CN111534293A - Temperature-responsive self-lubricating hydrogel profile control agent and preparation method thereof - Google Patents
Temperature-responsive self-lubricating hydrogel profile control agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a temperature-responsive self-lubricating hydrogel profile control agent and a preparation method thereof, wherein a hydrophilic polymer matrix is subjected to amide-hydroxyl dehydration condensation chemical crosslinking reaction under the action of a crosslinking agent A to generate a high-strength temperature-resistant polymer network in a water environment by a one-pot method, and simultaneously, a furfuryl amine-bisphenol A diglycidyl ether oligomer is subjected to Diels-Alder chemical crosslinking reaction under the action of a crosslinking agent B to generate a dynamic covalent network, and the two networks are compounded to generate the temperature-responsive self-lubricating hydrogel profile control agent. The profile control agent has good temperature resistance and self-lubricating performance, so that the problems of poor deep profile control effect, water flooding and low efficiency caused by high frictional resistance of the gel profile control agent in a high-temperature oil reservoir are solved.
Description
Technical Field
The invention belongs to the field of oil exploitation, and relates to a temperature-responsive self-lubricating hydrogel profile control agent, and a preparation method and application thereof.
Background
Reservoir heterogeneity is one of the main reasons that limit its water drive efficiency. Along with the extension of water drive time, crude oil in shallow stratum is gradually displaced out, and the stratum permeability obviously improves, forms high permeable formation, leads to the poor apart from grow of permeability between the different degree of depth ground, and follow-up rivers often pass high permeable formation and form the cross flow, have seriously restricted crude oil recovery and have promoted the effect. To solve this problem, researchers have developed a variety of materials to plug high permeability layers, of which gel is the most economical and efficient. The gel profile control agent commonly used at present is high-molecular hydrogel, such as polyacrylamide gel, guar gum, xanthan gum and the like, has high strength, good plugging performance on stratum large pore canals, and has strong shear resistance, acid and alkali resistance and salt resistance. However, as the depth of the formation increases, the temperature of the formation gradually rises, and the deep oil reservoir rich in oil has high temperature and strong heterogeneity, so that profile control needs to be performed by adopting temperature-resistant gel. The common high-molecular hydrogel has poor temperature resistance, partial chemical crosslinking of the hydrogel can be damaged at high temperature, and the supermolecule function among high-molecular chains is greatly weakened, so that the water-locking and water-retaining capacity, the overall strength and the plugging performance of the gel are obviously reduced. Therefore, in order to effectively improve the temperature resistance of the hydrogel, researchers develop efficient chemical cross-linking agents (such as modified phenolic resin and the like), construct double-network hydrogel (such as polyacrylamide-polyacrylic acid double-network hydrogel and the like), add reinforcing agents with strong temperature resistance (such as modified silicon dioxide nano-particles and the like) and the like to increase the cross-linking density of a polymer network or the content of temperature-resistant reinforcing particles in the polymer network, so that the temperature resistance of the gel is effectively improved.
However, because the width of the pore canal at the deep part of the stratum is small, the friction force between the temperature-resistant hydrogel and the rock wall is large, and the application of the temperature-resistant hydrogel in the profile control of the deep part of the oil reservoir has certain defects. The method specifically comprises the following steps: 1) the high frictional resistance results in poor longitudinal profile control between temperature resistant gel layers. With the water drive, part of crude oil in the medium and low permeability oil layers is displaced by water flow to generate a high permeability middle layer. Due to higher frictional resistance between the gel and the rock wall, the gel has poorer migration performance in the stratum, and is difficult to enter a low-permeability layer from a high-permeability layer for plugging, so that subsequent water flows form channeling through a high-permeability middle layer, and the oil extraction efficiency is reduced. 2) High frictional resistance results in poor lateral migration capabilities within the gel layer. High, medium and low permeability zones which are transversely and randomly distributed still exist in the stratum of the same depth of the high-temperature oil reservoir, and the porosity, permeability, pore diameter and the like of different transverse areas have larger differences. The higher frictional resistance causes the gel to collect mainly in the large channels and to be difficult to enter the medium, micro and slits. This results in a large number of channels not being plugged by gel, and lower water flooding efficiency and crude oil recovery enhancement.
Disclosure of Invention
The invention aims to provide a preparation method of a temperature-responsive self-lubricating hydrogel profile control agent, which can enable the gel profile control agent to have better temperature resistance and self-lubricating property simultaneously, thereby solving the problems of poor deep profile control effect, water flooding and low efficiency caused by high frictional resistance of the gel profile control agent in a high-temperature oil reservoir.
According to the invention, a double-network double-crosslinking hydrogel PAM-FA-BGPP (PAFB) is constructed by introducing a dynamic covalent bond crosslinked polymer network into a temperature-resistant hydrogel network, so that the gel has a self-lubricating characteristic of temperature response, the frictional resistance of the gel in deep migration of a stratum is effectively reduced, and the deep profile control performance of the gel is improved.
