CN104178102B - Cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid and preparation method thereof - Google Patents
Cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid and a preparation method thereof. The preparation method comprises the following steps: (1) the preparation method comprises the following steps of (1) preparation of a fracturing fluid thickening agent, (2) preparation of a crosslinking agent for a fracturing fluid, (3) preparation of a gel breaker for the fracturing fluid, and (4) crosslinkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid. The fracturing fluid prepared by the invention has excellent viscoelasticity, temperature resistance, shearing resistance and sand carrying performance, is wide in application temperature range, can well meet the fracturing construction requirement, has very low residue content, and has small secondary damage to a reservoir after fracturing, so that the fracturing effect is improved, and the reservoir capacity is increased.
Description
Technical Field
The invention relates to the technical field of oilfield chemistry and fracturing yield increase, in particular to a crosslinkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid and a preparation method thereof.
Background
The method comprises the steps of applying high pressure through ground equipment, injecting a proper fluid into a developed reservoir, after the fracture pressure of a stratum is exceeded, splitting the reservoir by the fluid to generate cracks, carrying a propping agent and spreading the propping agent into the cracks, after the pressure is released and the fluid is broken and flows back out of the stratum, filling the propping agent into the newly generated cracks to form a fluid channel with high flow conductivity, and thus improving the productivity of an oil-gas well or enhancing the injection capacity of a water well. The oil reservoir yield increasing mode is hydraulic fracturing, and the used fluid is fracturing fluid, which is one of the key factors for determining success or failure of fracturing construction.
With the continuous reduction of petroleum recoverable and easily recoverable reserves, the development of oil field exploration and development has been developed towards oceans, deep wells, medium-deep wells and ultra-deep wells, and the development of high-temperature deep wells is one of the major problems, the temperature of high-temperature oil and gas wells is above 120 ℃, and the temperature of oil and gas wells with abnormally high temperature gradients can reach 160 ℃ or above. From the fracturing reformation experience at home and abroad, the main difficult problems brought by high-temperature fracturing are as follows: the reservoir temperature is high, and the fracturing fluid is required to have good temperature resistance; the high shear time is long, and the fracturing fluid is required to have good shear resistance and viscosity recovery performance; secondly, the damage of the fracturing fluid to the reservoir must be paid attention to, and the development of the fracturing fluid with low damage to the reservoir is also a great problem.
Many currently used cross-linked guanidine gum fracturing fluids have wide applicable temperature range and can also meet the high-temperature requirement, but a guanidine gum fracturing fluid system needs to be added with chemical additives such as a cross-linking agent and a bactericide, the content of residues after gel breaking is high, the residues are not easy to flow back and have large damage to the stratum, and cross-linked jelly has high viscosity and increased friction resistance, so that the difficulty of fracturing construction is further improved; the VES fracturing fluid reported in recent years has the advantages of greatly reducing the residue problem of the fracturing fluid and having better friction resistance reduction, but has no general applicability due to poor temperature resistance.
In recent years, water-soluble polymers with little damage to the stratum have become the main direction of domestic and foreign research. Compared with natural polymers, the polymers have the characteristics of strong thickening capacity, good gel breaking performance, little residue (even no residue) and the like, but the synthetic polymer fracturing fluid also has the defect of poor temperature resistance, so that the applicable temperature range is small. Therefore, on the basis of the thought and research of water-soluble polymers, the research of a fracturing liquid system with excellent temperature and shear resistance, low damage, no residue and low friction resistance is particularly important.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art in preparing fracturing fluid, and provides a cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid and a preparation method thereof.
