CN105273145B - A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof - Google Patents
A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof Download PDFInfo
- Publication number
- CN105273145B CN105273145B CN201410643122.2A CN201410643122A CN105273145B CN 105273145 B CN105273145 B CN 105273145B CN 201410643122 A CN201410643122 A CN 201410643122A CN 105273145 B CN105273145 B CN 105273145B
- Authority
- CN
- China
- Prior art keywords
- water
- parts
- dissolved
- solution
- control agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention provides a kind of new weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof.The profile control agent is triggered by acrylamide monomer and compound crosslinking system through initiator to be polymerized.Its preparation method is：100 parts of acrylamides are dissolved in wiring solution-forming in 200 ~ 250 parts of water, 0.2 ~ 0.5 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in wiring solution-forming in 30 ~ 50 parts of water, 0.0002 ~ 0.001 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 20 ~ 40 parts of water, sequentially add in three-necked bottle, be placed in 10 DEG C ~ 15 DEG C of water-bath；0.01 0.03 parts of ammonium persulfates are dissolved in the solution being made into 30 ~ 50 parts of water and add three-necked bottle by logical nitrogen after 30 minutes.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 70 ~ 85 DEG C of water-baths and is incubated 2 ~ 6 hours, afterwards takes out gel by reaction after terminating, and shreds, drying, crushing, can obtain powdery product after screening.
Description
Technical field
The present invention relates to technical field of tertiary oil recovery, more particularly to a kind of weak cross-linked particles for improving oil recovery to adjust
Drive agent and preparation method thereof.
Background technology
Major part oil field in China's has been enter into the middle and later periods of secondary recovery at present, by long-term waterflooding extraction, reservoir geology
Become complicated, anisotropism is further serious, and oil well is average aqueous up to more than 80%, imply that China's main oilfield has been enter into middle height
Water-cut Period, oil saturation have substantially reduced.Therefore it is difficult to the 60- for producing underground residual by conventional increasing yield and injection measure
70% crude oil, production technique difficulty is increasing, and economic benefit is worse and worse, and tertiary oil recovery technology, which turns into, improves oil
The important means of recovery ratio.Linear polyacrylamide solution is widely used due to its unique viscoplasticity in tertiary oil recovery.
But under high temperature and high salt and the reservoir condition of serious heterogeneity, linear polyacrylamide aging is serious, and viscosity drastically declines, right
The bad adaptability of inhomogeneous formation, it is difficult to meet the requirement for improving recovery ratio；Furthermore it is possible to effectively adjust heterogeneous reservoir infiltration
The profile-controlling and plugging agent of rate, because the degree of cross linking is high, hardness is big, and morphotropism is poor, is migrated in hole difficult, it is impossible to play oil displacement agent
Effect.
Linear polyacrylamide and its polymer-modified facing challenges, patent CN101775275 disclose viscoelastic
Property particle oil displacement agent and preparation method thereof, using dimethylaminoethyl methacrylate as function monomer coordinate potassium peroxydisulfate-
Sodium hydrogensulfite trigger system, it is synthetically prepared go out it is partial cross-linked and containing a large amount of branched structures polyacrylamide viscoelastic particle
Oil displacement agent.Its part branched moiety cross-linked structure can effectively improve it while its aqueous dispersion system viscosity is not reduced
Modulus of elasticity, and long-term anti-ageing performance of the polyacrylamide in high temperature and high salt environment can be improved.
The application is compared with aforementioned patent CN101775275, introducing crosslinked agent polyethyleneglycol diacrylate, with methyl-prop
Olefin(e) acid diformazan ammonia ethyl ester forms compound crosslinking system, and formation cross-linked network structure is finer and close, and ageing-resistant performance improves, synthesis
Profile control agent granule strength increases, the achievable fluid diversion in porous media, less permeable layer in big great development, under a certain pressure
Deformable flowing again, realizes oil displacement efficiency.
The content of the invention
It is an object of the invention to provide a kind of weak cross-linked particles profile control agent and preparation method thereof, this profile control agent has profile control concurrently
Double effects with the displacement of reservoir oil are improving oil recovery.
In order to reach one of above-mentioned purpose, the present invention adopts the technical scheme that：
A kind of weak cross-linked particles profile control agent for improving oil recovery, it is by acrylamide monomer and compound crosslinking system warp
Initiator triggers the ter-polymers being polymerized, and the profile control agent structural formula is：
Wherein, n=14；A in above formula, b, c, d represent the degree of polymerization, using acrylamide quality as 100 parts of calculating, methyl-prop
Olefin(e) acid diformazan ammonia ethyl ester is 0.2~0.5 part, and polyethyleneglycol diacrylate is 0.0002~0.001 part.
