CN110305651B - Nano particle crosslinked polymer oil displacement agent and preparation method and application thereof - Google Patents

Nano particle crosslinked polymer oil displacement agent and preparation method and application thereof Download PDF

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CN110305651B
CN110305651B CN201810262575.9A CN201810262575A CN110305651B CN 110305651 B CN110305651 B CN 110305651B CN 201810262575 A CN201810262575 A CN 201810262575A CN 110305651 B CN110305651 B CN 110305651B
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polyacrylamide
acid
solution
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CN110305651A (en
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卢刚
吕成远
马涛
许关利
刘平
谭中良
贾红育
周国华
聂俊
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China Petroleum and Chemical Corp
Sinopec Exploration and Production Research Institute
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    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K8/86—Compositions based on water or polar solvents containing organic compounds
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    • C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract

The invention belongs to the technical field of oilfield development, and particularly provides a nanoparticle crosslinked polymer oil-displacing agent, and a preparation method and application thereof2Nano particles and water, wherein the concentration of the polyacrylamide is 90-3000 mg/L, and the ZrO content is ZrO2The concentration of the nanoparticles is 0.001-1 mg/L. The polymer oil-displacing agent adopts activated nano ZrO2As a cross-linking agent, the cross-linking agent is beneficial to controlling intermolecular cross-linking reaction of polymers and improving the efficiency of the cross-linking reaction, thereby reducing the dosage of the cross-linking agent, increasing the viscosity of polymer solution and achieving the aim of improving the recovery ratio of crude oil.

Description

Nano particle crosslinked polymer oil displacement agent and preparation method and application thereof
Technical Field
The invention belongs to the technical field of oilfield development, and particularly relates to a nanoparticle crosslinked polymer oil-displacing agent, a preparation method thereof and application of the nanoparticle crosslinked polymer oil-displacing agent.
Background
At present, most oil fields in China are in the middle and later development stages, the water content rapidly rises even to be more than 90%, and the existing water injection technology is difficult to meet the requirements of the oil fields. Enhanced oil recovery is achieved primarily from two aspects: on one hand, the sweep coefficient of the injected fluid in an oil layer is improved, the main method is to improve the heterogeneity of an oil reservoir or reduce the mobility of a displacement phase, stabilize the displacement front, and generally realize the displacement by profile control or increase the viscosity of the displacement fluid; another aspect is to improve the efficiency of oil washing, mainly by changing the wettability of the rock surface and reducing the adverse effects of capillarity, and by reducing the saturation of residual oil, typically by lowering the oil-water interfacial tension with surfactants. In recent years, the polymer flooding technology has become a mature and perfect practical technology for improving the oil recovery ratio in China, the pilot test of a mine site is mostly successful, Daqing oil fields enter a large-area industrialized popularization and application stage, and the polymer flooding technology research is also carried out in the Zhongpetrochemical Shengli oil field and the Henan oil field, so that a good effect is achieved in the mine site.
The polymer flooding is the most important technology of chemical flooding, and the oil displacement efficiency can be greatly improved by adding a water-soluble polymer into injected water, increasing the viscosity of a displacement phase, adjusting the oil-water fluidity ratio, expanding the wave and volume of the displacement phase and enhancing the oil washing efficiency. The polymer flooding agent is simple to operate, low in cost, capable of being combined with a profile control water shutoff agent for use, and has a certain permeability adjusting effect. The synthetic water-soluble polymer mainly comprising polyacrylamide and derivatives thereof is the polymer oil displacement agent which is most widely applied in chemical flooding and has the most remarkable effect at present. According to the structural division of polyacrylamide, the polyacrylamide can be divided into linear polyacrylamide and crosslinking polyacrylamide. The use of partially hydrolyzed linear polyacrylamide (HPAM) as an oil displacement agent is mainly based on the effect of increasing the viscosity of an aqueous solution, so as to increase the swept volume and improve the fluidity ratio. The poor temperature resistance and salt resistance of the linear polyacrylamide solution are technical bottlenecks in the application of the linear polyacrylamide solution in high-temperature oil reservoirs and polymer flooding oil reservoirs, and the actual using effect of the linear polyacrylamide solution is seriously influenced.
