these materials. Any dispersant may be used (again provided that it is compatible with all the other components); examples include lignosulfonates, lignites, humic acids, sulfonated styrene maleic anhydride copolymers, sulfonated naphthalene formaldehyde copolymers, polyacrylates, polyphosphates, modified tannins, zirconium citrate, and dextrins. The FLA (fluid loss additive) may be any known in the industry; it is optional, but is recommended if the fluid is to be pumped through small restrictions, for example bit nozzles. Suitable materials include polyethyleneimines, acrylamide-AMPS copolymers, hydroxyethyl cellulose, carboxymethyl cellulose, crosslinked microgels, bentonite, latexes, and polyvinyl alcohols. Suitable concentrations are from 0 to about 123 l/m 3  (about 5 gal/bbl) for liquids and from 0 to about 28.54 kg/m 3  (about 10 lb/bbl) for solids. 
     Weighting agents, for example silica sand, barite, fly ash, calcium carbonate and hematite, may be added to achieve higher fluid densities. Microspheres (cenospheres or glass bubbles) may be used to achieve lower fluid densities. 
     Although Fluids C, D and E did pass through the small 0.635 mm restriction ( 8/32″ nozzle), these fluids may also be pumped through a ball-operated valve placed above the drilling bottom hole assembly. In some cases, this may be preferred. 
     It was observed that in order for the gilsonite to compact and fuse in the fracture or fissure, water must be filtered out from the fluid loss control pill; therefore it is necessary for some water to be lost inside the fracture. 
     Fluid C was cured at 76.7° C. (170° F.) and 6.90 MPa (1000 psi) for 1 hour. The cell was then cooled to ambient temperature, the piston was removed, and 250-300 ml water was placed on the piston side of the sample. Pressure was applied at 0, 0.345, 0.689, 1.379, 2.758 and 4.137 MPa (0, 50, 100, 200, 400, and 600 psi) for 5-10 minutes. The plug was tightly compacted under these conditions and maintained its structure even after water exposure at differential pressures up to 4.137 MPa (600 psi). 
     Example 2 
     The four tests conducted were the same as in Example 1, except that the durability was evaluated by holding the fluid in the modified fluid loss cell after the slot (fracture) test at 76.7° C. (170° F.) and 6.90 MPa (1000 psi) for about 1 hour. 
     Four fluids were tested. Each contained 0.25 to 0.42 mm (40/60 mesh) Accupak Ottawa sand coated with about 2 to 4% curable phenolic resin, and having a specific gravity of about 2.56. Each also contained as an activator a Santrol (Fresno, Tex., U.S.A.) product, Superset P, which is a mixture of 25% methanol, 25% poly(oxyethylene)nonylphenol ether, and 50% di(ethyleneglycol) ethyl ether acetate. When compressed at elevated temperature, preferably with an activator, such materials fuse and create a solid mass. This material acts as both a plugging agent (fusing sold) and as a bridging agent. All other components, if used in the mixtures, were the same as in Example 1. 
     The four fluids tested are shown below in Table IV; all were made up in deionized water. The concentration of the antisettling agent was based on the water; all other concentrations were based on the total fluid. SVF is Solid Volume Fraction. The activator in these tests was a blend of toluene sulfonic acid and xylene sulfonic acid. 
     
       
         
               
               
               
               
               
             
           
               
                 TABLE IV 
               
               
                   
               
               
                   
                 Fluid F 
                 Fluid G 
                 Fluid H 
                 Fluid I 
               
               
                   
                 (density 1.536 kg/L 
                 (density 1.512 kg/L 
                 (density 1.50 kg/L 
                 (density 1.776 kg/L 
               
               
                   
                 (12.8 ppg); 
                 (12.6 ppg); 
                 (12.5 ppg);  
                 (14.8 ppg); 
               
               
                 Component 
                 SVF 35%) 
                 SVF 35%) 
                 SVF 35%) 
                 SVF 50%) 
               
               
                   
               
             
             
               
                 Antisettling 
                 45.65 (16) 
                 45.65 (16)   
                 45.65 (16)   
                 5.71 (2)   
               
               
                 agent, kg/m 3   
               
               
                 (lb/bbl) 
               
