CN102952533B - Composite cross-linked polymer weak gel oil displacement agent and preparation method thereof - Google Patents
Composite cross-linked polymer weak gel oil displacement agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to composite cross-linked polymer weak gel oil displacement agent and a preparation method thereof; the displacement agent is formed by polymer AM/AA/NVP and compound cross-linking agent formaldehyde/phenol which have dehydration condensation reaction; the prescription is as follows: 0.12 percent to 0.3 percent of polymer AM/AA/NVP, 0.0002 percent to 0.0006 percent of compound cross-linking agent, 0.005 percent to 0.025 percent of stabilizer, and the rest water. The composite cross-linked polymer weak gel oil displacement agent has good anti-shear thinning performance; the viscosity retention rate of the sheared gel oil reaches above 80 percent, the plugging rate reaches above 99 percent, the breakthrough pressure is higher than 7MPa, stronger erosion-resistant capability and selective plugging capability are realized, and the selective plugging capability reaches above 80 percent.
Description
Technical field
The invention belongs to water injection well in oil fields transfer drive technical field, particularly a kind of complex cross-linked polymer Application of weak gel profile agent and preparation method thereof.
Background technology
When oil field enters High water cut or ultra-high water-containing after date, oilfield water flooding problem will become increasingly complex, and the oil recovery rate how improving high water-cut stage is oil circle question of common concern.In water drive process, because the reasons such as oil water interfacial tension is high, wettability of rock surface is poor cause water drive displacement efficiency low, and the nonuniformity of oil reservoir and disadvantageous mobility ratio can cause injection water along most permeable zone and the uneven propelling of high permeability zones, in the vertical formed individual layer advance by leaps and bounds, tonguing, form fingering in the horizontal, cause before injecting water extraction and break through, middle low permeability layer sweep efficiency is low, oil displacement efficiency is poor, has had a strong impact on the development effectiveness of water drive.
In order to improve oil recovery factor further after water drive, people in succession propose and improve sweep efficiency (as polymer flooding, crosslinked polymer flooding) and improve the method that displacement efficiency (as surfactant flooding, mixed phase drive) etc. improves recovery ratio.
In recent years, adopt the tertiary oil recovery technology such as polymer flooding, combination flooding to achieve good effect, but also exist displacement of reservoir oil cost high, have a big risk, the problem such as field conduct is difficult.Although polymer waterflooding Technical comparing is simple, because formation pore is sheared and the impact of the factor such as stratum high-temperature, high salinity, after polymkeric substance injects stratum, the loss of its virtual viscosity is very large, does not often reach expection object.And for the higher stratum of non-homogeneous degree, polymkeric substance then can along high permeability zone channelling.
China is in the oil field of high water-cut stage, in raising recovery ratio, it is master that the approach usually adopted at present remains to expand injection water swept volume and improve injection water displacement efficiency, therefore, improve the main method injecting water development effectiveness and remain the sweep efficiency improving and inject water, basically, transfer drive technology must be taked to improve intake profile, make injection water feed through to the high region of oil saturation as far as possible, thus the crude oil in residual oil area is displaced.
Although transfer drive technology can play the effect of improving ecology exploitation to some specific oil reservoir, to improve for the purpose of sweep efficiency, to improve the transfer drive technology of intake profile, exist significantly not enough in raising displacement efficiency.Conventional transfer drive technology, because in system, chemical agent concentration is high, gelation rate is fast, wayward, thus limits its injection rate and operating range, and along with the increase repeatedly repeating transfer drive, the effect that transfer drive measure improves section is deteriorated gradually, and its volume increase validity period shortens.Equally, reducing oil water interfacial tension, improve reservoir rocks wettability, in raising sweep efficiency, also there is obvious deficiency in the technology of reservoir sweep improved for the purpose of displacement efficiency.So, on the basis giving full play to transfer drive technical role, the oil displacement efficiency of microcosmic must be improved by efficient technology of reservoir sweep, thus proposes transfer drive technology.
At present, the advantage that the adjusting driving agnet of polymer weak gel class scope that is controlled with its gelation time, that be suitable for is wider is widely used in oil field.Weak Gels also can be described as " flow-gel ", and primarily of polymkeric substance and linking agent two portions composition, exist with the form of entirety, cross-linked state is mainly intermolecular cross-linking.
Application of weak gel profile agent can reach the dual purpose of deep fluid changed course and the displacement of reservoir oil, and the preferential path that Weak Gels has in certain intensity energy formation on the one hand produces certain plugging action, makes follow-up injection water stream to low permeability layer, plays transfer drive effect; On the other hand, because cross-link intensity is not high, Weak Gels slowly can also move to earth formation deep the effect producing and be similar to polymer flooding in preferential path under the promotion of follow-up injection water, thus can expand swept volume to a greater extent and improve oil displacement efficiency.
Summary of the invention
The object of the present invention is to provide a kind of complex cross-linked polymer Application of weak gel profile agent and preparation method thereof, its have anti-shearing, gelation time is controlled, sealing ratiod is high, plugging strength greatly and stronger resistance to erosion ability and select the feature such as shut-off capacity, and the preparation method of this adjusting driving agnet is simple, result of use is good, for improving oil recovery factor.
The technical solution used in the present invention is: the agent of complex cross-linked polymer Application of weak gel profile, and the weight part of each component is:
A, polymer A M/AA/NVP:0.12% ~ 0.3%;
B, linking agent: 0.0002% ~ 0.0006%;
C, stablizer: 0.005% ~ 0.025%;
All the other are water.
Described polymkeric substance, the weight part of each component is:
A、AM：10%～18%；
B、AA：4%～8%；
C, NVP (NVP): 0.1% ~ 1.1%;
D, initiator: 0.4% ~ 0.7%.
All the other are water.
Described linking agent is formaldehyde/phenol, and the mol ratio of formaldehyde and phenol is 4:1.
Described stablizer is thiocarbamide.
Described pH adjusting agent is one or both in vinylformic acid or sodium hydroxide.
Described initiator is ammonium persulphate/sodium bisulfite, and its mol ratio is 1:1.
The preparation method of complex cross-linked polymer Application of weak gel profile agent is as follows:
1, take 1000ml experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP 5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely;
2, by distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is 10000mg/L, leaves standstill 48 hours;
3, get a certain amount of polymer mother liquor, be diluted to target liquid with experimental water, then add linking agent, stablizer and pH adjusting agent, stir, obtain reaction mixture;
4, reaction mixture is incubated 20h ~ 60h in the baking oven of 50 DEG C ~ 80 DEG C, makes its crosslinking polymerization, obtain viscous solution and be the agent of complex cross-linked polymer Application of weak gel profile.
The preparation process that present invention also offers preparation complex cross-linked polymer Weak Gels polymkeric substance used is as follows:
1, in wide-necked bottle, add a certain amount of AM, AA, add suitable quantity of water and dissolve, then add a certain amount of NVP, stirring and dissolving;
2, above-mentioned joined solution pH adjusting agent is adjusted to pH=6 ~ 7, then reaction system is put into thermostat water bath;
3, after temperature rises to 30 DEG C ~ 50 DEG C, in reaction system, add a certain amount of ammonium persulphate/sodium bisulfite initiator under agitation, until initiator dissolves completely, make it react 8 hours under constant temperature;
4, after having reacted, polymkeric substance is shredded, then use ethyl alcohol purification, and dry in 40 DEG C of baking ovens, grind into powder, namely obtain polymer A M/AA/NVP.
The viscosity retention ratio of complex cross-linked polymer Application of weak gel profile provided by the invention agent after shearing reaches more than 80%, sealing ratiod is greater than 99%, gel-strength is high, breakthrough pressure reaches more than 7MPa, can shutoff most permeable zone and adjustment profile-log of water injection in the earth formation, reach not only the object of " tune " but also " driving ".In addition, this complex cross-linked polymer Application of weak gel profile agent preparation method is simple, and validity period is long, and result of use is good.
Accompanying drawing explanation
Fig. 1 is the impact of Application of weak gel profile agent by shearing action.
Embodiment
In order to have understanding clearly and understanding to technical characteristic of the present invention, object and result of use, below by embodiment, the invention will be further described.