The compound crosslinking system is dimethylaminoethyl acrylate methyl ammonia ethyl ester and polyethyleneglycol diacrylate.
One of the object of the invention can also be realized by following measure：
The initiator is ammonium persulfate；
Each reactive component parts by weight of the weak cross-linked particles profile control agent are：
In order to reach the two of above-mentioned purpose, the technical scheme that the present invention takes is：
The synthetic method of above-mentioned ter-polymers profile control agent, comprises the following steps：
100 parts of acrylamides are dissolved in wiring solution-forming in 200~250 parts of water, 0.2~0.5 part of dimethylaminoethyl acrylate methyl ammonia
Ethyl ester is dissolved in wiring solution-forming in 30~50 parts of water, and 0.0002~0.001 part of polyethyleneglycol diacrylate is dissolved in 20~40 parts of water
Middle wiring solution-forming, is sequentially added in three-necked bottle, is placed in 10 DEG C~15 DEG C of water-bath；Logical nitrogen is after 30 minutes, by 0.01-
0.03 part of ammonium persulfate is dissolved in the solution being made into 30~50 parts of water and adds three-necked bottle.The temperature rise of question response solution stops after being more than 1 DEG C
Only lead to nitrogen, three-necked bottle is put into 70~85 DEG C of water-baths and is incubated 2~6 hours, afterwards takes out gel, cut by reaction after terminating
Powdery product is can obtain after broken, drying, crushing, screening.
The weak cross-linked particles profile control agent of the present invention, introducing crosslinked agent polyethyleneglycol diacrylate, with dimethylaminoethyl acrylate methyl
Ammonia ethyl ester forms compound crosslinking system, and formation cross-linked network structure is finer and close, and ageing-resistant performance improves, the profile control agent of synthesis
Grain intensity increase, both can adjust heterogeneous reservoir, the achievable fluid diversion in porous media, less permeable layer in big great development,
Deformable flowing again under a certain pressure, realizes oil displacement efficiency.Therefore the profile control agent is in postpolymerflooded reservoirs, high water-cut reservoir
And high permeable cement has a wide range of applications.The inventive method synthetic route is reasonable, and synthetic method is simple, and raw material is cheap
It is easy to get, there are important promotion and application to be worth.
Brief description of the drawings
Fig. 1 show rock core seepage apparatus schematic diagram；
Fig. 2 is suspension that particle profile control agent of the present invention is formed in salinity is 19334mg/L salt solution in fill out sand tube
Injection pressure change；
Fig. 3 show two-tube rock core parallel laboratory test schematic diagram；
Fig. 4 is the two-tube parallel laboratory test fractional flow curves of a specific embodiment of the invention.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but is not intended to limit the protection model of the present invention
Enclose.
Embodiment 1：
25 parts of acrylamides are dissolved in wiring solution-forming in 62 parts of water, 0.05 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in 8 parts
Wiring solution-forming in water, 0.00025 part of polyethyleneglycol diacrylate are dissolved in wiring solution-forming in 5 parts of water, sequentially added in three-necked bottle,
It is placed in 15 DEG C of water-bath；0.0025 part of ammonium persulfate is dissolved in the solution being made into 12 parts of water and added by logical nitrogen after 30 minutes
Enter three-necked bottle.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 75 DEG C of water-baths by reaction after terminating
Insulation 4 hours, afterwards takes out gel, shreds, drying, crushing, can obtain powdery product after screening.
Embodiment 2：
50 parts of acrylamides are dissolved in wiring solution-forming in 100 parts of water, 0.15 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in 20
Wiring solution-forming in part water, 0.00025 part of polyethyleneglycol diacrylate are dissolved in wiring solution-forming in 15 parts of water, sequentially add three-necked bottle
In, it is placed in 12 DEG C of water-bath；0.01 part of ammonium persulfate is dissolved in the solution being made into 25 parts of water and added by logical nitrogen after 30 minutes
Enter three-necked bottle.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 70 DEG C of water-baths by reaction after terminating
Insulation 6 hours, afterwards takes out gel, shreds, drying, crushing, can obtain powdery product after screening.