The cross-linked polyacrylamide is mostly formed by underground in-situ cross-linking, and the cross-linking agent is organic chromium, organic aluminum, organic zirconium, water-soluble phenolic resin and the like, and is formed by underground cross-linking with the linear HPAM by utilizing the cross-linking agent. The cross-linked polyacrylamide can be used as a profile control water shutoff agent and an oil displacement agent, and the high permeability layer can be subjected to profile control treatment to adjust the permeability of the high permeability layer due to the good volume swelling property of the cross-linked polyacrylamide. However, the use of fully crosslinked polyacrylamide in tertiary oil recovery is limited because of its high degree of crosslinking, high hardness, poor deformability, difficulty in migration through pores, and difficulty in functioning as an oil-displacing agent. When the polymer suspension is used as an oil displacement agent, the polymer suspension is required to have better migration capacity, can deform and pass through pores, has excellent viscoelastic performance, and can effectively increase the viscosity of a displacement phase and improve the fluidity ratio of the displacement phase.
Patent document CN93115276.3 discloses a crosslinked polymer oil displacement agent prepared by using polyacrylamide (or xanthan gum) as a gelling agent and chromium lactate as a crosslinking agent, which utilizes the crosslinking agent chromium lactate to change a polymer into a crosslinked polymer, thereby solving the problems of poor salt resistance and easy mechanical shearing of the polymer, wherein the concentration of a polyacrylamide aqueous solution in the patent document is preferably 800-8000 mg/L, and the dosage of the crosslinking agent chromium lactate is preferably 300-3000 mg/L, and the technical scheme has the following disadvantages: because the use of the small molecular crosslinking agent can cause intramolecular crosslinking reaction of a large amount of polymers, the use amount of the crosslinking agent is large. Patent document CN97104045.1 discloses that the injection cost is reduced by using aluminum citrate as a cross-linking agent to replace part of polyacrylamide in the polymer flooding technology and reducing the usage amount of polyacrylamide under the condition of ensuring that the injection viscosity is not reduced and is increased properly, but the injection viscosity is not increased much and is increased by only 0-25%. Patent document CN201510484051.0 provides a crosslinked polymer oil-displacing agent synthesized by taking triamines as raw materials, acrylamide adopts Pentamethyldiethylenetriamine (PMTDA) as a functional monomer and a crosslinking agent, potassium sulfate-sodium bisulfite is used as an initiation system, and the polymer oil-displacing agent which is partially crosslinked and contains a large number of branched structures is prepared.
Disclosure of Invention
Aiming at the defect that a small molecular cross-linking agent in the prior art generates a large amount of polymer intramolecular cross-linking reaction, the invention aims to provide a polymer oil-displacing agent crosslinked by nano particles, a preparation method thereof, and application of the polymer oil-displacing agent crosslinked by nano particles, wherein activated nano ZrO is selected2As a cross-linking agent, the cross-linking agent is beneficial to controlling intermolecular cross-linking reaction of polymers and improving the efficiency of the cross-linking reaction, thereby reducing the dosage of the cross-linking agent, increasing the viscosity of polymer solution and achieving the aim of improving the recovery ratio of crude oil.
The first aspect of the invention provides a nanoparticle crosslinked polymer oil displacement agent, which comprises polyacrylamide and ZrO2Nano particles and water, wherein the concentration of the polyacrylamide is 90-3000 mg/L, and the ZrO content is ZrO2The concentration of the nanoparticles is 0.001-1 mg/L.
The second aspect of the invention provides a preparation method of a nanoparticle crosslinked polymer oil-displacing agent, which comprises the following steps:
1) preparing polyacrylamide into a solution with the concentration of 100-3000 mg/L;
2) ZrO 2 is mixed with2Preparing the nano particles into a solution with the concentration of 1-100 mg/L;
3) mixing the solutions prepared in the steps 1) and 2) according to a volume ratio of 100-1000: 1 to obtain the polymer oil-displacing agent.
The third aspect of the invention provides a nanoparticle cross-linked polymer oil displacement agent prepared by the preparation method.
A fourth aspect of the invention provides the use of a nanoparticle crosslinked polymer oil-displacing agent as described above, preferably a polyacrylamide solution and ZrO2The nanoparticle solution is mixed and then injected, or mixed during the injection process.
The polymer oil displacement agent is prepared by adding a small amount of ZrO subjected to acid activation treatment into a polyacrylamide solution2Nanoparticles as inorganic cross-linking agent, ZrO of suitable particle size2The size of the nano particle cross-linking agent is equivalent to that of polymer molecules in the solution, so that the cross-linking between molecules of polyacrylamide is facilitated, the effective cross-linking efficiency is improved, and ZrO2The nano particles can be used as a cross-linking agent without special organic group modification, so that the viscosity of a polymer solution is increased, and the polymer flooding is facilitated to improve the oil recovery rate. The viscosity of the crosslinked polymer solution is 20-85 mPas, the viscosity after aging for 1-10 days is 30-184 mPas, and the viscosity is increased by 2-11 times compared with the initial polymer viscosity.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
In order that the present invention may be more readily understood, the following detailed description of the invention is given with reference to the accompanying embodiments, which are given by way of illustration only and are not intended to limit the invention.
