CN110305651A - A kind of polymer oil-displacing agent and its preparation method and application of nanoparticle crosslinking - Google Patents
A kind of polymer oil-displacing agent and its preparation method and application of nanoparticle crosslinking Download PDFInfo
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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 oil field development technical fields, specifically provide a kind of polymer oil-displacing agent and its preparation method and application of nanoparticle crosslinking, which includes polyacrylamide, ZrO2Nanoparticle and water, wherein the concentration of the polyacrylamide is 90~3000mg/L, the ZrO2The concentration of nanoparticle is 0.001~1mg/L.The polymer oil-displacing agent selects the nanometer ZrO of activation2As crosslinking agent, is conducive to control the intermolecular cross-linking reaction of polymer generation, improves the efficiency of cross-linking reaction, to reduce the dosage of crosslinking agent, increase the viscosity of polymer solution, achieve the purpose that improve oil recovery factor.
Description
Technical field
The invention belongs to oil field development technical fields, and in particular to a kind of polymer oil-displacing agent of nanoparticle crosslinking and its
The application of preparation method and the polymer oil-displacing agent of nanoparticle crosslinking.
Background technique
Major part oil field in China's is in mid-later development phase at present, and moisture content rises rapidly, and even as high as 90% or more, it is existing
Water injection technology be difficult to meet the needs in oil field.It improves oil recovery factor mainly to realize in terms of two: on the one hand mention
Sweep efficiency of the height injection fluid in oil reservoir, main method are the heterogeneity for improving oil reservoir or the stream for reducing displacing phase
Degree, stable displacement forward position generally take profile control or the viscosity by increasing displacement fluid to realize；It is exactly on the other hand
Displacement efficiency is improved, main method is the wetability for changing rock surface and the adverse effect for reducing capillarity, is reduced
Residual oil saturation usually reduces oil water interfacial tension using surfactant to realize.In recent years, technique of polymer flooding
It has become China and improves the perfect practical technique of oil recovery comparative maturity, mining site pilot test succeeds mostly, grand celebration
Oil field has entered the large area industrial application stage, and middle petrochemical industry Shengli Oil Field, Henan Oil Field also all carried out polymer
Technical research is driven, and obtains good effect in mining site.
Polymer flooding is the mostly important technology of chemical flooding, by the way that water-soluble polymer is added in injection water, increases and drives
For phase viscosity, oil and water mobility ratio is adjusted, expands displacing phase swept volume, enhances displacement efficiency, oil displacement efficiency can be greatly improved.
Polymer flooding is easy to operate, and cost is relatively low, can be used in combination with profile-controlling and plugging agent, has both certain permeability and adjusts and makees
With.As synthesis class water soluble polymer, the synthesis quasi polymer based on polyacrylamide and its derivative is current chemical flooding
In it is most widely used, obtain effect polymer oil-displacing agent the most outstanding.It divides, and can divide according to the structure of polyacrylamide
For linear polyacrylamide and crosslinked polyacrylamide.The linear polyacrylamide (HPAM) of partial hydrolysis makes as oil displacement agent
The increase swept volume played the role of with its viscosity for increasing aqueous solution is mainly based upon, improves mobility ratio.Linear polypropylene
Undesirable temperature-resistant anti-salt performance of amide solution etc. is the technical bottleneck that it is applied in high-temperature oil reservoir and postpolymerflooded reservoirs, sternly
Important place affects its practical effect.
Crosslinked polyacrylamide mostly uses greatly ground in-situ crosslinking method, and crosslinking agent is generally Organic Chromium, organo-aluminium, has
Machine zirconium, water soluble phenol resin etc., using crosslinking agent and line style HPAM underground crosslinked and formed.Crosslinked polyacrylamide can
Make profile-controlling and plugging agent and oil displacement agent uses, because its good swollen property of body can carry out profile control processing to high permeability formation to adjust its infiltration
Rate.But fully crosslinked polyacrylamide, due to degree of cross linking height, hardness is big, and morphotropism is poor, migrates in hole difficult, it is difficult
Use to play the role of oil displacement agent, therefore in tertiary oil recovery is restricted.As oil displacement agent in use, requiring polymer
Suspension possesses preferable migration ability, and the viscoelastic property for passing through, while having excellent can be deformed in hole, can be effective
Ground increases the viscosity of displacing phase, improves its mobility ratio.
