CN112442347A - Salt-resistant and high-temperature-resistant gel plugging agent crosslinked by adopting bisphenol propane and formaldehyde - Google Patents
Salt-resistant and high-temperature-resistant gel plugging agent crosslinked by adopting bisphenol propane and formaldehyde Download PDFInfo
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Abstract
The invention discloses a salt-resistant and high-temperature-resistant gel plugging agent crosslinked by bisphenol propane and formaldehyde. The salt-resistant and high-temperature-resistant gel plugging agent comprises the following components in percentage by mass: 0.2 to 1.0 percent of formaldehyde; bisphenol propane 0.3-2.0 wt%; 0.2 to 1.0 percent of terpolymer; 0.01 to 0.10 percent of stabilizer; 0.01 to 0.10 percent of delayed crosslinking agent; the balance of water. The high-temperature resistant gel plug has the gelling time of 4-70 h at the ambient temperature of 90-170 ℃, and has a stable structural state at the temperature of 120-200 ℃. The gel has the characteristics of low initial viscosity, gel formation at high temperature, stable viscosity at high temperature and good salt resistance, has good plugging property at high temperature, and can be used for high-salt and high-temperature oil and gas reservoirs with deep burial or thermal recovery of high-salt and high-temperature oil reservoirs.
Description
Technical Field
The invention relates to a salt-resistant and high-temperature-resistant gel plugging agent, in particular to a salt-resistant and high-temperature-resistant gel plugging agent which adopts terpolymer as a main body and is crosslinked by bisphenol propane and formaldehyde.
Background
The deeper the oil and gas reservoir is buried, the higher the oil and gas reservoir temperature is, and the higher the temperature resistance of the plugging agent is required to be when performing profile control of a water injection well, water plugging of an oil production well (gas production well) and temporary plugging and killing of the well during operation of the oil production well (gas production well). In addition, in the water plugging process, the gel plugging agent is required to have certain salt resistance. Meanwhile, the high-temperature resistant plugging agent is also adopted when profile control or water plugging is carried out on the oil reservoir thermally extracted by adopting modes of steam injection or in-situ combustion and the like. Currently, the most widely studied and used plugging agent is the gel plugging agent. The gel blocking agent is generally an inorganic metal ion crosslinked polymer gel system, a phenolic resin crosslinked polymer gel system and a polyethyleneimine crosslinked polymer gel system. Wherein the gel system formed by the organic cross-linking agent has better high-temperature resistance than the gel system formed by the metal cross-linking agent. The conventional organic crosslinked polymer gel has a low gelling temperature and becomes poor in plugging ability at a temperature higher than 120 ℃. In addition, under the condition of high mineralization, a large amount of inorganic salt ions can compress the diffusion double electron layers on the polymer molecular chains, so that the polymer molecules are compressed, and in the crosslinking process, the crosslinking points are limited, so that the strength of the gel blocking agent is influenced. The conventional gel plugging agent has limited salt resistance and temperature resistance, and the gel has poor stability under the conditions of high salt and high temperature, so that when the conventional organic cross-linked polymer gel is used for plugging the high-temperature oil-gas reservoir or thermal-recovery high-temperature oil reservoir which is deeply buried, the plugging effect is not ideal due to the fact that the salt resistance and the temperature resistance of the plugging agent cannot meet the temperature requirement of the oil-gas reservoir. In order to overcome the defect of poor temperature resistance of the conventional gel plugging agent, the research on the salt-resistant and high-temperature-resistant gel plugging agent is needed, and the requirements of a deeply-buried high-salt and high-temperature oil-gas reservoir or a thermally-produced high-salt and high-temperature oil reservoir are met.
Disclosure of Invention
The invention aims to provide a salt-tolerant and high-temperature-resistant gel plugging agent, which is crosslinked by adopting bisphenol propane and formaldehyde, and can profile control or plug an oil and gas reservoir under the condition of salt tolerance and high temperature, so that the exploitation effect of the oil and gas reservoir is improved.
