CN109135700B - Emulsion suspension polymer selective water shutoff agent and preparation method thereof - Google Patents
Emulsion suspension polymer selective water shutoff agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an emulsion suspension polymer selective water shutoff agent, which comprises the following components: (1) an aqueous solution containing acrylamide and N, N-dimethylacrylamide, wherein the total content of acrylamide and N, N-dimethylacrylamide is 0.5 to 15% by mass, preferably 1 to 10% by mass; (2) an oil-soluble monomer styrene or octyl methacrylate, (3) an emulsifier, and (4) an initiator, wherein the content of the oil-soluble monomer is 1.0 to 10 mass%, preferably 1.5 to 8 mass%, based on the total amount of the components (1) to (3). The invention also relates to a preparation method of the selective water shutoff agent.
Description
Technical Field
The invention relates to an emulsion suspension polymer selective water shutoff agent and a preparation method thereof.
Background
The water plugging process for the oil well is a key technology for optimizing the development result of water injection of the oil and gas field. The water layer and the oil layer in the stratum are mutually interwoven, the heterogeneity is serious, the two reservoirs are difficult to be effectively isolated by the existing construction technology, but oil field enterprises need to stabilize the yield of crude oil and reduce the comprehensive water content of an oil well as far as possible, and therefore higher requirements are provided for the water shutoff agent with high oil/water selectivity. Although the existing water-based, oil-based and polymer gel water-blocking systems have certain selectivity, the water-blocking and oil-blocking systems block water and oil, and the results of laboratory physical model experiments show that the oil-blocking rate of the existing water-blocking agents is more than 35%, the temperature resistance and salt resistance of the systems are poor, and the popularization and application range is small. Although the water-soluble polymer water shutoff agent can preferentially enter a stratum with higher water saturation, part of the water-soluble polymer water shutoff agent can enter an oil layer in stratum migration, and the water-soluble polymer water shutoff agent is very difficult to discharge because the water shutoff agent has no self-plugging removal capability. Although the oil-based cement water shutoff agent can also improve the crude oil recovery efficiency to a greater extent, the oil-based cement water shutoff agent has the great disadvantage that a stratum with higher water saturation is generally plugged, and when the oil-based cement water shutoff agent flows into an oil-water mixed stratum, even if only a small part of stratum water is mixed in an oil layer, the oil-based cement water shutoff agent can react with the stratum water to solidify the cement, which shows that the water shutoff selectivity of the oil-based cement water shutoff agent is also greatly deficient. The polymer gel water shutoff agent enables the oil-water phase permeability to be reduced unevenly by means of the change of the effective movable volume under the action of oil and water, but the oil-water channel physical shutoff can be caused by the treatment mode, so that the seepage capability of a porous medium is reduced, the oil production capability is also reduced while the water production of an oil well is greatly reduced, the liquid production amount is too low due to improper treatment, and the yield of crude oil is reduced.
At present, selective water shutoff agents and deep profile control technologies at home and abroad are improved day by day, and the selective water shutoff agent has been developed greatly on the technologies of research and development, construction process and the like of selective water shutoff materials, but with the development of oil fields, the characteristics of oil layers and the environment are changed continuously, particularly in the later development period, the contradiction of oil reservoir development is more prominent due to long-term adoption of the water shutoff materials, and new selective water shutoff materials need to be developed to improve the water shutoff effect of a selective system.
At present, most of selective plugging agents used for water plugging of oil wells are formed by gel or jelly formed by water-soluble polymers such as polyacrylamide and derivatives thereof in stratums, or oil-based plugging agents are used for gelling or curing when meeting water to plug water channeling passages, but due to poor selectivity, the oil phase permeability can be greatly reduced while water is plugged, so that low liquid after plugging is caused, and the application of the water plugging technology of the oil wells is restricted. Therefore, a novel selective water plugging material is developed, the water plugging and oil plugging of an oil layer are realized, and the selective water plugging material has important significance for improving the productivity of an oil well in an ultrahigh water cut period.
Disclosure of Invention
The invention provides an emulsion suspension polymer selective water shutoff agent, which comprises the following components:
(1) an aqueous solution containing acrylamide and N, N-dimethylacrylamide, wherein the total content of acrylamide and N, N-dimethylacrylamide is 0.5 to 15% by mass, preferably 1 to 10% by mass;
(2) oil-soluble monomers such as styrene or octyl methacrylate,
(3) an emulsifying agent, and a water-soluble emulsifier,
(4) an initiator, wherein the initiator is selected from the group consisting of,
wherein the content of the oil-soluble monomer is 1.0 to 10% by mass, preferably 1.5 to 8% by mass, based on the total amount of the components (1) to (3).
