CN103773342B - Large-pore composite plugging system and preparation method thereof - Google Patents
Large-pore composite plugging system and preparation method thereof Download PDFInfo
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- CN103773342B CN103773342B CN201310681417.4A CN201310681417A CN103773342B CN 103773342 B CN103773342 B CN 103773342B CN 201310681417 A CN201310681417 A CN 201310681417A CN 103773342 B CN103773342 B CN 103773342B
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Abstract
The invention provides a large-pore composite plugging system and a preparation method thereof, belonging to the technical field of oil exploitation. The large-pore composite plugging system comprises amphoteric polyacrylamide solution with concentration of 0.2-0.5wt%, a flocculation agent solution and inorganic granules, wherein the flocculation agent solution is a cationic polymer solution with concentration of 0.2-0.5wt% or cationic surface active agent with concentration of 1-4wt%. The large-pore composite plugging system has the advantages of high elasticity, high plugging capability, movability and good thermal stability.
Description
Technical field
The present invention relates to a kind of macropore is combined closure system, belong to technical field of petroleum extraction.
Background technology
In oil extraction process, waterflooding extraction is main oil production method, but during long-term injecting water exploitation,
Because water rinses, clay runs off, and so that the anisotropism on stratum is deteriorated, so that the permeability on higher permeability stratum is improved further,
Injection water often flows along high permeability zone, and water further causes the permeability of high permeability zone and significantly carries to washing away of high permeability zone
Height, some high permeability zones even form macropore channelling, inject the serious low effective circulation of water, some oil reservoir produced liquid moisture content are
Reach more than 90%, or even 95%, cost for oil production significantly rises.
In order that injection water uniformly advances, reduce well water, frequently with water shutoff agent, macropore is blocked.Conventional
Water shutoff agent includes polymer gel type water shutoff agent and polymer gel type water shutoff agent, and wherein polymer gel type water shutoff agent comes because of it
Source is extensive, it is simple to prepare, it has also become the research organic water plugging profile control agent of a most widely used class both at home and abroad.In prior art, gather
The polymer that compound gel-type water shutoff agent is adopted is mainly polyacrylamide.Such as, Chinese patent literature
CN102807849A discloses a kind of polyacrylamide gel plugging agent, and it includes following material non-ionic polyacrylamide
0.3～0.8%, cross-linking agent A0.6～1.3%, crosslinking agent B 0.45～1.44%, temperature stability agent 0.02～0.04%, pH adjusting agent
0.01～0.08%, and the water of surplus, wherein said cross-linking agent A is hexamethylenamine, and crosslinking agent B is hydroquinone or resorcinol；
Described temperature stability agent is sodium thiosulfate, sodium sulfite or sodium sulfite；Described pH value regulator is sodium hydroxide, hydrogen-oxygen
Change potassium, sodium carbonate or sodium bicarbonate.
In above-mentioned technology, amide groups mainly and on polyacrylamide amine molecule for the organic crosslinking agent crosslink reaction, preparation
Obtain gel plugging agent.When this gel plugging agent is used for profile control and water plugging, because the temperature on stratum is typically all higher, and in high temperature bar
Under part, the amide groups on polyacrylamide amine molecule not crosslinked can hydrolyze first, under the alkaline environment on stratum, shape
Become carboxylic sodio；After being that crosslinked amide groups are all hydrolyzed into carboxylic sodio in polyacrylamide amine molecule, further hydrolysis meeting
Occur with the polyacrylamide amine molecule amide groups place of link in organic crosslinking agent, cross-linking agent is gradually dissociated with polyacrylamide crosslinking,
Macroscopically it is seen that polymer gel breaks glue dehydration.Therefore this gel plugging agent is applied under the conditions of high temperature, high salinity
When, have that the heat stability time is short, effect duration is short, do not reach the problem of plugging effect.