The salt-resistant and high-temperature-resistant gel plugging agent has the characteristics of salt resistance (such as NaCl concentration of 10000mg/L) and high-temperature (such as 90-170 ℃) gelling, and has the characteristic of stable structure at high temperature (such as 120-200 ℃).
The salt-resistant and high-temperature-resistant gel plugging agent provided by the invention comprises the following components in percentage by mass:
0.2 to 1.0 percent of terpolymer;
0.2 to 1.0 percent of formaldehyde;
bisphenol propane 0.3-2.0 wt%;
0.01 to 0.10 percent of stabilizer;
0.01 to 0.10 percent of delayed crosslinking agent;
the balance of water;
wherein formaldehyde and bisphenol propane are used as cross-linking agents;
the terpolymer is polymerized by monomers of Acrylamide (AM), methyl propane sulfonic Acid (ATBS) and vinyl pyrrolidine (NVP); the polymerization steps are as follows:
adjusting the pH value of the aqueous solution of the acrylamide, the methyl propanesulfonic acid and the vinyl pyrrolidine to 6-8; introducing nitrogen into the aqueous solution to remove oxygen, and adding an initiator to react; when the temperature of the reactor is reduced to 35-45 ℃, taking out the colloidal reaction product; and mixing the colloidal reaction product with sodium hydroxide (granular), sealing, performing hydrolysis reaction at 85-95 ℃, and drying the obtained hydrolysis reaction product (for example, drying at 60 ℃ for 8 hours) to obtain the terpolymer (white powder).
In the above polymerization step, the aqueous solution may be prepared by:
firstly, deionized water is utilized to prepare an aqueous solution of acrylamide, and the mass fraction of the aqueous solution can be 25-30%; and then adding the methyl propane sulfonic acid and the vinyl pyrrolidine into the mixture, wherein the mass of the methyl propane sulfonic acid can be 12-13% of that of the acrylamide, and the mass of the vinyl pyrrolidine can be 12-13% of that of the acrylamide.
In the polymerization step, the initiator can be ammonium persulfate or sodium bisulfite, the addition amount is 0.03-0.07% of the total mass of the acrylamide, the methylpropanesulfonic acid and the vinylpyrrolidine, and the system temperature is not more than 5 ℃ in the process of adding the initiator.
In the above polymerization step, after the initiator was added, the change of the solution in the reactor was observed, and the temperature change was recorded.
In the polymerization step, the addition amount of the sodium hydroxide is 12-18% of the total mass of the acrylamide, the methylpropanesulfonic acid and the vinylpyrrolidine.
In the salt-resistant and high-temperature-resistant gel plugging agent, the molecular weight of the terpolymer can be 300-2000 ten thousand, and the hydrolysis degree can be 10-20%.
In the salt-resistant and high-temperature-resistant gel plugging agent, the chemical name of the bisphenol propane is 2, 2-bis (4-hydroxyphenyl) propane.
In the salt-resistant and high-temperature-resistant gel plugging agent, the stabilizing agent can be ammonium chloride and/or ammonium sulfate.
In the salt-resistant and high-temperature-resistant gel plugging agent, the delayed crosslinking agent can be oxalic acid and/or sodium phosphate.