The first aspect of the invention provides a nanoparticle crosslinked polymer oil displacement agent, which comprises polyacrylamide and ZrO2Nano particles and water, wherein the concentration of the polyacrylamide is 90-3000 mg/L, and the ZrO content is ZrO2The concentration of the nanoparticles is 0.001-1 mg/L.
Preferably, the concentration of the polyacrylamide is 750-3000 mg/L, and the ZrO content is high2The concentration of the nano particles is 0.02-1 mg/L.
In the present invention, the ZrO2Nano particleZrO activated by acid2Nanoparticles. Acid activated ZrO2The nano particles are ZrO2The nano particles are prepared by activating under the condition of low acidity, and the preparation method comprises the following steps: ZrO 2 is mixed with2The nanoparticles are ultrasonically dispersed in an acid solution with the pH value of 3-4 to be activated for 1-10 min, and the activation temperature is 10-50 ℃.
According to the present invention, the acid in the acid solution for activation may be selected from at least one of hydrochloric acid, acetic acid, sulfuric acid, and oxalic acid.
In the present invention, the ZrO2The particle size of the nanoparticles may be 1 to 200nm, preferably 10 to 100 nm.
According to the invention, the polyacrylamide is partially hydrolyzed polyacrylamide with a molecular weight range of 5-20 × 106The degree of hydrolysis is 10-30%.
The second aspect of the invention provides a preparation method of a nanoparticle crosslinked polymer oil-displacing agent, which comprises the following steps:
1) preparing polyacrylamide into a solution with the concentration of 100-3000 mg/L;
2) ZrO 2 is mixed with2Preparing the nano particles into a solution with the concentration of 1-100 mg/L;
3) mixing the solutions prepared in the steps 1) and 2) according to a volume ratio of 100-1000: 1 to obtain the polymer oil-displacing agent.
In the invention, the polyacrylamide is partially hydrolyzed polyacrylamide, and the molecular weight range of the polyacrylamide is 5-20 multiplied by 106The degree of hydrolysis is 10-30%. Preparing an aqueous solution of polyacrylamide under stirring at room temperature as a gelling agent, preferably, preparing a solution of polyacrylamide with a concentration of 800-3000 mg/L.
According to the invention, the ZrO2The nanoparticles being acid-activated ZrO2The particle size of the nanoparticles may be 1 to 200nm, preferably 10 to 100 nm.
Acid activated ZrO2The nano particles are nano-sized ZrO2The particles are activated under low acidity conditions, which can be routinely selected with reference to the art. Preferably, the acid-activated ZrO2Nano meterThe preparation method of the particles comprises the following steps: ZrO 2 is mixed with2Ultrasonically dispersing the nanoparticles in an acid solution with the pH value of 3-4, and activating for 1-10 min at the activation temperature of 10-50 ℃; the acid in the acid solution is at least one selected from hydrochloric acid, acetic acid, sulfuric acid and oxalic acid.
Activated ZrO2The nano particles are prepared into solution as a cross-linking agent, and ZrO with concentration2The nano particle activating solution can be directly used as a cross-linking agent solution for standby, and the activating solution can also be centrifuged to obtain activated ZrO2The nano particles are washed by deionized water and then are dispersed in the deionized water to be used as a cross-linking agent solution for standby.
The third aspect of the invention provides a nanoparticle cross-linked polymer oil displacement agent prepared by the preparation method.
In a fourth aspect the present invention provides the use of a nanoparticle crosslinked polymer oil-displacing agent as described above.
Preferably, the gel former (polyacrylamide solution) and the crosslinking agent (ZrO) constituting the polymer oil-displacing agent2Nanoparticle solution) may be mixed and then injected, or may be mixed during the injection process. When the gelling agent and the crosslinking agent are mixed first, the mixing mode is preferably as follows: adding a cross-linking agent (ZrO) with corresponding concentration into a prepared polymer (polyacrylamide) solution with a certain concentration under the condition of stirring2Nanoparticle) solution, mixing, stirring for 1-20 minutes, and then preparing for injection. When mixed during injection: the prepared polymer solution with a certain concentration and the cross-linking agent solution with a corresponding concentration are respectively injected at the same time, and the gelling agent and the cross-linking agent are automatically mixed and stirred in the injection process. No matter what mixing method is adopted, the volume ratio of the polymer solution to the cross-linking agent solution is preferably 100: 1-200: 1.
The present invention will be described in detail below with reference to examples.
In the following examples and comparative examples:
the viscosity of the crosslinking system is measured by adopting a Brookfield viscometer under the conditions of temperature of 40-70 ℃ and shearing rate of 6 r/min.
The core used in the core displacement experiment is beret sandstone, the length is 10cm, the inner diameter is 2.5cm, the permeability is 500mD, the pore volume is 45mL, the whole displacement experiment is carried out in a digital temperature control box, the fluid injection speed is 0.5mL/min, and the experiment temperature is 60 ℃.
Examples 1-5 are presented to illustrate nanoparticle crosslinked polymer oil-displacing agents of the present invention.
Example 1
Firstly, preparing polyacrylamide into 1000mg/L solution, and then preparing ZrO with the particle size of 20nm2Ultrasonically dispersing the particles in an oxalic acid solution with the pH value of 3 to activate for 5 minutes at the activation temperature of 30 ℃, centrifuging, washing with deionized water, and dispersing in the deionized water to be used as a cross-linking agent solution for later use, wherein the concentration of the particles is 10 mg/L. 200mL of the polymer solution was used as a gum, 1mL of the crosslinking agent solution was added, and the resulting mixture was stirred at 60 ℃ for 10 minutes to determine the viscosity of the crosslinked polymer solution to be 23 mPas, and after aging for 3 days, the viscosity was 38 mPas. The core displacement experiment result shows that the cross-linking system can improve the crude oil recovery rate by 8.3 percent.
Example 2
Firstly preparing polyacrylamide into 3000mg/L solution, and then preparing ZrO with particle size of 50nm2Ultrasonically dispersing the particles in a sulfuric acid solution with the pH value of 3 to activate for 5 minutes at the activation temperature of 10 ℃, centrifuging, washing with deionized water, and dispersing in the deionized water to be used as a cross-linking agent solution for later use, wherein the concentration of the particles is 100 mg/L. 100mL of the polymer solution was used as a gum, 1mL of the crosslinking agent solution was added, and the resulting mixture was stirred at 60 ℃ for 10 minutes to determine the viscosity of the crosslinked polymer solution to 85 mPas, and aged for 3 days to determine the viscosity to 184 mPas. The core displacement experiment result shows that the cross-linking system can improve the crude oil recovery by 23 percent.
Example 3
Firstly preparing polyacrylamide into 1000mg/L solution, and then preparing ZrO with particle size of 10nm2Ultrasonically dispersing the particles in an acetic acid solution with the pH value of 3 to activate for 10 minutes at the activation temperature of 40 ℃, centrifuging, washing with deionized water, and dispersing in the deionized water to be used as a cross-linking agent solution for later use, wherein the concentration of the particles is 20 mg/L. 500mL of the polymer solution was used as a gum, 5mL of the crosslinking agent solution was added, and the mixture was stirred at 60 ℃ for 10 minutes to measure the crosslinking polymerizationThe viscosity of the solution was 56 mPas, which was 63 mPas after aging for 2 days. The core displacement experiment result shows that the cross-linking system can improve the crude oil recovery rate by 15 percent.
Example 4
Firstly preparing polyacrylamide into 800mg/L solution, and then preparing ZrO with the particle size of 100nm2Ultrasonically dispersing the particles in a sulfuric acid solution with the pH value of 3 to activate for 5 minutes at the activation temperature of 20 ℃, centrifuging, washing with deionized water, and dispersing in the deionized water to be used as a cross-linking agent solution for later use, wherein the concentration of the particles is 100 mg/L. 1000mL of the polymer solution was used as a gum, 5mL of the crosslinking agent solution was added, and the resulting mixture was stirred at 60 ℃ for 10 minutes to determine the viscosity of the crosslinked polymer solution to be 32 mPas, and after 3 days of aging, the viscosity was 30 mPas. The core displacement experiment result shows that the cross-linking system can improve the crude oil recovery rate by 11 percent.
