阅读说明：本技术 一种制备高渗透油藏采收用高温交联堵剂的方法 (Method for preparing high-temperature cross-linking plugging agent for high-permeability oil reservoir recovery ) 是由 牛太同 张武生 马小丽 和严斌 杨炳杰 王哲 高萌 冯四利 于 2021-10-12 设计创作，主要内容包括：本发明涉及油田化学品技术领域,公开了一种制备高渗透油藏采收用高温交联堵剂的方法,所述高温交联堵剂包括以下重量百分比的原材料：丙烯酰胺单体13-25％、丙烯酸单体2-5％、功能性单体3.5-15％、交联剂1-2％、引发剂0.02-0.6％、余量为去离子水；包括混合溶液配置、聚合、一次造粒、二次造粒等步骤。本发明获得的凝胶颗粒成品容易进入裂缝、孔洞或高渗通道及地层深部,适应于高渗透高温高盐类型油藏领域；遇水后吸水膨胀,能有效的进行封堵,从而达到调整吸水剖面,改变液流方向,起到增油和提高采收率的作用。(The invention relates to the technical field of oil field chemicals, and discloses a method for preparing a high-temperature cross-linking plugging agent for high-permeability oil reservoir recovery, which comprises the following raw materials in percentage by weight: 13-25% of acrylamide monomer, 2-5% of acrylic acid monomer, 3.5-15% of functional monomer, 1-2% of cross-linking agent, 0.02-0.6% of initiator and the balance of deionized water; comprises the steps of mixed solution preparation, polymerization, primary granulation, secondary granulation and the like. The gel particle finished product obtained by the invention can easily enter cracks, holes or high-permeability channels and deep parts of stratums, and is suitable for the field of high-permeability high-temperature high-salinity oil reservoirs; the water-absorbing agent can absorb water to expand after meeting water, and can effectively perform plugging, thereby achieving the purposes of adjusting the water-absorbing profile, changing the direction of liquid flow, increasing oil and improving the recovery ratio.)

1. A method for preparing a high-temperature crosslinking plugging agent for high-permeability oil reservoir recovery is characterized in that,

the high-temperature cross-linking plugging agent comprises the following raw materials in percentage by weight: 13-25% of acrylamide monomer, 2-5% of acrylic acid monomer, 3.5-15% of functional monomer, 1-2% of cross-linking agent, 0.02-0.6% of initiator and the balance of deionized water;

the reaction steps are as follows:

s1, preparing mixed solution

Sequentially adding an acrylamide monomer, an acrylic acid monomer, a functional monomer and deionized water into a reaction device, stirring and mixing uniformly, adding a pH regulator to regulate the pH value to 6-7, then adding a cross-linking agent and mixing uniformly to obtain a mixed solution; controlling the temperature to be 25-40 ℃ in the mixing process;

s2, polymerization

Continuously introducing nitrogen into the reaction device, and replacing oxygen; controlling the temperature in the reaction kettle to be 25-40 ℃, and adding an initiator to initiate polymerization; controlling the temperature in the reaction kettle to be 60-75 ℃, and stirring for reaction for 120-180 min; reacting to generate gel;

s3, primary granulation

Grinding the gel obtained in the step S2 to obtain primary gel particles;

s4, secondary granulation

And (4) adding deionized water and solvent oil into the primary gel particles obtained in the step (S3), stirring and mixing uniformly, and then grinding to obtain a finished product of the gel particles.

2. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 1, wherein the method comprises the following steps: the functional monomer comprises a temperature-resistant monomer and a salt-resistant monomer.

3. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 2, wherein the method comprises the following steps: the mass ratio of the temperature-resistant monomer to the salt-resistant monomer is 1-3: 1.

4. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 3, wherein the method comprises the following steps: the salt-resistant monomer is at least one of 3-acrylamide-3-methylbutyrate sodium, N-alkyl acrylamide, sulfonated vinyl toluene and diallyl dimethyl ammonium chloride.

5. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 4, wherein the method comprises the following steps: the temperature-resistant monomer is at least one of 2-acrylamide-2-methylpropanesulfonic acid, N-acryloyl morpholine, N-vinyl-2-pyrrolidone and sodium styrene sulfonate.

6. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 1, wherein the method comprises the following steps: the cross-linking agent is at least one of N, N-methylene bisacrylamide, N-methylene bismethacrylamide, epichlorohydrin, polyethylene glycol diacrylate, ethylene glycol dimethacrylate and pentaerythritol triacrylate.

7. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 1, wherein the method comprises the following steps: the initiator is a redox initiator; the redox initiator comprises an oxidizing agent and a reducing agent; the mass ratio of the oxidant to the reducing agent is 1-1.5: 1.

8. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 7, wherein the method comprises the following steps: the oxidant is one of potassium persulfate, ammonium persulfate and sodium persulfate; the reducing agent is one of sodium sulfite, potassium sulfite and sodium thiosulfate.

9. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 1, wherein the method comprises the following steps: in step S4, the mass ratio of the primary gel particles to the deionized water to the solvent oil is 2:1: 1; the solvent oil is at least one of kerosene, white oil, gasoline and diesel oil.

10. The method for preparing the high-temperature cross-linking plugging agent for the recovery of the high-permeability oil reservoir according to claim 1, wherein the method comprises the following steps: the particle size range of the finished gel particle is as follows: d50 is more than or equal to 100 mu m and less than or equal to 400 mu m.

Technical Field

The invention relates to the technical field of oil field chemicals, and discloses a method for preparing a high-temperature cross-linking plugging agent for high-permeability oil reservoir recovery.

Background

Along with the rapid development of economy in China, the demand for petroleum is increasing day by day, the shortage of petroleum is more and more serious, according to statistics, the medium and high permeability reservoir resources account for more than 60% of the total resources, and after long-term water drive development, the medium and high permeability reservoir has reached the middle and later periods of high water content, the yield is seriously decreased, and the difficulty in stable production is large. Because of long-term water flooding development, a local large pore channel is formed in a medium and high permeability reservoir, and conventional water flooding is difficult to further improve the recovery ratio, at present, microbial oil flooding is implemented for medium and high permeability reservoirs by using a plugging agent to perform deep plugging and profile control on the reservoir and then performing surfactant oil flooding, on one hand, deep profile control is used for improving the swept volume of the reservoir, and on the other hand, chemical flooding is used for improving the oil washing efficiency of the reservoir.

The plugging agent in the prior art is unstable in a high-temperature environment, cannot be applied to the high-temperature environment, and greatly influences the recovery of an oil reservoir in the high-temperature stratum environment.

Disclosure of Invention

The invention aims to overcome the defects and provide a method for preparing a high-temperature crosslinking plugging agent for high-permeability oil reservoir recovery.

In order to achieve the purpose, the invention is implemented according to the following technical scheme:

a method for preparing a high-temperature crosslinking plugging agent for high-permeability oil reservoir recovery,

the high-temperature cross-linking plugging agent comprises the following raw materials in percentage by weight: 13-25% of acrylamide monomer, 2-5% of acrylic acid monomer, 3.5-15% of functional monomer, 1-2% of cross-linking agent, 0.02-0.6% of initiator and the balance of deionized water;

the reaction steps are as follows:

s1, preparing mixed solution

Sequentially adding an acrylamide monomer, an acrylic acid monomer, a functional monomer and deionized water into a reaction device, stirring and mixing uniformly, adding a pH regulator to regulate the pH value to 6-7, then adding a cross-linking agent and mixing uniformly to obtain a mixed solution; controlling the temperature to be 25-40 ℃ in the mixing process;

s2, polymerization

Continuously introducing nitrogen into the reaction device, and replacing oxygen; controlling the temperature in the reaction kettle to be 25-40 ℃, and adding an initiator to initiate polymerization; controlling the temperature in the reaction kettle to be 60-75 ℃, and stirring for reaction for 120-180 min; reacting to generate gel;

s3, primary granulation

Grinding the gel obtained in the step S2 to obtain primary gel particles;

s4, secondary granulation

And (4) adding deionized water and solvent oil into the primary gel particles obtained in the step (S3), stirring and mixing uniformly, and then grinding to obtain a finished product of the gel particles.

Preferably, the functional monomer comprises a temperature-resistant monomer and a salt-resistant monomer.

Preferably, the mass ratio of the temperature-resistant monomer to the salt-resistant monomer is 1-3: 1.

Preferably, the salt-resistant monomer is at least one of sodium 3-acrylamide-3-methylbutyrate, N-alkyl acrylamide, sulfonated vinyl toluene and diallyl dimethyl ammonium chloride.