The salt-resistant and high-temperature-resistant gel plugging agent can be any one of the following 1) to 9):
1)0.2 to 1.0 percent of formaldehyde, 0.38 to 1.90 percent of bisphenol-based propane, 0.3 to 1.0 percent of terpolymer, 0.02 to 0.10 percent of delayed crosslinking agent, 0.02 to 0.10 percent of stabilizer and the balance of water;
2)0.2 to 0.6 percent of formaldehyde, 0.38 to 1.14 percent of bisphenol-based propane, 0.3 to 0.6 percent of terpolymer, 0.02 to 0.06 percent of delayed crosslinking agent, 0.02 to 0.06 percent of stabilizer and the balance of water;
3)0.2 to 0.5 percent of formaldehyde, 0.38 to 0.95 percent of bisphenol-based propane, 0.3 to 0.5 percent of terpolymer, 0.02 to 0.05 percent of delayed crosslinking agent, 0.02 to 0.05 percent of stabilizer and the balance of water;
4)0.2 to 0.4 percent of formaldehyde, 0.38 to 0.76 percent of bisphenol-based propane, 0.3 to 0.4 percent of terpolymer, 0.02 to 0.04 percent of delayed crosslinking agent, 0.02 to 0.04 percent of stabilizer and the balance of water;
5) 0.3% of formaldehyde, 0.57% of bisphenol-based propane, 0.3% of terpolymer, 0.03% of delayed crosslinking agent, 0.03% of stabilizer and the balance of water;
6) 0.4% of formaldehyde, 0.76% of bisphenol-based propane, 0.4% of terpolymer, 0.04% of delayed crosslinking agent, 0.04% of stabilizer and the balance of water;
7) 0.5% of formaldehyde, 0.95% of bisphenol-based propane, 0.5% of terpolymer, 0.05% of delayed crosslinking agent, 0.05% of stabilizer and the balance of water;
8) 0.6% of formaldehyde, 1.14% of bisphenol-based propane, 0.6% of terpolymer, 0.06% of delayed crosslinking agent, 0.06% of stabilizer and the balance of water;
9)1.0 percent of formaldehyde, 1.90 percent of bisphenol propane, 1.0 percent of terpolymer, 0.10 percent of delayed crosslinking agent, 0.10 percent of stabilizer and the balance of water.
The salt-resistant and high-temperature-resistant gel plugging agent can be prepared by the following method:
preparing the aqueous solution of the terpolymer, then adding the formaldehyde, the bisphenol propane, the delayed crosslinking agent and the stabilizing agent into the aqueous solution of the terpolymer, and stirring to obtain the salt-resistant and high-temperature-resistant gel plugging agent.
After the salt-resistant and high-temperature-resistant gel plugging agent is prepared, the gel plugging agent is kept at the constant temperature of 90-170 ℃ for 4-70 h, and then the salt-resistant, high-temperature-resistant, high-profile-control and plugging gel can be formed.
The high-temperature-resistant gel plugging agent can be used for profile control of injection wells and plugging of oil production wells or gas production wells of high-salinity and high-temperature oil and gas reservoirs in deep burial, or profile control of injection wells or plugging of oil production wells of high-salinity and high-temperature oil reservoirs in thermal recovery.
Specifically, the salt-resistant and high-temperature-resistant gel plugging agent can be used for exploitation of high-salt and high-temperature oil and gas reservoirs with deep burial depths;
specifically, the salt-resistant and high-temperature-resistant gel plugging agent can be used for steam flooding heavy oil reservoir exploitation;
specifically, the salt-resistant and high-temperature-resistant gel plugging agent can be used for steam stimulation heavy oil reservoir exploitation;
specifically, the salt-resistant and high-temperature-resistant gel plugging agent can be used for the exploitation of a fire flooding heavy oil reservoir;
specifically, the salt-resistant and high-temperature-resistant gel plugging agent can be used for high-temperature hot water flooding heavy oil reservoir exploitation.
The salt-resistant and high-temperature-resistant gel plugging agent has the characteristics of low initial viscosity, gelling at high temperature, stable viscosity at high temperature and good salt resistance, has good plugging property at high temperature, and can be used for high-salt and high-temperature oil and gas reservoirs with deep burial depths or thermal recovery high-salt and high-temperature oil reservoirs.
Drawings
Fig. 1 is a structural state diagram of the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention after gelling (at 120 ℃).
Fig. 2 is a structural state diagram of the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention after gelling (at 150 ℃).