               
                 FLA, L/m 3   
                   36.9 (1.5) 
                 36.9 (1.5) 
                 36.9 (1.5) 
                 36.9 (1.5) 
               
               
                 (gal/bbl) 
               
               
                 Antifoam, L/m 3   
                   7.38 (0.3) 
                 7.38 (0.3) 
                 7.38 (0.3) 
                 7.38 (0.3) 
               
               
                 (gal/bbl) 
               
               
                 Fiber, kg/m 3   
                 2.85 (1) 
                 5.71 (2)   
                 9.99 (3.5) 
                 1.14 (0.4) 
               
               
                 (lb/bbl) 
               
               
                 Medium flakes, 
                 5.71 (2) 
                 11.41 (4)   
                 19.97 (7)   
                 2.28 (0.8) 
               
               
                 kg/m 3  (lb/bbl) 
               
               
                 Fine flakes, 
                 5.71 (2) 
                 11.41 (4)   
                 19.97 (7)   
                 2.28 (0.8) 
               
               
                 kg/m 3  (lb/bbl) 
               
               
                 Activator, L/m 3   
                   7.87 (0.32) 
                  7.87 (0.32) 
                  7.87 (0.32) 
                  7.87 (0.32) 
               
               
                 (gal/bbl) 
               
               
                 40/60 Accupak, 
                   821.38 (287.9) 
                 800.27 (280.5) 
                 768.60 (269.4) 
                 1237.92 (433.9)  
               
               
                 kg/m 3  (lb/bbl) 
               
               
                   
               
             
          
         
       
     
     A summary of the tests results is shown in Table V: 
     
       
         
               
               
               
               
               
             
           
               
                 TABLE V 
               
               
                   
               
               
                 Fluid 
                 Slot Test 
                 Nozzle Test 
                 Mixability 
                 Durability 
               
               
                   
               
             
             
               
                 Fluid F 
                 Passed 
                 Passed 
                 Pumpable - 
                 Not Tested 
               
               
                   
                 Through Slot 
                 through 
                 Thick 
               
               
                   
                   
                 Nozzle* 
               
               
                 Fluid G 
                 Plugged Slot 
                 Passed 
                 Pumpable - 
                 Solid - Set 
               
               
                   
                   
                 through 
                 Thick 
                 After 24 
               
               
                   
                   
                 Nozzle* 
                   
                 Hours 
               
               
                 Fluid H 
                 Plugged Slot 
                 Plugged 
                 Pumpable - 
                 Solid - Set 
               
               
                   
                   
                 Nozzle** 
                 Very Thick 
                 After 24 
               
               
                   
                   
                   
                   
                 Hours 
               
               
                 Fluid I 
                 Not Tested 
                 Not Tested 
                 Too Thick 
                 Not Tested 
               
               
                   
               
               
                 *Small amounts of wet 0.25 to 0.42 mm (40/60 mesh) Accupak and FLA material were left inside the cell above the nozzle 
               
               
                 *A large plug was left inside the cell above the nozzle 
               
             
          
         
       
     
     In more detail, fluid F passed the nozzle test but failed the slot test; the durability test was not done. Fluid F had the lowest concentrations of fibers and flakes, so it was the most pumpable, but it did not plug either the nozzle or the slot. Fluid G plugged off above the slot and passed all four tests; it was the only fluid to pass through the nozzle and yet plug the slot. It therefore is able to pass through the smallest bit nozzle currently in commercial use and plug fractures up to at least 0.318 mm (⅛ inch) in width. It was thick but pumpable due to the intermediate levels of fibers and flakes.  FIG. 7  shows Fluid G plugging off above the ⅛ inch (0.318 cm) slot. 
     Fluid H contained the highest concentrations of fibers and flakes, so it plugged the slot very efficiently, but it also plugged the nozzle. Fluid I was too thick during preparation, and could not be pumped and was not tested further. 
     Although Fluid G did pass through the small restriction, in this case an 0.635 mm ( 8/32 inch) nozzle, the fluid of the Invention may also be pumped through a ball-operated valve placed above the drilling bottom hole assembly. In some cases, this may be preferred. 
     It was observed that in order for the curable resin coated particles to compact and fuse in the fracture or fissure, water must be filtered out from the fluid loss control pill; therefore it is necessary for some water to be lost inside the fracture.