The invention also provides a preparation method of the selective water shutoff agent for the emulsion suspension polymer, which comprises the following steps:
(1) weighing acrylamide and N, N-dimethylacrylamide to prepare an aqueous solution, and adjusting the pH value of the aqueous solution to 6-10;
(2) adding an oil-soluble monomer and an emulsifier into the solution, and fully stirring to form a stable emulsion;
(3) and (3) adding a water-soluble initiator and an oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, heating, and initiating polymerization to obtain the emulsion suspension polymer selective water shutoff agent.
Compared with the prior art, the invention has the following beneficial effects:
the invention introduces oil-soluble polymer particles into the emulsion of water-based acrylamide copolymer, the oil-soluble polymer particles can be stably suspended in the water-based emulsion and can be smoothly injected into the oil reservoir stratum by a high-pressure pump. The existence of the oil-soluble particles can greatly improve the temperature resistance, salt resistance and scouring resistance of the water plugging agent material. In the stratum, when the water shutoff agent is influenced by the environmental temperature and the pressure of a water layer, the water shutoff agent can deform, and a large amount of gathered oil-soluble particle water shutoff agents interact with each other to effectively block the stratum with the rock pore with higher water saturation, so that the water yield of an oil well is greatly reduced. After part of the oil-soluble particle water plugging agent flows into an oil layer, the oil-soluble particle water plugging agent can be dissolved into crude oil due to good oil solubility of the oil-soluble particle water plugging agent and is returned to the ground together with underground crude oil, so that the oil/water selectivity of the water plugging material is remarkably improved, and the effect of preventing water plugging and oil plugging is achieved.
After the water plugging material is injected into an oil reservoir stratum and enters a water phase layer, oil-soluble particles in the water plugging material can effectively plug a pore so as to reduce the water phase permeability and increase the water phase plugging effect; after entering the oil phase layer, the oil-soluble particles are dissolved in the crude oil without affecting the oil phase permeability, thereby achieving the effect of selectively blocking water and not blocking oil.
Detailed Description
The invention provides an emulsion suspension polymer selective water shutoff agent, which comprises the following components:
(1) an aqueous solution containing acrylamide and N, N-dimethylacrylamide, wherein the total content of acrylamide and N, N-dimethylacrylamide is 0.5 to 15% by mass, preferably 1 to 10% by mass;
(2) oil-soluble monomers such as styrene or octyl methacrylate,
(3) an emulsifying agent, and a water-soluble emulsifier,
(4) an initiator, wherein the initiator is selected from the group consisting of,
wherein the content of the oil-soluble monomer is 1.0 to 10% by mass, preferably 1.5 to 8% by mass, based on the total amount of the components (1) to (3).
In a preferred embodiment, the emulsifier consists of a primary emulsifier A and a co-emulsifier B,
wherein the primary emulsifier A is selected from sodium dodecyl sulfate (SBS), Sodium Dodecyl Sulfate (SDS), Sodium Dodecyl Benzene Sulfonate (SDBS), or a mixture thereof;
wherein the coemulsifier B is selected from span 20, span 40, span 60, span 80, Tween 20, Tween 40, Tween 60, Tween 80, or their mixture.
In a preferred embodiment, the concentration of N, N-dimethylacrylamide in the aqueous solution of component (1) is 0.1 to 8% by mass, preferably 0.2 to 5% by mass.
In a preferred embodiment, the content of the emulsifier is 1.0 to 5% by mass based on the total amount of the components (1) to (3); and the content of the main emulsifier A is 0.5-4.5 mass%.
In a preferred embodiment, the initiator consists of a water-soluble initiator and an oil-soluble initiator, wherein the water-soluble initiator is an oxidation-reduction initiation system consisting of a persulfate oxidizer and a sulfite reducer;
wherein the oil-soluble initiator is azobisisobutyronitrile, dimethyl azobisisobutyrate, or a mixture thereof.
In a preferred embodiment, the persulfate oxidant is added in an amount of 0.01 to 0.1 mass% and the sulfite reductant is added in an amount of 0.005 to 0.05 mass%, based on the total mass of acrylamide and N, N-dimethylacrylamide used;
wherein the oil-soluble initiator is added in an amount of 0.01 to 0.1 mass% based on the total mass of the oil-soluble monomer used, and is directly added after weighing.