Example 5
Firstly, preparing polyacrylamide into 2000mg/L solution, and then preparing ZrO with the particle size of 20nm2The particles were ultrasonically dispersed in acetic acid solution of pH 4 for 5 minutes at 30 deg.C and a particle concentration of 2 mg/L. The gel forming agent and the cross-linking agent are injected into the polymer displacement experiment after water flooding according to the volume ratio of 100: 1, and the gel forming agent and the cross-linking agent are automatically mixed and stirred in the injection process, so that the result shows that the cross-linking system can improve the crude oil recovery rate by 12%.
Comparative examples 1 to 3
The following polyacrylamide solutions were each measured for viscosity with a Brookfield viscometer at a temperature of 60 ℃ and a shear rate of 6 r/min.
The viscosity of the 1000mg/L polyacrylamide solution was 8.2 mPas.
The viscosity of a 3000mg/L polyacrylamide solution was 29 mPas.
The viscosity of the 800mg/L polyacrylamide solution was 7.6 mPas.
As can be seen from the data of examples and comparative examples, ZrO2The addition of the nano particles is beneficial to controlling the intermolecular crosslinking reaction of polyacrylamide and improving the efficiency of the crosslinking reaction, thereby reducing the dosage of the crosslinking agent and increasing the polymer solutionThe viscosity of the cross-linking system is increased by 2-11 times compared with the viscosity of the initial polymer, and the recovery ratio is increased by 6-29% in an indoor polymer displacement experiment.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.

Claims (8)

1. A nano particle crosslinked polymer oil displacement agent, which is characterized in that the polymer oil displacement agent comprises polyacrylamide and ZrO2Nano particles and water, wherein the concentration of the polyacrylamide is 90-3000 mg/L, and the ZrO content is ZrO2The concentration of the nano particles is 0.001-1 mg/L;
the ZrO2The nanoparticles being acid-activated ZrO2Nanoparticles having a particle diameter of 1 to 200 nm;
the acid-activated ZrO2The preparation method of the nano-particles comprises the following steps: ZrO 2 is mixed with2Ultrasonically dispersing the nanoparticles in an acid solution with the pH value of 3-4, activating for 1-10 min, wherein the activation temperature is 10-50 ℃, and the acid in the acid solution is selected from at least one of hydrochloric acid, acetic acid, sulfuric acid and oxalic acid;
the polyacrylamide is partially hydrolyzed polyacrylamide, and the molecular weight range of the polyacrylamide is 5-20 multiplied by 106The degree of hydrolysis is 10-30%.
2. The polymer oil-displacing agent according to claim 1, wherein the concentration of the polyacrylamide is 750 to 3000mg/L, and the ZrO is ZrO2The concentration of the nano particles is 0.02-1 mg/L.
3. The polymer oil-displacing agent according to claim 1, wherein the ZrO2The particle size of the nanoparticles is 10-100 nm.
4. A method for preparing a nanoparticle crosslinked polymer oil-displacing agent, the method comprising:
1) preparing polyacrylamide into a solution with the concentration of 100-3000 mg/L;
2) ZrO 2 is mixed with2Preparing the nano particles into a solution with the concentration of 1-100 mg/L;
3) mixing the solutions prepared in the steps 1) and 2) according to a volume ratio of 100-1000: 1 to obtain the polymer oil-displacing agent;
the polyacrylamide is partially hydrolyzed polyacrylamide, and the molecular weight range of the polyacrylamide is 5-20 multiplied by 106The degree of hydrolysis is 10-30%;
the ZrO2The nanoparticles being acid-activated ZrO2Nanoparticles having a particle diameter of 1 to 200 nm;
the acid-activated ZrO2The preparation method of the nano-particles comprises the following steps: ZrO 2 is mixed with2Ultrasonically dispersing the nanoparticles in an acid solution with the pH value of 3-4, and activating for 1-10 min at the activation temperature of 10-50 ℃; the acid in the acid solution is at least one selected from hydrochloric acid, acetic acid, sulfuric acid and oxalic acid.
5. The production method according to claim 4, wherein the ZrO2The particle size of the nanoparticles is 10-100 nm.
6. A nanoparticle-crosslinked polymer oil-displacing agent prepared by the preparation method of claim 4 or 5.
7. Use of a nanoparticle crosslinked polymer oil-displacing agent of claim 6.
8. Use according to claim 7, wherein the polyacrylamide solution and ZrO2The nanoparticle solution is mixed and then injected, or mixed during the injection process.
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纳米t-ZrO2的制备及交联胍胶压裂液的研究;李治鹏;杨洋;谷卓然;陈奇;叶世贵;卢宏涛;《石油化工》;20191115;第48卷(第11期);第1151-1156页 *

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