Fig. 3 is a structural state diagram of the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention after gelling (at 170 ℃).
FIG. 4 is a distribution diagram of NaCl solution (100000mg/L) and gel system before gelation of the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention.
FIG. 5 is a distribution diagram of NaCl solution (100000mg/L) and gel system after the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention is gelled.
Fig. 6 is a diagram of the upper gel structure of the gel system after the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention is gelled.
Fig. 7 is a diagram of the gel structure in the middle of the gel system after the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention is gelled.
Fig. 8 is a gel structure state diagram of the interface between the lower gel system of the gel system and the NaCl solution after the salt-resistant and high-temperature-resistant gel plugging agent prepared in example 4 of the present invention is gelled.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The terpolymer used in the following embodiment has a molecular weight of 400-800 ten thousand and a hydrolysis degree of 10-20%, and is prepared by the following method:
preparing an AM solution with a certain mass fraction (25%) by using deionized water, adding functional monomers ATBS and NVP (accounting for about 12% of the mass of the AM monomer respectively), stirring to fully dissolve, adjusting the pH of a system to about 7 by using a pH regulator, and cooling to 0 ℃; introducing nitrogen to remove oxygen for 30min, adding a small amount of initiator ammonium persulfate/sodium bisulfite (accounting for about 0.05% of the total mass of the monomers), keeping the temperature not exceeding 5 deg.C, and continuing to introduce nitrogen for 30 min; observing the change of the solution in the bottle and recording the temperature change; taking out the rubber block-shaped reaction product when the temperature in the bottle is reduced to 40 ℃, filling the rubber block-shaped reaction product into a bag, adding 15% of granular sodium hydroxide, sealing, and placing the bag into a 90 ℃ oven for reaction for 4 hours; and taking out the reactant, drying the reactant at the temperature of 60 ℃ for 8 hours, and crushing the reactant to obtain a white powdery terpolymer sample.
Example 1:
0.3g of terpolymer is added into 98.77g of water and stirred for 2 hours, and then 0.3g of formaldehyde, 0.57g of bisphenol propane, 0.03g of oxalic acid and 0.03g of ammonium chloride are added and stirred for 20 minutes to form the salt-resistant and temperature-resistant gel plugging agent.
The high temperature resistant gel blocking agent prepared in this example comprises the following components (by mass percent): 0.3% terpolymer + 0.3% formaldehyde + 0.57% bisphenol based propane + 0.03% oxalic acid + 0.03% ammonium chloride.
The salt-resistant and high-temperature-resistant gel plugging agent prepared by the embodiment has gelling time of 50h at the environmental temperature of 120 ℃; the gelling time is 34h at the ambient temperature of 150 ℃.
Example 2:
0.4g of terpolymer is added into 98.36g of water, stirred for 2 hours, and then added with 0.4g of formaldehyde, 0.76g of bisphenol propane, 0.04g of oxalic acid and 0.04g of ammonium chloride, and stirred for 20 minutes to form the salt-resistant and temperature-resistant gel plugging agent.
The salt-resistant and high-temperature-resistant gel plugging agent prepared in the embodiment comprises the following components (by mass percent): 0.4% terpolymer + 0.4% formaldehyde + 0.76% bisphenol based propane + 0.04% oxalic acid + 0.04% ammonium chloride.
The salt-resistant and high-temperature-resistant gel plugging agent prepared by the embodiment has gelling time of 38h at the environmental temperature of 120 ℃; the gelling time is 22h at the ambient temperature of 150 ℃.
Example 3:
adding 0.5g of terpolymer into 97.95g of water, stirring for 2 hours, adding 0.5g of formaldehyde, 0.95g of bisphenol propane, 0.05g of oxalic acid and 0.05g of ammonium chloride, and continuously stirring for 20 minutes to form the salt-resistant and temperature-resistant gel plugging agent.