The technical scheme of the invention is as follows:
a preparation method of a cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid comprises the following steps:
(1) preparation of fracturing fluid densifier
Adding acrylic acid, acrylamide, a cationic unsaturated monomer, an anionic unsaturated monomer and water into a reaction kettle, uniformly mixing, adding caustic soda flakes to adjust the pH value of a system to 8-9, adding an emulsifier sodium dodecyl benzene sulfonate, adding a redox initiator ammonium persulfate-sodium bisulfite, reacting at the reaction temperature of 40-45 ℃ for 4-6 h, hydrolyzing at the temperature of 90 ℃ for 5h to obtain a colloidal product, and granulating, drying and crushing the colloid to obtain a fracturing fluid thickening agent;
(2) preparation of cross-linking agent for fracturing fluid
Adding dimethylbenzene serving as a solvent into a reaction kettle, adding dodecyl dimethyl tertiary amine, n-octadecyl alcohol and dimethyl sulfate serving as reactants, adding sodium carbonate to adjust the pH value to 7-8, adding azodiisobutyronitrile serving as a catalyst, carrying out a alkylation reaction for 4-5 hours at the temperature of 45-55 ℃, and after the reaction is finished, cooling and filtering to obtain a crosslinking agent solid product for fracturing fluid; dissolving a crosslinking agent solid product for the fracturing fluid in water to prepare a solution with the mass fraction of 25%, and stirring and mixing uniformly after completely dissolving to obtain the crosslinking agent for the fracturing fluid;
(3) preparation of gel breaker for fracturing fluid
Adding polyimide and ethyl acetate serving as composite capsule coat materials into a reaction kettle, stirring and dissolving, adding potassium persulfate, introducing nitrogen and stirring, controlling the temperature of the solution to be 80 ℃, reacting for 30min, adding span 85 and tween 60 serving as emulsifiers and polyethylene glycol 600 serving as a thickening agent, adding water, keeping the reaction temperature at 80 ℃, continuing to react for 60min, stopping the reaction, spraying and granulating reactants through a spray drying device, and drying at 70 ℃ until constant weight is achieved to obtain the gel breaker for the fracturing fluid;
(4) crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid
The fracturing fluid base fluid comprises the following components in percentage by weight: 0.3 to 0.65 percent of fracturing fluid thickening agent and the balance of water;
the additives during construction comprise a cross-linking agent for fracturing fluid, a gel breaker for fracturing fluid or ammonium persulfate; when the ground temperature is 90-160 ℃, the components of the additive account for the base fluid in percentage by weight during construction: 0.2 to 0.6 percent of cross-linking agent for fracturing fluid and 0.02 to 0.05 percent of gel breaker for fracturing fluid; when the ground layer temperature is 30-90 ℃, the components of the additive account for the base fluid in percentage by weight during construction: 0.2 to 0.6 percent of cross-linking agent for fracturing fluid and 0.05 to 0.08 percent of ammonium persulfate.
In the preparation method, in the step (1), the cationic unsaturated monomer is n-alkyl dimethyl diallyl ammonium chloride, wherein n is 12, 14, 16 or 18; the anionic unsaturated monomer is 2-acrylamide-2-methylpropanesulfonic acid or methacrylic acid sodium salt.
The preparation method comprises the following steps of (1), according to mass percent, 2-5% of acrylic acid, 35-45% of acrylamide, 8-10% of cationic unsaturated monomer, 1-3% of anionic unsaturated monomer, 0.1-0.5% of initiator ammonium persulfate-sodium bisulfite, wherein the mass ratio of ammonium persulfate to sodium bisulfite is 3:1, 5-8% of flake caustic soda, 3% of emulsifier sodium dodecyl benzene sulfonate, and the balance of water.
According to the preparation method, in the step (2), the mass percent of the dodecyl dimethyl tertiary amine is 16-18%, the mass percent of the n-octadecanol is 22-27%, the mass percent of the dimethyl sulfate is 15-20%, the mass percent of the sodium carbonate is 1.5-3%, the mass percent of the azobisisobutyronitrile is 1-3%, and the balance is the solvent xylene.
According to the preparation method, in the step (3), by mass percentage, the polyimide accounts for 35%, the ethyl acetate accounts for 14%, the potassium persulfate accounts for 25%, and the emulsifier accounts for 8%, wherein the mass ratio of span 85 to tween 60 is 1:1, the thickening agent polyethylene glycol 600 accounts for 2%, and the balance is water.
The crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid prepared by the preparation method.
The gel breaker for the fracturing fluid is a capsule gel breaker and is prepared by using an oxidant as a main raw material through processes of spraying, granulating and the like, wherein the main component of the oxidant is potassium persulfate. The addition of the gel breaker for the fracturing fluid can ensure good liquid performance of the fracturing fluid during fracturing construction, and can thoroughly break the gel of the fracturing fluid after fracturing is completed, wherein the corresponding gel breaking time is 2.0-5.0 hours at the formation temperature.
The invention provides a preparation method of a cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid base fluid in a laboratory, which comprises the following steps:
in a laboratory, according to the weight percentage of the components of the base fluid, adding water into a waring stirrer, slowly adding a fracturing fluid thickening agent into the water under the stirring condition, and uniformly stirring to obtain the cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid base fluid.
The invention provides a preparation method of a crosslinkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid base fluid on a construction site, which comprises the following steps:
on a construction site, adding water into a liquid preparation tank according to the weight percentage of the components of the base liquid, sucking a fracturing fluid thickening agent of the base liquid from a jet gun under the stirring condition of a large tank, wherein the sucking of the thickening agent needs to be slow, namely the thickening agent does not cake and form fish eyes; and after the thickening agent is added, stirring for 20min, and standing the liquid for 2 hours to obtain the base liquid of the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid.
