CN103773342A - 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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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 the compound shutoff system of a kind of macropore, belong to technical field of petroleum extraction.
Background technology
In oil extraction process, waterflooding is main oil production method, but in the process of long-term injecting water exploitation, because water rinses, clay runs off, the nonuniformity on stratum is worsened, the rate of permeation on higher permeability stratum is further improved, injected water often flows along most permeable zone, water has further caused the rate of permeation of most permeable zone greatly to improve to washing away of most permeable zone, some most permeable zones even form macropore channelling, the serious low effective circulation of injected water, some oil reservoir produced liquid water ratio has reached 90%, even more than 95%, cost for oil production significantly rises.
For injected water is evenly advanced, reduce well water, often adopt plugging agent to carry out shutoff to macropore.Conventional plugging agent comprises polymer gel type plugging agent and polymer gel type plugging agent, and wherein polymer gel type plugging agent is simple because of its wide material sources, preparation, has become the organic water plugging profile control agent of the most widely used class of domestic and international research.In prior art, the polymkeric substance that polymer gel type plugging agent adopts is mainly polyacrylamide.Such as, Chinese patent literature CN102807849A discloses a kind of polyacrylamide gel plugging agent, it comprises following material non-ionic polyacrylamide 0.3～0.8%, linking agent A0.6～1.3%, crosslinking agent B 0.45～1.44%, temperature stabilising agent 0.02～0.04%, pH adjusting agent 0.01～0.08%, with the water of surplus, wherein said linking agent A is urotropine, and crosslinking agent B is Resorcinol or Resorcinol; Described temperature stabilising agent is Sulfothiorine, sodium bisulfite or S-WAT; Described pH value conditioning agent is sodium hydroxide, potassium hydroxide, sodium carbonate or sodium bicarbonate.
In above-mentioned technology, the amide group generation crosslinking reaction of organic crosslinking agent mainly and on polyacrylamide amine molecule, prepares gel plugging agent.When this gel plugging agent is used for profile control and water plugging, because the temperature on stratum is generally all higher, and under hot conditions, first the amide group not occurring on crosslinked polyacrylamide amine molecule can be hydrolyzed, and under the alkaline environment on stratum, forms carboxylic sodium base; When being all hydrolyzed into after carboxylic sodium base for crosslinked amide group in polyacrylamide amine molecule, further hydrolysis reaction can occur with the polyacrylamide amine molecule amide group place of link at organic crosslinking agent, linking agent and polyacrylamide are crosslinked to be dissociated gradually, and what in macroscopic view, see is the broken glue dehydration of polymer gel.Therefore when this gel plugging agent is applied under high temperature, high salinity condition, have that the thermostability time is short, validity period is short, do not reach the problem of plugging effect.
Summary of the invention
Technical problem to be solved by this invention be in prior art gel plugging agent in the time that hot conditions is applied, have that the thermostability time is short, shutoff validity period is short, do not reach the problem of plugging effect, and then provide macropore long, that plugging effect is good of a kind of thermostability time compound shutoff system.
In order to solve the problems of the technologies described above, the invention provides the compound shutoff system of a kind of macropore, comprise that concentration is amphiprotic polyacrylamide solution, flocculation agent solution and the inorganic particle of 0.2～0.5wt%;
Wherein, described flocculation agent solution is that concentration is the cation type polymer solution of 0.2～0.5wt% or the cats product solution that concentration is 1～4wt%.
Cation type polymer in described cation type polymer solution is any one or a few in your glue of cationic modified starch, cationic polyacrylamide, cation-modified Mierocrystalline cellulose or cation-modified guanidine; Cats product in described cats product solution is quaternary ammonium salt cationic surfactant.
Described quaternary ammonium salt cationic surfactant is any one or a few in Dodecyl trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride, octadecyl dimethyl hydroxyethyl ammonium nitrate.
Cation type polymer in described flocculation agent solution or the cationic degree of cats product are 20%-25%.
The addition of described inorganic particle accounts for 3～8wt% of described amphiprotic polyacrylamide solution total mass.
The particle diameter of described inorganic particle is 100 order～200 orders.
In mass, described amphiprotic polyacrylamide solution is 1:1～3:1 with the addition ratio of described flocculation agent solution.
The present invention also further provides the preparation method of the compound shutoff system of described macropore, comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added to the water, stirs, obtain amphiprotic polyacrylamide solution;
(2) to the inorganic particle that adds specified quantitative in the amphiprotic polyacrylamide solution in described step (1), stir, obtain mixing solutions;
(3) cation type polymer of specified quantitative or cats product are slowly added to the water, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions contacts and generates compound shutoff system with described flocculation agent solution.