Content of the invention
The technical problem to be solved is that in prior art, gel plugging agent, when hot conditionss are applied, has heat
Stability time is short, closure effect duration is short, does not reach the problem of plugging effect, and then provides a kind of heat stability time length, envelope
The good macropore of stifled effect is combined closure system.
In order to solve above-mentioned technical problem, the invention provides a kind of macropore is combined closure system, it is 0.2 including concentration
The amphiprotic polyacrylamide solution of～0.5wt%, coacervation agent solution and inorganic particle；
Wherein, described coacervation agent solution for concentration be 0.2～0.5wt% cation type polymer solution or concentration be 1～
The cationic surfactant solution of 4wt%.
Cation type polymer in described cation type polymer solution is cationic modified starch, cation polypropylene
Any one or a few in amide, your glue of cation-modified cellulose or cation-modified guanidine；Described cation surface activating
Cationic surfactant in agent solution is quaternary ammonium salt cationic surfactant.
Described quaternary ammonium salt cationic surfactant is Dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl
Any one or a few in ammonium chloride, octadecyldimethyl hydroxyethyl ammonium nitrate.
The cationic degree of the cation type polymer in described coacervation agent solution or cationic surfactant is 20%-
25%.
The addition of described inorganic particle accounts for 3～8wt% of described amphiprotic polyacrylamide solution gross mass.
The particle diameter of described inorganic particle is 100 mesh～200 mesh.
In mass, the addition of described amphiprotic polyacrylamide solution and described coacervation agent solution is than for 1:1～3:1.
The present invention still further provides the preparation method that described macropore is combined closure system, comprises the steps：
（1）The amphiprotic polyacrylamide of specified quantitative is slowly added in water, stirs, obtain amphiprotic polyacrylamide molten
Liquid；
（2）To described step（1）In amphiprotic polyacrylamide solution in add the inorganic particle of specified quantitative, stirring is all
Even, obtain mixed solution；
（3）The cation type polymer of specified quantitative or cationic surfactant are slowly added in water, stir, obtain
To coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, described mixing
Solution is contacted with described coacervation agent solution and generates compound closure system.
Described step（1）In, after amphiprotic polyacrylamide and water stir 30min under 680-720r/min mixing speed,
Mixing speed is dropped to 380-420r/min, the amphiprotic polyacrylamide solution being uniformly mixed after continuously stirred 1.5-2h.
Described step（2）In, described amphiprotic polyacrylamide solution is fast in the stirring of 680～720r/min with inorganic particle
Degree is lower to stir 15min, the mixed solution being uniformly mixed.
Described step（3）In, described cationic surfactant and water stir under the mixing speed of 380-420r/min
10min, or described cation type polymer and water stirs 30min-2h under the mixing speed of 380-420r/min, is mixed
Uniform coacervation agent solution.
Described step（4）In, by described mixed solution and described coacervation agent solution 50～100 times/min concussion speed
Lower concussion, so as to quick mix homogeneously complete to react, obtains compound closure system.