The persulfate oxidizer may be selected from alkali metal or ammonium persulfate salts, such as potassium persulfate, sodium persulfate, or ammonium persulfate. When in use, the persulfate oxidizer is preferably a potassium persulfate aqueous solution with the mass concentration of 0.1-0.2% or an ammonium persulfate aqueous solution with the mass concentration of 0.1-0.2%.
The sulfite reducing agent can be selected from alkali sulfite, and when in use, the sulfite reducing agent is preferably potassium bisulfite water solution with mass concentration of 0.1-0.2% or sodium bisulfite water solution with mass concentration of 0.1-0.2%.
The invention also provides a preparation method of the selective water shutoff agent for the emulsion suspension polymer, which comprises the following steps:
(1) weighing acrylamide and N, N-dimethylacrylamide to prepare an aqueous solution, and adjusting the pH value of the aqueous solution to 6-10;
(2) adding an oil-soluble monomer and an emulsifier into the solution, and fully stirring to form a stable emulsion;
(3) and (3) adding a water-soluble initiator and an oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, heating, and initiating polymerization to obtain the emulsion suspension polymer selective water shutoff agent.
In a preferred embodiment, in step (3), the temperature is raised to 40-60 ℃ and the polymerization is initiated for more than 6 hours, for example 6-8 hours.
In a preferred embodiment, in step (3), the water-soluble initiator is used in the form of an aqueous solution of 0.1 to 0.2 mass%.
In one embodiment, the method for preparing the water shutoff agent of the present invention comprises the following steps:
step 1, weighing acrylamide and N, N-dimethylacrylamide, adding the acrylamide and the N, N-dimethylacrylamide into a heat-preservation polymerization bottle to prepare an aqueous solution, and adjusting the pH value of the aqueous solution to 6-10 by using alkali (such as sodium hydroxide or sodium carbonate);
step 2, weighing oil-soluble monomers, a main emulsifier A and an auxiliary emulsifier B, adding the oil-soluble monomers, the main emulsifier A and the auxiliary emulsifier B into the solution, and fully stirring to form stable emulsion;
and 3, adding a water-soluble initiator and an oil-soluble initiator into the emulsion obtained in the step 2, fully stirring and emulsifying, raising the temperature to 40-60 ℃, and initiating polymerization for 6-8 hours to obtain the water plugging material.
In the present invention, unless otherwise specified, the operation is carried out under normal pressure.
In the present invention, all parts and percentages are by mass unless otherwise specified.
In the present invention, the substances used are all known substances, and are commercially available or synthesized by known methods.
In the present invention, the apparatus or equipment used is conventional apparatus or equipment known in the art, and is commercially available.
In the invention, the plugging rate is carried out on a rock core flow test device according to the plugging rate test procedure in 'indoor test method for bridging plugging material for drilling fluid' SY/T5840-2007.
And (3) measuring the water plugging rate: loading the artificial core into core holder, saturating with water, and measuring its pore volume PV and water phase permeability (K)w1) Then injecting 1.0PV water shutoff agent, curing for 24h at 90 ℃, and measuring the permeability (K) of the mixture after adding the water shutoff agent by using waterw2)，Kw2And Kw1Ratio (K)w2/Kw1) Namely the water plugging rate.
And (3) measuring the oil plugging rate: loading the artificial core into core holder, saturating with oil, and measuring its pore volume PV and oil phase permeability (K)o1) Then injecting 1.0PV water shutoff agent, curing for 24h at 90 deg.C, and measuring the permeability (K) after adding water shutoff agent with oilo2)，Ko2And Ko1Ratio (K)o2/Ko1) Namely the oil plugging rate.
And (3) measuring the scouring resistance multiple: after the water plugging rate is measured, water with 50 times of pore volume multiple (PV) is continuously injected into the rock core, the permeability under different PV numbers is recorded, the water plugging rate under different PV numbers is calculated according to the measuring method of the water plugging rate, and the scouring resistance multiple is the maximum PV number of the injected water when the water plugging rate is more than or equal to 80%. Normally, the water blocking rate at 50PV number is measured, and the value is more than or equal to 80 percent, which indicates that the material has excellent flushing resistance.
Wherein the artificial core is obtained by filling quartz sand of 40-60 meshes in a mould.