The shear resistant of complex cross-linked polymer Application of weak gel profile provided by the present invention agent, sealing ratiod, plugging strength, selection shut-off capacity, resistance to erosion ability are tested, wherein: Fig. 1 is shown in the anti-shear performance test of Application of weak gel profile agent, sealing ratiod is in table 2, plugging strength is in table 3, select shut-off capacity in table 4, resistance to erosion ability is in table 5.
Embodiment 1: the anti-shear performance of Application of weak gel profile agent
This example provides a kind of Application of weak gel profile agent, and its preparation process is as follows:
Take 1000ml experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely; With distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is as 10000mg/L, leaves standstill 48 hours; Get 40g polymer mother liquor, add the water of 0.04g formaldehyde/phenol mother liquor and 1g stablizer mother liquor and 58.96g wherein, and then add sodium hydroxide wherein and regulate its pH to 7, stir, the baking oven putting into 60 DEG C is incubated 30h makes its crosslinking polymerization, obtains Application of weak gel profile agent.
Sheared by the adjusting driving agnet of preparation Wu Yin agitator, in the time that the rotating speed down cut of 3500r/min is different, the viscosity after then shearing by BrookfieldDV-III viscometer determining Weak Gels system, the results are shown in Figure 1.
As can be seen from Figure 1, the viscosity degradation of system after high speed shear, after shearing 50s, gel viscosity retention rate is 91.38%, illustrate that gelling system has good shear resistant, when can ensure that solution arrives earth formation deep, still there is higher viscosity, be conducive to expanding swept volume, improve oil recovery factor.
Embodiment 2: the sealing characteristics of Application of weak gel profile agent
This example provides a kind of Application of weak gel profile agent, and its preparation process is as follows:
Take 1000ml experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP 5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely; With distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is as 10000mg/L, leaves standstill 48 hours; Get 40g polymer mother liquor, add the water of 0.04g formaldehyde/phenol mother liquor and 1g stablizer mother liquor and 58.96g wherein, and then add sodium hydroxide wherein and regulate its pH to 7, stir, the baking oven putting into 60 DEG C is incubated 30h makes its crosslinking polymerization, obtains Application of weak gel profile agent.
As follows to the concrete test procedure of the sealing ratiod test experiments of rock core:
In fill out sand tube, inject the simulated formation water of human configuration with the constant flow rate of 2mL/min, to constant pressure, record flow and pressure, calculate the rate of permeation K1 of fill out sand tube;
In fill out sand tube, inject above-mentioned Application of weak gel profile agent with 1mL/min flow velocity, put into 60 DEG C of thermostat container plastics, soaking time 42h; Sequent water flooding, injects local water with 1mL/min flow velocity in fill out sand tube, record breakthrough pressure and steadily after pressure, calculate rate of permeation K2.
Sealing ratiod the results are shown in Table 2.
Table 2 sealing ratiod experimental result
As known from Table 2, the sealing ratiod of the Weak Gels developed in fill out sand tube simulated experiment is more than 99%, is up to 99.95%, and sealing ratiod is very high, and plugging effect is fine.
Embodiment 3: the plugging strength of Application of weak gel profile agent
This example provides a kind of Application of weak gel profile agent, and its preparation process is as follows:
Take 1000ml experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP 5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely; With distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is as 10000mg/L, leaves standstill 48 hours; Get 40g polymer mother liquor, add the water of 0.04g formaldehyde/phenol mother liquor and 1g stablizer mother liquor and 58.96g wherein, and then add sodium hydroxide wherein and regulate its pH to 7, stir, the baking oven putting into 60 DEG C is incubated 30h makes its crosslinking polymerization, obtains Application of weak gel profile agent.
Carry out shutoff experiment to above-mentioned Application of weak gel profile agent, the plugging strength breakthrough pressure of Weak Gels describes, and concrete test procedure is as follows:
First by saturated for fill out sand tube local water;
Inject a certain amount of Weak Gels with the flow of 2mL/min, after airtight for the fill out sand tube two ends injecting Weak Gels, putting design temperature into is wait for plastic in the baking oven of reservoir temperature;
Under temperature is reservoir temperature, local water is injected with 1mL/min flow, until fill out sand tube exit end flows out the first drop of liquid, and constantly have liquid to flow out later, now the manometric reading of entrance end is the breakthrough pressure Pmax of Weak Gels, and the ratio of this value and rock core length is breakthrough pressure gradient Pm.