Embodiment 3：
100 parts of acrylamides are dissolved in wiring solution-forming in 250 parts of water, 0.4 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in 40
Wiring solution-forming in part water, 0.0008 part of polyethyleneglycol diacrylate are dissolved in wiring solution-forming in 20 parts of water, sequentially add three-necked bottle
In, it is placed in 12 DEG C of water-bath；0.02 part of ammonium persulfate is dissolved in the solution being made into 30 parts of water and added by logical nitrogen after 30 minutes
Enter three-necked bottle.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 80 DEG C of water-baths by reaction after terminating
Insulation 3 hours, afterwards takes out gel, shreds, drying, crushing, can obtain powdery product after screening.
Embodiment 4：
200 parts of acrylamides are dissolved in wiring solution-forming in 400 parts of water, 1 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in 100 parts
Wiring solution-forming in water, 0.0004 part of polyethyleneglycol diacrylate are dissolved in wiring solution-forming in 80 parts of water, sequentially added in three-necked bottle,
It is placed in 10 DEG C of water-bath；0.06 part of ammonium persulfate is dissolved in the solution being made into 60 parts of water and added by logical nitrogen after 30 minutes
Three-necked bottle.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 85 DEG C of water-baths and protected by reaction after terminating
Temperature 2 hours, afterwards takes out gel, shreds, drying, crushing, can obtain powdery product after screening.
Embodiment 5
100 parts of acrylamides are dissolved in wiring solution-forming in 200 parts of water, 0.2 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in 30
Wiring solution-forming in part water, 0.0002 part of polyethyleneglycol diacrylate are dissolved in wiring solution-forming in 20 parts of water, sequentially add three-necked bottle
In, it is placed in 10 DEG C of water-bath；0.01 part of ammonium persulfate is dissolved in the solution being made into 30 parts of water and added by logical nitrogen after 30 minutes
Enter three-necked bottle.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 75 DEG C of water-baths by reaction after terminating
Insulation 5 hours, afterwards takes out gel, shreds, drying, crushing, can obtain powdery product after screening.
Embodiment 6
100 parts of acrylamides are dissolved in wiring solution-forming in 250 parts of water, 0.5 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester is dissolved in 50
Wiring solution-forming in part water, 0.001 part of polyethyleneglycol diacrylate are dissolved in wiring solution-forming in 40 parts of water, sequentially add three-necked bottle
In, it is placed in 15 DEG C of water-bath；0.03 part of ammonium persulfate is dissolved in the solution being made into 50 parts of water and added by logical nitrogen after 30 minutes
Enter three-necked bottle.The temperature rise of question response solution stops logical nitrogen after being more than 1 DEG C, three-necked bottle is put into 80 DEG C of water-baths by reaction after terminating
Insulation 3 hours, afterwards takes out gel, shreds, drying, crushing, can obtain powdery product after screening.
Embodiment 7：
The injectability of particle profile control agent of the present invention is evaluated using rock core seepage apparatus
Experimental procedure is as follows：By 0.2g 100-150 mesh profile control agent powder of the present invention, it is slowly added under magnetic stirring
100mL salinities are that mixing speed is set to 500r/min, mixing time 10-15min, obtains transfer drive in 19334mg/L salt solution
Agent suspension.
Fig. 1 show rock core seepage apparatus schematic diagram, by high-accuracy low speed compression pump, fluid reservoir, pressure gauge and fill out sand tube
Composition, to ensure that system is homogeneous during injecting suspension, uses magnetic stirrer fluid reservoir, rotating speed 200r/min.
Whole Seepage Experiment is carried out in digital temperature-controlled box, and fluid injection rate is 0.5mL/min, and experimental temperature is 70 DEG C.Experiment institute
Porous media is self-control fill out sand tube, and a length of 30cm, internal diameter 2.5cm, the permeability of fill out sand tube is (1500 ± 15) × 10- 3um2, pore volume (PV) is 50 ± 0.5cm3。
The salt solution for injecting that salinity is 19334mg/L first into fill out sand tube is tested, records inlet-pressure at regular intervals
Power；After pressure balance, change note 2000mg/L profile control agent suspension, time recording pressure, carried out after pressure balance follow-up
For water drive to balancing, test result is shown in Fig. 2.