Patent document CN93115276.3 discloses one kind using polyacrylamide (or xanthan gum) as gelatinizing agent, with lactic acid
Chromium is the cross-linked polymer oil-displacing agent of crosslinking agent preparation, and polymer is become cross-linked polymer using crosslinking agent Chromic lactate, from
And solving the problems, such as polymer salt tolerance difference and vulnerable to mechanical shearing, the concentration of polyacrylamide solution is most in the patent document
It is well 800~8000mg/L, the shortcomings that dosage of crosslinking agent Chromic lactate is preferably 300~3000mg/L, the technical solution are as follows: because
Intramolecular crosslinking reaction occurs to will lead to number of polymers using small molecule crosslinking agent, the usage amount of crosslinking agent is bigger.Specially
Sharp document CN97104045.1, which is disclosed, replaces polypropylene segment using crosslinking agent aluminium citrate in polymer displacement of reservoir oil tech
Amide reduces the usage amount of polyacrylamide, to reduce note in the case where guaranteeing that injection viscosity does not reduce simultaneously appropriate increased situation
Enter cost, but injects viscosity and improve few, only raising 0~25%.Patent document CN201510484051.0 provides one kind
Tertiary amine participates in the crosslinking polymer oil displacement agent of synthesis, and acrylamide is used as function using pentamethyl-diethylenetriamine (PMTDA)
Energy monomer and crosslinking agent, potassium sulfate-sodium hydrogensulfite are prepared partial cross-linked and contain a large amount of branched structures as initiation system
Polymer oil-displacing agent.
Summary of the invention
The deficiency of number of polymers intramolecular crosslinking reaction is generated for small molecule crosslinking agent in the prior art, it is of the invention
Purpose is to provide the polymer of polymer oil-displacing agent of a kind of nanoparticle crosslinking and preparation method thereof and nanoparticle crosslinking
The nanometer ZrO of activation is selected in the application of oil displacement agent2As crosslinking agent, be conducive to control the intermolecular crosslinking of polymer generation instead
It answers, improves the efficiency of cross-linking reaction, to reduce the dosage of crosslinking agent, increase the viscosity of polymer solution, reach raising crude oil
The purpose of recovery ratio.
The first aspect of the present invention provides a kind of polymer oil-displacing agent of nanoparticle crosslinking, the polymer oil-displacing agent packet
Containing polyacrylamide, ZrO2Nanoparticle and water, wherein the concentration of the polyacrylamide is 90~3000mg/L, the ZrO2
The concentration of nanoparticle is 0.001~1mg/L.
The second aspect of the present invention provides a kind of preparation method of the polymer oil-displacing agent of nanoparticle crosslinking, the system
Preparation Method includes:
1) polyacrylamide is configured to the solution that concentration is 100~3000mg/L；
2) by ZrO2Nanoparticle is configured to the solution that concentration is 1~100mg/L；
3) solution made from step 1) and step 2) is mixed according to 100~1000: 1 volume ratio, obtains the polymerization
Object oil displacement agent.
The third aspect of the present invention provides a kind of polymer displacement of reservoir oil of the crosslinking of nanoparticle made from above-mentioned preparation method
Agent.
The fourth aspect of the present invention provides the application of the polymer oil-displacing agent of above-mentioned nanoparticle crosslinking, it is preferable that
Polyacrylamide solution and ZrO2It injects after nano-particle solution mixing, or is mixed in injection process.
Polymer oil-displacing agent of the invention is handled by adding a small amount of acid activation of passing through in polyacrylamide solution
ZrO2Nanoparticle is as inorganic crosslinking agent, the ZrO of appropriate particle size2Nanoparticle crosslinker and polymer molecule in solution are big
It is small quite, be conducive to polyacrylamide and carry out intermolecular cross-linking, improves the efficiency being effectively crosslinked, ZrO2Nanoparticle is without carrying out
Special organic group modification, can be used as crosslinking agent, increases the viscosity of polymer solution, is conducive to polymer flooding and improves petroleum
Recovery ratio.The viscosity of cross-linked polymer solution is 20~85mPas, viscosity after aging in 1~10 day is 30~
184mPas increases by 2~11 times than initial polymer viscosity.
Other features and advantages of the present invention will then part of the detailed description can be specified.
Specific embodiment
To keep the present invention easier to understand, below in conjunction with embodiment, the present invention will be described in detail, these embodiment party
Formula only serves illustrative, is not intended to restrict the invention.
The first aspect of the present invention provides a kind of polymer oil-displacing agent of nanoparticle crosslinking, the polymer oil-displacing agent packet
Containing polyacrylamide, ZrO2Nanoparticle and water, wherein the concentration of the polyacrylamide is 90~3000mg/L, the ZrO2
The concentration of nanoparticle is 0.001~1mg/L.