The salt-resistant and high-temperature-resistant gel plugging agent prepared in the embodiment comprises the following components (by mass percent): 0.5% terpolymer + 0.5% formaldehyde + 0.95% bisphenol based propane + 0.05% oxalic acid + 0.05% ammonium chloride.
The salt-resistant and high-temperature-resistant gel plugging agent prepared by the embodiment has gelling time of 24 hours at the environmental temperature of 120 ℃; the gelling time is 14h at the ambient temperature of 150 ℃.
Example 4:
0.6g of terpolymer is added into 97.54g of water, stirred for 2 hours, and then added with 0.6g of formaldehyde, 1.14g of bisphenol propane, 0.06g of oxalic acid and 0.06g of ammonium chloride, and stirred for 20 minutes to form the salt-resistant and temperature-resistant gel plugging agent.
The salt-resistant and high-temperature-resistant gel plugging agent prepared in the embodiment comprises the following components (by mass percent): 0.6% terpolymer + 0.6% formaldehyde + 1.14% bisphenol based propane + 0.06% oxalic acid + 0.06% ammonium chloride.
The salt-resistant and high-temperature-resistant gel plugging agent prepared by the embodiment has gelling time of 13h at the environmental temperature of 120 ℃; the gelling time is 5h at the ambient temperature of 150 ℃.
Example 5:
adding 1.0g of terpolymer into 95.90g of water, stirring for 2h, adding 1.0g of formaldehyde, 1.90g of bisphenol propane, 0.10g of oxalic acid and 0.10g of ammonium chloride, and continuously stirring for 20min to form the salt-resistant and temperature-resistant gel plugging agent.
The salt-resistant and high-temperature-resistant gel plugging agent prepared in the embodiment comprises the following components (by mass percent): 1.0% terpolymer + 1.0% formaldehyde + 1.90% bisphenol based propane + 0.10% oxalic acid + 0.10% ammonium chloride.
The salt-resistant and high-temperature-resistant gel plugging agent prepared by the embodiment has the gelling time of 6 hours at the environmental temperature of 120 ℃; the gelling time is 4h at the ambient temperature of 150 ℃.
Example 6:
the salt-resistant, high temperature resistant gel plugging formulations of examples 1 to 5 were subjected to gel formation time (120 ℃) and viscosity tests before and after gel formation, with the results shown in table 1. As can be seen from table 1, the salt and high temperature resistant plugging formulation of example 4 has the highest strength after gelling under the conditions that the injectability is satisfied (viscosity is less than 400mPa · s).
TABLE 1 gelling time (Experimental 120 ℃ C.) and viscosity test results
Example 7:
a physical simulation experiment was performed on the formulation of the salt-resistant and high-temperature-resistant gel plugging agent in example 4.
Permeability measured at initial water as K1Respectively injecting 0.5PV of salt-resistant and high-temperature-resistant gel plugging agent into the sand-filled pipe model, keeping the temperature of the sand-filled pipe model constant at 120 ℃ for 18 hours to ensure that the salt-resistant and high-temperature-resistant gel plugging agent gels, and measuring the water permeability K again2And breakthrough pressure. The plugging rate calculation formula is as follows: f1＝(K1-K2)/K1X 100%, after subsequent water flooding by 10PV, measuring the water permeability K again3And the plugging rate calculation formula is as follows: f2＝(K1-K3)/K1X 100%, the results are shown in table 2.
As can be seen from Table 2, the salt-resistant and high-temperature-resistant gel plugging agent has good plugging capability and scouring resistance, and the system is suitable for profile control and water plugging work, and is particularly suitable for high-salt and high-temperature oil and gas reservoir plugging work.
Table 2 sand-packed pipe model plugging experimental results
Example 8:
after the salt-resistant and high-temperature-resistant gel plugging agent formula in example 4 is gelled at different temperatures (120 ℃, 150 ℃ and 170 ℃), the gel structure state is observed, and the results are shown in fig. 1, fig. 2 and fig. 3, so that the gel formula can form the gel plugging agent with stable property at high temperature, and the high-temperature-resistant performance requirement of the plugging agent in the oilfield field can be met.