The invention has the beneficial effects that: the synthesis method of the high-temperature-resistant residue-free multi-component copolymerization thickening agent and the method for preparing the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid by using the thickening agent are provided, and the excellent performances of the thickening agent and the fracturing fluid are mainly summarized as follows:
(1) the apparent viscosity of the fracturing fluid thickening agent increases with the use concentration, and the apparent viscosity of the fracturing fluid thickening agent reaches 90 mPas (170 s) at the concentration of 0.50 percent at normal temperature-1) The thickening agent has strong thickening capability;
(2) the thickening agent has low residue content, and has small secondary damage to a reservoir after fracturing, so that the fracturing effect is improved, and the reservoir productivity is increased;
(3) the molecules of the fracturing fluid densifier are provided with hydrophobic groups, so that a fluid with a reversible structure can be formed in water, and the fracturing fluid densifier has good viscoelasticity and obvious elastic behavior, thereby realizing viscoelasticity sand carrying;
(4) after the cross-linking agent for the fracturing fluid is mixed with the fracturing fluid base fluid, hydrogen bonds in solution molecules can be connected in a physical cross-linking mode, the apparent viscosity and the structural strength of the fracturing fluid are improved, and jelly with a reversible structure is formed, so that the temperature and shear resistance of the fracturing fluid can be improved during fracturing construction;
(5) the viscosity of the fracturing fluid is reduced along with the increase of the speed gradient due to the reversible structure of the fracturing fluid, and after the shearing action is stopped, the structure of the fracturing fluid is recovered, and the viscosity is recovered, so that the fracturing fluid is determined to have thixotropy, the flow resistance can be greatly reduced on the premise of ensuring good sand carrying performance in fracturing construction, and the friction resistance is obviously lower than that of the conventional guanidine gum fracturing fluid;
(6) in a certain hydraulic jet horizontal well of a Qinghai oilfield, the high-temperature-resistant residue-free multi-component copolymerization type crosslinkable fracturing fluid provided by the invention is applied to a certain exploratory well in China, the construction of the low-temperature well is smooth, the yield-increasing effect is obvious, the high-temperature-resistant residue-free multicomponent copolymerization type crosslinkable fracturing fluid is successful in a reservoir with poor geological conditions of a high-temperature oil layer, and the good yield-increasing effect is obtained. The fracturing fluid provided by the invention is wide in application temperature range, not only can well meet the requirements of fracturing construction, but also has small damage to the stratum, and the fracturing fluid is proved to be a cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid.
Drawings
FIG. 1 is a thickening capacity curve of a crosslinkable high-temperature-resistant residue-free multicomponent copolymer fracturing fluid thickening agent.
FIG. 2 is a test of the stability of a solution of a crosslinkable, high-temperature-resistant, residue-free multicomponent copolymer fracturing fluid densifier provided in the present invention.
FIG. 3 is a picture showing the hanging performance of the crosslinkable high-temperature-resistant residue-free multicomponent copolymer fracturing fluid.
FIG. 4 is a 60 ℃ temperature-resistant and shear-resistant test curve of the crosslinkable high-temperature-resistant residue-free multicomponent copolymerization fracturing fluid provided by the invention.
FIG. 5 is a 90 ℃ temperature-resistant and shear-resistant test curve of the crosslinkable high-temperature-resistant residue-free multicomponent copolymerization fracturing fluid provided by the invention.
FIG. 6 is a 120 ℃ temperature-resistant and shear-resistant test curve of the cross-linkable high-temperature-resistant residue-free multi-copolymerization fracturing fluid provided by the invention.
FIG. 7 is a 160 ℃ temperature-resistant shear-resistant test curve of the crosslinkable high-temperature-resistant residue-free multicomponent copolymerization fracturing fluid provided by the invention.
FIG. 8 is a viscoelastic test curve of a crosslinkable high-temperature-resistant residue-free multicomponent copolymer fracturing fluid.
FIG. 9 is a shear thinning test curve of the crosslinkable high-temperature-resistant residue-free multicomponent copolymerization fracturing fluid.
FIG. 10 is a flow conductivity damage test curve of a crosslinkable high-temperature-resistant residue-free multicomponent copolymer fracturing fluid provided by the invention.
FIG. 11 is a construction curve 1 for the field application of the crosslinkable high-temperature-resistant residue-free multicomponent copolymer fracturing fluid.
Detailed Description
The present invention will be described in detail with reference to specific examples.
If not specifically indicated, the experimental conditions and the experimental methods for evaluating the performance of the fracturing fluid, which are referred to in the examples, refer to the petroleum industry standard "SY/T6376-2008 general technical conditions of the fracturing fluid" and "SY/T5107-2005 water-based fracturing fluid performance evaluation method"; the percentages in the examples are given by mass unless otherwise indicated.
EXAMPLE 1 Synthesis of crosslinkable, high temperature resistant, residue free multicomponent copolymer fracturing fluid densifier
Adding acrylic acid, acrylamide, hexadecyl dimethyl diallyl ammonium chloride, 2-acrylamide-2-methyl propanesulfonic acid and water into a reaction kettle, uniformly mixing, adding caustic soda flakes to adjust the pH value, measuring the pH value to be 8.8 by using a precise pH value, adding an emulsifier sodium dodecyl benzene sulfonate, adding a redox initiator ammonium persulfate-sodium bisulfite, reacting for 5.5 hours at the temperature of 42 ℃, hydrolyzing for 5 hours at the temperature of 90 ℃ to obtain a colloidal product, and granulating, drying and crushing the colloid to obtain a fracturing fluid thickening agent;
the mass of the total reaction system is 100%, wherein acrylic acid accounts for 3% of the total mass, acrylamide accounts for 33% of the total mass, hexadecyl dimethyl diallyl ammonium chloride accounts for 8% of the total mass, 2-acrylamide-2-methyl propane sulfonic Acid (AMPS) accounts for 2% of the total mass, an initiator ammonium persulfate-sodium bisulfite accounts for 0.3% of the total mass, the mass ratio of ammonium persulfate to sodium bisulfite is 3:1, caustic soda flakes accounts for 6% of the total mass, an emulsifier sodium dodecyl benzene sulfonate accounts for 3% of the total mass, and the balance is water.
