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WO2014176188A1 - Procédé servant au traitement et au recyclage de fluide de fracturation hydraulique - Google Patents

Procédé servant au traitement et au recyclage de fluide de fracturation hydraulique Download PDF

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Publication number
WO2014176188A1
WO2014176188A1 PCT/US2014/034865 US2014034865W WO2014176188A1 WO 2014176188 A1 WO2014176188 A1 WO 2014176188A1 US 2014034865 W US2014034865 W US 2014034865W WO 2014176188 A1 WO2014176188 A1 WO 2014176188A1
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WO
WIPO (PCT)
Prior art keywords
metal ion
hydraulic fracturing
salts
source fluid
aqueous
Prior art date
Application number
PCT/US2014/034865
Other languages
English (en)
Inventor
Raymond EHRHART
Thomas Peter Tufano
Robert Harvey Moffett
Original Assignee
E. I. Du Pont De Nemours And Company
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Filing date
Publication date
Application filed by E. I. Du Pont De Nemours And Company filed Critical E. I. Du Pont De Nemours And Company
Publication of WO2014176188A1 publication Critical patent/WO2014176188A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/60—Compositions for stimulating production by acting on the underground formation
    • C09K8/62—Compositions for forming crevices or fractures
    • C09K8/66—Compositions based on water or polar solvents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56—Macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/722—Oxidation by peroxides
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/203—Iron or iron compound
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/206—Manganese or manganese compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH OR ROCK DRILLING; MINING
    • E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
    • E21B43/25—Methods for stimulating production
    • E21B43/26—Methods for stimulating production by forming crevices or fractures
    • E21B43/2607—Surface equipment specially adapted for fracturing operations

Definitions

  • the present invention relates to an improved process for removing certain contaminants from hydraulic fracturing fluids.
  • the treated fracturing fluids can be recycled and used in subsequent hydraulic fracturing processes.
  • the production of oil and natural gas from an underground well can be stimulated by a technique called hydraulic fracturing in which a fracturing fluid is introduced into an oil or gas well via a conduit, such as tubing or casing, at a flow rate and a pressure to create, reopen and/or extend a fracture into the well, allowing access to the oil or gas within the formation.
  • hydraulic fracturing in which a fracturing fluid is introduced into an oil or gas well via a conduit, such as tubing or casing, at a flow rate and a pressure to create, reopen and/or extend a fracture into the well, allowing access to the oil or gas within the formation.
  • the fracturing fluid is typically a water based solution and may comprise components such as suspended proppants (e.g., sand, bauxite); biocides to inhibit growth of bacteria and other microorganisms; corrosion inhibitors and scale inhibitors which reduce rust formation and other deposits on the conduit; and friction reducers to promote laminar flow of the hydraulic fracturing fluid into the formation and reduce the pumping pressure necessary to achieve the desired fracturing fluid flow rate.
  • suspended proppants e.g., sand, bauxite
  • biocides to inhibit growth of bacteria and other microorganisms
  • corrosion inhibitors and scale inhibitors which reduce rust formation and other deposits on the conduit
  • friction reducers to promote laminar flow of the hydraulic fracturing fluid into the formation and reduce the pumping pressure necessary to achieve the desired fracturing fluid flow rate.
  • flow back water contains contaminants such as hydrocarbons, minerals, and salts that are extracted from the formation during the fracturing process in addition to components of the fracturing fluid, including biocides, friction reducers, etc. that were introduced as part of the fracturing fluid.
  • the water becomes "produced water", which is the naturally occurring water in the formation. Flow back and produced water cannot simply be disposed of in a local stream, river, or shallow aquifer, but must be treated to remove contaminants.
  • Aerial oxidation is a relatively slow process, but oxidizing biocides rapidly and quantitatively oxidize Fe 2+ to Fe 3+ and Mn 2+ to Mn 4+ with the concomitant precipitation of colloidal Fe(OH) 3 and MnO 2 , respectively, at or near neutral pH.
  • Fe 2+ is generally more abundant than Mn 2+ , therefore precipitation of Fe(OH) 3 is potentially more of a problem than MnO2.
  • colloidal Fe(OH) 3 in high-enough concentration, can interfere with hydraulic fracturing operations (e.g., due to complexing and
  • the present invention provides a method for reducing the concentration of soluble and suspended oxidizable metal ion salts in an aqueous, hydraulic fracturing source fluid comprising the steps of:
  • an aqueous, hydraulic fracturing source fluid containing oxidizable metal ion salts oxidizing at least some of the oxidizable metal ion salts; contacting the aqueous, hydraulic fracturing source fluid with an anionic silica-based colloid for a time sufficient to coagulate at least a portion of the suspended oxidized metal ion salts; and separating the oxidized metal ion salts from the hydraulic fracturing source fluid.