Example 9:
for the formulation of the salt-tolerant and high-temperature-resistant gel plugging agent in example 4, the experiment adopted that the lower part in the ampoule bottle was the NaCl solution (100000mg/L), the upper part was the salt-tolerant and salt-tolerant gel solution, the gel was formed at 120 ℃, and the observation and test showed the gel structure state after the formation of the gel, and the results are shown in fig. 4 to 8, it was not known from the gel structure state and the viscosity test that the high salt did not significantly affect the formation of the salt-tolerant and high-temperature-resistant gel system and the gel structure, the upper and middle gel system structures were completely preserved, and the gel at the interface between the lower gel system and the NaCl solution still could maintain a higher gel structure. The salt-resistant and high-temperature-resistant gel system can meet the requirements of the oil field on the salt-resistant and high-temperature-resistant performance of the plugging agent.
Claims (7)
1. A salt-resistant and high-temperature-resistant gel plugging agent comprises the following components in percentage by mass:
0.2 to 1.0 percent of terpolymer;
0.2 to 1.0 percent of formaldehyde;
bisphenol propane 0.3-2.0 wt%;
0.01 to 0.10 percent of stabilizer;
0.01 to 0.10 percent of delayed crosslinking agent;
the balance of water;
wherein formaldehyde and bisphenol propane are used as cross-linking agents;
the terpolymer is formed by polymerizing an acrylamide monomer, a methyl propanesulfonic acid monomer and a vinyl pyrrolidine monomer.
2. The salt-tolerant, high temperature-resistant gel blocking agent of claim 1, wherein: the molecular weight of the terpolymer is 300-2000 ten thousand, and the degree of hydrolysis is 10-20%.
3. The salt-tolerant, high temperature-resistant gel blocking agent of claim 1 or 2, wherein: the stabilizer is ammonium chloride and/or ammonium sulfate.
4. The salt-tolerant, high-temperature-resistant gel blocking agent according to any one of claims 1 to 3, characterized in that: the delayed crosslinking agent is oxalic acid and/or sodium phosphate.
5. The method for preparing the salt-resistant and high-temperature-resistant gel plugging agent according to any one of claims 1 to 4, comprising the following steps:
preparing the aqueous solution of the terpolymer, then adding the formaldehyde, the bisphenol propane, the delayed crosslinking agent and the stabilizing agent into the aqueous solution of the terpolymer, and stirring to obtain the salt-resistant and high-temperature-resistant gel plugging agent.
6. The use of the salt-tolerant, high temperature-resistant gel plugging agent of any of claims 1-4 for injection well profile control and plugging of oil or gas production wells of deep-buried high-salt, high-temperature oil and gas reservoirs.
7. The application of the salt-resistant and high-temperature-resistant gel plugging agent of any one of claims 1 to 4) in the exploitation of any one of the following thermal recovery heavy oil reservoirs:
1) steam stimulation heavy oil reservoirs;
2) steam flooding heavy oil reservoir;
3) fire flooding heavy oil reservoirs;
4) high-temperature hot water flooding heavy oil reservoir.
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Cited By (1)
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| CN115785929A (en) * | 2022-12-02 | 2023-03-14 | 西南石油大学 | Preparation and application of high-temperature-resistant and hypersalinity-resistant double-crosslinked gel system |
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| CN109385259A (en) * | 2018-11-15 | 2019-02-26 | 中国石油大学(北京) | A kind of AM-AMPS-NVP terpolymer-PR heatproof profile control agent and the preparation method and application thereof |
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| CN104449618A (en) * | 2015-01-06 | 2015-03-25 | 西南石油大学 | Temperature-resisting salt-tolerant high-temperature self-cross-linking onsite polymerization water plugging gel |
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Application publication date: 20210305 |