In order to achieve the purpose of the invention, the technical scheme of the invention is as follows:
a temperature-responsive self-lubricating hydrogel profile control agent and a preparation method thereof are disclosed, wherein the method comprises the following steps: through a one-pot method, in a water environment, a hydrophilic polymer matrix is subjected to amide-hydroxyl dehydration condensation chemical crosslinking reaction under the action of a crosslinking agent A to generate a high-strength temperature-resistant polymer network, meanwhile, a furfuryl amine-bisphenol A diglycidyl ether oligomer is subjected to Diels-Alder chemical crosslinking reaction under the action of a crosslinking agent B to generate a dynamic covalent network, and the two networks are compounded to generate the temperature-response self-lubricating hydrogel profile control agent.
The method comprises the following specific steps:
(1) adding a hydrophilic polymer matrix, a furfuryl amine-bisphenol A diglycidyl ether oligomer, a crosslinking agent A and a crosslinking agent B into water at 60-80 ℃, and stirring to dissolve the hydrophilic polymer matrix, the furfuryl amine-bisphenol A diglycidyl ether oligomer, the crosslinking agent A and the crosslinking agent B to obtain a reaction solution;
(2) and continuously stirring the reaction solution until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing for 24-72 hours at 60-80 ℃ to obtain the temperature response self-lubricating hydrogel profile control agent.
Preferably, the hydrophilic polymer matrix includes any one of polyacrylamide, polyacrylic acid, polyethylene oxide, polyvinyl pyrrolidone and polyethylene glycol, and polyacrylamide is preferred.
Preferably, the crosslinking agent A comprises hexamethylenetetramine-hydroquinone, N' -methylenebisacrylamide, phenolic resin and Cr3+、Fe3+And N, N' -methylenebisacrylamide, preferably hexamethylenetetramine-hydroquinone.
Preferably, the crosslinking agent B is a maleimide crosslinking agent, preferably N, N '- (4, 4' -methylenediphenyl) bismaleimide.
Preferably, the mass ratio of the hydrophilic polymer matrix to the furfuryl amine-bisphenol A diglycidyl ether oligomer to the crosslinking agent A to the crosslinking agent B is 3-7: 5-9: 1-5: 0.1-0.5.
Preferably, the stirring speed is 300-600 rpm, and the stirring time is 0.5-1 h.
A method for producing oil from a temperature-responsive self-lubricating hydrogel profile control agent, the method comprising:
(1) adding the self-lubricating hydrogel profile control agent and distilled water into a colloid mill according to the mass ratio of 1-3: 1, grinding gel at the rotating speed of 7000-12000 rpm for 20-60 min, and drying to obtain micron-grade temperature response self-lubricating hydrogel profile control agent particles;
(2) adding 5-10 wt% of temperature response self-lubricating hydrogel profile control agent particles into formation water, injecting the obtained mixed solution into a high-temperature (90-120 ℃) oil reservoir, transporting the self-lubricating hydrogel profile control agent particles to a high-permeability area by utilizing water flow, standing for 3-6 hours, and enabling the self-lubricating hydrogel profile control agent particles to absorb water and expand and block the high-permeability area.
According to the oil recovery method, the temperature response self-lubricating hydrogel profile control agent is particularly suitable for a non-homogeneous oil reservoir stratum at the temperature of 90-120 ℃.
According to the oil extraction method, the temperature response self-lubricating hydrogel profile control agent can be used as a channeling sealing, water plugging, profile control and deep profile control and displacement diverting agent in a heterogeneous oil reservoir at the temperature of 90-120 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the temperature response self-lubricating hydrogel profile control agent prepared by the invention has good self-lubricating performance at high temperature (90-120 ℃), and can secrete lubricating liquid on the surface of the profile control agent under the action of external force, so that the friction force between the gel and the formation rock wall is effectively reduced, and the migration capability of the gel in the formation is improved.
2. The temperature response self-lubricating hydrogel profile control agent prepared by the invention has stronger temperature resistance, can keep higher strength at high temperature, has stronger shear resistance and tear resistance, and can better adapt to the high-shear environment of the stratum.
3. The temperature response self-lubricating hydrogel profile control agent prepared by the invention has a larger plugging range, higher plugging strength and excellent oil recovery capability, and can effectively improve the water flooding efficiency.
4. The temperature response self-lubricating hydrogel profile control agent prepared by the invention has no pollution to the environment, the raw materials are easy to obtain, and the preparation method is simple and is suitable for large-scale popularization and production.
Drawings
FIG. 1 is the NMR spectrum of the mixed solution of temperature-responsive self-lubricating hydrogel profile control agent PAFB and its reactants in example 1: (1H-NMR) chart.
FIG. 2 is the NMR spectrum of the mixture of temperature-responsive self-lubricating hydrogel profile control agent PAFB and its reactants in example 1: (13C-NMR).
FIG. 3 is a graph of the infrared spectra (FTIR) of the temperature responsive self-lubricating hydrogel profile control agent PAFB of example 1, the temperature resistant PAM gel and the FA-BGPP gel of comparative example 1.
FIG. 4 is a bar graph of the friction coefficients of temperature-responsive self-lubricating hydrogel profile control agent PAFB in example 1 and temperature-resistant PAM gel in comparative example 1 at room temperature.
FIG. 5 is the Diels-Alder reaction equation that occurs between FA-BGPP oligomer and BM in example 1.