Preferably, the temperature-resistant monomer is at least one of 2-acrylamido-2-methylpropanesulfonic acid, N-acryloylmorpholine, N-vinyl-2-pyrrolidone and sodium styrene sulfonate.

Preferably, the crosslinking agent is at least one of N, N-methylene bisacrylamide, N-methylene bismethacrylamide, epichlorohydrin, polyethylene glycol diacrylate, ethylene glycol dimethacrylate and pentaerythritol triacrylate.

Preferably, the initiator is a redox initiator; the redox initiator comprises an oxidizing agent and a reducing agent; the mass ratio of the oxidant to the reducing agent is 1-1.5: 1.

Preferably, the oxidant is one of potassium persulfate, ammonium persulfate and sodium persulfate; the reducing agent is one of sodium sulfite, potassium sulfite and sodium thiosulfate.

Preferably, in step S4, the mass ratio of the primary gel particles to the deionized water to the solvent oil is 2:1: 1; the solvent oil is at least one of kerosene, white oil, gasoline and diesel oil.

Preferably, the particle size range of the finished gel particle is as follows: d50 is more than or equal to 100 mu m and less than or equal to 400 mu m.

Compared with the prior art, the invention has the beneficial effects that:

temperature-resistant monomers and salt-resistant monomers are added into the gel particle finished product prepared by the method, so that the gel particle has salt-resistant and high-temperature-resistant performances; the gel particle finished product obtained by the invention can easily enter cracks, holes or high-permeability channels and deep parts of stratums, and is suitable for high-permeability high-temperature high-salinity oil reservoirs; the water-absorbing agent can absorb water to expand after meeting water, and can effectively perform plugging, thereby achieving the purposes of adjusting the water-absorbing profile, changing the direction of liquid flow, increasing oil and improving the recovery ratio.

Detailed Description

The present invention will be further described with reference to specific examples, which are illustrative of the invention and are not to be construed as limiting the invention.

Example 1

A method for preparing a high-temperature crosslinking plugging agent for high-permeability oil reservoir recovery,

the high-temperature cross-linking plugging agent comprises the following raw materials in percentage by weight: 25% of acrylamide monomer, 5% of acrylic acid monomer, 3.5% of functional monomer, 2% of cross-linking agent, 0.6% of initiator and the balance of deionized water.

The functional monomer comprises a temperature-resistant monomer and a salt-resistant monomer; the mass ratio of the temperature-resistant monomer to the salt-resistant monomer is 3: 1; the salt-resistant monomer is in diallyl dimethyl ammonium chloride. The temperature-resistant monomer is 2-acrylamide-2-methylpropanesulfonic acid.

The cross-linking agent is N, N-methylene bisacrylamide.

The initiator is a redox initiator; the redox initiator comprises an oxidizing agent and a reducing agent; the mass ratio of the oxidizing agent to the reducing agent is 1.5: 1. The oxidant is sodium persulfate; the reducing agent is sodium thiosulfate.

The reaction steps are as follows:

s1, preparing mixed solution

Sequentially adding an acrylamide monomer, an acrylic acid monomer, a functional monomer and deionized water into a reaction device, stirring and mixing uniformly, adding a pH regulator to regulate the pH value to 6, then adding a cross-linking agent and mixing uniformly to obtain a mixed solution; the temperature was controlled at 40 ℃ during the mixing.

S2, polymerization

Continuously introducing nitrogen into the reaction device, and replacing oxygen; controlling the temperature in the reaction kettle to be 40 ℃, and adding an initiator to initiate polymerization; controlling the temperature in the reaction kettle to be 75 ℃, and stirring to react for 120 min; the reaction produced a gel.

S3, primary granulation

Grinding the gel obtained in the step S2 to obtain primary gel particles;

s4, secondary granulation

And (4) adding deionized water and solvent oil into the primary gel particles obtained in the step (S3), stirring and mixing uniformly, and then grinding to obtain a finished product of the gel particles.

The mass ratio of the primary gel particles to the deionized water to the solvent oil is 2:1: 1; the solvent oil is kerosene.

The particle size range of the finished gel particles prepared in this example is as follows: d50 is more than or equal to 100 mu m and less than or equal to 200 mu m.