Test result is as table 3, and the shutoff that Weak Gels is formed needs elevated pressures to break through, and illustrates that Weak Gels can form very strong plugging action in the earth formation.
Table 3 breakthrough pressure and breakthrough pressure gradient
Embodiment 4: the selection shut-off capacity of Application of weak gel profile agent
This example provides a kind of Application of weak gel profile agent, and its preparation process is as follows:
Take 1000ml experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP 5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely; With distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is as 10000mg/L, leaves standstill 48 hours; Get 40g polymer mother liquor, add the water of 0.04g formaldehyde/phenol mother liquor and 1g stablizer mother liquor and 58.96g wherein, and then add sodium hydroxide wherein and regulate its pH to 7, stir, the baking oven putting into 60 DEG C is incubated 30h makes its crosslinking polymerization, obtains Application of weak gel profile agent.
Above-mentioned Application of weak gel profile agent is carried out to the selection shut-off capacity test experiments of rock core.
Weak Gels, to the shutoff situation on different permeability grade stratum, carrys out quantitative description with profile improvement rate.Simulation stratum condition, by fill out sand tube parallel connections different for two rate of permeation, measure the water regain of high low permeability layer before and after transfer drive, then reference section improves degree.Experimental result is in table 4.
Shut-off capacity selected by table 4
As shown in Table 4, when two fill out sand tube with permeability contrast are in parallel, the amount of the Weak Gels that the fill out sand tube that rate of permeation is larger absorbs is more, and sealing ratiod is higher, this illustrates that this adjusting driving agnet has certain selectively blocking off ability, can first shutoff most permeable zone and macropore; And Weak Gels injection rate is larger, it is stronger that section improves ability.
Embodiment 5: the resistance to erosion ability of Application of weak gel profile agent
This example provides a kind of Application of weak gel profile agent, and its preparation process is as follows:
Take 1000ml experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP 5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely; With distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is as 10000mg/L, leaves standstill 48 hours; Get 40g polymer mother liquor, add the water of 0.04g formaldehyde/phenol mother liquor and 1g stablizer mother liquor and 58.96g wherein, and then add sodium hydroxide wherein and regulate its pH to 7, stir, the baking oven putting into 60 DEG C is incubated 30h makes its crosslinking polymerization, obtains Application of weak gel profile agent.
Above-mentioned Application of weak gel profile agent is carried out to the resistance to erosion aptitude tests experiment of rock core.Concrete test procedure is as follows:
First by saturated for fill out sand tube local water;
Inject a certain amount of Weak Gels with the flow of 2mL/min, after airtight for the fill out sand tube two ends injecting Weak Gels, putting design temperature into is wait for plastic in the baking oven of reservoir temperature;
Continue to inject local water in fill out sand tube, measure the rate of permeation after often injecting certain pore volume injected simulated formation water and plugging rate.Experimental result, as table 5, along with the increase of water injection rate, is washed away pressure and is not significantly reduced, but fluctuate within the specific limits, and illustrate that the shutoff that Weak Gels used is formed can keep for a long time, shutoff has good resistance to erosion ability.
Table 5 resistance to erosion aptitude tests result
The above embodiment is only used to further illustrate the present invention; can not be interpreted as can the restriction of practical range to the present invention; the researchist in this field can make some nonessential adjustment and improvement according to above content of the present invention, but is included within protection scope of the present invention.
Claims (1)
1. the preparation method of complex cross-linked polymer Application of weak gel profile agent, it is characterized in that, this adjusting driving agnet carries out dehydration condensation by polymer A M/AA/NVP by the hydroxyl in its amide group and multiple crosslinking agent formaldehyde/phenol to form, and the weight part of each component is: polymkeric substance: 0.12% ~ 0.3%; Linking agent: 0.0002% ~ 0.0006%; Stablizer: 0.005% ~ 0.025%, all the other are water, adjusting driving agnet temperature be 50 DEG C ~ 80 DEG C, pH value be 6 ~ 7.5 conditions under plastic;
Described polymkeric substance is AM/AA/NVP, it is using acrylamide (AM), vinylformic acid (AA) and NVP (NVP) as polymerization single polymerization monomer, issue raw radical polymerization in the effect of initiator ammonium persulfate/sodium bisulfite to obtain, its preparation process is as follows:
(1) in wide-necked bottle, add a certain proportion of AM, AA, then add suitable quantity of water dissolving, then add a certain amount of NVP, stirring and dissolving is complete;
(2) above-mentioned joined solution pH adjusting agent is adjusted to pH=6 ~ 7, then reaction system is put into thermostat water bath;
(3) after temperature rises to 30 DEG C ~ 50 DEG C, in reaction system, add a certain amount of ammonium persulphate/sodium bisulfite under agitation as initiator, until initiator dissolves completely, react 8 hours under constant temperature;
(4) after having reacted, polymkeric substance is shredded, then use ethyl alcohol purification, and dry in 40 DEG C of baking ovens, grind into powder, namely obtain polymer A M/AA/NVP;
Described linking agent is formaldehyde/phenol, and its mol ratio is 4:1;
Described stablizer is thiocarbamide;
Described polymkeric substance is synthesized by AM, AA, NVP and initiator, and the weight part of each component is: AM:10% ~ 18%; AA:4% ~ 8%; NVP:0.1% ~ 1.1%; Initiator: 0.4% ~ 0.7%; All the other are water;
Described pH adjusting agent is vinylformic acid or sodium hydroxide;
Described initiator is ammonium sulfate/sodium bisulfite, and its mol ratio is 1:1;
The preparation process of described complex cross-linked polymer Application of weak gel profile agent is as follows:
(1) take 1000mL experimental water, joining volume is in the beaker of 1L; Then add AM/AA/NVP multipolymer 5.00g, be mixed with 5000mg/L polymers soln, stirring and dissolving latter aging 24 hours completely;
(2) with distilled water preparation linking agent formaldehyde/phenol, stablizer thiocarbamide mother liquor, concentration is 10000mg/L, leaves standstill 48 hours;
(3) get a certain amount of polymers soln, be diluted to target liquid with experimental water, then add linking agent, stablizer and pH adjusting agent, stir, obtain reaction mixture;
(4) reaction mixture is incubated 20h ~ 60h in the baking oven of 50 DEG C ~ 80 DEG C, makes its crosslinking polymerization, obtain viscous solution and be the agent of complex cross-linked polymer Application of weak gel profile.
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| CN104371681A (en) * | 2014-10-17 | 2015-02-25 | 西南石油大学 | AA/AM/SSS underground cross-linked polymer gel plugging agent and preparation method thereof |
| CN104342101A (en) * | 2014-10-23 | 2015-02-11 | 西南石油大学 | AA/AM/NVP (Acrylic Acid/Acrylamide/N-Vinyl Pyrrolidone) copolymer water flooding direction change agent and synthesis method thereof |
| CN106318361A (en) * | 2015-07-09 | 2017-01-11 | 中国石油化工股份有限公司 | Modifying and flooding agent for high-temperature high-calcium-magnesium oil pool and preparation method thereof |
| CN110055046A (en) * | 2018-01-19 | 2019-07-26 | 中国石油天然气股份有限公司 | High-viscoelasticity polymer oil-displacing agent prepared from high-temperature high-salt reservoir injection water and preparation method thereof |
| CN111073625B (en) * | 2018-10-22 | 2022-10-04 | 中国石油化工股份有限公司 | Modifying and flooding agent and preparation method thereof |
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| CN116554846B (en) * | 2023-01-02 | 2024-07-19 | 西南石油大学 | Gel plugging agent suitable for hypotonic ultra-hypotonic fractured reservoir and preparation method thereof |
| CN116375926A (en) * | 2023-05-04 | 2023-07-04 | 武汉晶顺科技开发有限公司 | Ternary polymerization heat-insulating fireproof glass gel and preparation method and application thereof |
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| CN1903974A (en) * | 2005-07-26 | 2007-01-31 | 中国科学院理化技术研究所 | Nano water-soluble microgel oil displacement material and preparation method thereof |
| CN102329599A (en) * | 2011-08-19 | 2012-01-25 | 西南石油大学 | Novel selective water shutoff agent for oil well water shutoff |
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