FIG. 6 is a bar graph of the strength (G') of the temperature-responsive self-lubricating hydrogel profile control agent PAFB of example 1 and the temperature-resistant PAM gel of comparative example 1 at room temperature.
FIG. 7 is a bar graph of loss factor (tan) at room temperature for the temperature responsive self-lubricating hydrogel profile control agent PAFB of example 1 and the temperature resistant PAM gel of comparative example 1.
FIG. 8 is a plot of the amplitude sweep of the rheology test of the temperature responsive self-lubricating hydrogel profile control agent PAFB of example 1 at room temperature.
Fig. 9 is an amplitude scan curve of rheology test at room temperature for temperature resistant PAM gels in comparative example 1.
FIG. 10 is a low field nuclear magnetic resonance (LF-NMR) spectrum of temperature-responsive self-lubricating hydrogel profile control agent PAFB from example 1.
FIG. 11 is a low field nuclear magnetic resonance (LF-NMR) spectrum of the temperature resistant PAM gel of comparative example 1.
FIG. 12 is a graph of the overall transverse relaxation times (T.sub.L) in low field nuclear magnetic analysis of the temperature-responsive self-lubricating hydrogel profile control agent PAFB of example 1 and the temperature-resistant PAM gel of comparative example 12,avg) And a histogram of the percentage of peak area of polymer-water nmr.
FIG. 13 is a surface coefficient of friction versus temperature curve for the temperature responsive self-lubricating hydrogel profile control agent PAFB of example 1 and the temperature resistant PAM gel of comparative example 1.
FIG. 14 is a representation (photograph) of the thermoreversibility of FA-BGPP gel.
FIG. 15 is a graph of strength (G') -temperature of the temperature-responsive self-lubricating hydrogel profile control agent PAFB of example 1 and the temperature-resistant PAM gel of control 1.
FIG. 16 is a Differential Scanning Calorimetry (DSC) chart of a mixture of FA-BGPP oligomer and BM.
FIG. 17 is a Differential Scanning Calorimetry (DSC) plot of the temperature responsive self-lubricating hydrogel profile control agent PAFB of example 1 and the temperature resistant PAM gel of control 1.
FIG. 18 is a displacement differential pressure, high/low permeability sand pack pipe flow rate and crude oil recovery-injection volume curve of temperature-responsive self-lubricating hydrogel profile control agent PAFB in example 1 and temperature-resistant PAM gel profile control at 120 ℃ in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail below with reference to examples.
Aiming at the problems in the prior art, the invention constructs the double-network double-crosslinking hydrogel PAM-FA-BGPP (PAFB) by introducing a dynamic covalent bond crosslinked polymer network into a temperature-resistant hydrogel network, so that the gel has the self-lubricating characteristic of temperature response, thereby effectively reducing the frictional resistance of the gel in deep migration of a stratum and improving the deep profile control performance of the gel. Specifically, the reversible covalent cross-linking network FA-BGPP-BM based on the Diels-Alder reaction can be broken and degraded into polymer water-based lubricating liquid with moderate viscosity under the action of high temperature (90-120 ℃), and the polymer water-based lubricating liquid is secreted to the surface of gel under the external force extrusion, so that a self-lubricating layer with an ultralow friction coefficient is formed between the gel and a rock wall, and the self-lubricating property of gel temperature response is endowed. And the temperature-resistant PAM network chemically crosslinked (amide-hydroxyl dehydration condensation reaction) by the high-efficiency crosslinking agent (HMTA-HQ) forms a protective support of the FA-BGPP network, so that the gel still has high strength at high temperature (90-120 ℃). Compared with the traditional temperature-resistant hydrogel, the PAFB applied to the deep profile control of the oil reservoir has the following advantages: 1) the PAFB gel is easy to transfer longitudinally to realize deep profile control. In the process of migrating towards the deep part of the stratum, the PAFB gel can secrete more lubricating liquid along with the temperature rise, has better longitudinal migration capability in the stratum and is easy to enter a low-permeability layer to realize profile control. 2) The PAFB gel can effectively improve the transverse water flooding and efficiency of the low-permeability layer. Due to the existence of the double-network structure and the dynamic covalent bond, the PAFB gel has good self-lubricating performance and high mechanical strength in a low-permeability layer at high temperature (90-120 ℃), and can block more middle and micro channels under the pushing of water flow, so that the water flooding efficiency is improved.
The synthetic route of the temperature response self-lubricating hydrogel profile control agent is as follows:
some of the raw materials referred to in the following examples were self-made, in which,
FA-BGPP was synthesized by reacting furfurylamine (FA, Shanghai Michellin Biochemical Co., Ltd.) and bisphenol A diglycidyl ether (BGPP, Shanghai Michellin Biochemical Co., Ltd.) in a molar ratio of 1:1 in N', N-dimethylformamide (DMF, Shanghai Michellin Biochemical Co., Ltd.) at 120 ℃ for 12 h.
HMTA-HQ is synthesized by reacting hexamethylene tetramine (HMTA, Shanghai Michelin Biochemical technology Co., Ltd.) and hydroquinone (HQ, Shanghai Michelin Biochemical technology Co., Ltd.) in a mass ratio of 1:1 in deionized water at 70 ℃ for 3h, and is prepared for use.