Example 2

A method for preparing a high-temperature crosslinking plugging agent for high-permeability oil reservoir recovery,

the high-temperature cross-linking plugging agent comprises the following raw materials in percentage by weight: 19% of acrylamide monomer, 3.5% of acrylic acid monomer, 9% of functional monomer, 1.5% of cross-linking agent, 0.33% of initiator and the balance of deionized water.

The functional monomer comprises a temperature-resistant monomer and a salt-resistant monomer; the mass ratio of the temperature-resistant monomer to the salt-resistant monomer is 2: 1; the salt-resistant monomer is N-alkyl acrylamide. The temperature-resistant monomer is N-acryloyl morpholine.

The cross-linking agent is polyethylene glycol diacrylate.

The initiator is a redox initiator; the redox initiator comprises an oxidizing agent and a reducing agent; the mass ratio of the oxidizing agent to the reducing agent is 1.3: 1. The oxidant is ammonium persulfate; the reducing agent is potassium sulfite.

The reaction steps are as follows:

s1, preparing mixed solution

Sequentially adding an acrylamide monomer, an acrylic acid monomer, a functional monomer and deionized water into a reaction device, stirring and mixing uniformly, adding a pH regulator to regulate the pH value to 6.5, then adding a cross-linking agent and mixing uniformly to obtain a mixed solution; the temperature was controlled at 35 ℃ during the mixing.

S2, polymerization

Continuously introducing nitrogen into the reaction device, and replacing oxygen; controlling the temperature in the reaction kettle to be 35 ℃, and adding an initiator to initiate polymerization; controlling the temperature in the reaction kettle to be 70 ℃, and stirring for reaction for 140 min; the reaction produced a gel.

S3, primary granulation

Grinding the gel obtained in the step S2 to obtain primary gel particles;

s4, secondary granulation

And (4) adding deionized water and solvent oil into the primary gel particles obtained in the step (S3), stirring and mixing uniformly, and then grinding to obtain a finished product of the gel particles.

The mass ratio of the primary gel particles to the deionized water to the solvent oil is 2:1: 1; the solvent oil is white oil.

The particle size range of the finished gel particles prepared in this example is as follows: d50 is more than or equal to 200 mu m and less than or equal to 300 mu m.

Example 3

A method for preparing a high-temperature crosslinking plugging agent for high-permeability oil reservoir recovery,

the high-temperature cross-linking plugging agent comprises the following raw materials in percentage by weight: 13% of acrylamide monomer, 2% of acrylic acid monomer, 15% of functional monomer, 1% of cross-linking agent, 0.05% of initiator and the balance of deionized water.

The functional monomer comprises a temperature-resistant monomer and a salt-resistant monomer; the mass ratio of the temperature-resistant monomer to the salt-resistant monomer is 1: 1; the salt-resistant monomer is 3-acrylamide-3-sodium methylbutyrate. The temperature-resistant monomer is sodium styrene sulfonate.

The cross-linking agent is epichlorohydrin.

The initiator is a redox initiator; the redox initiator comprises an oxidizing agent and a reducing agent; the mass ratio of the oxidizing agent to the reducing agent is 1: 1. The oxidant is potassium persulfate; the reducing agent is sodium sulfite.

The reaction steps are as follows:

s1, preparing mixed solution

Sequentially adding an acrylamide monomer, an acrylic acid monomer, a functional monomer and deionized water into a reaction device, stirring and mixing uniformly, adding a pH regulator to regulate the pH value to 7, then adding a cross-linking agent and mixing uniformly to obtain a mixed solution; the temperature was controlled at 25 ℃ during the mixing.

S2, polymerization

Continuously introducing nitrogen into the reaction device, and replacing oxygen; controlling the temperature in the reaction kettle to be 25 ℃, and adding an initiator to initiate polymerization; controlling the temperature in the reaction kettle to be 60 ℃, and stirring and reacting for 180 min; the reaction produced a gel.

S3, primary granulation

Grinding the gel obtained in the step S2 to obtain primary gel particles;

s4, secondary granulation

And (4) adding deionized water and solvent oil into the primary gel particles obtained in the step (S3), stirring and mixing uniformly, and then grinding to obtain a finished product of the gel particles.

The mass ratio of the primary gel particles to the deionized water to the solvent oil is 2:1: 1; the solvent oil is diesel oil.

The particle size range of the finished gel particles prepared in this example is as follows: d50 is more than or equal to 300 mu m and less than or equal to 400 mu m.

The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.