Under preferable case, the concentration of the polyacrylamide is 750~3000mg/L, the ZrO2The concentration of nanoparticle
For 0.02~1mg/L.
In the present invention, the ZrO2Nanoparticle is the ZrO of acid activation2Nanoparticle.The ZrO of acid activation2Nanoparticle is
By ZrO2Nanoparticle activates under the conditions of Low acid to be made, and preparation method includes: by ZrO2Nanoparticle ultrasonic disperse is in pH
1~10min is activated in=3~4 acid solution, activation temperature is 10~50 DEG C.
According to the present invention, it can be selected from least one in hydrochloric acid, acetic acid, sulfuric acid and oxalic acid for the acid in the acid solution of activation
Kind.
In the present invention, the ZrO2The partial size of nanoparticle can be 1~200nm, preferably 10~100nm.
According to the present invention, the polyacrylamide be partially hydrolyzed polyacrylamide (PHPA), molecular weight ranges be 5~20 ×
106, degree of hydrolysis is 10~30%.
The second aspect of the present invention provides a kind of preparation method of the polymer oil-displacing agent of nanoparticle crosslinking, the system
Preparation Method includes:
1) polyacrylamide is configured to the solution that concentration is 100~3000mg/L；
2) by ZrO2Nanoparticle is configured to the solution that concentration is 1~100mg/L；
3) solution made from step 1) and step 2) is mixed according to 100~1000: 1 volume ratio, obtains the polymerization
Object oil displacement agent.
In the present invention, the polyacrylamide is partially hydrolyzed polyacrylamide (PHPA), and molecular weight ranges are 5~20 × 106,
Degree of hydrolysis is 10~30%.Polyacrylamide is configured to aqueous solution as gelatinizing agent, preferably feelings under agitation under room temperature
Under condition, the compound concentration of polyacrylamide is the solution of 800~3000mg/L.
According to the present invention, the ZrO2Nanoparticle is the ZrO of acid activation2Nanoparticle, partial size can be 1~200nm,
Preferably 10~100nm.
The ZrO of acid activation2Nanoparticle is by the ZrO of nanoscale2Particle activates under the conditions of Low acid, acid activation item
Part can refer to this field and carry out conventional selection.Under preferable case, the ZrO of the acid activation2The preparation method of nanoparticle includes:
By ZrO2Nanoparticle ultrasonic disperse activates 1~10min in the acid solution of pH=3~4, and activation temperature is 10~50 DEG C；Acid
Acid in solution is selected from least one of hydrochloric acid, acetic acid, sulfuric acid and oxalic acid.
By the ZrO of activation2Nanoparticle is configured to solution as crosslinking agent, meets the ZrO of concentration2Nanoparticle activating solution
Can be spare directly as cross-linking agent solution, activating solution can also be centrifuged, the ZrO activated2Nano particles by using deionized water
After washing, redisperse is used as cross-linking agent solution spare in deionized water.
The third aspect of the present invention provides a kind of polymer displacement of reservoir oil of the crosslinking of nanoparticle made from above-mentioned preparation method
Agent.
The fourth aspect of the present invention provides the application of the polymer oil-displacing agent of above-mentioned nanoparticle crosslinking.
Preferably, the gelatinizing agent (polyacrylamide solution) and crosslinking agent (ZrO of polymer oil-displacing agent are constituted2Nanoparticle
Solution) can mix after reinject, can also be mixed in injection process.When mixing gelatinizing agent and crosslinking agent in the ban, mixing side
Formula is preferred are as follows: in prepared a certain concentration polymer (polyacrylamide) solution, respective concentration is added under agitation
Crosslinking agent (ZrO2Nanoparticle) solution, it is stirred for after mixing 1~20 minute, is ready for injecting.When in injection process
When mixing: prepared a certain concentration polymer solution and the cross-linking agent solution of respective concentration inject simultaneously respectively, are injecting
Automatic mixed stirring gelatinizing agent and crosslinking agent in journey.No matter which kind of hybrid mode is used, preferred polymers solution and crosslinking agent are molten
The volume ratio of liquid is 100: 1~200: 1.
The present invention is described in detail by the following examples.
In embodiment and comparative example below:
The viscosity of cross-linking system uses Brookfield viscosimeter, at 40~70 DEG C of temperature, the item of shear rate 6r/min
It is measured under part.