The present invention compared with prior art has the advantage that：
（1）Macropore of the present invention is combined closure system, using amphiprotic polyacrylamide solution, due to both sexes polypropylene
Amide can be along C-C key in water（σ key）Structure is curled in interior rotation formation, but its bond angle remains 109 ° 28 ', both sexes poly- third
The curling structure and can occur mutually to tangle of acrylamide, entanglement of formation " key ", additionally ,-NH2 the quilt in amphiprotic polyacrylamide chain link
When anion and cation replace simultaneously, in addition to entanglement of formation " key " between amphiprotic polyacrylamide molecule, can also divide
In son and intermolecular generation ionic bond and association key, ionic bond, association key and tangle " key ", Macintosh can be produced, Macintosh is common
Amphiprotic polyacrylamide can be connected into a supramolecular structure by same-action；Form supramolecular structure in amphiprotic polyacrylamide
Meanwhile, the cation group in amphiprotic polyacrylamide can also adsorb inorganic particle, and anionic group exposed so that inorganic
Granule can be dispersed in amphiprotic polyacrylamide solution；When amphiprotic polyacrylamide solution is contacted with coacervation agent solution
When, the cation group in the exposed anionic group in amphiprotic polyacrylamide solution and coacervation agent solution can rapidly with from
The mode of sub-key combines, and forms compound closure system；Additionally due to stratum sandstone surface is elecrtonegativity, such both sexes polyacrylamide
The anionic group being not combined with cation group in amine aqueous solution and stratum sandstone are due to the effect of electrically repelling each other so that compound seal
Stifled system dispersion stabilization in the earth formation is good.Because compound closure system of the present invention is by amphiprotic polyacrylamide
In anionic group be bonded with the cation group in flocculation agent, instead of in prior art and typically require in polyacrylamide
In amido link at crosslinked mode, be easy to hydrolyze under high temperature, high salinity, lead to when also just overcoming crosslinked at amido link
Water shutoff agent heatproof, the problem of resistance to salinity effect difference.Macropore of the present invention is combined closure system, can adopt high salinity
Oil field water prepared, have that elasticity is strong, blocking ability is strong, good, the resistance to salinity effect of resistance to temp effect is good, closure effect duration is long
Advantage.
（2）Macropore of the present invention is combined closure system, selects the apparent viscous of amphiprotic polyacrylamide solution further
During degree ＞ 150mPa s, amphiprotic polyacrylamide solution can play good suspension effect to inorganic particle；Equally, enter one
Step selects the addition of described inorganic particle to account for 3～8wt% of described amphiprotic polyacrylamide solution gross mass, is also to make both sexes
Polyacrylamide solution plays good suspension effect to inorganic particle, and inorganic particle so can be made molten with amphiprotic polyacrylamide
Liquid mixes well, will not produce lamination；Further, described amphiprotic polyacrylamide solution and described coacervation agent solution
Interpolation mass ratio be 1:1～3:When 1, compound occluding body cording can be made to have suitable strength, when using it for Water in Water Shutoff in Oil Field,
There is optimal resistance to temp effect and optimal closure effect duration.
（3）Macropore of the present invention is combined the preparation method of closure system, first by the both sexes polyacrylamide of specified quantitative
Amine is slowly added in water, stirs, and so can make to pass through between polymer molecular chain to be wound around " key " mutually winding more
Stable, and it is enriched with certain inner chamber being wound around near " key ", carry out with stirring, part hydrone can enter inner chamber, finally can
Form the amphiprotic polyacrylamide solution with rock-steady structure；Again to stating in amphiprotic polyacrylamide solution addition inorganic particle,
Now continuing stirring can make cation group in amphiprotic polyacrylamide solution adsorb inorganic particle, anionic group exposed
Outward, thus there is good suspended dispersed effect to inorganic particle；The cation type polymer of specified quantitative or cationic surface are lived
Property agent is slowly added in water, stirs, after obtaining coacervation agent solution, then will carry the amphiprotic polyacrylamide of inorganic particle
Solution is mixed with described coacervation agent solution, due to having substantial amounts of exposed anion in amphiprotic polyacrylamide solution, and gathers
Substantial amounts of cation is contained, two kinds of solution one contact, and cation can be combined by ionic bond with anion, wink in solidifying agent solution
Between complete to react, generate compound closure system.Macropore of the present invention is combined the preparation method of closure system, has reaction fast
Speed, the advantage of easy construction.
Specific embodiment
With reference to embodiments, the present invention is further described in detail, but is not limited to this.
Embodiment 1
Macropore described in the present embodiment is combined closure system, including 1kg concentration be 0.2wt% both sexes polyacrylamide
Amine aqueous solution, the concentration of 1kg be the PAMC solution of 0.2wt% and 0.03kg particle diameter be 100 mesh active carbonic acid
Calcium.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field injection of 3000mg/L
In water, after stirring 30min under 680r/min mixing speed, mixing speed is dropped to 420r/min, obtains after continuously stirred 2h
The amphiprotic polyacrylamide solution of mix homogeneously.
