CN104178102A - Cross-linkable high-temperature-resistant residue-free polybasic copolymerizable fracturing fluid and preparation method thereof - Google Patents
Cross-linkable high-temperature-resistant residue-free polybasic copolymerizable fracturing fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cross-linkable high-temperature-resistant residue-free polybasic copolymerizable fracturing fluid and a preparation method thereof. The preparation method comprises the following steps of (1) preparing a thickener for the fracturing fluid; (2) preparing a cross-linking agent for the fracturing fluid; (3) preparing a gel breaker for the fracturing fluid and (4) preparing the cross-linkable high-temperature-resistant residue-free polybasic copolymerizable fracturing fluid. The fracturing fluid prepared by adopting the preparation method has the characteristics of excellent viscoelasticity, temperature resistance and shear resistance, sand-carrying performance and wide applicable temperature range; the fracturing fluid can well meet the requirement on the fracturing construction, and the content of the residue is very low; after the fracturing, the secondary harm to a reservoir is small and thus the fracturing effect is improved and the production capacity of the reservoir is increased.
Description
Technical field
The present invention relates to oilfield chemistry and fracturing yield increasing technical field, in particular a kind of crosslinkable high temperature resistance is without residue multi-component copolymer type fracturing liquid and preparation method thereof.
Background technology
Apply high pressure by uphole equipment, in exploitation reservoir, inject a kind of suitable fluid, exceed after formation-parting pressure, fluid can rive reservoir make its produce crack, carry propping agent simultaneously and spread in crack, treat pressure release, the broken glue of fluid returns discharges behind stratum, proppant pack, in the new crack producing, forms the fluid channel of a high flow conductivity, thereby improves the injectability of Oil & Gas Productivity or enhancing well.This oil reservoir yield increase is waterfrac treatment, and fluid used is fracturing liquid, is one of key factor determining pressing crack construction success or failure.
The continuous minimizing that can adopt, easily adopt reserves along with oil, In Oil Field Exploration And Development to ocean, deep-well, middle-deep well and ultra deep well future development, and the exploitation of high temperature deep well is one of great difficult problem, high temperature oil gas well temperature all more than 120 DEG C, and the temperature of the Oil/gas Well of those abnormal high temperature degree gradients can reach 160 DEG C and more than.From domestic and international fracturing reform experience, the main bugbear that high temperature pressure break is brought is: reservoir temperature is high, requires fracturing liquid to have good heat resistance; The high-shear time of experience is long, requires fracturing liquid to possess good anti-shear performance and viscosity recovery performance; Secondly, fracturing liquid must be paid attention to the injury of reservoir, and exploitation is also a great problem to the low fracturing liquid of reservoir damage.
The a lot of crosslinked guanidine gum fracturing fluid Applicable temperature scope using is at present wider, also can meet high temperature requirement, but guanidine gum fracturing fluid system will be added the chemical additive such as linking agent and sterilant, after broken glue, residue content is high, be difficult for the row of returning, large to formation damage, and crosslinked frozen glue is because viscosity is high, frictional resistance increases, and has further improved the difficulty of pressing crack construction; Although and the VES fracturing liquid of report had reduced of the fracturing fluid residue problem dramatically in recent years, fall frictional resistance also better, because its heat-resisting property is poor and do not have a general applicability simultaneously.
In recent years, the little water-soluble polymers of formation damage is become the main direction of domestic and international research.Compared with natural polymer, features such as (even without residues) that these polymkeric substance have strong, the broken colloidality of thickening capabilities can be good, residue is few, but also there is the imperfect shortcoming of heat resistance in synthetic polymer hydrofracturing fluid, makes applicable temperature range little.Therefore in the thinking and basis of water-soluble polymers research, it is particularly important without residue and the low fracturing fluid system of frictional resistance that research possesses good, the low injury of temperature resistance anti-shear performance.
Summary of the invention
Technical problem to be solved by this invention be for prior art preparing the deficiency existing in fracturing liquid, provide a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid and preparation method thereof.