The product obtained by the synthesis scheme has excellent performance, and is used as a thickening agent of the fracturing fluid system.
Example 2 Synthesis of a crosslinking agent for fracturing fluids
Adding dimethylbenzene serving as a solvent into a reaction kettle, adding dodecyl dimethyl tertiary amine, n-octadecyl alcohol and dimethyl sulfate serving as reactants, adding sodium carbonate to adjust the pH value, measuring the pH value to be 7.9 by using a precise pH test paper, adding azodiisobutyronitrile serving as a catalyst, carrying out a alkylation reaction for 4 hours at the temperature of 51 ℃, cooling and filtering after the reaction is finished, and thus obtaining a crosslinking agent solid product for fracturing fluid.
In the reaction system, the total mass of the reaction system is 100%, wherein dodecyl dimethyl tertiary amine accounts for 18% of the total mass, n-octadecyl alcohol accounts for 25% of the total mass, dimethyl sulfate accounts for 16% of the total mass, sodium carbonate accounts for 2% of the total mass, azobisisobutyronitrile accounts for 1% of the total mass, and the balance is solvent xylene.
And adding water to dissolve the obtained crosslinking agent solid product for the fracturing fluid to prepare a solution with the mass fraction of 25%, and stirring and mixing uniformly after complete dissolution to obtain the crosslinking agent for the fracturing fluid of the fracturing fluid system.
Example 3 preparation of a breaker for fracturing fluids
Adding composite capsule coat materials of polyimide and ethyl acetate (oil phase) into a reaction kettle, stirring and dissolving, adding potassium persulfate, introducing nitrogen and stirring, controlling the temperature of the solution to be 80 ℃, after reacting for 30min, adding an emulsifier (span 85 and Tween 60) and a thickening agent polyethylene glycol 600, adding water, keeping the reaction temperature at 80 ℃, continuing to react for 60min, stopping the reaction, spraying and granulating reactants through a spray drying device, and drying at 70 ℃ until the weight is constant, thereby obtaining the gel breaker for the fracturing fluid.
In the reaction system, the mass of the total reaction system is 100%, wherein the polyimide accounts for 35% of the total mass, the potassium persulfate accounts for 25% of the total mass, the ethyl acetate accounts for 14% of the total mass, the emulsifier accounts for 8% of the total mass (wherein the mass ratio of span 85 to tween 60 is 1:1), the thickening agent polyethylene glycol 600 accounts for 2% of the total mass, and the balance is water.
The fracturing fluid thickeners used in the following examples are all the products described in example 1, the crosslinking agents for fracturing fluids are all the products described in example 2, and the breakers for fracturing fluids are all the products described in example 3.
Example 4 crosslinkable, high temperature resistant, residue free multicomponent copolymer fracturing fluid suitable for 30 ℃ formation fracturing
The base liquid part comprises the following components in percentage by weight: 0.3% of fracturing fluid thickening agent and the balance of water;
the weight percentage of the added part in the base fluid during the site construction is as follows: 0.2 percent of cross-linking agent for fracturing fluid and 0.08 percent of ammonium persulfate.
Laboratory preparation of base solutions: the fracturing fluid base fluid is prepared according to a laboratory preparation method of the base fluid.
And adding a cross-linking agent for the fracturing fluid and ammonium persulfate during gel breaking test or field construction.
Example 5 crosslinkable, high temperature resistant, residue free multicomponent copolymer fracturing fluids suitable for 60 deg.C formation fracturing
The base liquid part comprises the following components in percentage by weight: 0.4% of fracturing fluid thickening agent and the balance of water;
the weight percentage of the added part in the base fluid in the rheological test is as follows: 0.3 percent of cross-linking agent for fracturing fluid;
the weight percentage of the added part in the base fluid during the site construction is as follows: 0.3% of a crosslinking agent for fracturing fluid, and ammonium persulfate: 0.05 percent.
Laboratory preparation of base solutions: the fracturing fluid base fluid is prepared according to a laboratory preparation method of the base fluid.
And (3) rheological testing: and (3) adding a crosslinking agent for the fracturing fluid into the base fluid according to a proportion, and testing the temperature resistance and the shearing resistance of the fracturing fluid by using a Haake RS6000 rheometer.
And adding a cross-linking agent for the fracturing fluid and ammonium persulfate during gel breaking test or field construction.