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter activated carbon
Sour calcium, stirs 15min under the mixing speed of 680r/min, stirs, obtain mixed solution；
（3）The salinity that the PAMC of specified quantitative is slowly added to specified quantitative is the oil field note of 3000mg/L
Enter in water, stir 30min under the mixing speed of 380r/min, stir, obtain coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, described mixing
Solution is shaken under the concussion speed of 50 times/min with described coacervation agent solution so as to quickly mixing homogeneously and be quickly generated compound
Closure system.
Embodiment 2
Macropore described in the present embodiment is combined closure system, including 1.5kg concentration be 0.3wt% both sexes polypropylene
Amide solution, the concentration of 1kg be the Dodecyl trimethyl ammonium chloride solution of 1wt% and 0.075kg particle diameter be 120 mesh work
Property Calcium Carbonate.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field injection of 5000mg/L
In water, after stirring 30min under 680r/min mixing speed, mixing speed is dropped to 420r/min, obtains after continuously stirred 2h
The amphiprotic polyacrylamide solution of mix homogeneously.
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter activated carbon
Sour calcium, stirs 15min under the mixing speed of 680r/min, stirs, obtain mixed solution；
（3）The salinity that the Dodecyl trimethyl ammonium chloride of specified quantitative is slowly added to specified quantitative is the oil of 5000mg/L
In field injection water, stir 10min under the mixing speed of 380r/min, stir, obtain coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, described mixing
Solution is shaken under the concussion speed of 90 times/min with described coacervation agent solution so as to quickly mixing homogeneously and be quickly generated compound
Closure system.
Embodiment 3
Macropore described in the present embodiment is combined closure system, including 2kg concentration be 0.35wt% both sexes polyacrylamide
Amine aqueous solution, the concentration of 1kg are the dodecyl dimethyl benzyl ammonium chloride solution of 2.5wt% and the particle diameter of 0.12kg is 150 purposes
Flyash.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field note of 10000mg/L
Enter in water, after stirring 30min under 700r/min mixing speed, mixing speed is dropped to 400r/min, after continuously stirred 1.8h
Obtain, the amphiprotic polyacrylamide solution of mix homogeneously；
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter flyash,
Stir 15min under the mixing speed of 700r/min, stir, obtain mixed solution；
（3）The salinity that the dodecyl dimethyl benzyl ammonium chloride of specified quantitative is slowly added to specified quantitative is 10000mg/
In the oilfield injection water of L, stir 10min under the mixing speed of 400r/min, stir, obtain coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, described mixing
Solution is shaken under the concussion speed of 50 times/min with described coacervation agent solution so as to quickly mixing homogeneously and be quickly generated compound
Closure system.
Embodiment 4
Macropore described in the present embodiment is combined closure system, including 2.5kg concentration be 0.4wt% both sexes polypropylene
Amide solution, the concentration of 1kg be the cation-modified cellulose of 0.3wt% and 0.175kg particle diameter be 170 mesh active carbonic acid
Calcium.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field note of 15000mg/L
Enter in water, after stirring 30min under 720r/min mixing speed, mixing speed is dropped to 380r/min, after continuously stirred 2h
Arrive, the amphiprotic polyacrylamide solution of mix homogeneously；
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter activated carbon
Sour calcium, stirs 15min under the mixing speed of 720r/min, stirs, obtain mixed solution；
（3）The salinity that the cation-modified cellulose of specified quantitative is slowly added to specified quantitative is the oil field of 15000mg/L
In injection water, stir 2h under the mixing speed of 380r/min, stir, obtain coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, described mixing
Solution is shaken under the concussion speed of 60 times/min with described coacervation agent solution so as to quickly mixing homogeneously and be quickly generated compound
Closure system.
Embodiment 5
Macropore described in the present embodiment is combined closure system, including 3kg concentration be 0.5wt% both sexes polyacrylamide
Amine aqueous solution, the concentration of 1kg be the cationic modified starch solution of 0.5wt% and 0.24kg particle diameter be 200 mesh active carbonic acid
Calcium.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field note of 20000mg/L
Enter in water, after stirring 30min under 680r/min mixing speed, mixing speed is dropped to 420r/min, after continuously stirred 2h
Amphiprotic polyacrylamide solution to mix homogeneously.
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter activated carbon
Sour calcium, stirs 15min under the mixing speed of 690r/min, stirs, obtain mixed solution；
（3）The salinity that the cationic modified starch of specified quantitative is slowly added to specified quantitative is the oil field note of 20000mg/L
Enter in water, stir 1h under the mixing speed of 400r/min, stir, obtain coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, described mixing
Solution is shaken under the concussion speed of 70 times/min with described coacervation agent solution so as to quickly mixing homogeneously and be quickly generated compound
Closure system.
Embodiment 6
Macropore described in the present embodiment is combined closure system, including 1.2kg concentration be 0.25wt% both sexes polypropylene
The cation that amide solution, the concentration of 0.5kg are the cation-modified guanidine that glue of 0.4wt%, the concentration of 0.5kg is 0.4wt% changes
The particle diameter of property starch and 0.06kg is the Calcium Carbonate of 100～200 mesh.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field note of 25000mg/L
Enter in water, after stirring 30min under 700r/min mixing speed, mixing speed is dropped to 400r/min, after continuously stirred 1.8h
The amphiprotic polyacrylamide solution being uniformly mixed；
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter Calcium Carbonate,
Stir 15min under the mixing speed of 710r/min, stir, obtain mixed solution；
（3）The salinity that your glue of cation-modified guanidine of specified quantitative is slowly added to specified quantitative is the oil field of 25000mg/L
In injection water, stir 30min under the mixing speed of 420r/min, stir, obtain the first coacervation agent solution；By specified quantitative
Cationic modified starch be slowly added to specified quantitative salinity be 25000mg/L oilfield injection water in, 380r/min's
Stir 2h under mixing speed, stir, obtain the second coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In the first coacervation agent solution, the second coacervation
Agent solution mixes, and described mixed solution is fast in the concussion of 80 times/min with described first coacervation agent solution and the second coacervation agent solution
The lower concussion of degree is so as to quick mix homogeneously be quickly generated compound closure system.
Embodiment 7
Macropore described in the present embodiment is combined closure system, including 1.8kg concentration be 0.45wt% both sexes polypropylene
Amide solution, the concentration of 0.5kg are the octadecyldimethyl hydroxyethyl ammonium nitrate of 4wt%, the concentration of 0.5kg is the ten of 4wt%
The particle diameter of dialkyl group trimethyl ammonium chloride and 0.099kg is the silicon powder of 200 mesh.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field note of 30000mg/L
Enter in water, after stirring 30min under 720r/min mixing speed, mixing speed is dropped to 380r/min, after continuously stirred 2h
Amphiprotic polyacrylamide solution to mix homogeneously；
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter silicon powder,
Stir 15min under the mixing speed of 680r/min, stir, obtain mixed solution；
（3）The salinity that the octadecyldimethyl hydroxyethyl ammonium nitrate of specified quantitative is slowly added to specified quantitative is
In the oilfield injection water of 30000mg/L, stir 10min under the mixing speed of 420r/min, stir, obtain the first coacervation
Agent solution；The salinity that the Dodecyl trimethyl ammonium chloride of specified quantitative is slowly added to specified quantitative is the oil field of 30000mg/L
In injection water, stir 10min under the mixing speed of 420r/min, stir, obtain the second coacervation agent solution
（4）By described step（2）In mixed solution and described step（3）In the first coacervation agent solution, the second coacervation
Agent solution mixing, described mixed solution and described first coacervation agent solution and the second coacervation agent solution, in the concussion of 100 times/min
Concussion under speed is so as to quick mix homogeneously be quickly generated compound closure system.
Embodiment 8
Macropore described in the present embodiment is combined closure system, including 1.2kg concentration be 0.45wt% both sexes polypropylene
Amide solution, the concentration of 1.2kg are the octadecyldimethyl hydroxyethyl ammonium nitrate of 4wt% and the particle diameter of 0.1kg is 245 purposes
Activated Calcium carbonate.
The preparation method that macropore described in the present embodiment is combined closure system comprises the steps：
（1）The salinity that the amphiprotic polyacrylamide of specified quantitative is slowly added to specified quantitative is the oil field note of 22000mg/L
Enter in water, after stirring 30min under 720r/min mixing speed, mixing speed is dropped to 420r/min, after continuously stirred 2h
Amphiprotic polyacrylamide solution to mix homogeneously；
（2）To described step（1）In amphiprotic polyacrylamide solution in add specified quantitative specified particle diameter activated carbon
Sour calcium, stirs 15min under the mixing speed of 720r/min, stirs, obtain mixed solution；
（3）The salinity that the PAMC of specified quantitative is slowly added to specified quantitative is the oil field of 22000mg/L
In injection water, stir 1.5h under the mixing speed of 420r/min, stir, obtain coacervation agent solution；
（4）By described step（2）In mixed solution and described step（3）In coacervation agent solution mixing, 100 times/
Concussion under the concussion speed of min is so as to quick mix homogeneously be quickly generated compound closure system.
Example is evaluated in performance measurement
（1）Quantitative measurement evaluates example
Comprcssive strength is carried out to the compound closure system preparing in above-mentioned all embodiments 1～8 using CT3 Texture instrument
Test, test result is shown in Table 1.
Table 1 is combined the quantitative measurement result of closure system
| Embodiment is numbered | Comprcssive strength/N |
| 1 | 1000 |
| 2 | 1025 |
| 3 | 1285 |
| 4 | 1725 |
| 5 | 2025 |
| 6 | 1680 |
| 7 | 3100 |
| 8 | 3615 |
As shown in Table 1, the comprcssive strength of the core simulating test that compound closure system of the present invention is carried out can reach
More than 1000N, shows compound occluding body system of the present invention at high temperature, have very strong closure stability under high salinity,
Ensure that effective macropore plugging in site operation, improve oil recovery factor.
（2）Sealing ratiod test evaluation example
Macropore of the present invention is combined in the preparation process of closure system, the both sexes due to mixing with inorganic particle poly- third
Acrylamide solution is when contacting with coacervation agent solution, you can moment generates compound closure system, and its feature is combined conventional on oil field
Water plugging and profile controlling method in two-fluid process（Two-fluid process refers to the working solutions different using two kinds, is separated with insulating liquid, alternately injection ground
Layer, through being extrapolated to after certain distance in the earth formation, two kinds of working solution contacts occur chemical reaction to produce closure material）, therefore exist
The rock core of the compound closure system simulated field reservoir condition described in embodiment 1～8 is carried out blocking in process of the test using double
Liquid method is simulated test.
The proportioning being respectively adopted the compound closure system described in embodiment 1～8 carries out following simulation tests, simulation test
Temperature be 60～80 DEG C, the rock core test of simulated field reservoir condition is:Take length 0.9m-1.1m, diameter 0.03m-0.04m
Rock core, survey after water drive to pressure stability its stifled before permeability Kw0, carry out closure test using following steps：Water drive is surveyed rock core and is oozed
Rate injects the specific of the coacervation agent solution injection insulating liquid 4ml injection specified quantitative of the certain concentration of specified quantitative thoroughly
The amphiprotic polyacrylamide solution of concentration is injected with the mixed solution injection insulating liquid 4ml of the inorganic particle of specified quantitative
The both sexes that the coacervation agent solution of the certain concentration of specified quantitative injects the certain concentration that insulating liquid 4ml injects specified quantitative gather
Acrylamide solution and the mixed solution sequent water flooding of the inorganic particle of specified quantitative, after water drive to pressure stability, survey rock
Stifled rear permeability K of the heartw1, and press formulaCalculate reservoir core plugging rate.Experimental result is shown in Table 2.
In order to further illustrate the concrete grammar of above-mentioned simulation test, the present invention further, with using institute in embodiment 2
The method that the compound closure system proportioning stated is simulated test is described in detail, other embodiments all using with the method phase
Same simulation test is tested, specific as follows：
Take length 1.1m, the rock core of diameter 0.04m, be 70 DEG C in temperature, after water drive to pressure stability, survey its stifled front infiltration
Rate Kw0=14.6μm2, carry out closure test using following steps：Water drive surveys ten that core permeability implantation concentration is 1wt%
Dialkyl group trimethyl ammonia chloride ammonium salt solution 0.04PV (wherein PV refers to rock pore volume) injection insulating liquid 4ml injection
The concentration of 1.5kg be amphiprotic polyacrylamide solution and the 0.075kg of 0.3wt% particle diameter be 120 mesh activated Calcium carbonate mixed
Close solution 0.06PV and inject the coacervation agent solution 0.04PV injection isolation that insulating liquid 4ml implantation concentration is 1wt%
The concentration that liquid 4ml injects 1.5kg is the amphiprotic polyacrylamide solution of 0.3wt% is 120 purposes with the particle diameter of 0.075kg
The mixed solution 0.06PV sequent water flooding 3PV of activated Calcium carbonate, after water drive to pressure stability, survey rock core stifled after permeate
Rate Kw1=0.9928μm2, and press formulaCalculate reservoir core plugging rate, experimental result is shown in Table 2.
Need to above-mentioned simulation test be with further illustrating, due to density and the described both sexes polypropylene of coacervation agent solution
The density of amide solution is essentially identical, so, replace the mass ratio in embodiment to carry out rock core using volume ratio in simulation test
Simulation test.Further for above-mentioned simulation test, all carry out three core simulating test by the proportioning in each embodiment, take it
The meansigma methodss of test result are as final testing result.
Rock core test method through respectively above-described embodiment 1～8 is pressed with above-mentioned simulated field reservoir condition is simulated examination
After testing, the sealing ratiod of testing rock core, result is as shown in table 2：
Table 2 core simulating test sealing ratiod test result
| Embodiment is numbered | Kwo/μm2 | Kw1/μm2 | E/% |
| 1 | 15.2 | 1.3072 | 91.4 |
| 2 | 14.6 | 0.9928 | 93.2 |
| 3 | 14.8 | 0.8436 | 94.3 |
| 4 | 14.8 | 0.6068 | 95.9 |
| 5 | 14.9 | 0.4321 | 97.1 |
| 6 | 15.0 | 0.72 | 95.2 |
| 7 | 14.7 | 0.2793 | 98.1 |
| 8 | 15.1 | 0.1208 | 99.2 |
As shown in Table 2, the sealing ratiod of the core simulating test being carried out using compound closure system of the present invention can reach
To more than 90%, result shows, compound occluding body of the present invention ties up to high temperature, has very strong sealing characteristics under high salinity,
Ensure that effective macropore plugging in site operation, improve oil recovery factor.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.Right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment, and the obvious change thus extended out or
Change among still in the invention scope of the claims.
Claims (15)
1. a kind of macropore is combined closure system it is characterised in that including the both sexes polyacrylamide that concentration is 0.2～0.5wt%
Amine aqueous solution, coacervation agent solution and inorganic particle；
Wherein, the cation type polymer solution that described coacervation agent solution is 0.2～0.5wt% for concentration；
In mass, the addition of described amphiprotic polyacrylamide solution and described coacervation agent solution is than for 1:1～3:1.
2. macropore is combined closure system it is characterised in that in described cation type polymer solution according to claim 1
Cation type polymer be cationic modified starch, PAMC, cation-modified cellulose or cation change
Property your glue of guanidine in any one or a few.