As seen from the figure, the water drive stage, pressure change is smaller, quickly reaches poised state；Profile control agent suspension of the present invention drives
After beginning, pressure increases sharply, and shows the formation of plugging action, the permeability reduction of fill out sand tube；After pressure reaches maximum,
Pressure fluctuates, until balance.After sequent water flooding starts, partial particulate is rushed to open, and fill out sand tube permeability increase, pressure is also opened
Begin to decline.
The test shows that particle profile control agent of the present invention has excellent injectability in fill out sand tube.
Embodiment 8：
The heterogeneous ability of regulation oil reservoir of profile control agent of the present invention is evaluated using two-tube rock core parallel laboratory test
Experimental procedure is as follows：The preparation of profile control agent suspension is the same as embodiment 5.As shown in figure 3, high permeability and low-permeability
The permeability of fill out sand tube is respectively (1000 ± 10) × 10-3μm2(5000 ± 15) × 10-3μm2, total hole of two parallel seepage flow pipes
Gap volume is 101.6 ± 0.5cm3.Salt solution and suspension of the salinity for 19334mg/L are successively injected in a manner of closing note point and adopt
Liquid, injection rate 0.5mL/min, experimental temperature are 70 DEG C.It is 19334mg/L salt solution that experiment, which is initially injected 1PV salinities, it
Change note 1PV 2000mg/L profile control agent suspension afterwards, carry out sequent water flooding followed by.Time recording pressure becomes in experimentation
Change and the Liquid output of high and low permeability fill out sand tube, by analyzing fractional flow curves come comparative study profile control agent suspension of the present invention
The heterogeneous ability of regulation oil reservoir, test result is shown in Fig. 4.
As seen from the figure, when water drive balances, the shunt volume of hypertonic fill out sand tube and hypotonic fill out sand tube be respectively 83.5% and
16.5%, the ratio between the two is about 5:1, meet the ratio between the two permeability.After profile control agent suspension is injected, the stream of hypertonic fill out sand tube
Amount tapers into and hypotonic fill out sand tube flow becomes big, and obvious reversal development occurs in the shunt volume of high hyposmosis fill out sand tube, is referred to as
" fluid diversion ".After sequent water flooding starts, the shunt volume of hyposmosis fill out sand tube slowly declines and Thief zone fill out sand tube shunt volume is opened
Beginning increases, and after 2 PV, high hyposmosis fill out sand tube shunt volume is equal, then gradually recovers shunt volume level, i.e. profile control agent before poly- drive
Suspension persistently carries out profile control after sequent water flooding starts to fill out sand tube, and fluid diversion still maintains 2PV in the sequent water flooding stage
Time.
Claims (1)
- A kind of 1. weak cross-linked particles profile control agent for improving oil recovery, by acrylamide monomer and compound crosslinking system through triggering Agent, which triggers, to be polymerized, it is characterised in that the compound crosslinking system is dimethylaminoethyl acrylate methyl ammonia ethyl ester and polyethylene glycol two Acrylate, the initiator are ammonium persulfate, and the parts by weight of each component are：Acrylamide 100Dimethylaminoethyl acrylate methyl ammonia ethyl ester 0.2~0.5Polyethyleneglycol diacrylate 0.0002~0.001Ammonium persulfate 0.01~0.03Water 280~390；The weak cross-linked particles profile control agent of the raising oil recovery is made as follows：100 parts of acrylamides are dissolved in wiring solution-forming in 200~250 parts of water, 0.2~0.5 part of dimethylaminoethyl acrylate methyl ammonia ethyl ester Wiring solution-forming in 30~50 parts of water is dissolved in, 0.0002~0.001 part of polyethyleneglycol diacrylate, which is dissolved in 20~40 parts of water, matches somebody with somebody Into solution, sequentially add in three-necked bottle, be placed in 10 DEG C~15 DEG C of water-bath；Logical nitrogen is after 30 minutes, by 0.01~0.03 Part ammonium persulfate is dissolved in the solution being made into 30~50 parts of water and adds three-necked bottle, and the temperature rise of question response solution stops logical after being more than 1 DEG C Three-necked bottle is put into 70~85 DEG C of water-baths and is incubated 2~6 hours, afterwards takes out gel by nitrogen, reaction after terminating, shred, Powdery product is can obtain after drying, crushing, screening.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410643122.2A CN105273145B (en) | 2014-11-07 | 2014-11-07 | A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410643122.2A CN105273145B (en) | 2014-11-07 | 2014-11-07 | A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105273145A CN105273145A (en) | 2016-01-27 |