Example 6 crosslinkable, high temperature resistant, residue free multicomponent copolymer fracturing fluids suitable for 90 ℃ formation fracturing
Base liquid portion: 0.45% of fracturing fluid thickening agent and the balance of water;
the weight percentage of the added part in the base fluid in the rheological test is as follows: 0.35 percent of cross-linking agent for fracturing fluid;
the weight percentage of the added part in the base fluid during the site construction is as follows: 0.35 percent of cross-linking agent for fracturing fluid and 0.03 percent of ammonium persulfate.
Laboratory preparation of base solutions: the fracturing fluid base fluid is prepared according to a laboratory preparation method of the base fluid.
And (3) rheological testing: and (3) adding a crosslinking agent for the fracturing fluid into the base fluid according to a proportion, and testing the temperature resistance and the shearing resistance of the fracturing fluid by using a Haake RS6000 rheometer.
And adding a cross-linking agent for the fracturing fluid and ammonium persulfate during gel breaking test or field construction.
Example 7 crosslinkable, high temperature resistant, residue free multicomponent copolymer fracturing fluids suitable for 120 ℃ formation fracturing
Base liquid portion: 0.5% of fracturing fluid thickening agent and the balance of water;
the weight percentage of the added part in the base fluid in the rheological test is as follows: 0.4 percent of cross-linking agent for fracturing fluid;
the weight percentage of the added part in the base fluid during the site construction is as follows: 0.4% of a crosslinking agent for the fracturing fluid, and a gel breaker for the fracturing fluid: 0.04 percent.
Laboratory preparation of base solutions: the fracturing fluid base fluid is prepared according to a laboratory preparation method of the base fluid.
And (3) rheological testing: and (3) adding a crosslinking agent for the fracturing fluid into the base fluid according to a proportion, and testing the temperature resistance and the shearing resistance of the fracturing fluid by using a Haake RS6000 rheometer.
And adding a crosslinking agent for the fracturing fluid and a gel breaker for the fracturing fluid during gel breaking test or site construction.
Example 8 crosslinkable, high temperature resistant, residue free multicomponent copolymer fracturing fluids suitable for 160 deg.C formation fracturing
Base liquid portion: 0.65% of fracturing fluid thickening agent and the balance of water;
the weight percentage of the added part in the base fluid in the rheological test is as follows: 0.6 percent of cross-linking agent for fracturing fluid;
the weight percentage of the added part in the base fluid during the site construction is as follows: 0.6% of cross-linking agent for fracturing fluid, and gel breaker for fracturing fluid: 0.02 percent.
Laboratory preparation of base solutions: the fracturing fluid base fluid is prepared according to a laboratory preparation method of the base fluid.
And (3) rheological testing: and (3) adding a crosslinking agent for the fracturing fluid into the base fluid according to a proportion, and testing the temperature resistance and the shearing resistance of the fracturing fluid by using a Haake RS6000 rheometer.
And adding a crosslinking agent for the fracturing fluid and a gel breaker for the fracturing fluid during gel breaking test or site construction.
Example 9
1. The performance evaluation of the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid thickening agent provided by the invention is as follows:
the invention provides a crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid thickening agent, the apparent viscosity of the solution of the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid thickening agent is increased along with the increase of the using concentration of the thickening agent, and a specific change curve is shown in figure 1. At room temperature, the thickening agent has an apparent viscosity of 90 mPas (170 s) at 0.50%-1) Thus, the thickening agent has strong thickening ability.
The cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid thickening agent provided by the invention does not contain a food source of bacteria in a solution system, and has a certain sterilization effect, so that the cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid thickening agent has good stability. And after the solution is placed at 25 ℃ for one week, the apparent viscosity of the solution is kept stable, no precipitation is generated, and the experimental result is shown in figure 2. The thickening agent solution is not corroded by bacteria, and is beneficial to industrial construction in field or field.
2. The invention provides a cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid, which has the following evaluation on the hanging performance:
according to the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid provided by the invention, after the action of the viscosity synergist of the fracturing fluid and the base fluid of the fracturing fluid, jelly with certain strength can be formed, and the fracturing fluid has certain suspension property, the experimental phenomenon is shown in figure 3, and experiments show that the strength of the fracturing fluid can be improved by crosslinking the multi-component copolymerization water-soluble polymer solution, so that the temperature resistance of the fracturing fluid is improved.
3. The temperature resistance and shear resistance of the crosslinkable high-temperature-resistant residue-free multicomponent copolymerization fracturing fluid provided by the invention are evaluated as follows:
(1) the fracturing fluid of example 5 was tested for temperature and shear resistance.
An experimental instrument: haake RS6000 rheometer, rotating cylinder test system, using rotor PZ 38;
and (3) testing conditions are as follows: temperature 60 ℃ and shear rate 170s-1And the testing time is 120 min.
(2) The fracturing fluid of example 6 was tested for temperature and shear resistance.
An experimental instrument: haake RS6000 rheometer, rotating cylinder test system, using rotor PZ 38;
and (3) testing conditions are as follows: temperature 90 ℃ and shear rate 170s-1And the testing time is 120 min.
(3) The fracturing fluid of example 7 was tested for temperature and shear resistance.
An experimental instrument: haake RS6000 rheometer, rotating cylinder test system, using rotor PZ 38;
and (3) testing conditions are as follows: temperature 120 ℃ and shear rate 170s-1And the testing time is 120 min.
(4) The fracturing fluid of example 8 was tested for temperature and shear resistance.
An experimental instrument: haake RS6000 rheometer, rotating cylinder test system, using rotor PZ 38;
and (3) testing conditions are as follows: temperature 160 ℃ and shear rate 170s-1And the testing time is 120 min.
Temperature-resistant and shear-resistant performance test of four groups of fracturing fluidsThe experimental results are shown in fig. 4, fig. 5, fig. 6 and fig. 7, respectively. At 60 deg.C, 90 deg.C, 120 deg.C, 160 deg.C, 170s-1And shearing for 120min, wherein the fracturing fluid has certain temperature sensitivity in the temperature rising process, the apparent viscosity is reduced along with the temperature rise, and after the fracturing fluid reaches a certain temperature, the crosslinking agent added into the fracturing fluid has a weak crosslinking effect with the base fluid, so that the apparent viscosity has a rising process and then is reduced. When the temperature is stable, the apparent viscosity of the fracturing fluid has no dependence on time, a structural dynamic balance exists in the system, and the apparent viscosity does not change along with the time but is kept in a relatively stable numerical range.
The results show that: the cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid provided by the invention has excellent temperature resistance and shearing resistance at 30-160 ℃, is stable in structure, and can meet the requirement of long-time fracturing construction wells in a temperature range through formula adjustment.
4. The invention provides a crosslinkable high-temperature-resistant residue-free multicomponent copolymer fracturing fluid, which has the following viscoelasticity test:
the fracturing fluid of example 6 was sheared at 160 ℃ for 120min and then subjected to viscoelasticity testing, i.e., fixed frequency and fixed stress sweep (Osc Time Curve).
Testing an instrument: haake RS6000 rheometer, rotating cylinder test system, using rotor PZ 38;
and (3) testing conditions are as follows: the shear stress τ was set to 0.5Pa and the frequency f was set to 6.18 HZ.
The viscoelastic performance test result of the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid is shown in figure 8. The experimental results show that: in the whole experiment process, the storage modulus G ' of the fracturing fluid provided by the invention is kept at a stable value, G ' is approximately equal to G and is far greater than the energy consumption modulus G ', the elasticity is obviously greater than the viscosity, and the elastic behavior is obvious, so that the suspension and sand carrying capacity of the fracturing fluid can completely meet the construction requirement.
5. The shear thinning test of the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid provided by the invention is as follows:
the fracturing fluid of example 6 was subjected to shear thinning test and the n, K values of the fracturing fluid were calculated.
Testing an instrument: haake RS6000 rheometer, cone plate test system, using rotor C60/1 degree Ti;
and (3) testing conditions are as follows: room temperature, shear rate 0s-1～1000s-1～0s-1。
The test results are shown in fig. 9, and the parameters of the fracturing fluid calculated by the software are as follows: k is 1.596, n is 0.4925, the consistency coefficient k of the fracturing fluid system is larger, the flow index n is smaller, namely the fluid has strong viscosity increasing property and good shearing diluting property.
Experimental results show that the apparent viscosity of the crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid provided by the invention is reduced along with the increase of the shearing speed, but the viscosity of the fracturing fluid can be recovered after the shearing is stopped, so that the fluid flow resistance can be greatly reduced on the premise of ensuring good sand carrying performance, the low-friction resistance characteristic can be reflected, and the fracturing of a high-temperature deep well is facilitated.
6. The invention provides a cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid, which comprises the following components in percentage by weight:
in order to improve the flowback of the fracturing fluid and reduce the damage to a reservoir, the fracturing fluid is required to realize rapid and thorough gel breaking when the construction is finished, and the gel breaking time of the fracturing fluid is required to be matched with the fracture closing time. For this reason, several formulations in the examples were used to prepare fracturing fluids and gel breaking tests were performed, and the test results of several groups of fracturing fluids are shown in table 1.
Table 1 example gel breaking test results
The experimental results show that: under the condition of stratum temperature, the gel breaker is added according to the formula proportion, the fracturing fluid can be completely broken within 5 hours, the gel breaking performance is good, and the viscosity of the gel breaker liquid is low; the solution after gel breaking is transparent liquid, the content of residues in the fracturing fluid is measured according to a water-based fracturing fluid performance evaluation method SYT5107-2005, and the residues can not be measured; the surface tension of the gel breaking solution was measured to be low (27mN/m or less). Therefore, the glue breaking liquid is more favorable for returning and the damage of the glue liquid to the stratum is reduced.
7. The invention provides a cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid which is used for testing the damage of the diversion capability of a supporting crack as follows:
the testing device comprises: API diversion trench, electronic balance, magnetic stirrer, graduated cylinder and other instruments;
the test method comprises the following steps: installing an API diversion trench, selecting 20/40-mesh ceramsite proppant, and setting the sand laying concentration to be 20kg/m generally2The tested fluid is put in a special conical flask, enters an API diversion trench under the action of specified liquid column differential pressure (△ H is 1m), the liquid passing through the diversion trench enters a beaker, is measured by a balance, and the mass and the corresponding time are recorded by a computer every 0.5min, so that the flowing conditions of the fracturing fluid system gel breaking liquid, the conventional HPG fracturing fluid gel breaking liquid and the experimental flowing medium 2% KCl (or standard saline) are respectively tested.
Data processing: and (3) plotting the accumulated volume against time to obtain a curve, averaging the volumes in each time period to obtain the average flow Q in the time period, wherein the ratio Ki/KKcl of the permeability of the supporting crack after the gel breaking liquid and the 2% KCl solution flow through the diversion trench is Qi/QKcl, and plotting the accumulated volume with the Qi/QKcl to obtain the damage condition of the gel breaking liquid of the BCG fracturing liquid and the HPG fracturing liquid to the flow conductivity of the supporting crack, which is shown in figure 10.
The conductivity damage test shows that the conductivity retention rate of the BCG fracturing fluid gel breaking liquid flowing through the supporting filling layer is over 90 percent, which shows that the system has very little damage to the supporting filling layer. And the conductivity retention rate after the boron crosslinked HPG fracturing fluid is treated is very low.
Example 10
A horizontal well of a Qinghai oilfield is positioned in the southern winged mountain area of the mountain of the vast cliff town in Haizhou, Qinghai province, and the horizontal section is as follows: 1784.47-2085.00 m, the length of the fracturing layer is 295.53m, the pressure of the middle part of the oil layer is 28.056Mpa, and the temperature of the middle part is as follows: 84.37 ℃, the well is a large-scale construction wellThe method adopts hydraulic jet fracturing construction, seven layers are fractured in total, in order to reduce the damage of fracturing modification to a reservoir layer, the well uses crosslinkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid (the formula of the fracturing fluid in example 6), low-density high-strength ceramsite is added as a fracturing propping agent, and the total fluid volume is designed to be 2700m3Design sand addition amount of 180m3. The construction condition of the fourth layer is as follows: perforating stage, low replacement liquid 14.04m3Blasting liquid 31.41m3Adding sand 2.00m310.72m of displacing liquid3(ii) a The fracturing stage has construction highest pressure of 60.80MPa, fracture pressure of 28.00MPa and maximum discharge capacity of 2.95m3Min, pad fluid 44.90m3Slug adding sand 2.00m375.79m of sand-carrying liquid3Adding 16.90m of sand3The average sand ratio is 22.29%, and the construction curve is shown in FIG. 11. Closing the well for 4 hours after fracturing is finished, discharging an oil nozzle with the diameter of 8mm, breaking the gel of the flowback liquid completely, and discharging liquid of more than 800m after 5 days3The average oil production is 10.2 tons per day after the production, and the oil production period is long.
On-site application proves that the cross-linkable high-temperature-resistant residue-free multi-component copolymerization type fracturing fluid provided by the invention has good high-temperature resistance, and also has good yield-increasing effect in a stratum with poor geological condition, and the residue-free low-damage characteristic of the fracturing fluid is reflected.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (2)
1. A preparation method of a cross-linkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid is characterized by comprising the following steps:
(1) preparation of fracturing fluid densifier
Adding acrylic acid, acrylamide, a cationic unsaturated monomer, an anionic unsaturated monomer and water into a reaction kettle, uniformly mixing, adding caustic soda flakes to adjust the pH value of a system to 8-9, adding an emulsifier sodium dodecyl benzene sulfonate, adding a redox initiator ammonium persulfate-sodium bisulfite, reacting at the reaction temperature of 40-45 ℃ for 4-6 h, hydrolyzing at the temperature of 90 ℃ for 5h to obtain a colloidal product, and granulating, drying and crushing the colloid to obtain a fracturing fluid thickening agent; the cationic unsaturated monomer is n-alkyl dimethyl diallyl ammonium chloride, wherein n is 12, 14, 16 or 18; the anionic unsaturated monomer is 2-acrylamide-2-methylpropanesulfonic acid or methacrylic acid sodium salt; according to the mass percentage, the acrylic acid is 2-5%, the acrylamide is 35-45%, the cation unsaturated monomer is 8-10%, the anion unsaturated monomer is 1-3%, the initiator ammonium persulfate-sodium bisulfite is 0.1-0.5%, wherein the mass ratio of the ammonium persulfate to the sodium bisulfite is 3:1, the flake caustic soda is 5-8%, the emulsifier sodium dodecyl benzene sulfonate is 3%, and the balance is water;
(2) preparation of cross-linking agent for fracturing fluid
Adding dimethylbenzene serving as a solvent into a reaction kettle, adding dodecyl dimethyl tertiary amine, n-octadecyl alcohol and dimethyl sulfate serving as reactants, adding sodium carbonate to adjust the pH value to 7-8, adding azodiisobutyronitrile serving as a catalyst, carrying out a alkylation reaction for 4-5 hours at the temperature of 45-55 ℃, and after the reaction is finished, cooling and filtering to obtain a crosslinking agent solid product for fracturing fluid; dissolving a crosslinking agent solid product for the fracturing fluid in water to prepare a solution with the mass fraction of 25%, and stirring and mixing uniformly after completely dissolving to obtain the crosslinking agent for the fracturing fluid; according to the mass percentage, 16 to 18 percent of dodecyl dimethyl tertiary amine, 22 to 27 percent of n-octadecanol, 15 to 20 percent of dimethyl sulfate, 1.5 to 3 percent of sodium carbonate, 1 to 3 percent of azobisisobutyronitrile and the balance of solvent xylene;
(3) preparation of gel breaker for fracturing fluid
Adding polyimide and ethyl acetate serving as composite capsule coat materials into a reaction kettle, stirring and dissolving, adding potassium persulfate, introducing nitrogen and stirring, controlling the temperature of the solution to be 80 ℃, reacting for 30min, adding span 85 and tween 60 serving as emulsifiers and polyethylene glycol 600 serving as a thickening agent, adding water, keeping the reaction temperature at 80 ℃, continuing to react for 60min, stopping the reaction, spraying and granulating reactants through a spray drying device, and drying at 70 ℃ until constant weight is achieved to obtain the gel breaker for the fracturing fluid; calculated by mass percent, the polyimide accounts for 35 percent, the ethyl acetate accounts for 14 percent, the potassium persulfate accounts for 25 percent, and the emulsifier accounts for 8 percent, wherein the mass ratio of span 85 to Tween 60 is 1:1, the thickening agent polyethylene glycol 600 accounts for 2 percent, and the balance is water;
(4) crosslinkable high-temperature-resistant residue-free multi-component copolymerization fracturing fluid
The fracturing fluid base fluid comprises the following components in percentage by weight: 0.3 to 0.65 percent of fracturing fluid thickening agent and the balance of water;
the additives during construction comprise a cross-linking agent for fracturing fluid, a gel breaker for fracturing fluid or ammonium persulfate; when the ground temperature is 90-160 ℃, the components of the additive account for the base fluid in percentage by weight during construction: 0.2 to 0.6 percent of cross-linking agent for fracturing fluid and 0.02 to 0.05 percent of gel breaker for fracturing fluid; when the ground layer temperature is 30-90 ℃, the components of the additive account for the base fluid in percentage by weight during construction: 0.2 to 0.6 percent of cross-linking agent for fracturing fluid and 0.05 to 0.08 percent of ammonium persulfate.
2. The crosslinkable high-temperature residue-free multicomponent copolymer type fracturing fluid prepared by the preparation method of claim 1.
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| WO2017096055A1 (en) * | 2015-12-02 | 2017-06-08 | Saudi Arabian Oil Company | High temperature crosslinked fracturing fluids |
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| CN108192588B (en) * | 2018-01-24 | 2020-08-18 | 西南石油大学 | Self-repairing low-damage ultrahigh-temperature-resistant fracturing fluid |
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| CN109054799A (en) * | 2018-07-25 | 2018-12-21 | 中国石油集团川庆钻探工程有限公司 | Environment-friendly multipurpose thickening agent for shale gas reservoir volume reconstruction and preparation method thereof |
| CN109536154A (en) * | 2018-12-13 | 2019-03-29 | 新疆科力新技术发展股份有限公司 | Realize that oil field fracturing returns the pressure break thickener and preparation method thereof of drain recycling |
| CN109652053B (en) * | 2019-01-22 | 2021-09-21 | 西南石油大学 | High-temperature-resistant full-suspension low-damage fracturing fluid and preparation method thereof |
| CN110358519A (en) * | 2019-06-12 | 2019-10-22 | 欧志飞 | A kind of preparation method of low residue salt tolerant fracturing fluid |
| CN113583653A (en) * | 2020-04-30 | 2021-11-02 | 爱森（中国）絮凝剂有限公司 | Novel aqueous fracturing fluid composition and fracturing method using the same |
| CN111892921B (en) * | 2020-07-31 | 2022-04-22 | 东营东方化学工业有限公司 | Viscoelastic surfactant type sand-carrying fluid and processing technology thereof |
| CN115677904A (en) * | 2021-07-29 | 2023-02-03 | 中国石油天然气股份有限公司 | Water shutoff agent and preparation method and application thereof |
| CN116751336B (en) * | 2023-08-15 | 2023-10-13 | 东营市百扬石油科技有限责任公司 | Preparation method of temperature-resistant emulsion type fracturing fluid thickener |
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