  • the step of oxidizing at least some of the oxidizable metal ion salts is achieved by aerial oxidation.
  • the step of oxidizing at least some of the oxidizable metal ion salts is achieved by treating the aqueous, hydraulic fracturing source fluid with an oxidizing biocide.
  • the pH of the source fluid it may be desirable to adjust the pH of the source fluid.
  • the pH can be adjusted either before or after contacting the source fluid with the anionic silica-based colloid. It may be desirable to control the pH in the range of about 5.0 to about 8.0. It may be even more desirable to control the pH in the range of about 6.0 to about 7.0.
  • the pH can be achieved by any suitable means as one skilled in the art will understand.
  • a suitable base such as sodium hydroxide or ammonium hydroxide can be used to control the pH in the above ranges.
  • the present invention provides a method for reducing the concentration of soluble and suspended oxidizable metal ion salts in an aqueous, hydraulic fracturing source fluid consisting essentially of the following steps: providing an aqueous, hydraulic fracturing source fluid containing oxidizable metal ion salts; treating the aqueous, hydraulic fracturing source fluid with an oxidizing biocide to oxidize at least some of the oxidizable metal ion salts;
  • the oxidizing biocide can comprise a material selected from the group consisting of chlorine bleach, peroxides, peracids, persulfates, ozone, chlorine dioxide, and combinations thereof.
  • the oxidizing biocide can comprise chlorine dioxide.
  • the anionic silica-based colloid can comprise a material selected from the group consisting of polysilicic acid, polysilicic acid microgels, polysilicate microgels, polyaluminosilicate microgels, colloidal silicas and combinations thereof.
  • the oxidizable metal ion can comprise a material selected from the group consisting of ferrous ion and manganous ion. In one aspect the oxidizable metal ion comprises ferrous ion.
  • the aqueous, hydraulic fracturing source fluid can further comprise at least one material selected from the group consisting of alkali metal salts, alkaline-earth metal salts, friction reducing polymer, scale inhibitor, corrosion inhibitor, hydrocarbon and proppant.
  • the method may further include the step of adding a cationic organic polymer to the hydraulic fracturing source fluid.
  • the present invention provides a method for reducing the concentration of soluble and suspended oxidizable metal ion salts in an aqueous, hydraulic fracturing source fluid comprising the steps of:
  • an aqueous, hydraulic fracturing source fluid containing oxidizable metal ion salts oxidizing at least some of the oxidizable metal ion salts; contacting the aqueous, hydraulic fracturing source fluid with an anionic silica-based colloid for a time sufficient to coagulate at least a portion of the suspended oxidized metal ion salts; and separating the oxidized metal ion salts from the hydraulic fracturing source fluid.
  • the step of oxidizing at least some of the oxidizable metal ion salts is achieved by aerial oxidation.
  • the step of oxidizing at least some of the oxidizable metal ion salts is achieved by treating the aqueous, hydraulic fracturing source fluid with an oxidizing biocide.
  • the pH of the source fluid it may be desirable to adjust the pH of the source fluid.
  • the pH can be adjusted either before or after contacting the source fluid with the anionic silica-based colloid. It may be desirable to control the pH in the range of about 5.0 to about 8.0. It may be even more desirable to control the pH in the range of about 6.0 to about 7.0.
  • the pH can be achieved by any suitable means as one skilled in the art will understand.
  • a suitable base such as sodium hydroxide or ammonium hydroxide can be used to control the pH in the above ranges.
  • the present invention provides a method for reducing the concentration of soluble and suspended oxidizable metal ion salts in an aqueous, hydraulic fracturing source fluid consisting essentially of the following steps: providing an aqueous, hydraulic fracturing source fluid containing oxidizable metal ion salts;
  • At least a portion of the suspended metal ion salts are allowed to settle before the salts are separated from the hydraulic fluid.
  • oxidizing biocide is meant herein a compound that has biocidal activity, meaning reduces the amount of bacteria and other
  • oxidizing biocides include chlorine bleach (sodium hypochlorite,
  • peroxides such as hydrogen peroxide
  • peracids such as peracetic acid, persulfates, ozone, chlorine dioxide, and combinations thereof.
  • Preferred biocides include chlorine bleach, peracetic acid and chlorine dioxide.
  • the oxidizing biocide is generally added in an amount to provide a free residual in the fracturing fluid.
  • the residual may be about 1 -5 ppm of the oxidizing biocide.
  • the biocide is chlorine dioxide, for example, a dose of as great as 150 ppm CIO2 may be required to provide a target of 1 -5 ppm residual to achieve an appropriate level of disinfection.
  • Chlorine dioxide is a preferred oxidizing biocide. Chlorine dioxide is a gas and can be generated onsite at the oil or gas well location. Various methods are known for generating chlorine dioxide, including chemical and electrochemical processes as disclosed for example in Ulllmann's Encyclopedia of Industrial Chemistry, Wiley Online Library,
  • One particular method of generating chlorine dioxide involves reaction in aqueous solution of an alkali metal chlorite salt, such as sodium chlorite, with sodium hypochlorite and a source of strong acid as illustrated below.
  • an alkali metal chlorite salt such as sodium chlorite
  • the anionic silica-based colloids may have an S value of less than about 50%, as defined in Her and Dalton in J. Phys. Chem., 1956, vol. 60, pp. 955-957.
  • the S value is a measure of the degree of aggregate or microgel formation and a lower S value indicates a higher microgel content and is determined by the measure of the amount of silica, in weight percent, in the disperse phase.
  • the disperse phase consists of particles of anhydrous silica together with any water that is immobilized at the surface or in the interior of the particles.
  • anionic silica-based colloids which can be used in the process of this invention include colloidal silica, polysilicic acid, polysilicic acid microgels, polysilicate microgels, polyaluminosilicate microgels, colloidal silicas with a high microgel content, and mixtures thereof.
  • the anionic silica-based colloids have an S value of less than about 50% and preferably less than 40%.
  • Polysilicate microgels also known as active silicas, have
  • Polysilicic acid generally refers to those silicic acids that have been formed and partially polymerized in the pH range 1 -4 and comprise silica particles generally smaller than 4 nm diameter, which thereafter polymerize into chains and three-dimensional networks.
  • Polysilicic acid can be prepared, for example, in accordance with the methods disclosed in U. S. Patent 5,127,994, incorporated herein by reference.
  • Polyaluminosilicates are polysilicate or polysilicic acid microgels in which aluminum has been incorporated within the particles, on the surface of the particles, or both.
  • polysilicate microgels and polyaluminosilicate microgels useful in this invention are commonly formed by the activation of an alkali metal silicate under conditions described in U. S. Patents 4,954,220 and
  • polyaluminosilicates can be formed by the acidification of silicate with mineral acids containing dissolved aluminum salts as described in U. S. Patent 5,482,693, incorporated herein by reference.
  • Alumina/silica microgels can be formed by the acidification of silicate with an excess of alum, as described in U. S. Patent 2,234,285, incorporated herein by reference.
  • the anionic silica-based colloid can be provided in any suitable amount.
  • the anionic silica-based colloid can be provided in an amount from about 0.1 to about 1000 ppm, and more preferably in an amount from about 1 .0 to about 1000 ppm, based on the S1O2 content.
  • the oxidizable metal ion can comprise a material selected from the group consisting of ferrous ion and manganous ion. In one aspect the oxidizable metal ion comprises ferrous ion.
  • the method may further include the step of adding a cationic organic polymer to the hydraulic fracturing source fluid.
  • the cationic organic polymer may be added after the anionic silica-based colloid. High molecular weight and low molecular weight polymers may be used.
  • the cationic organic polymer can be provided in any suitable amount. In an aspect of the invention the cationic organic polymer can be provided in an amount from about 0.5 to about 1000 mg of polymer per liter of aqueous fluid, and preferably in an amount from about 1 to about 100 mg per liter of aqueous fluid.
  • High molecular weight cationic organic polymers include natural and synthetic cationic polymers. Natural cationic polymers include cationic starch, cationic guar gum, and chitosan. High molecular weight synthetic cationic polymers typically have number average molecular weights greater than 1 ,000,000, such as cationic polyacrylannide.
  • Cationic starches include those formed by reacting starch with a tertiary or quaternary amine to provide cationic products with a degree of substitution of from 0.01 to 1 .0, containing from about 0.01 to 1 .0 wt. % nitrogen. Suitable starches include potato, corn, waxy maize, wheat, rice and oat.
  • the high molecular weight cationic organic polymer is polyacrylannide.
  • Low molecular weight cationic organic polymers have a number average molecular weight in the range between about 2,000 to about 1 ,000,000, preferably between 10,000 and 500,000.
  • the low molecular weight polymer can be polyethylene imine, polyamines, polycyandiamide formaldehyde polymers, amphoteric polymers, diallyl dimethyl ammonium chloride polymers, diallylaminoalkyl (meth)acrylate polymers and dialkylaminoalkyl (meth)acrylamide polymers, a copolymer of acrylamide and diallyl dimethyl ammonium chloride, a copolymer of acrylamide and diallylaminoalkyl (meth)acrylates, a copolymer of acrylamide and dialkyldiaminoalkyl (meth)acrylamides, and a polymer of dimethylamine and epichlorohydrin.
  • the aqueous, hydraulic fracturing source fluid can further comprise at least one material selected from the group consisting of alkali metal salts, alkaline-earth metal salts, friction reducing polymer, scale inhibitor, corrosion inhibitor, hydrocarbon, and proppant.
  • a friction reducer can be added to the fracturing fluid to promote laminar flow of the fracturing fluid, which is important to achieve desired fracturing at lower pressures while maintaining high flow rates into the formation. Performance of the friction reducer is critical to achieve desired flow rates at desired pump pressure. Poor performance of a friction reducer causes increased pressure or reduced flow rate, either of which will negatively impact the fracturing process by increasing energy costs for higher pressure or increasing time and/or efficiency to achieve the desired fracturing at a lower pressure.
  • Suitable friction reducers can include organic polymers such as acrylic acid and acrylamide polymers and copolymers. Friction reducers may be anionic, cationic, and nonionic. Anionic friction reducers are lower cost and are the most widely used.
  • Friction reducers are typically dosed in an amount of 50 - 1000 ppm (parts per million by volume of polymer dispersion) based on the volume of the fracturing fluid.
  • Proppant which keeps an induced hydraulic fracture open during or following a fracturing treatment, is most commonly sand but can also be any other such particulate material with adequate mechanical properties to withstand closure stresses including, for example, ceramic, glass, and bauxite.
  • the fracturing fluid may comprise other components, including, for example, polymers, breaking agents, scale inhibitors, corrosion inhibitors, etc. These other components may be added to the biocide or to the water, or still other options for adding are available.
  • Turbidity At each indicated time point, a 25 mL sample of the supernatant was withdrawn from the reaction vessel by pipette and reserved for analysis. At the conclusion of each experiment, each sample was well-mixed, transferred to a sample cell, and the turbidity was measured using a Hach Model 2100N turbidimeter (Hach Company, Loveland, CO). Results are reported in Nephelometric turbidity units (NTU). Total iron analysis was carried out on the same sample used for turbidity measurements by one of two methods as indicated in the examples:
  • ICP- OES Inductively coupled plasma optical emission spectroscopy
  • Redox/ORP electrode (#9678BNWP).
  • Example 2 Another 100-mL sample of produced water was treated with chlorine dioxide as described in Example 1 .
  • a dose of 100 mg/L (SiO2 basis) of a 1 .0 wt.% (SiO2 basis) solution of polysilicic acid microgel was used.
  • the pH was adjusted from 3.91 to 6.71 with aqueous ammonia.
  • the stirrer was turned off, the rust-colored coagulum was found to settle in about 17 seconds, even more rapidly than in Example 1 .
  • Example 2 Another 100-mL sample of produced water was treated with chlorine dioxide as described in Example 1 . In this case, no polysilicic acid microgel was added. The pH was adjusted from 4.17 to 6.88 with aqueous ammonia. When the stirrer was turned off, the rust-colored coagulum was found to settle in about 138 seconds, more slowly than in Examples 1 and 2.
  • Example B and Examples 3-6 another produced water from the Marcellus region was obtained and characterized as follows: pH 4.5 Ba 183 mg/kg Ca 14,500 mg/kg Fe 201 mg/kg K 953 mg/kg Mg 1620 mg/kg Mn 14 mg/kg Na 40,300 mg/kg Sr 2930 mg/kg
  • Example 3 As described in Example 3, another 200-mL sample of produced water was treated with chlorine dioxide and 5 mg/L (SiO2 basis) of polysilicic acid microgel. The stir rate was increased from 50 to 200 rpm and the pH was adjusted dropwise with aqueous ammonia from 3.18 to 6.47. At this point 50 mg/L Zetag ® 8818 cationic polyacrylamide polymer solution (BASF Corporation North America, Florham Park, NJ; 40% active) was added using a 1/400 aqueous dilution of the product. The sample was allowed to stir until a flocculated solid suspension was fully-formed (about 1 -2 minutes). At this point the stirrer was turned off and the solids were allowed to settle.