| CN105273145B true CN105273145B (en) | 2017-11-17 |
Family
ID=55143033
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410643122.2A Active CN105273145B (en) | 2014-11-07 | 2014-11-07 | A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105273145B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009131937A2 (en) * | 2008-04-21 | 2009-10-29 | Nalco Company | Composition and method for recovering hydrocarbon fluids from a subterranean reservoir |
| CN101775275A (en) * | 2010-01-18 | 2010-07-14 | 四川大学 | Novel viscoelastic particle oil displacement agent and preparation method thereof |
| CN102304200A (en) * | 2011-05-27 | 2012-01-04 | 中国海洋石油总公司 | Crosslinked polymer microspheres and preparation method thereof |
| CN102408518A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Microcrosslinking polymer for oil displacement and preparation method thereof |
| CN102585093A (en) * | 2012-02-24 | 2012-07-18 | 中国石油天然气股份有限公司 | Pre-crosslinked gel particles for profile control and polymer flooding, and preparation method and application thereof |
-
2014
- 2014-11-07 CN CN201410643122.2A patent/CN105273145B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009131937A2 (en) * | 2008-04-21 | 2009-10-29 | Nalco Company | Composition and method for recovering hydrocarbon fluids from a subterranean reservoir |
| CN101775275A (en) * | 2010-01-18 | 2010-07-14 | 四川大学 | Novel viscoelastic particle oil displacement agent and preparation method thereof |
| CN102408518A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Microcrosslinking polymer for oil displacement and preparation method thereof |
| CN102304200A (en) * | 2011-05-27 | 2012-01-04 | 中国海洋石油总公司 | Crosslinked polymer microspheres and preparation method thereof |
| CN102585093A (en) * | 2012-02-24 | 2012-07-18 | 中国石油天然气股份有限公司 | Pre-crosslinked gel particles for profile control and polymer flooding, and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105273145A (en) | 2016-01-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11015109B2 (en) | Particulate profile control agent self-adaptive to size of formation pore throat and preparation method thereof | |
| CN104087275B (en) | A kind of high-temperature-resistant high-salt tiny gels granular profile control agent and its preparation method and application | |
| CN100543106C (en) | The preparation of composite cation blocking agent and stifled poly-using method | |
| CN103555305B (en) | Hyperbranched slow-swelling profile control particles and preparation method thereof | |
| CN103216211B (en) | Profile control method for fractured reservoir | |
| CN103184040B (en) | Stratum pre-crosslinked gel water shutoff agent | |
| CN103374342B (en) | A kind of oil field profile-controlling and plugging agent and oil field profile control and water shutoff method | |
| CN104371682A (en) | AA-AM-AMPS-DAC (acrylic acid-acrylamide-2-acrylamido-methylpropanesulfonic acid-acryloyloxyethyl ammonium chloride) polymer gel plugging agent and synthesis method thereof | |
| CN105112034B (en) | High-temperature-resistant gel diverting agent and preparation method and application thereof | |
| WO2020248309A1 (en) | Mine application method for increasing crude oil recovery rate by nano-micropheres in situ | |
| CN104610950A (en) | Suspended gel particle plugging agent and application thereof | |
| CN102952533A (en) | Composite cross-linked polymer weak gel oil displacement agent and preparation method thereof | |
| CN104371681A (en) | AA/AM/SSS underground cross-linked polymer gel plugging agent and preparation method thereof | |
| WO2014033233A1 (en) | Use of thermo-thickening polymers in the gas- and oilfield industry | |
| CN104098737A (en) | Heterogeneous nano-active oil-displacing agent and preparation method thereof | |
| CN103375153A (en) | Oil field profile control and water shutoff method | |
| CN103483497B (en) | A kind of physisorption type selective water shutoff agent and synthetic method thereof | |
| CN103484087B (en) | Viscoelasticity well cementation packer material | |
| CN105153361B (en) | A kind of part branched moiety cross-linked polymer oil-displacing agent and preparation method thereof | |
| CN105085798B (en) | A kind of partial cross-linked partially branched polymer oil displacement agent of dual-network and preparation method thereof | |
| CN112980407A (en) | Temperature-controllable gel plugging agent and preparation method and application thereof | |
| CA2791420C (en) | Methods and compositions for sand control in injection wells | |
| CN104100224A (en) | Oil well water plugging method | |
| CN105273145B (en) | A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof | |
| CN106753297A (en) | A kind of anti-salt type polymer gel profile control agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |