CN105273145A - Weak-crosslinking particle modifying and flooding agent capable of raising petroleum recovery efficiency and preparation method therefor - Google Patents

Weak-crosslinking particle modifying and flooding agent capable of raising petroleum recovery efficiency and preparation method therefor Download PDF

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CN105273145A
CN105273145A CN201410643122.2A CN201410643122A CN105273145A CN 105273145 A CN105273145 A CN 105273145A CN 201410643122 A CN201410643122 A CN 201410643122A CN 105273145 A CN105273145 A CN 105273145A
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water
parts
dissolved
solution
necked bottle
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CN105273145B (en
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李振泉
曹绪龙
姜祖明
宋新旺
陈晓彦
王红艳
刘煜
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China Petroleum and Chemical Corp
Sinopec Shengli Geological Scientific Reserch Institute
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China Petroleum and Chemical Corp
Sinopec Shengli Geological Scientific Reserch Institute
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Abstract

The invention provides a weak-crosslinking particle modifying and flooding agent capable of raising petroleum recovery efficiency and a preparation method therefor. The modifying and flooding agent is prepared from acrylamide monomers and a composite crosslinking system through polymerization under initiation of initiators. The preparation method is as follows: 100 parts of acrylamide is dissolved in 200-250 parts of water to prepare a solution, 0.2-0.5 part of 2-(dimethylamino)ethyl methacrylate is dissolved in 30-50 parts of water to prepare a solution, 0.0002-0.001 part of poly(ethylene glycol) diacrylate is dissolved in 20-40 parts of water to prepare a solution, the three solutions are added in a three-necked bottle in order, the three-necked bottle is placed in water-bath at a temperature of 10 DEG C-15 DEG C, after nitrogen is inputted for 30 min, 0.01-0.03 part of ammonium persulfate is dissolved in 30-50 parts of water to prepare a solution, and then the solution is added in the three-necked bottle. When the temperature rise of the reaction solution is more than 1 DEG C, nitrogen input is stopped, the three-necked bottle is placed in a water-bath kettle with a temperature of 70-85 DEG C after the reaction is finished, thermal insulation is carried out for 2-6h, then gel is taken out, the gel is cut, dried, crushed and screened, and a powdery product can be obtained.

Description

A kind of weak cross-linked particles adjusting driving agnet improving oil recovery and preparation method thereof
Technical field
The present invention relates to technical field of tertiary oil recovery, particularly relate to a kind of weak cross-linked particles adjusting driving agnet improving oil recovery and preparation method thereof.
Background technology
Current China's major part oil field has entered the middle and later periods of secondary recovery, and through long-term waterflooding, reservoir geology becomes complicated, nonuniformity is further serious, oil well is on average moisture reaches more than 80%, and imply that China's main oilfield enters high water cut rate, oil saturation reduces greatly.Therefore rely on conventional increasing yield and injection measure to be difficult to exploit out the crude oil of the 60-70% that underground remains, production technique difficulty is increasing, and economic benefit worse and worse, and tertiary oil recovery technology becomes the important means improving oil recovery.Linear polyacrylamide solution, due to the visco-elasticity of its uniqueness, is widely used in tertiary oil recovery.But under the reservoir condition of high temperature and high salt and serious heterogeneity, linear polyacrylamide is seriously aging, and viscosity sharply declines, to the bad adaptability of inhomogeneous formation, be difficult to meet the requirement improving recovery ratio; In addition, effectively can regulate the profile-controlling and plugging agent of heterogeneous reservoir rate of permeation, because degree of crosslinking is high, hardness is large, and deformability is poor, and in hole, migration difficulty, can not play the effect of oil-displacing agent.
Linear polyacrylamide and polymer-modified facing challenges thereof, patent CN101775275 discloses viscoelastic particle oil displacement agent and preparation method thereof, adopt dimethylaminoethyl methacrylate to coordinate Potassium Persulphate-sodium bisulfite initiator system as function monomer, partial cross-linked and containing a large amount of branched structure polyacrylamide viscoelastic particle oil displacement agent is prepared in synthesis.Its part branched moiety crosslinking structure while not reducing its aqueous dispersion system viscosity, effectively can improve its Young's modulus, and can improve the resisting ageing for long time performance of polyacrylamide in high temperature and high salt environment.
The application is compared with aforementioned patent CN101775275, introduce linking agent polyethyleneglycol diacrylate, compound crosslinking system is formed with dimethylaminoethyl acrylate methyl ammonia ethyl ester, form cross-linked network structure finer and close, ageing-resistant performance improves, and the adjusting driving agnet granule strength of synthesis increases, fluid diversion can be realized in porous medium, low permeability layer in large great development, deformable flowing again, realizes oil displacement efficiency under a certain pressure.
Summary of the invention
The object of this invention is to provide a kind of weak cross-linked particles adjusting driving agnet and preparation method thereof, this adjusting driving agnet has the double effects of profile control and the displacement of reservoir oil concurrently in order to improve oil recovery.
In order to reach one of above-mentioned purpose, the technical scheme that the present invention takes is:
Improving a weak cross-linked particles adjusting driving agnet for oil recovery, is that this adjusting driving agnet structural formula is by acrylamide monomer and the compound crosslinking system ter-polymers through initiator initiated polymerization:
Wherein, n=14; A in above formula, b, c, d represent the polymerization degree, and be 100 parts of calculating with acrylamide quality, dimethylaminoethyl acrylate methyl ammonia ethyl ester is 0.2 ~ 0.5 part, and polyethyleneglycol diacrylate is 0.0002 ~ 0.001 part.
Described compound crosslinking system is dimethylaminoethyl acrylate methyl ammonia ethyl ester and polyethyleneglycol diacrylate.
One of the object of the invention also realizes by following measure:
Described initiator is ammonium persulphate;
Each reactive component weight part of described weak cross-linked particles adjusting driving agnet is:
In order to reach above-mentioned purpose two, the technical scheme that the present invention takes is:
The synthetic method of above-mentioned ter-polymers adjusting driving agnet, comprises the 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, 0.0002 ~ 0.001 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 20 ~ 40 parts of water, add in three-necked bottle successively, and be placed in the water-bath of 10 DEG C ~ 15 DEG C; 0.01-0.03 part ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 30 ~ 50 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 70 ~ 85 DEG C of water-baths insulations 2 ~ 6 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
The weak cross-linked particles adjusting driving agnet of the present invention, introduce linking agent polyethyleneglycol diacrylate, form compound crosslinking system with dimethylaminoethyl acrylate methyl ammonia ethyl ester, form cross-linked network structure finer and close, ageing-resistant performance improves, the adjusting driving agnet granule strength of synthesis increases, both adjustable heterogeneous reservoir, can realize fluid diversion in porous medium, low permeability layer in large great development, deformable flowing again, realizes oil displacement efficiency under a certain pressure.Therefore this adjusting driving agnet has a wide range of applications at postpolymerflooded reservoirs, high water-cut reservoir and high permeable cement.The inventive method synthetic route is reasonable, and synthetic method is simple, and cheaper starting materials is easy to get, and has important promotion and application and is worth.
Accompanying drawing explanation
Figure 1 shows that rock core seepage apparatus schematic diagram;
Fig. 2 is particle adjusting driving agnet of the present invention is the injection pressure change of suspension in fill out sand tube formed in 19334mg/L salt solution in salinity;
Figure 3 shows that two-tube rock core parallel laboratory test schematic diagram;
Fig. 4 is the two-tube parallel laboratory test fractional flow curves of the present invention one specific embodiment.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but be not used for limiting the scope of the invention.
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 wiring solution-forming in 8 parts of water, 0.00025 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 5 parts of water, adds in three-necked bottle successively, and is placed in the water-bath of 15 DEG C; 0.0025 part of ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 12 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 75 DEG C of water-baths insulations 4 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained 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 wiring solution-forming in 20 parts of water, 0.00025 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 15 parts of water, adds in three-necked bottle successively, and is placed in the water-bath of 12 DEG C; 0.01 part of ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 25 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 70 DEG C of water-baths insulations 6 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained 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 wiring solution-forming in 40 parts of water, 0.0008 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 20 parts of water, adds in three-necked bottle successively, and is placed in the water-bath of 12 DEG C; 0.02 part of ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 30 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 80 DEG C of water-baths insulations 3 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained 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 wiring solution-forming in 100 parts of water, 0.0004 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 80 parts of water, adds in three-necked bottle successively, and is placed in the water-bath of 10 DEG C; 0.06 part of ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 60 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 85 DEG C of water-baths insulations 2 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained 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 wiring solution-forming in 30 parts of water, 0.0002 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 20 parts of water, adds in three-necked bottle successively, and is placed in the water-bath of 10 DEG C; 0.01 part of ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 30 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 75 DEG C of water-baths insulations 5 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained 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 wiring solution-forming in 50 parts of water, 0.001 part of polyethyleneglycol diacrylate is dissolved in wiring solution-forming in 40 parts of water, adds in three-necked bottle successively, and is placed in the water-bath of 15 DEG C; 0.03 part of ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 50 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 80 DEG C of water-baths insulations 3 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
Embodiment 7:
Rock core seepage apparatus is adopted to evaluate the injectability of particle adjusting driving agnet of the present invention
Experimental procedure is as follows: by adjusting driving agnet powder of the present invention for 0.2g100-150 order, and slowly adding 100mL salinity is under magnetic stirring that in 19334mg/L salt solution, stirring velocity is set to 500r/min, and churning time is 10-15min, obtains adjusting driving agnet suspension.
Figure 1 shows that rock core seepage apparatus schematic diagram, be made up of high-accuracy low speed pressure pump, container for storing liquid, tensimeter and fill out sand tube, homogeneous for ensureing to inject suspension process system, use magnetic stirrer container for storing liquid, rotating speed is 200r/min.Whole Seepage Experiment carries out in digital temperature-controlled box, and fluid injection speed is 0.5mL/min, and experimental temperature is 70 DEG C.Test porous medium used for self-control fill out sand tube, long is 30cm, and internal diameter is 2.5cm, and the rate of permeation of fill out sand tube is (1500 ± 15) × 10 -3um 2, volume of voids (PV) is 50 ± 0.5cm 3.
First experiment injects the salt solution that salinity is 19334mg/L in fill out sand tube, records intake pressure at regular intervals; When after pressure equilibrium, change the adjusting driving agnet suspension of note 2000mg/L, time recording pressure, after pressure equilibrium, carry out sequent water flooding to balance, test result is shown in Fig. 2.
As seen from the figure, in the water drive stage, pressure change is less, reaches equilibrium state very soon; After adjusting driving agnet suspension of the present invention drives beginning, pressure increases sharply, and shows the formation of plugging action, the permeability reduction of fill out sand tube; After pressure reaches maximum value, there is fluctuation in pressure, until balance.After sequent water flooding starts, partial particulate is rushed to open, and fill out sand tube rate of permeation increases, and pressure also starts to decline.
This test shows that particle adjusting driving agnet of the present invention has excellent injectability in fill out sand tube.
Embodiment 8:
Two-tube rock core parallel laboratory test is utilized to evaluate the adjustment oil reservoir heterogeneous body ability of adjusting driving agnet of the present invention
Experimental procedure is as follows: the preparation of adjusting driving agnet suspension is with embodiment 5.As shown in Figure 3, the rate of permeation of high permeability and low permeability fill out sand tube is respectively (1000 ± 10) × 10 -3μm 2(5000 ± 15) × 10 -3μm 2, the total pore size volume of two parallel seepage flow pipes is 101.6 ± 0.5cm 3.The mode of adopting to close note point successively injects the salt solution and suspension that salinity is 19334mg/L, and injection speed is 0.5mL/min, and experimental temperature is 70 DEG C.First experiment injects 1PV salinity is 19334mg/L salt solution, changes the adjusting driving agnet suspension of note 1PV2000mg/L afterwards, in addition carries out sequent water flooding afterwards.The Liquid output of time recording pressure change and high and low rate of permeation fill out sand tube in experimentation, carry out the adjustment oil reservoir heterogeneous body ability of comparative study adjusting driving agnet suspension of the present invention by analyzing fractional flow curves, test result is shown in Fig. 4.
As seen from the figure, during water drive balance, the fractional flow that height oozes fill out sand tube and hypotonic fill out sand tube is respectively 83.5% and 16.5%, and the ratio of the two is about 5:1, meets the ratio of the two rate of permeation.When after injection adjusting driving agnet suspension, the flow that height oozes fill out sand tube diminishes gradually and hypotonic fill out sand tube flow becomes large, and obvious reversal development appears in the fractional flow of high hyposmosis fill out sand tube, is called " fluid diversion ".After sequent water flooding starts, the fractional flow of hyposmosis fill out sand tube slowly declines and Thief zone fill out sand tube fractional flow starts to increase, after 2 PV, high hyposmosis fill out sand tube fractional flow is equal, then recover poly-gradually and drive front fractional flow level, namely adjusting driving agnet suspension continues to carry out profile control to fill out sand tube after sequent water flooding starts, and fluid diversion still maintains the time of 2PV in the sequent water flooding stage.