Rock core used in rock core displacement test be Berea sandstone, a length of 10cm, internal diameter 2.5cm, permeability 500mD,
Pore volume is 45mL, and entire displacement test carries out in digital temperature-controlled box, and fluid injection rate is 0.5mL/min, experiment temperature
Degree is 60 DEG C.
Embodiment 1-5 is used to illustrate the polymer oil-displacing agent of nanoparticle crosslinking of the invention.
Embodiment 1
Polyacrylamide is configured to the solution of 1000mg/L first, the ZrO for being then 20nm by partial size2Particle ultrasound point
It is dispersed in the oxalic acid solution of pH=3 and activates 5 minutes, activation temperature is 30 DEG C, using centrifugation, after deionized water washing, dispersion
It is spare as cross-linking agent solution in deionized water, particle concentration 10mg/L.It takes 200mL polymer solution to make gelatinizing agent, adds
After entering 1mL cross-linking agent solution, stirring at 60 DEG C and measuring the viscosity of cross-linked polymer solution after ten minutes is 23mPas, by 3
It is 38mPas that its viscosity is surveyed after its aging.Rock core displacement test is the result shows that oil recovery factor can be improved in this cross-linking system
8.3%.
Embodiment 2
Polyacrylamide is configured to the solution of 3000mg/L first, the ZrO for being then 50nm by partial size2Particle ultrasound point
It is dispersed in the sulfuric acid solution of pH=3 and activates 5 minutes, activation temperature is 10 DEG C, using centrifugation, after deionized water washing, dispersion
It is spare as cross-linking agent solution in deionized water, particle concentration 100mg/L.It takes 100mL polymer solution to make gelatinizing agent, adds
After entering 1mL cross-linking agent solution, stirring at 60 DEG C and measuring the viscosity of cross-linked polymer solution after ten minutes is 85mPas, by 3
It is 184mPas that its viscosity is surveyed after its aging.Rock core displacement test is the result shows that oil recovery factor can be improved in this cross-linking system
23%.
Embodiment 3
Polyacrylamide is configured to the solution of 1000mg/L first, the ZrO for being then 10nm by partial size2Particle ultrasound point
It is dispersed in the acetum of pH=3 and activates 10 minutes, activation temperature is 40 DEG C, using centrifugation, after deionized water washing, dispersion
It is spare as cross-linking agent solution in deionized water, particle concentration 20mg/L.It takes 500mL polymer solution to make gelatinizing agent, adds
After entering 5mL cross-linking agent solution, stirring at 60 DEG C and measuring the viscosity of cross-linked polymer solution after ten minutes is 56mPas, by 2
It is 63mPas that its viscosity is surveyed after its aging.Rock core displacement test is the result shows that oil recovery factor can be improved in this cross-linking system
15%.
Embodiment 4
Polyacrylamide is configured to the solution of 800mg/L first, the ZrO for being then 100nm by partial size2Particle ultrasound point
It is dispersed in the sulfuric acid solution of pH=3 and activates 5 minutes, activation temperature is 20 DEG C, using centrifugation, after deionized water washing, dispersion
It is spare as cross-linking agent solution in deionized water, particle concentration 100mg/L.1000mL polymer solution is taken to make gelatinizing agent,
After 5mL cross-linking agent solution is added, stirring at 60 DEG C and measuring the viscosity of cross-linked polymer solution after ten minutes is 32mPas, is passed through
It is 30mPas that its viscosity is surveyed after aging in 3 days.Rock core displacement test is the result shows that oil recovery factor can be improved in this cross-linking system
11%.
Embodiment 5
Polyacrylamide is configured to the solution of 2000mg/L first, the ZrO for being then 20nm by partial size2Particle ultrasound point
It is dispersed in the acetum of pH=4 and activates 5 minutes, activation temperature is 30 DEG C, particle concentration 2mg/L.By gelatinizing agent and crosslinking
Two kinds of solution of agent are 100: 1 while injecting the polymer flooding experiment after carrying out water drive by volume, automatic in injection process
Gelatinizing agent and crosslinking agent is mixed, the results showed that oil recovery factor 12% can be improved in this cross-linking system.
Comparative example 1~3
Under conditions of temperature 60 C, shear rate 6r/min, following poly- third is measured respectively with Brookfield viscosimeter
The viscosity of acrylamide solution.
The viscosity of 1000mg/L polyacrylamide solution is 8.2mPas.
The viscosity of 3000mg/L polyacrylamide solution is 29mPas.
The viscosity of 800mg/L polyacrylamide solution is 7.6mPas.