3. macropore is combined closure system it is characterised in that cation in described coacervation agent solution according to claim 1
The cationic degree of type polymer is 20%-25%.
4. macropore according to any one of claims 1 to 3 is combined closure system it is characterised in that described inorganic particle
Addition accounts for 3～8wt% of described amphiprotic polyacrylamide solution gross mass.
5. macropore is combined closure system it is characterised in that the particle diameter of described inorganic particle is 100 according to claim 4
Mesh～200 mesh.
6. macropore described in any one of Claims 1 to 5 is combined the preparation method of closure system, comprises the steps：
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in water, stirs, obtain amphiprotic polyacrylamide solution；
(2) add the inorganic particle of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), stir, obtain
To mixed solution；
(3) cation type polymer of specified quantitative is slowly added in water, stirs, obtain coacervation agent solution；
(4) mixed solution in described step (2) is mixed with the coacervation agent solution in described step (3), described mixed solution
Contact with described coacervation agent solution and generate compound closure system.
7. preparation method according to claim 6 is it is characterised in that in described step (1), amphiprotic polyacrylamide and water
After stirring 30min under 680-720r/min mixing speed, mixing speed is dropped to 380-420r/min, continuously stirred 1.5-2h
The amphiprotic polyacrylamide solution being uniformly mixed afterwards.
8. the preparation method according to claim 6 or 7 is it is characterised in that in described step (2), described both sexes polypropylene
Amide solution and inorganic particle stir 15min under the mixing speed of 680～720r/min, and the mixing being uniformly mixed is molten
Liquid.
9. the preparation method according to claim 6 or 7 is it is characterised in that in described step (3), described cationic poly
Compound and water stir 30min-2h, the coacervation agent solution being uniformly mixed under the mixing speed of 380-420r/min.
10. the preparation method according to claim 6 or 7 is it is characterised in that in described step (4), by described mixed solution
Shake under the concussion speed of 50～100 times/min with described coacervation agent solution so as to quickly mixing homogeneously and completing to react, obtain
To compound closure system.
A kind of 11. macropores are combined the preparation method of closure system, comprise the steps：
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in water, stirs, obtain amphiprotic polyacrylamide solution；
(2) add the inorganic particle of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), stir, obtain
To mixed solution；
(3) cationic surfactant of specified quantitative is slowly added in water, stirs, obtain coacervation agent solution；
(4) mixed solution in described step (2) is mixed with the coacervation agent solution in described step (3), described mixed solution
Contact with described coacervation agent solution and generate compound closure system；
In mass, the addition of described amphiprotic polyacrylamide solution and described coacervation agent solution is than for 1:1～3:1；
The concentration of described amphiprotic polyacrylamide solution is 0.2～0.5wt%；
The concentration of described coacervation agent solution is 1～4wt%.
12. preparation methoies according to claim 11 it is characterised in that in described step (1), amphiprotic polyacrylamide with
After water stirs 30min under 680-720r/min mixing speed, mixing speed is dropped to 380-420r/min, continuously stirred 1.5-
The amphiprotic polyacrylamide solution being uniformly mixed after 2h.
13. preparation methoies according to claim 11 or 12 it is characterised in that in described step (2), described both sexes poly- third
Acrylamide solution and inorganic particle stir 15min under the mixing speed of 680～720r/min, and the mixing being uniformly mixed is molten
Liquid.
14. preparation methoies according to claim 11 or 12 it is characterised in that in described step (3), described cation form
Face activating agent and water stir 10min, the coacervation agent solution being uniformly mixed under the mixing speed of 380-420r/min.
15. preparation methoies according to claim 11 or 12 will be it is characterised in that in described step (4), will described mix molten
Liquid shakes so as to quickly mixing homogeneously and completing to react under the concussion speed of 50～100 times/min with described coacervation agent solution,
Obtain compound closure system.
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