Example 1:
the preparation experiment steps of the temperature response self-lubricating hydrogel profile control agent are as follows:
(1) at 70 ℃. + -. 10 ℃, 0.3g of polyacrylamide (PAM, Shanghai Michelin Biochemical technology Co., Ltd.), 0.5g of furfurylamine-bisphenol A diglycidyl ether oligomer (FA-BGPP, by itself), 0.1g of hexamethylenetetramine-hydroquinone crosslinking agent (HMTA-HQ, by itself), and 0.01g N, N '- (4, 4' -methylenediphenyl) bismaleimide (BM, Shanghai Michelin Biochemical technology Co., Ltd.) were added to 100mL of water and stirred to be dissolved, thereby obtaining a reaction solution.
(2) Continuously stirring the reaction solution at the stirring speed of 500rpm until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing in an oven at 70 +/-10 ℃ for 48 hours to obtain the temperature response self-lubricating hydrogel profile control agent PAFB-1.
Example 2:
the preparation experiment steps of the temperature response self-lubricating hydrogel profile control agent are as follows:
(1) at 70 ℃. + -. 10 ℃, 0.5g of polyacrylamide (PAM, Shanghai Michelin Biochemical technology Co., Ltd.), 0.7g of furfurylamine-bisphenol A diglycidyl ether oligomer (FA-BGPP, by itself), 0.3g of hexamethylenetetramine-hydroquinone (HMTA-HQ, by itself), and 0.03g N, N '- (4, 4' -methylenediphenyl) bismaleimide (BM, Shanghai Michelin Biochemical technology Co., Ltd.) were added to 100mL of water and stirred to be dissolved, thereby obtaining a reaction solution.
(2) Continuously stirring the reaction solution at the stirring speed of 500rpm until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing in an oven at 70 +/-10 ℃ for 48 hours to obtain the temperature response self-lubricating hydrogel profile control agent PAFB-2.
Example 3:
the preparation experiment steps of the temperature response self-lubricating hydrogel profile control agent are as follows:
(1) at 70 ℃. + -. 10 ℃, 0.7g of polyacrylamide (PAM, Shanghai Michelin Biochemical technology Co., Ltd.), 0.9g of furfurylamine-bisphenol A diglycidyl ether oligomer (FA-BGPP, by itself), 0.5g of hexamethylenetetramine-hydroquinone (HMTA-HQ, by itself), and 0.05g N, N '- (4, 4' -methylenediphenyl) bismaleimide (BM, Shanghai Michelin Biochemical technology Co., Ltd.) were added to 100mL of water and stirred to be dissolved, thereby obtaining a reaction solution.
(2) Continuously stirring the reaction solution at the stirring speed of 500rpm until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing in an oven at 70 +/-10 ℃ for 48 hours to obtain the temperature response self-lubricating hydrogel profile control agent PAFB-3.
Comparative example 1:
the preparation experiment steps of the reference temperature-resistant PAM gel are as follows:
(1) 0.7g of polyacrylamide (PAM, Shanghai Michelin Biochemical Co., Ltd.), 0.5g of hexamethylenetetramine-hydroquinone (HMTA-HQ, manufactured by Kogyo Co., Ltd.) and 0.05g N, N '- (4, 4' -methylenediphenyl) bismaleimide (BM, Shanghai Michelin Biochemical Co., Ltd.) were added to 100mL of water at 70. + -. 10 ℃ and stirred to be dissolved, thereby obtaining a reaction solution.
(2) And continuously stirring the reaction solution at the stirring speed of 500rpm until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing in an oven at 70 +/-10 ℃ for 48 hours to obtain the temperature-resistant PAM gel 1.
Comparative example 2:
the preparation experiment steps of the reference temperature-resistant PAM gel are as follows:
(1) at 70 ℃. + -. 10 ℃, 0.7g of polyacrylamide (PAM, available from Mecanum Biochemical Co., Ltd., Shanghai) and 0.5g of hexamethylenetetramine-hydroquinone (HMTA-HQ, available from Korea) were added to 100mL of water and stirred to be dissolved, thereby obtaining a reaction solution.
(2) And continuously stirring the reaction solution at the stirring speed of 500rpm until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing in an oven at 70 +/-10 ℃ for 48 hours to obtain the temperature-resistant PAM gel 2.
Characterization and its use
Nuclear magnetic resonance hydrogen spectrum of temperature response self-lubricating hydrogel profile control agent PAFB-1: (1H-NMR), see FIG. 1.
As shown in FIG. 1, after one-pot reaction (one-pot method), the proton peaks (7.6ppm and 6.3ppm) of the furan group in the reactant are completely replaced by the corresponding proton peaks (6.7ppm, 6.6ppm and 5.1ppm) of the Diels-Alder reaction product, which indicates that the Diels-Alder reaction between furfuryl amine-bisphenol A diglycidyl ether oligomer (FA-BGPP) and N, N '- (4, 4' -methylenediphenyl) Bismaleimide (BM) in the PAM network protective scaffold is completely performed, the PAM network does not influence the Diels-Alder reaction, and the PAFB gel is successfully synthesized by the one-pot method.