Example 1
The preparation of the emulsion suspension polymer selective water shutoff agent of the invention comprises the following steps:
(1) weighing 2.9g of acrylamide and 0.6g N, N-dimethylacrylamide, adding into 300mL of water, stirring and fully dissolving, and then adjusting the pH value of the aqueous solution to 6.0 by using alkali to obtain a stable aqueous solution;
(2) 6.0g of styrene, 1.5g of a main emulsifier SDBS and 1.5g of a co-emulsifier span 20 are weighed and added into the solution, and a stable emulsion is formed after full stirring;
(3) and (3) sequentially adding 0.15g of 0.2% potassium persulfate aqueous solution, 0.15g of 0.1% sodium bisulfite aqueous solution and 0.6mg of oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, raising the temperature to 40 ℃, and initiating polymerization for 6-8 hours to obtain the polymer water plugging material DSJ 1.
Tests show that under the conditions of high temperature (90 ℃) and high salt (the mineralization is 50,000mg/L), the water plugging rate of the water plugging material is 94.5%, the oil plugging rate is 12.3%, and the scouring resistance multiple is more than 50 PV. This shows that the water plugging material prepared in this example has excellent selective plugging rate and flushing resistance to oil/water, and particularly still has good selective plugging rate to oil/water under high temperature and high salt conditions.
Example 2
The preparation of the emulsion suspension polymer selective water shutoff agent of the invention comprises the following steps:
(1) weighing 9.0g of acrylamide and 6.0g N, N-dimethylacrylamide, adding into 300mL of water, stirring and fully dissolving, and then adjusting the pH value of the aqueous solution to 7.0 by using alkali to obtain a stable aqueous solution;
(2) weighing 15.0g of styrene, 6.0g of SBS (styrene butadiene styrene) as a main emulsifier and 3.0g of span 40 as a co-emulsifier, adding into the solution, and fully stirring to form stable emulsion;
(3) and (3) sequentially adding 3.75g of 0.2% potassium persulfate aqueous solution, 3.75g of 0.1% sodium bisulfite aqueous solution and 7.5mg of oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, raising the temperature to 45 ℃, and initiating polymerization for 7 hours to obtain the polymer water plugging material DSJ 2.
Tests show that under the conditions of high temperature (90 ℃) and high salt (the mineralization is 50,000mg/L), the water plugging rate of the water plugging material is 96.2 percent, the oil plugging rate is 10.3 percent, and the scouring resistance multiple is more than 50 PV. This shows that the water plugging material prepared in this example has excellent selective plugging rate and flushing resistance to oil/water, and particularly still has good selective plugging rate to oil/water under high temperature and high salt conditions.
Example 3
The preparation of the emulsion suspension polymer selective water shutoff agent of the invention comprises the following steps:
(1) weighing 15.0g of acrylamide and 15.0g of 15.0g N, N-dimethylacrylamide, adding the acrylamide and the 15.0g of g N into 300mL of water, stirring and fully dissolving, and then adjusting the pH value of the aqueous solution to 7.0 by using alkali to obtain a stable aqueous solution;
(2) weighing 30.0g of styrene, 10.0g of SDS (sodium dodecyl sulfate) serving as a main emulsifier and 5.0g of Tween 80 serving as a co-emulsifier, adding the weighed materials into the solution, and fully stirring to form stable emulsion;
(3) and (3) sequentially adding 15.0g of 0.2% potassium persulfate aqueous solution, 15.0g of 0.1% sodium bisulfite aqueous solution and 30mg of oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, raising the temperature to 60 ℃, and initiating polymerization for 8 hours to obtain the polymer water plugging material DSJ 3.
Tests show that under the conditions of high temperature (90 ℃) and high salt (the mineralization is 50,000mg/L), the water plugging rate of the water plugging material is 96.5 percent, the oil plugging rate is 8.9 percent, and the scouring resistance multiple is more than 50 PV. This shows that the water plugging material prepared in this example has excellent selective plugging rate and flushing resistance to oil/water, and particularly still has good selective plugging rate to oil/water under high temperature and high salt conditions.
Example 4
The preparation of the emulsion suspension polymer selective water shutoff agent of the invention comprises the following steps:
(1) weighing 10.0g of acrylamide and 8.0g of 8.0g N, N-dimethylacrylamide, adding into 300mL of water, stirring and fully dissolving, and then adjusting the pH value of the aqueous solution to 7.0 by using alkali to obtain a stable aqueous solution;
(2) weighing 12.0g of octyl methacrylate, 6.0g of SDBS (sodium dodecyl benzene sulfonate) as a main emulsifier and 6.0g of Tween 40 as a co-emulsifier, adding into the solution, and fully stirring to form stable emulsion;
(3) and (3) sequentially adding 1.8g of 0.2% potassium persulfate aqueous solution, 1.8g of 0.1% sodium bisulfite aqueous solution and 6.0mg of oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, raising the temperature to 50 ℃, and initiating polymerization for 7 hours to obtain the polymer water plugging material DSJ 4.