Claims (4)

1. improve a weak cross-linked particles adjusting driving agnet for oil recovery, formed, it is characterized in that by acrylamide monomer and compound crosslinking system through initiator initiated polymerization, described compound crosslinking system is dimethylaminoethyl acrylate methyl ammonia ethyl ester and polyethyleneglycol diacrylate.
2. a kind of weak cross-linked particles adjusting driving agnet improving oil recovery as claimed in claim 1, it is characterized in that, described initiator is ammonium persulphate.
3. a kind of weak cross-linked particles adjusting driving agnet improving oil recovery as claimed in claim 1, it is characterized in that, the weight part of described each component is:
4. a method for the weak cross-linked particles adjusting driving agnet of synthesis described raising oil recovery as arbitrary in claim 1-3, is characterized in that, carry out 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 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, add in three-necked bottle successively, and be placed in the water-bath of 10 DEG C ~ 15 DEG C; 0.01-0.03 part ammonium persulphate, after 30 minutes, is dissolved in the solution be made in 30 ~ 50 parts of water and adds three-necked bottle by logical nitrogen.Stop logical nitrogen after the temperature rise of question response solution is greater than 1 DEG C, after reaction terminates, three-necked bottle is put into 70 ~ 85 DEG C of water-baths insulations 2 ~ 6 hours, afterwards gel is taken out, shred, drying, pulverizing, can powdery product be obtained after screening.
CN201410643122.2A 2014-11-07 2014-11-07 A kind of weak cross-linked particles profile control agent for improving oil recovery and preparation method thereof Active CN105273145B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
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 granulate for profile control and polymer flooding as well as preparation method and application of pre-crosslinked gel granulates

Patent Citations (5)

* Cited by examiner, † Cited by third party
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 granulate for profile control and polymer flooding as well as preparation method and application of pre-crosslinked gel granulates

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