Nuclear magnetic resonance carbon spectrum of temperature response self-lubricating hydrogel profile control agent PAFB-1 (13C-NMR), see FIG. 2.
As shown in FIG. 2, after one-step reaction, the furan group carbon nuclear resonance peaks (151ppm, 143ppm, 112ppm and 111ppm) in the reactant are completely replaced by the corresponding carbon nuclear resonance peaks (140ppm, 92ppm and 81ppm) of the Diels-Alder reaction product, which indicates that FA-BGPP-BM dynamic covalent network has been successfully introduced into the temperature-resistant PAM gel, and the PAFB gel is successfully synthesized by a one-pot method.
Infrared Spectroscopy (FTIR) analysis of temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 is shown in FIG. 3.
As shown in FIG. 3, the infrared spectrogram of the gel shows that the PAFB gel has a C ═ O stretching vibration peak (PAFB: 1668 cm) belonging to the amide group of the temperature-resistant PAM gel-1(ii) a Temperature resistant PAM gels: 1672cm-1) And the N-H in-plane bending vibration peak (PAFB: 1616cm-1(ii) a Temperature resistant PAM gels: 1610cm-1) And also contains a benzene ring proton stretching vibration peak belonging to FA-BGPP gel (PAFB: 3066cm-1；FA-BGPP：3043cm-1) Out-of-plane deformation vibration peak (PAFB: 850-684 cm-1；FA-BGPP：831cm-1～721cm-1) And characteristic peaks of Diels-Alder reaction product (PAFB: 1778cm-1；FA-BGPP：1774cm-1) The FA-BGPP-BM dynamic covalent network is successfully introduced into the temperature-resistant PAM gel, and the synthesized PAFB gel conforms to the design.
The self-lubricating properties of the PAFB gel at room temperature were determined by measuring the surface friction coefficients of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1 and the temperature-resistant PAM gel 1 of comparative example 1 at room temperature (25 ℃) using a friction and abrasion tester. The results of the experiment are shown in FIG. 4.
When tested, Al2O3The ceramic ball (diameter 6mm) is acted on the gel surface under the action of load force to do linear reciprocating motion, and one reciprocating linear motion is a shearing cycle. One shear cycle has a length of 5mm, a ceramic ball motion frequency of 0.06Hz, and a corresponding shear rate of 0.3mm · s-1The load force was 70 mN. Since all the gel samples tended to stabilize their friction coefficients after undergoing 20 shears, the data from the 20 th shear was used as an index for evaluating the gel friction performance.
According to fig. 4, the introduction of FA-BGPP at room temperature does not effectively reduce the friction coefficient between the temperature-resistant PAM gel and the solid wall surface, because DA reaction tends to proceed forward at room temperature (fig. 5), and the dynamic covalent network is difficult to break, resulting in PAFB gel having no self-lubricating property at room temperature.
The mechanical properties of the gels were determined by measuring the strength (G'), loss factor (tan) gel-to-sol transition strain of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1 and the temperature-resistant PAM gel 1 of comparative example 1 at room temperature (25 ℃ C.) using a rotational rheometer. The experimental results are shown in FIGS. 6 to 9.
During testing, the gel is scanned in amplitude and time by adopting an oscillation mode, and parameters such as elastic modulus (G ', Pa), viscous modulus (G', Pa), gel-sol transition strain, loss factor (tan) and the like of the gel are measured. The strain corresponding to the gel G '-strain and the G' -strain curve intersection point is the gel-sol transformation strain. The testing temperature is 25 ℃, the strain range adopted by amplitude scanning is 0.01-400%, and the frequency is 1.0 Hz. The frequency selected for the time sweep was 1.0Hz, the amplitude was 0.5%, and the duration was 200 s.
According to the figures 6-9, the addition of FA-BGPP can make the temperature-resistant PAM gel network more compact and the gel strength significantly improved (figure 6). Meanwhile, according to fig. 7-9, compared with the temperature-resistant PAM gel, the PAFB gel has higher gel-sol transition strain and lower loss factor (tan), which indicates that the PAFB gel has stronger shear resistance and solidification-like property. That is, the PAFB gel is more elastically deformed under external stress, and the gel has stronger tear resistance.
LF-NMR analysis was performed on the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1 and the temperature-resistant PAM gel 1 in comparative example 1 using a nuclear magnetic resonance cross-linking densitometer, and the influence of the introduced FA-BGPP network on the cross-linking degree of the temperature-resistant PAM gel was analyzed accordingly. The experimental results are shown in FIGS. 10 to 12.
For the test, the maximum transverse relaxation time was 3000.000ms, and the number of scans was 8.
According to fig. 10-12, it was found that the formation of the double network increased the overall degree of crosslinking of the PAFB gel compared to the temperature resistant PAM gel. According to the low-field nuclear magnetic spectrum (figure 10-12), compared with the temperature-resistant PAM gel, the PAFB gel has lower T2,avgAnd higher polymer-water peak areaThe ratio indicates that FA-BGPP enhances the overall degree of cross-linking of the PAFB gel mainly by effectively enhancing the supramolecular interaction between the polymer and water molecules.
The surface friction coefficients of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1 and the temperature-resistant PAM gel 1 in the comparative example 1 at different temperatures were measured by a friction and wear tester, and the rule of the influence of the temperature on the self-lubricating property of the PAFB gel was analyzed accordingly. The results of the experiment are shown in FIG. 13.
When tested, Al2O3The ceramic ball (diameter 6mm) is acted on the gel surface under the action of load force to do linear reciprocating motion, and one reciprocating linear motion is a shearing cycle. One shear cycle has a length of 5mm, a ceramic ball motion frequency of 0.06Hz, and a corresponding shear rate of 0.3mm · s-1The load force was 70 mN. When the surface friction coefficient of the gel sample tends to be stable, the value is recorded and the gel friction performance is evaluated based on the value.
From fig. 13, it was found that the surface friction coefficient of the temperature-resistant PAM gel remained stable with increasing temperature. In contrast, above 80 ℃, the PAFB gel surface friction coefficient decreased significantly. The high temperature can ensure that the PAFB gel has better self-lubricating property, thereby greatly reducing the self surface friction coefficient and being beneficial to improving the deep profile control effect of the gel. This is because: 1) due to the thermal reversibility of the Diels-Alder reaction (figure 5), a dynamic covalent network (FA-BGPP network) in the PAFB gel can be decomposed at high temperature (90-120 ℃) and precipitated to the surface of the gel to form a lubricating layer (figure 14), so that the friction coefficient of the PAFB gel is remarkably reduced. According to FIG. 14, the FA-BGPP gel network can be rapidly decomposed at 100 ℃ to form sol and can be regenerated at 70 ℃, which shows that the thermally reversible Diels-Alder reaction between FA-BGPP and BM endows the PAFB gel with a better self-lubricating function at high temperature (90-120 ℃).
The strength of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1 and the temperature-resistant PAM gel 1 in the comparative example 1 at different temperatures was measured by using a rotational rheometer, and the rule of the influence of the temperature on the mechanical properties of the PAFB gel was analyzed. The results of the experiment are shown in FIG. 15.
In the test, the mechanical properties of the gel were analyzed by measuring the elastic modulus (G', Pa) of the gel by time-scanning the gel in an oscillation mode. The scanning frequency is 1.0Hz, the amplitude is 0.5%, the duration is 200s, and the testing temperature range is 30-140 ℃.
From fig. 15, it was found that the temperature-resistant PAM gel strength slightly decreased with increasing temperature. Compared with the PAB gel, the strength of the PAFB gel is greatly reduced but still higher than that of the temperature-resistant PAM gel at the temperature of more than 80 ℃. The PAM network in the PAFB gel ensures that the PAFB gel still has higher strength at high temperature (90-120 ℃).
The thermal behavior of the PAFB gel was explored by DSC analysis of the FA-BGPP & BM mixture, the temperature responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1, and the temperature resistant PAM gel 1 of control 1 using a differential scanning calorimeter. The results are shown in FIGS. 16 and 17.
For the test, 5mg of the sample was sealed in a 40. mu.L aluminum crucible and heated at a rate of 10 ℃ min-1The temperature is raised from 25 ℃ to 300 ℃.
According to the DSC curve (figure 16) of the FA-BGPP & BM mixture, an endothermic peak of the Diels-Alder reaction exists at 63 ℃ and an exothermic peak of the retro-Diels-Alder reaction exists at 106 ℃, which proves that the Diels-Alder reaction in the dynamic covalent network has better thermal reversibility. Meanwhile, in a PAFB gel DSC curve (figure 17), the exothermic peak of retro-Diels-Alder reaction is shifted to 112 ℃, which shows that the high crosslinking density caused by the PAFB gel double-network structure delays the progress of retro-Diels-Alder reaction to a certain extent, and is beneficial to prolonging the effective self-lubricating time of the gel at high temperature (90-120 ℃). On the other hand, comparing DSC curves of PAFB and temperature-resistant PAM gel (figure 17), finding that the endothermic peak of PAM-crosslinking agent (HMTA-HQ) chemical bond fracture is increased from 143 ℃ (temperature-resistant PAM gel DSC curve) to 178 ℃ (PAFB gel DSC curve), which shows that after full retro-Diels-Alder reaction, PAFB gel still has a certain double-network structure, and the double-network structure enhances PAM network temperature resistance, so that PAFB gel has higher strength at high temperature (90-120 ℃).
The profile control and plugging performances of the temperature response self-lubricating hydrogel profile control agents PAFB-1, PAFB-2 and PAFB-3 prepared in examples 1 to 3 and the temperature-resistant PAM gel 1 and the temperature-resistant PAM gel 2 in comparative examples 1 and 2 in high-temperature (120 ℃) and low-temperature (60 ℃) environments are measured by utilizing an indoor simulated oil recovery experiment (core displacement experiment), the influence of self-lubrication on the gel profile control effect is analyzed according to the profile control and plugging performances, and the experimental result is shown in FIG. 18 (example 1 and comparative example 1) and tables 1 and 2.
During testing, in order to effectively simulate the heterogeneity of an oil reservoir, a double-pipe parallel core displacement device is adopted, wherein the average permeability of the high-permeability core is 1.38 mu m2Average porosity of 21.37%, and low permeability core of 0.37 μm2The average porosity was 23.57%. The total pore volume of the core was 143.62mL on average, and the total oil saturation was 78.52% on average. The specific experimental procedures are as follows: 1) the artificial core was saturated. Respectively at a rate of 1 mL/min-1And 0.5 mL. min-1And injecting water and crude oil into the sand filling pipe in sequence at the speed until the pressure difference between the two sides of the sand filling pipe tends to be stable, so that the sand filling pipe is saturated by the water and the crude oil in sequence. And then placing the saturated sand filling pipe in a 60 ℃ or 120 ℃ oven for aging for 120h, weighing the sand filling pipe and calculating the crude oil saturation of the core. 2) And (5) water flooding. Stratum water is added at 1 mL/min-1The rate of (2) is injected into the sand-packed pipe, and the sand-packed pipe is displaced until the injection pressure is maintained stable and the water content of the produced liquid reaches 98 percent. 3) And (5) injecting gel. 0.5PV (PV: pore volume) gel at 0.5mL min-1Injecting the mixture into a sand filling pipe, and then placing the sand filling pipe in an oven at 60 ℃ or 120 ℃ for standing for 120 h. 4) And (5) performing subsequent water flooding. The formation water (1 mL. min.) is injected into the sand-filled pipe again-1) And respectively representing the plugging and oil production performance of the gel in the stratum by breakthrough pressure, plugging rate and crude oil recovery ratio until the water content of the produced liquid reaches 98%, wherein the calculation formula of the plugging rate (η) is shown as formula (1).
Wherein, KiPermeability before plugging, μm2；KfIn terms of post-plugging permeability, μm2。
TABLE 1120 deg.C indoor simulated oil recovery experimental results
Indoor simulation oil extraction experimental result at 260 ℃ in table
Referring to fig. 18(a) and (b) and table 1, the blocking rates and the subsequent water drive pressure differences of the temperature-resistant PAM gel 1 and the temperature-resistant PAM gel 2 in comparative examples 1 and 2 were 58.7% and 60.2% and 75KPa and 81KPa, respectively, at 120 ℃. Compared with temperature-resistant PAM gel, the PAFB gel has higher blocking rate and subsequent water drive pressure difference, the blocking rate and the subsequent water drive pressure difference of the PAFB-1, the PAFB-2 and the PAFB-3 gel in the examples 1-3 respectively reach 83.1%, 86.2% and 80.3%, 118 KPa, 137KPa and 181KPa, and the blocking strength and the blocking range are enlarged due to the double-network structure and the self-lubricating property of the PAFB gel. Meanwhile, according to fig. 18(c) and (d), the flow rate ratio of the high-permeability core to the low-permeability core in the initial water flooding process is 90:10, which indicates that the water flow is mainly concentrated in the high-permeability layer due to the reservoir heterogeneity, so that the oil recovery efficiency of the low-permeability layer is low. After profile control by the temperature-resistant PAM gel and the PAFB gel (shown in figures 18(c), (d) and table 1), the flow diversion ratio of the high-permeability core to the low-permeability core is respectively changed into 50:50 and 20:80, which shows that the PAFB gel has stronger flow diversion capability, so that the displacement fluid is mainly concentrated in the low-permeability core, and the recovery ratio of crude oil in the low-permeability layer of the oil reservoir is favorably improved. In addition, the total crude oil recovery rate and the hypotonic core crude oil recovery rate of the indoor simulated oil recovery experiments of the temperature-resistant PAM gel 1 and the temperature-resistant PAM gel 2 in the comparative examples 1 and 2 are 52.3 percent, 55.6 percent (total crude oil recovery rate), 49.7 percent and 45.3 percent (hypotonic core crude oil recovery rate) respectively at 120 ℃. Compared with temperature-resistant PAM gel, the total crude oil recovery rate is remarkably improved after the PAFB gel profile control, the total crude oil recovery rate of a low-permeability core is higher than that of a high-permeability core, the total crude oil recovery rates of PAFB-1, PAFB-2 and PAFB-3 gel indoor simulated oil recovery experiments in examples 1-3 respectively reach 75.6%, 78.1% and 76.2%, and the total crude oil recovery rates of low-permeability cores respectively reach 81.7%, 85.1% and 82.2%, so that the PAFB gel has stronger oil recovery capability, a main oil production area can be converted from a high-permeability layer to a low-permeability layer, and the exploitation degree of the low-permeability layer is effectively improved. The above experimental phenomena illustrate that,
compared with temperature-resistant PAM gel, PAFB gel has stronger deep profile control capability at high temperature (120 ℃), and can effectively increase total oil production and low permeability oil production.
On the other hand, comparing the profile control results of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1 and the temperature-resistant PAM gel 1 in the comparative example 1 at different temperatures (tables 1 and 2), it is found that the plugging range (plugging rate), the flow diversion capability (final hypotonic core flow ratio) and the oil recovery capability (oil recovery rate) of the temperature-resistant PAM gel are not significantly changed by temperature increase, and the gel plugging strength (breakthrough pressure) is only slightly reduced, which indicates that the temperature-resistant PAM gel network has strong temperature resistance. Compared with the PAFB gel, the temperature rise enhances the self-lubricating property of the PAFB gel, thereby effectively enlarging the gel plugging range, improving the gel flow diversion capability and obviously enhancing the oil extraction capability. In addition, the PAM network in the PAFB gel is used as a temperature-resistant high-strength protective support, so that the PAM network still has higher (higher than the temperature-resistant PAM gel) plugging strength at high temperature (90-120 ℃).
Other product performance results of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-2 and the temperature-responsive self-lubricating hydrogel profile control agent PAFB-3 prepared in examples 2 and 3 are similar to those of the temperature-responsive self-lubricating hydrogel profile control agent PAFB-1 prepared in example 1, and other product performance results of the temperature-resistant PAM gel 2 prepared in comparative example 2 are similar to those of the temperature-resistant PAM gel 1 prepared in comparative example 1, and are not given one by one.
The temperature response self-lubricating hydrogel profile control agent prepared by the invention is easy to transfer longitudinally, and realizes deep profile control. The temperature response self-lubricating hydrogel profile control agent can secrete more lubricating liquid along with the increase of temperature in the process of migrating to the deep part of the stratum, has better longitudinal migration capability in the stratum, and is easy to enter a low-permeability layer to realize profile control. The temperature response self-lubricating hydrogel profile control agent prepared by the invention can effectively improve the transverse water flooding efficiency of the low-permeability layer. Due to the existence of the double-network structure and the dynamic covalent bond, the temperature response self-lubricating hydrogel profile control agent has better self-lubricating property and higher mechanical strength in a high-temperature (90-120 ℃) low-permeability layer of an oil reservoir, and can block more middle and micro channels under the pushing of water flow, so that the water flooding efficiency is improved.
Claims (9)
1. A temperature-responsive self-lubricating hydrogel profile control agent is characterized in that in a water environment, a hydrophilic polymer matrix is subjected to amide-hydroxyl dehydration condensation chemical crosslinking reaction under the action of a crosslinking agent A to generate a high-strength temperature-resistant polymer network, meanwhile, a furfuryl amine-bisphenol A diglycidyl ether oligomer is subjected to Diels-Alder chemical crosslinking reaction under the action of a crosslinking agent B to generate a dynamic covalent network, and the two networks are compounded to generate the temperature-responsive self-lubricating hydrogel profile control agent.
2. A self-lubricating hydrogel profile control agent as claimed in claim 1, wherein the hydrophilic polymer matrix comprises any one of polyacrylamide, polyacrylic acid, polyethylene oxide, polyvinylpyrrolidone, polyethylene glycol, preferably polyacrylamide.
3. The self-lubricating hydrogel profile control agent of claim 1, wherein the crosslinker a comprises hexamethylenetetramine-hydroquinone, N' -methylenebisacrylamide, phenolic resin, Cr3+、Fe3+And N, N' -methylenebisacrylamide, preferably hexamethylenetetramine-hydroquinone.
4. A self-lubricating hydrogel profile control agent according to claim 1, wherein the crosslinker B is a maleimide crosslinker, preferably N, N '- (4, 4' -methylenediphenyl) bismaleimide.
5. The self-lubricating hydrogel profile control agent as claimed in claim 1, wherein the mass ratio of the hydrophilic polymer matrix, the furfuryl amine-bisphenol A diglycidyl ether oligomer, the crosslinking agent A and the crosslinking agent B is 3-7: 5-9: 1-5: 0.1-0.5.
6. A method of preparing a temperature responsive self-lubricating hydrogel profile control agent as claimed in any one of claims 1 to 5, wherein a one-pot process is used comprising the steps of:
(1) adding a hydrophilic polymer matrix, a furfuryl amine-bisphenol A diglycidyl ether oligomer, a cross-linking agent A and a cross-linking agent B into water at 60-80 ℃, and stirring to dissolve the hydrophilic polymer matrix, the furfuryl amine-bisphenol A diglycidyl ether oligomer, the cross-linking agent A and the cross-linking agent B to obtain a reaction solution;
(2) and continuously stirring the reaction solution until the polymer in the reaction solution is uniformly swelled to obtain sol, sealing the sol, and standing for 24-72 hours at the temperature of 60-80 ℃ to obtain the temperature response self-lubricating hydrogel profile control agent.
7. The method according to claim 6, wherein in the step (2), the stirring speed is 300 to 600rpm, and the stirring time is 0.5 to 1 hour.
8. A method of oil recovery based on the temperature responsive self-lubricating hydrogel profile control agent of any of claims 1-5, the method comprising:
(1) adding the profile control agent and distilled water into a colloid mill according to the mass ratio of 1-3: 1, grinding the gel at the rotating speed of 7000-12000 rpm for 20-60 min, and drying to obtain micron-level particles;
(2) adding 5-10 wt% of particles into formation water, injecting the obtained mixed solution into a high-temperature oil reservoir, transporting the particles to a high-permeability area by using water flow, standing for 3-6 hours, and enabling the particles to absorb water and expand and block the high-permeability area.
9. A method of using as claimed in claim 8 wherein said high temperature reservoir is a reservoir at a temperature of not more than 120 ℃.
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