By the data of embodiment and comparative example it is found that ZrO2The addition of nanoparticle is conducive to control polyacrylamide generation
Intermolecular cross-linking reaction, improves the efficiency of cross-linking reaction, to reduce the dosage of crosslinking agent, increases the viscous of polymer solution
Degree achievees the purpose that raising oil recovery factor, and the viscosity of cross-linking system increases by 2~11 times than initial polymer viscosity, and interior is poly-
It closes object displacement test and improves recovery ratio 6~29%.
The embodiment of the present invention is described above, above description is exemplary, and non-exclusive, and also not
It is limited to disclosed embodiment.Without departing from the scope and spirit of illustrated embodiment, for the art
Many modifications and changes are obvious for those of ordinary skill.
Claims (10)
1. a kind of polymer oil-displacing agent of nanoparticle crosslinking, which is characterized in that the polymer oil-displacing agent include polyacrylamide,
ZrO2Nanoparticle and water, wherein the concentration of the polyacrylamide is 90~3000mg/L, the ZrO2Nanoparticle it is dense
Degree is 0.001~1mg/L.
2. polymer oil-displacing agent according to claim 1, wherein the concentration of the polyacrylamide is 750~3000mg/
L, the ZrO2The concentration of nanoparticle is 0.02~1mg/L.
3. polymer oil-displacing agent according to claim 1, wherein the ZrO2Nanoparticle is the ZrO of acid activation2Nanometer
Particle, partial size are 1~200nm, preferably 10~100nm.
4. polymer oil-displacing agent according to claim 3, wherein the ZrO of the acid activation2The preparation method of nanoparticle
It include: by ZrO2Nanoparticle ultrasonic disperse activates 1~10min in the acid solution of pH=3~4, and activation temperature is 10~50
DEG C, the acid in acid solution is selected from least one of hydrochloric acid, acetic acid, sulfuric acid and oxalic acid.
5. polymer oil-displacing agent according to claim 1, wherein the polyacrylamide is partial hydrolysis polyacrylamide
Amine, molecular weight ranges are 5~20 × 106, degree of hydrolysis is 10~30%.
6. a kind of preparation method of the polymer oil-displacing agent of nanoparticle crosslinking, which is characterized in that the preparation method includes:
1) polyacrylamide is configured to the solution that concentration is 100~3000mg/L；
2) by ZrO2Nanoparticle is configured to the solution that concentration is 1~100mg/L；
3) solution made from step 1) and step 2) is mixed according to 100~1000: 1 volume ratio, obtains the polymer
Oil displacement agent.
7. preparation method according to claim 6, wherein the polyacrylamide is partially hydrolyzed polyacrylamide (PHPA),
Molecular weight ranges are 5~20 × 106, degree of hydrolysis is 10~30%；.
8. preparation method according to claim 6, wherein the ZrO2Nanoparticle is the ZrO of acid activation2Nanoparticle,
Its partial size is 1~200nm, preferably 10~100nm；
Preferably, the ZrO of the acid activation2The preparation method of nanoparticle includes: by ZrO2Nanoparticle ultrasonic disperse is in pH=
1~10min is activated in 3~4 acid solution, activation temperature is 10~50 DEG C；Acid in acid solution is selected from hydrochloric acid, acetic acid, sulfuric acid
At least one of with oxalic acid.
9. a kind of polymer displacement of reservoir oil of the crosslinking of nanoparticle made from preparation method as described in any one of claim 6-8
Agent.
10. the application of the polymer oil-displacing agent of nanoparticle crosslinking as claimed in claim 9, it is preferable that polyacrylamide solution
And ZrO2It injects after nano-particle solution mixing, or is mixed in injection process.
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| CN114058342A (en) * | 2020-08-05 | 2022-02-18 | 中国石油化工股份有限公司 | Modified graphene oxide nanosheet tackifier, polymer system for oil displacement, application of polymer system and oil reservoir oil displacement method |
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| 李治鹏;杨洋;谷卓然;陈奇;叶世贵;卢宏涛: "纳米t-ZrO2的制备及交联胍胶压裂液的研究", 《石油化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114058342A (en) * | 2020-08-05 | 2022-02-18 | 中国石油化工股份有限公司 | Modified graphene oxide nanosheet tackifier, polymer system for oil displacement, application of polymer system and oil reservoir oil displacement method |
| CN114058342B (en) * | 2020-08-05 | 2023-05-23 | 中国石油化工股份有限公司 | Modified graphene oxide nano-sheet adhesion promoter, polymer system for oil displacement, application and oil reservoir oil displacement method |
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