  • Zetag ® 8818 cationic polyacrylamide polymer solution BASF Corporation North America, Florham Park, NJ; 40% active
  • This example illustrates the use of a cationic polyacrylamide friction reduction polymer in combination with an anionic silica-based colloid to accelerate solids settling in a produced water sample.
  • a cationic polyacrylamide friction reduction polymer in combination with an anionic silica-based colloid to accelerate solids settling in a produced water sample.
  • another 200-mL sample of produced water was treated with chlorine dioxide and 5 mg/L (SiO2 basis) of polysilicic acid microgel.
  • the stir rate was increased from 50 to 200 rpm and the pH was adjusted dropwise with aqueous ammonia from 3.17 to 6.38.
  • 50 mg/L KemFlowTM C4107 cationic polyacrylannide polymer solution was added using a 1/1000 aqueous dilution of the product.
  • This example illustrates the utility of a lower dose of cationic organic polymer in combination with an anionic silica-based colloidal microgel.
  • another 200-mL sample of produced water was treated with chlorine dioxide and 5 mg/L (SiO2 basis) of polysilicic acid microgel.
  • the stir rate was increased from 50 to 200 rpm and the pH was adjusted dropwise with aqueous ammonia from 3.17 to 6.41 .
  • 12.5 mg/L Zetag ® 8818 cationic polyacrylannide polymer solution was added using a 1/400 aqueous dilution of the product.
  • the sample was allowed to stir until a flocculated solid suspension was fully-formed (about 1 -2 minutes).
  • a synthetic brine solution (used to closely replicate a produced water sample) with the following composition was prepared in deionized water for use in Examples 7 and 8, and Comparative Examples C - F.
  • Example 8 Another 200 mL sample of synthetic brine solution was prepared as described in Example 7, treated with 35 mg/L chlorine dioxide and 10 mg/L (SiO2 basis) of polysilicic acid microgel. The stir rate was increased from 50 to 200 rpm and the pH was adjusted dropwise with aqueous ammonia from 2.91 to 6.65. At this point 50 mg/L Zetag 8818 cationic polyacrylamide polymer solution was added using a 1/400 aqueous dilution of the product. The sample was allowed to stir until a flocculated solid suspension was fully-formed (about 1 -2 minutes). At this point the stirrer was turned off and the solids were allowed to settle.
  • Comparative Examples D and E show that without the addition of chlorine dioxide, reduction in the concentration of soluble and suspended oxidizable metal ion salts (e.g., iron salts) is not achieved.
  • soluble and suspended oxidizable metal ion salts e.g., iron salts
  • Comparative Example D Another 200 ml_ sample of synthetic brine solution was prepared as described in Example 7, but was not treated with chlorine dioxide.
  • Comparative Example E Another 200 ml_ sample of synthetic brine solution was prepared as described in Comparative Example D without chlorine dioxide treatment. In this case it was treated with 10 mg/L (SiO2 basis) of polysilicic acid microgel solution and 50 mg/L Zetag ® 8818 cationic polyacrylamide polymer solution as described in Example 8. The resultant pH after polmer addition was 6.14, so no further pH adjustment was required.
  • ICP-OES inductively coupled plasma optical emission spectroscopy

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

La présente invention concerne un nouveau procédé servant au traitement de fluide de fracturation hydraulique. Le fluide de fracturation hydraulique est traité avec un colloïde anionique à base de silice suivant une quantité et pendant une durée suffisantes pour coaguler certains contaminants contenus dans le fluide de fracturation hydraulique. Les contaminants peuvent par la suite être retirés du fluide de fracturation hydraulique.
PCT/US2014/034865 2013-04-23 2014-04-22 Procédé servant au traitement et au recyclage de fluide de fracturation hydraulique WO2014176188A1 (fr)

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US10377942B2 (en) 2017-04-06 2019-08-13 Nissan Chemical America Corporation Hydrocarbon formation treatment micellar solutions
US10563117B2 (en) 2017-09-13 2020-02-18 Nissan Chemical America Corporation Crude oil recovery chemical fluids
WO2020092920A1 (fr) 2018-11-02 2020-05-07 Nissan Chemical America Corporation Récupération améliorée d'huile à l'aide de fluides de traitement comprenant de la silice colloïdale avec un agent de soutènement
US10801310B2 (en) 2017-09-26 2020-10-13 Nissan Chemcial America Corporation Using gases and hydrocarbon recovery fluids containing nanoparticles to enhance hydrocarbon recovery
US10870794B2 (en) 2017-11-03 2020-12-22 Nissan Chemical America Corporation Using brine resistant silicon dioxide nanoparticle dispersions to improve oil recovery

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