Technical scheme of the present invention is as follows:
A kind of crosslinkable high temperature resistance is without the of the fracturing fluid preparation method of residue multi-component copolymer type, and its step is as follows:
(1) preparation of fracturing fluid gelatinizer
Vinylformic acid, acrylamide, positively charged ion unsaturated monomer, negatively charged ion unsaturated monomer and water are added in reactor and mixed, add sheet alkali regulation system pH value to 8～9, add emulsifying agent Sodium dodecylbenzene sulfonate, add redox initiator ammonium persulfate-sodium bisulfite, be to react 4h～6h at 40 DEG C～45 DEG C in temperature of reaction, after being hydrolyzed 5h at 90 DEG C, obtain colloidal product, colloid is carried out to granulation, dry, pulverizing, obtain fracturing fluid gelatinizer;
(2) preparation of linking agent for fracturing liquid
In reactor, add dimethylbenzene as solvent, add Dodecyl Dimethyl Amine, positive stearyl alcohol and methyl-sulfate as reactant, adding sodium carbonate to regulate pH value is 7～8, add catalyzer Diisopropyl azodicarboxylate, under 45 DEG C～55 DEG C conditions, carry out hydrocarbyl reaction 4h～5h, after reaction finishes, cold filtration obtains fracturing liquid linking agent solid product; Fracturing liquid is dissolved in water with linking agent solid product, is mixed with massfraction and is 25% solution, after dissolving completely, be uniformly mixed, obtain fracturing liquid linking agent;
(3) preparation of gel breaker for fracturing liquid
In reactor, add after composite sac clothing material polyimide, ethyl acetate stirring and dissolving, add Potassium Persulphate, logical nitrogen also stirs, and controlling solution temperature is 80 DEG C, reaction 30min, add emulsifier span 85 and polysorbate60, viscosifying agent Polyethylene Glycol-600, and add water, keep 80 DEG C of temperature of reaction, stopped reaction after continuation reaction 60min, reactant is sprayed and granulation by spray drying unit, and at 70 DEG C, dry straight constant weight, obtain fracturing liquid gel breaker;
(4) crosslinkable high temperature resistance is without residue multi-component copolymer type fracturing liquid
The weight percent of the component of fracturing liquid base fluid is: fracturing fluid gelatinizer is 0.3%～0.65%, and surplus is water;
When construction, additive comprises fracturing liquid linking agent and fracturing liquid gel breaker or ammonium persulphate; Wherein, in the time that formation temperature is 90～160 DEG C, when construction, the component of additive accounts for the weight percent of base fluid and is: fracturing liquid linking agent is 0.2%～0.6%, and fracturing liquid gel breaker is 0.02%～0.05%; When formation temperature is 30～90 DEG C, when construction, the component of additive accounts for the weight percent of base fluid and is: fracturing liquid linking agent is 0.2%～0.6%, and ammonium persulphate is 0.05%～0.08%.
Described preparation method, in step (1), described positively charged ion unsaturated monomer is n alkyl dimethyl diallyl ammonium chloride, wherein n is 12,14,16 or 18; Negatively charged ion unsaturated monomer is 2-acrylamide-2-methylpro panesulfonic acid or sodium salt of methacrylic acid.
Described preparation method, in step (1), calculate by mass percentage, vinylformic acid is 2%～5%, acrylamide is 35%～45%, positively charged ion unsaturated monomer is 8%～10%, and negatively charged ion unsaturated monomer is 1%～3%, and initiator ammonium persulfate-sodium bisulfite is 0.1%～0.5%, wherein the mass ratio of ammonium persulphate and sodium bisulfite is 3:1, sheet alkali is 5%-8%, and emulsifying agent Sodium dodecylbenzene sulfonate is 3%, and all the other are water.
Described preparation method, in step (2), calculate by mass percentage, hexadecyldimethyl benzyl ammonium tertiary amine is 16%～18%, positive stearyl alcohol is 22%～27%, and methyl-sulfate is 15%～20%, and sodium carbonate is 1.5%～3%, Diisopropyl azodicarboxylate is 1%～3%, and all the other are solvent xylene.
Described preparation method, in step (3), calculates by mass percentage, and polyimide is 35%, ethyl acetate is 14%, and Potassium Persulphate is 25%, and emulsifying agent is 8%, wherein the mass ratio of sorbester p37 and polysorbate60 is 1:1, and viscosifying agent Polyethylene Glycol-600 is 2%, and all the other are water.
The crosslinkable high temperature resistance that described preparation method makes is without residue multi-component copolymer type fracturing liquid.
Described fracturing liquid gel breaker is a kind of capsule breaker, and it is taking oxygenant as main raw material, makes through techniques such as spraying, granulations, and wherein the main component of oxygenant is Potassium Persulphate.Good liquid properties simultaneously, again can be by thoroughly broken glue of fracturing liquid after pressure break completes when the pressing crack construction with ensureing fracturing liquid adding of gel breaker for fracturing liquid, and under formation temperature, the corresponding broken glue time is 2.0～5.0 hours.
A kind of crosslinkable high temperature resistance provided by the invention is as follows without compound method in the laboratory of residue multi-component copolymer type fracturing liquid base fluid:
In laboratory, by the weight percent of base fluid component, in waring agitator, add water, under agitation condition, slowly in water, add fracturing fluid gelatinizer, after stirring, obtain crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid base fluid.
A kind of crosslinkable high temperature resistance provided by the invention is as follows without the working-yard compound method of residue multi-component copolymer type fracturing liquid base fluid:
At the construction field (site), by the weight percent of base fluid component, add water in Agitation Tank, suck the fracturing fluid gelatinizer of base fluid under large tank agitation condition from jet rifle, the suction of viscosifying agent must slowly, be as the criterion not lump and not form flake; After viscosifying agent adds, stir 20min, liquid leaves standstill 2 hours, obtains crosslinkable high temperature resistance without the of the fracturing fluid base fluid of residue multi-component copolymer type.