Tests show that under the conditions of high temperature (90 ℃) and high salt (the mineralization is 50,000mg/L), the water plugging rate of the water plugging material is 97.6 percent, the oil plugging rate is 6.8 percent, and the scouring resistance multiple is more than 50 PV. This shows that the water plugging material prepared in this example has excellent selective plugging rate and flushing resistance to oil/water, and particularly still has good selective plugging rate to oil/water under high temperature and high salt conditions.
Claims (6)
1. An emulsion suspension polymer selective water shutoff agent, which consists of the following components:
(1) an aqueous solution containing acrylamide and N, N-dimethylacrylamide, wherein the total content of acrylamide and N, N-dimethylacrylamide is 0.5 to 15% by mass, and wherein the concentration of N, N-dimethylacrylamide is 0.1 to 8% by mass;
(2) an oil-soluble monomer styrene or octyl methacrylate, wherein the content of the oil-soluble monomer is 1.0 to 10 mass% based on the total amount of the components (1) to (3);
(3) an emulsifier which consists of a main emulsifier A and a co-emulsifier B,
wherein the main emulsifier A is selected from sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, or their mixture; wherein the coemulsifier B is selected from span 20, span 40, span 60, span 80, Tween 20, Tween 40, Tween 60, Tween 80, or mixture thereof; wherein the content of the emulsifier is 1.0 to 5% by mass based on the total amount of the components (1) to (3); and the content of the main emulsifier A is 0.5-4.5 mass%;
(4) the initiator consists of a water-soluble initiator and an oil-soluble initiator, wherein the water-soluble initiator is an oxidation-reduction initiation system consisting of a persulfate oxidant and a sulfite reducing agent; wherein the oil-soluble initiator is azobisisobutyronitrile, dimethyl azobisisobutyrate, or a mixture thereof; wherein the persulfate oxidizer is added in an amount of 0.01 to 0.1 mass% and the sulfite reducer is added in an amount of 0.005 to 0.05 mass%, based on the total mass of acrylamide and N, N-dimethylacrylamide used; wherein the amount of the oil-soluble initiator added is 0.01 to 0.1 mass% based on the total mass of the oil-soluble monomer used;
the selective water shutoff agent for the emulsion suspension polymer is prepared by a method comprising the following steps of:
(1) weighing acrylamide and N, N-dimethylacrylamide to prepare an aqueous solution, and adjusting the pH value of the aqueous solution to 6-10;
(2) adding an oil-soluble monomer and an emulsifier into the solution, and fully stirring to form a stable emulsion;
(3) and (3) adding a water-soluble initiator and an oil-soluble initiator into the emulsion obtained in the step (2), fully stirring and emulsifying, heating, and initiating polymerization to obtain the emulsion suspension polymer selective water shutoff agent.
2. The emulsion suspension polymer selective water shutoff agent according to claim 1, wherein the total content of acrylamide and N, N-dimethylacrylamide is 1 to 10% by mass.
3. The emulsion suspension polymer selective water shutoff agent according to claim 1, wherein the content of the oil-soluble monomer is 1.5 to 8% by mass based on the total amount of the components (1) to (3).
4. The emulsion suspension polymer selective water shutoff agent according to claim 1, wherein the concentration of N, N-dimethylacrylamide in the aqueous solution of component (1) is 0.2 to 5% by mass.
5. The emulsion suspension polymer selective water shutoff according to claim 1, wherein in step (3), the temperature is raised to 40-60 ℃ and polymerization is initiated for more than 6 hours.
6. The emulsion suspension polymer selective water shutoff agent according to claim 1, wherein in the step (3), the water-soluble initiator is used in the form of an aqueous solution of 0.1 to 0.2 mass%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811238997.9A CN109135700B (en) | 2018-10-23 | 2018-10-23 | Emulsion suspension polymer selective water shutoff agent and preparation method thereof |
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| CN201811238997.9A CN109135700B (en) | 2018-10-23 | 2018-10-23 | Emulsion suspension polymer selective water shutoff agent and preparation method thereof |
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| CN109135700A CN109135700A (en) | 2019-01-04 |
| CN109135700B true CN109135700B (en) | 2021-05-14 |
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