Beneficial effect of the present invention is: the synthetic method of a kind of high temperature resistance without residue multi-component copolymer type viscosifying agent is provided, and utilize this viscosifying agent to prepare a kind of crosslinkable high temperature resistance without the of the fracturing fluid method of residue multi-component copolymer type, this viscosifying agent and of the fracturing fluid premium properties are mainly summarized as follows:
(1) aqueous solution apparent viscosity of fracturing fluid gelatinizer increases with the increase of working concentration, and at normal temperatures, when this viscosifying agent 0.50%, the apparent viscosity of solution can reach 90mPas (170s
-1) more than, there is stronger tackifying ability;
(2) this viscosifying agent residue content is very low, and the secondary injury to reservoir after pressure break is little, thereby improves fracturing effect, increases reservoir productivity;
(3) in fracturing fluid gelatinizer molecule with hydrophobic grouping, in water, can form a kind of fluid with reversible construction, there is good visco-elasticity, elastic behavior is obvious, takes sand thereby realize visco-elasticity;
(4) after fracturing liquid mixes with fracturing liquid base fluid with linking agent, can the hydrogen bond in solution molecule be coupled together by the form of physical crosslinking, improve fracturing liquid apparent viscosity and structural strength, form the frozen glue of reversible construction, so, when pressing crack construction, can improve fracturing liquid temperature resistance anti-shear performance;
(5) just because of the reversible structure of fracturing liquid, viscosity increases and declines with speed ladder, and after shearing action stops, its structure recovery, viscosity also can be recovered thereupon, thereby determined that this fracturing liquid has thixotropy, therefore in pressing crack construction ensure well take grittiness can prerequisite under can significantly reduce again resistance to flow, frictional resistance is starkly lower than conventional guanidine gum fracturing fluid;
(6) at Qinghai Oil Field hydrojet horizontal well, the a certain prospect pit in Central Plains is applied high temperature resistance provided by the invention without residue multi-component copolymer type crosslinkable fracturing liquid, smooth and effect of increasing production is obvious in the construction of low hot-well, still obtained success, and obtained good effect of increasing production at high temperature, the very poor reservoir of reservoir geology situation.This illustrates that fracturing liquid Applicable temperature scope provided by the invention is wide, not only can meet well pressing crack construction requirement, and little to formation damage, has confirmed that this fracturing liquid is that a kind of crosslinkable high temperature resistance is without residue multi-component copolymer type fracturing liquid.
Brief description of the drawings
Fig. 1 is for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing fluid gelatinizer thickening capabilities curve.
Fig. 2 tests without residue multi-component copolymer type fracturing fluid gelatinizer stability of solution for the invention provides a kind of crosslinkable high temperature resistance.
Fig. 3 hangs performance picture for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid.
Fig. 4 is for the invention provides a kind of crosslinkable high temperature resistance without 60 DEG C of heatproof curves of resistance to shearing test of residue multi-component copolymer type fracturing liquid.
Fig. 5 is for the invention provides a kind of crosslinkable high temperature resistance without 90 DEG C of heatproof curves of resistance to shearing test of residue multi-component copolymer type fracturing liquid.
Fig. 6 is for the invention provides a kind of crosslinkable high temperature resistance without 120 DEG C of heatproof curves of resistance to shearing test of residue multi-component copolymer type fracturing liquid.
Fig. 7 is for the invention provides a kind of crosslinkable high temperature resistance without 160 DEG C of heatproof curves of resistance to shearing test of residue multi-component copolymer type fracturing liquid.
Fig. 8 is for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid visco-elasticity test curve.
Fig. 9 is for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid shear thinning behavior test curve.
Figure 10 is for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid flow conductivity injury test curve.
Figure 11 is for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid rig-site utilization construction curve 1.
Figure 12 is for the invention provides a kind of crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid rig-site utilization construction curve 2.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
If do not particularly point out, the fracturing liquid performance evaluation experiment condition relating in embodiment and experimental technique are all with reference to PetroChina Company Limited.'s industry standard " SY/T6376-2008 fracturing liquid general technical specifications " and " SY/T5107-2005 aqueous fracturing fluid method of evaluating performance "; If do not particularly point out, the percentage sign " % " relating in embodiment is mass percent.
The crosslinkable high temperature resistance of embodiment 1 is synthetic without residue multi-component copolymer type fracturing fluid gelatinizer
Vinylformic acid, acrylamide, hexadecyldimethyl benzyl ammonium diallyl ammonium chloride, 2-acrylamide-2-methylpro panesulfonic acid and water are added in reactor and mixed, add sheet alkali to regulate pH value, recording pH by Accurate pH value is 8.8, add emulsifying agent Sodium dodecylbenzene sulfonate, add redox initiator ammonium persulfate-sodium bisulfite, be to react 5.5h at 42 DEG C in temperature, and obtain colloidal product be hydrolyzed 5h at 90 DEG C after, colloid is carried out to granulation, dry, pulverizing, obtain fracturing fluid gelatinizer;
To react total system quality as 100%, wherein, vinylformic acid accounts for 3% of total mass, acrylamide accounts for 33% of total mass, hexadecyldimethyl benzyl ammonium diallyl ammonium chloride accounts for 8% of total mass, 2-acrylamide-2-methylpro panesulfonic acid (AMPS) accounts for 2% of total mass, initiator ammonium persulfate-sodium bisulfite accounts for 0.3% of total mass, wherein the mass ratio of ammonium persulphate and sodium bisulfite is 3:1, sheet alkali accounts for 6% of total mass, emulsifying agent Sodium dodecylbenzene sulfonate accounts for 3% of total mass, and all the other are water.
The product performance that this synthetic schemes obtains are good, and adopt the viscosifying agent of this product as this fracturing fluid system.
Embodiment 2 fracturing liquids are synthetic with linking agent
In reactor, add dimethylbenzene as solvent, add Dodecyl Dimethyl Amine, positive stearyl alcohol and methyl-sulfate as reactant, add sodium carbonate to regulate pH value, recording pH with accurate pH test paper is 7.9, add catalyzer Diisopropyl azodicarboxylate, under 51 DEG C of conditions, carry out hydrocarbyl reaction 4h, after reaction finishes, cold filtration obtains fracturing liquid linking agent solid product.
In above-mentioned reaction system, to react total system quality as 100%, wherein, hexadecyldimethyl benzyl ammonium tertiary amine accounts for 18% of total mass, positive stearyl alcohol accounts for 25% of total mass, and methyl-sulfate accounts for 16% of total mass, and sodium carbonate accounts for 2% of total mass, Diisopropyl azodicarboxylate accounts for 1% of total mass, and all the other are solvent xylene.
The fracturing liquid obtaining is dissolved in water with linking agent solid product, is mixed with massfraction and is 25% solution, after dissolving completely, be uniformly mixed, obtain the fracturing liquid linking agent of this fracturing fluid system.
The preparation of gel breaker for embodiment 3 fracturing liquids
In reactor, add after composite sac clothing material polyimide, ethyl acetate (oil phase) stirring and dissolving, add Potassium Persulphate, logical nitrogen also stirs, and to control solution temperature be 80 DEG C, after reaction 30min, add emulsifying agent (sorbester p37 and polysorbate60), viscosifying agent Polyethylene Glycol-600, and add water, keep 80 DEG C of temperature of reaction, continue after reaction 60min, stopped reaction, sprays reactant granulation by spray drying unit, and at 70 DEG C, dry straight constant weight, obtain fracturing liquid gel breaker.
In above-mentioned reaction system, to react total system quality as 100%, wherein, polyimide accounts for 35% of total mass, Potassium Persulphate accounts for 25% of total mass, and ethyl acetate accounts for 14% of total mass, and emulsifying agent accounts for 8% (wherein the mass ratio of sorbester p37 and polysorbate60 is 1:1) of total mass, viscosifying agent Polyethylene Glycol-600 accounts for 2% of total mass, and all the other are water.
Following examples fracturing fluid gelatinizer used is product described in embodiment 1, and fracturing liquid is product described in embodiment 2 with linking agent, and fracturing liquid is product described in embodiment 3 with gel breaker.
The crosslinkable high temperature resistance that embodiment 4 is applicable to 30 DEG C of stratafracs is without residue multi-component copolymer type fracturing liquid
Count by weight percentage base fluid part: fracturing fluid gelatinizer 0.3%, surplus are water;
When site operation, adding the weight percent that part accounts for base fluid is: linking agent 0.2%, ammonium persulphate 0.08% for fracturing liquid.
The laboratory preparation of base fluid: press the laboratory preparation method of base fluid, preparation obtains fracturing liquid base fluid.
When broken glue test or site operation, add fracturing liquid linking agent and ammonium persulphate.
The crosslinkable high temperature resistance that embodiment 5 is applicable to 60 DEG C of stratafracs is without residue multi-component copolymer type fracturing liquid
Count by weight percentage base fluid part: fracturing fluid gelatinizer 0.4%, surplus are water;
When rheometer test, adding the weight percent that part accounts for base fluid is: linking agent 0.3% for fracturing liquid;
When site operation, adding the weight percent that part accounts for base fluid is: linking agent 0.3%, ammonium persulphate for fracturing liquid: 0.05%.
The laboratory preparation of base fluid: press the laboratory preparation method of base fluid, preparation obtains fracturing liquid base fluid.
Rheometer test: add fracturing liquid linking agent in proportion in base fluid, and adopt Haake RS6000 rheometer test fracturing liquid heatproof endurance of cutting energy.
When broken glue test or site operation, add fracturing liquid linking agent and ammonium persulphate.
The crosslinkable high temperature resistance that embodiment 6 is applicable to 90 DEG C of stratafracs is without residue multi-component copolymer type fracturing liquid
Base fluid part: fracturing fluid gelatinizer 0.45%, surplus is water;
When rheometer test, adding the weight percent that part accounts for base fluid is: linking agent 0.35% for fracturing liquid;
When site operation, adding the weight percent that part accounts for base fluid is: linking agent 0.35% for fracturing liquid, ammonium persulphate 0.03%.
The laboratory preparation of base fluid: press the laboratory preparation method of base fluid, preparation obtains fracturing liquid base fluid.
Rheometer test: add fracturing liquid linking agent in proportion in base fluid, and adopt Haake RS6000 rheometer test fracturing liquid heatproof endurance of cutting energy.
When broken glue test or site operation, add fracturing liquid linking agent and ammonium persulphate.
The crosslinkable high temperature resistance that embodiment 7 is applicable to 120 DEG C of stratafracs is without residue multi-component copolymer type fracturing liquid
Base fluid part: fracturing fluid gelatinizer 0.5%, surplus is water;
When rheometer test, adding the weight percent that part accounts for base fluid is: linking agent 0.4% for fracturing liquid;
When site operation, adding the weight percent that part accounts for base fluid is: linking agent 0.4% for fracturing liquid, fracturing liquid gel breaker: 0.04%.
The laboratory preparation of base fluid: press the laboratory preparation method of base fluid, preparation obtains fracturing liquid base fluid.
Rheometer test: add fracturing liquid linking agent in proportion in base fluid, and adopt Haake RS6000 rheometer test fracturing liquid heatproof endurance of cutting energy.
When broken glue test or site operation, add fracturing liquid linking agent and fracturing liquid gel breaker.
The crosslinkable high temperature resistance that embodiment 8 is applicable to 160 DEG C of stratafracs is without residue multi-component copolymer type fracturing liquid
Base fluid part: fracturing fluid gelatinizer 0.65%, surplus is water;
When rheometer test, adding the weight percent that part accounts for base fluid is: linking agent 0.6% for fracturing liquid;
When site operation, adding the weight percent that part accounts for base fluid is: linking agent 0.6% for fracturing liquid, fracturing liquid gel breaker: 0.02%.
The laboratory preparation of base fluid: press the laboratory preparation method of base fluid, preparation obtains fracturing liquid base fluid.
Rheometer test: add fracturing liquid linking agent in proportion in base fluid, and adopt Haake RS6000 rheometer test fracturing liquid heatproof endurance of cutting energy.
When broken glue test or site operation, add fracturing liquid linking agent and fracturing liquid gel breaker.
Embodiment 9
1, a kind of crosslinkable high temperature resistance provided by the invention is as follows without the performance evaluation of residue multi-component copolymer type fracturing fluid gelatinizer:
The crosslinkable high temperature resistance of one provided by the invention is without residue multi-component copolymer type fracturing fluid gelatinizer, and the apparent viscosity of its solution increases with the increase of viscosifying agent working concentration, and concrete change curve is shown in Fig. 1.At normal temperatures, the apparent viscosity of solution can reach 90mPas (170s when this viscosifying agent 0.50%
-1) more than, there is stronger tackifying ability.
The crosslinkable high temperature resistance of one provided by the invention, without residue multi-component copolymer type fracturing fluid gelatinizer, does not contain the food source of bacterium, and itself just has certain germicidal action in its solution system, therefore have satisfactory stability.And under 25 DEG C of conditions, place after one week, it is stable that the apparent viscosity of solution keeps, and can not produce precipitation, and experimental result is shown in Fig. 2.Illustrate that this viscosifying agent solution is not subject to the erosion of bacterium, be conducive at the scene or industrialized construction is carried out in field.
2, of the fracturing fluid to hang performance evaluation as follows without residue multi-component copolymer type for the crosslinkable high temperature resistance of one provided by the invention:
The crosslinkable high temperature resistance of one provided by the invention is without residue multi-component copolymer type fracturing liquid, after fracturing liquid viscosity synergistic agent and the effect of fracturing liquid base fluid, can form the frozen glue of some strength, and there is certain hanging property, experimental phenomena is shown in Fig. 3, experiment shows that multi-component copolymer type water-soluble polymer solution also can be by being cross-linked to improve fracturing liquid intensity, thereby improves fracturing liquid heat resistance.
3, the crosslinkable high temperature resistance of one provided by the invention can be evaluated as follows without the of the fracturing fluid heatproof endurance of cutting of residue multi-component copolymer type:
(1) embodiment 5 fracturing liquids having been carried out to heatproof endurance of cutting can test.
Laboratory apparatus: Haake RS6000 rheometer, rotor test macro, uses rotor PZ38;
Test condition: temperature 60 C, shearing rate 170s
-1, test duration 120min.
(2) embodiment 6 fracturing liquids having been carried out to heatproof endurance of cutting can test.
Laboratory apparatus: Haake RS6000 rheometer, rotor test macro, uses rotor PZ38;
Test condition: 90 DEG C of temperature, shearing rate 170s
-1, test duration 120min.
(3) embodiment 7 fracturing liquids having been carried out to heatproof endurance of cutting can test.
Laboratory apparatus: Haake RS6000 rheometer, rotor test macro, uses rotor PZ38;
Test condition: 120 DEG C of temperature, shearing rate 170s
-1, test duration 120min.
(4) embodiment 8 fracturing liquids having been carried out to heatproof endurance of cutting can test.
Laboratory apparatus: Haake RS6000 rheometer, rotor test macro, uses rotor PZ38;
Test condition: 160 DEG C of temperature, shearing rate 170s
-1, test duration 120min.
The experimental result that four groups of of the fracturing fluid heatproof endurance of cuttings can be tested is shown in respectively Fig. 4, Fig. 5, Fig. 6, Fig. 7.At 60 DEG C, 90 DEG C, 120 DEG C, 160 DEG C, 170s
-1shear 120min, there is certain temperature sensitivity in this fracturing liquid in temperature-rise period, and apparent viscosity raises and reduces with temperature, but reach after certain temperature, the linking agent adding in fracturing liquid and base fluid have effect crosslinked a little less than in the of, make apparent viscosity have a uphill process, decline subsequently.When after temperature-stable, fracturing liquid apparent viscosity does not have dependency to the time, has a structure running balance in system, and apparent viscosity does not change in time, but remains on a numerical range relatively stably.
Result shows: heatproof endurance of cutting at 30～160 DEG C can be good without residue multi-component copolymer type fracturing liquid for a kind of crosslinkable high temperature resistance provided by the invention, fracturing liquid Stability Analysis of Structures, by formula adjustment, the requirement of the long-time pressing crack construction well within the scope of can satisfied temperature.
4, the crosslinkable high temperature resistance of one provided by the invention is as follows without the of the fracturing fluid visco-elasticity test of residue multi-component copolymer type:
Fracturing liquid in embodiment 6, after 160 DEG C of down cut 120min, has done visco-elasticity test to it, determines frequency and determines stress scans (Osc Time Curve).
Testing tool: Haake RS6000 rheometer, rotor test macro, uses rotor PZ38;
Test condition: set shear-stress τ=0.5Pa, frequency f=6.18HZ.
The crosslinkable high temperature resistance of one provided by the invention carries out viscoelasticity energy test result without residue multi-component copolymer type fracturing liquid and sees Fig. 8.Experimental result shows: in whole experimentation, of the fracturing fluid storage modulus G' provided by the invention remains on stationary value, and G' ≈ G* is also far longer than Loss modulus G ", elasticity is greater than viscosity significantly; elastic behavior is obvious, so fracturing liquid suspends, prop-carrying capacity can meet construction requirement completely.
5, the crosslinkable high temperature resistance of one provided by the invention is as follows without the of the fracturing fluid shear thinning behavior test of residue multi-component copolymer type:
Fracturing liquid in embodiment 6 is carried out to shear thinning behavior test, and calculated this of the fracturing fluid n, K value.
Testing tool: Haake RS6000 rheometer, cone-plate test macro, uses C60/1 ° of Ti of rotor;
Test condition: room temperature, shearing rate 0s
-1～1000s
-1～0s
-1.
Test result is shown in Fig. 9, and the fracturing liquid parameter going out by computed in software is: k=1.596, n=0.4925, and the consistency index k of fracturing fluid system is larger, and flow stance index n is less, and liquid tackifying is strong, and shear thinning behavior is good.
Experimental result shows, the crosslinkable high temperature resistance of one provided by the invention is without residue multi-component copolymer type fracturing liquid, its apparent viscosity declines with shearing the increase of speed ladder, but stopping shearing rear fracturing liquid viscosity can recover again, therefore this of the fracturing fluid use is well taken in guarantee under the prerequisite of grittiness energy, can significantly reduce again fluid flow resistance, so more can embody its low friction loss characteristic, more be conducive to high temperature deep well pressure break.
6, the crosslinkable high temperature resistance of one provided by the invention is as follows without the of the fracturing fluid broken glue of residue multi-component copolymer type and residue content test:
In order to improve the of the fracturing fluid row of returning, reduce the injury to reservoir, require fracturing liquid in the time that construction finishes, to realize thoroughly broken glue fast, require again fluid break time and crack closure time to match.For this reason, adopt the several formulated fracturing liquids in embodiment, break glue test, several groups of of the fracturing fluid test results are in table 1.
Table 1 embodiment breaks glue test result
Experimental result shows: under formation temperature conditions, add gel breaker by formula rate, the interior fracturing liquid of 5h can break glue completely and broken glue is functional, and breaking glue solution viscosity is low; Solution after broken glue is transparent liquid, and according to aqueous fracturing fluid method of evaluating performance, SYT5107-2005 measures fracturing fluid residue content, and residue does not almost measure; Record breaking glue solution surface tension low (27mN/m is following).Be more conducive to like this breaking glue solution and return row, reduced the injury of glue to stratum.
7, the crosslinkable high temperature resistance of one provided by the invention is as follows to supporting crack flow conductivity injury test without residue multi-component copolymer type fracturing liquid:
Test set: the instruments such as API diversion trench, electronic balance, magnetic stirring apparatus, graduated cylinder;
Testing method: install API diversion trench, select 20/40 order ceramsite propping agent, sanding concentration is generally decided to be 20kg/m
2.The fluid of test is contained in special Erlenmeyer flask, under the fluid column differential pressure action (△ H=1m) of specifying, enters API diversion trench, enter in beaker by the liquid of diversion trench, with balance metering, the every 0.5min of computer records an inferior quality and corresponding time.This fracturing fluid system breaking glue solution, the HPG fracturing liquid rubber-breaking liquid of routine and the mobility status of experiment flow media 2%KCl (or normal saline solution) are tested respectively.
Data processing: with accumulative total volume to the time curve of mapping to obtain, volume in each time period is averaged, obtain the average discharge Q in this time period, the ratio K i/KKcl that breaking glue solution and 2%KCl solution stream are crossed diversion trench rear support fracture permeability is Qi/QKcl, with Qi/QKcl to accumulative total volume mapping, obtain BCG fracturing liquid and HPG fracturing liquid rubber-breaking liquid to the damage of supporting crack flow conductivity as Figure 10.
Flow conductivity infringement is tested and is shown, after BCG fracturing liquid rubber-breaking liquid flows through and supports filling bed, flow conductivity conservation rate, more than 90%, illustrates that this system is very little to the infringement of support filling bed.And the crosslinked HPG fracturing liquid flow conductivity conservation rate after treatment of boron is very low.
Embodiment 10
Qinghai Oil Field certain level well, be positioned at the Hai Xizhou of Qinghai Province Mangnai Zhen Nan Yi Mountain area, horizontal section: 1784.47～2085.00m, fractured layer length is 295.53m, oil reservoir middle part pressure is 28.056Mpa, middle part temperature: 84.37 DEG C, this well is extensive construction well, the construction of employing hydraulic jetting fracturing, seven layers of pressure breaks altogether, for reducing the injury of fracturing reform to reservoir, this well uses crosslinkable high temperature resistance without residue multi-component copolymer type fracturing liquid (fracturing liquid formula in embodiment 6), add low-density high-strength haydite as fracturing propping agents, designing total liquid measure is 2700m
3, design adds sand amount 180m
3.Wherein the condition of construction of the 4th layer is: the perforation stage, low for liquid 14.04m
3, sandblast liquid 31.41m
3, add sand 2.00m
3, displacing liquid 10.72m
3; The pressure break stage, construction top pressure 60.80MPa, parting pressure 28.00MPa, maximum delivery 2.95m
3/ min, spearhead 44.90m
3, slug adds sand 2.00m
3, sand-carrying agent 75.79m
3, add sand 16.90m
3, average sand is than 22.29%, and construction curve is shown in Figure 11.Closing well 4h after pressure break completes, 8mm oil nozzle open flow, returns the broken glue of discharge opeing thorough, and after 5 days, discharge opeing exceedes 800m
3, 10.2 tons of operation rear every day of average produce oils, and the produce oil cycle is long.
Embodiment 11
The northern textural a certain prospect pit in Pu city in Central Plains, fractured layer position is Shi Qian peak group, level number 159#; Fractured well section 4645.0～4654.3m; Net thickness 9.3m/1 layer, formation temperature is up to 153 DEG C, and zone permeability is low, and geological state is poor.This well adopts D127mm, and P110 (pressing 96.1MPa in anti-) light sleeve pipe injects form of construction work, uses the crosslinkable high temperature resistance of one provided by the invention without residue multi-component copolymer type fracturing liquid (fracturing liquid formula in embodiment 8), total liquid measure 438m
3(spearhead 230m
3+ sand-carrying agent 163m
3+ for putting liquid 45m
3), parting pressure 71.2MPa, construction pump pressure 69.5MPa, termination of pumping pressure 88.1MPa (seeing Figure 12), adds high-strength ceramsite 32m
3, average sand is than 17.8%, high sand ratio 23%, generally discharge capacity 4.75m
3/ min.Construction process is normal smoothly, presses rear discharge opeing normal, 6 days accumulative total water outlet 338 sides, and after going into operation, output is on average at 8.3 tons/day.
Rig-site utilization proves that a kind of crosslinkable high temperature resistance provided by the invention has good high temperature resistant property really without residue multi-component copolymer type fracturing liquid, and also obtained good effect of increasing production on the poor stratum of geological state, embody of the fracturing fluid without the low injury characteristic of residue.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (6)
1. crosslinkable high temperature resistance, without the of the fracturing fluid preparation method of residue multi-component copolymer type, is characterized in that, its step is as follows:
(1) preparation of fracturing fluid gelatinizer
Vinylformic acid, acrylamide, positively charged ion unsaturated monomer, negatively charged ion unsaturated monomer and water are added in reactor and mixed, add sheet alkali regulation system pH value to 8～9, add emulsifying agent Sodium dodecylbenzene sulfonate, add redox initiator ammonium persulfate-sodium bisulfite, be to react 4h～6h at 40 DEG C～45 DEG C in temperature of reaction, after being hydrolyzed 5h at 90 DEG C, obtain colloidal product, colloid is carried out to granulation, dry, pulverizing, obtain fracturing fluid gelatinizer;
(2) preparation of linking agent for fracturing liquid
In reactor, add dimethylbenzene as solvent, add Dodecyl Dimethyl Amine, positive stearyl alcohol and methyl-sulfate as reactant, adding sodium carbonate to regulate pH value is 7～8, add catalyzer Diisopropyl azodicarboxylate, under 45 DEG C～55 DEG C conditions, carry out hydrocarbyl reaction 4h～5h, after reaction finishes, cold filtration obtains fracturing liquid linking agent solid product; Fracturing liquid is dissolved in water with linking agent solid product, is mixed with massfraction and is 25% solution, after dissolving completely, be uniformly mixed, obtain fracturing liquid linking agent;
(3) preparation of gel breaker for fracturing liquid
In reactor, add after composite sac clothing material polyimide, ethyl acetate stirring and dissolving, add Potassium Persulphate, logical nitrogen also stirs, and controlling solution temperature is 80 DEG C, reaction 30min, add emulsifier span 85 and polysorbate60, viscosifying agent Polyethylene Glycol-600, and add water, keep 80 DEG C of temperature of reaction, stopped reaction after continuation reaction 60min, reactant is sprayed and granulation by spray drying unit, and at 70 DEG C, dry straight constant weight, obtain fracturing liquid gel breaker;
(4) crosslinkable high temperature resistance is without residue multi-component copolymer type fracturing liquid
The weight percent of the component of fracturing liquid base fluid is: fracturing fluid gelatinizer is 0.3%～0.65%, and surplus is water;
When construction, additive comprises fracturing liquid linking agent and fracturing liquid gel breaker or ammonium persulphate; Wherein, in the time that formation temperature is 90～160 DEG C, when construction, the component of additive accounts for the weight percent of base fluid and is: fracturing liquid linking agent is 0.2%～0.6%, and fracturing liquid gel breaker is 0.02%～0.05%; When formation temperature is 30～90 DEG C, when construction, the component of additive accounts for the weight percent of base fluid and is: fracturing liquid linking agent is 0.2%～0.6%, and ammonium persulphate is 0.05%～0.08%.
2. preparation method according to claim 1, is characterized in that, in step (1), described positively charged ion unsaturated monomer is n alkyl dimethyl diallyl ammonium chloride, and wherein n is 12,14,16 or 18; Negatively charged ion unsaturated monomer is 2-acrylamide-2-methylpro panesulfonic acid or sodium salt of methacrylic acid.
3. preparation method according to claim 1, is characterized in that, in step (1), calculate by mass percentage, vinylformic acid is 2%～5%, and acrylamide is 35%～45%, and positively charged ion unsaturated monomer is 8%～10%, negatively charged ion unsaturated monomer is 1%～3%, initiator ammonium persulfate-sodium bisulfite is 0.1%～0.5%, and wherein the mass ratio of ammonium persulphate and sodium bisulfite is 3:1, and sheet alkali is 5%-8%, emulsifying agent Sodium dodecylbenzene sulfonate is 3%, and all the other are water.
4. preparation method according to claim 1, it is characterized in that, in step (2), calculate by mass percentage, hexadecyldimethyl benzyl ammonium tertiary amine is 16%～18%, and positive stearyl alcohol is 22%～27%, methyl-sulfate is 15%～20%, sodium carbonate is 1.5%～3%, and Diisopropyl azodicarboxylate is 1%～3%, and all the other are solvent xylene.
5. preparation method according to claim 1, it is characterized in that, in step (3), calculate by mass percentage, polyimide is 35%, ethyl acetate is 14%, Potassium Persulphate is 25%, and emulsifying agent is 8%, and wherein the mass ratio of sorbester p37 and polysorbate60 is 1:1, viscosifying agent Polyethylene Glycol-600 is 2%, and all the other are water.
6. the crosslinkable high temperature resistance making according to the arbitrary described preparation method of claim 1～5 is without residue multi-component copolymer type fracturing liquid.
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