In described step (1), amphiprotic polyacrylamide and water stir after 30min under 680-720r/min stirring velocity, and stirring velocity is dropped to 380-420r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 1.5-2h.
In described step (2), described amphiprotic polyacrylamide solution and inorganic particle stir 15min under the stirring velocity of 680～720r/min, the mixing solutions that obtains mixing.
In described step (3), described cats product and water stir 10min under the stirring velocity of 380-420r/min, or described cation type polymer and water stir 30min-2h, the flocculation agent solution that obtains mixing under the stirring velocity of 380-420r/min.
In described step (4), described mixing solutions and described flocculation agent solution are shaken under the concussion speed of 50～100 times/min, make its short mix evenly and complete reaction, obtain compound shutoff system.
The present invention compared with prior art tool has the following advantages:
(1) the compound shutoff system of macropore of the present invention, adopt amphiprotic polyacrylamide solution, because amphiprotic polyacrylamide can be along rotating to form and curl structure in C-C key (σ key) in water, but its bond angle remain 109 ° 28 ', the curling structure and can occur mutually to tangle of amphiprotic polyacrylamide, entanglement of formation " key ", in addition, in amphiprotic polyacrylamide chain link-NH2 is while being replaced by negatively charged ion and positively charged ion simultaneously, entanglement of formation between amphiprotic polyacrylamide molecule " key ", can also be in molecule and intermolecular generation ionic linkage and association key, ionic linkage, association key and tangle " key ", can produce Macintosh, Macintosh acting in conjunction can connect into amphiprotic polyacrylamide a supramolecular structure, when amphiprotic polyacrylamide forms supramolecular structure, the cation group in amphiprotic polyacrylamide can also adsorb inorganic particle, and anionic group is exposed, and inorganic particle can be dispersed in amphiprotic polyacrylamide solution, in the time that amphiprotic polyacrylamide solution contacts with flocculation agent solution, the cation group of the exposed anionic group in amphiprotic polyacrylamide solution in flocculation agent solution can be combined in the mode of ionic linkage rapidly, forms compound shutoff system, in addition because stratum sandstone surface is electronegativity, the anionic group of being combined with cation group in amphiprotic polyacrylamide solution like this and stratum sandstone be due to the effect of electrically repelling each other, and makes compound occluding body tie up to dispersion stabilization in stratum good.Because compound shutoff system of the present invention is by the cation group bonding in anionic group and flocculation agent in amphiprotic polyacrylamide, replaced in prior art conventionally need to be in polyacrylamide the crosslinked mode in amido linkage place, also just overcome when amido linkage place is crosslinked the problem that is easy to hydrolysis under high temperature, high salinity, causes plugging agent heatproof, the weak effect of resistance to salinity.The compound shutoff system of macropore of the present invention, can adopt the oil-field water of high salinity to prepare, and has advantages of that elasticity is strong, blocking ability is strong, heatproof is effective, resistance to salinity is effective, shutoff validity period is long.
(2) the compound shutoff system of macropore of the present invention, while further selecting the apparent viscosity > 150mPas of amphiprotic polyacrylamide solution, amphiprotic polyacrylamide solution can play good suspension effect to inorganic particle; Equally, further select the addition of described inorganic particle to account for 3～8wt% of described amphiprotic polyacrylamide solution total mass, also be to make amphiprotic polyacrylamide solution play good suspension effect to inorganic particle, can make like this inorganic particle well mix with amphiprotic polyacrylamide solution, can not produce demixing phenomenon; Further, when the mass ratio of the interpolation of described amphiprotic polyacrylamide solution and described flocculation agent solution is 1:1～3:1, can make compound occluding body cording have suitable strength, while using it for Water in Water Shutoff in Oil Field, there is best heatproof effect and best shutoff validity period.
(3) preparation method of the compound shutoff system of macropore of the present invention, first the amphiprotic polyacrylamide of specified quantitative is slowly added to the water, stir, can make like this between polymer molecular chain by being wound around more stable that " key " is wound around mutually, near and the certain inner chamber of enrichment winding " key ", along with stirring is carried out, part water molecules can enter inner chamber, finally can form the amphiprotic polyacrylamide solution with rock steady structure; Add inorganic particle to stating in amphiprotic polyacrylamide solution again, now continue stirring and can make the cation group absorption inorganic particle in amphiprotic polyacrylamide solution, anionic group is outside exposed, thereby inorganic particle is had to good suspended dispersed effect; The cation type polymer of specified quantitative or cats product are slowly added to the water, stir, obtain after flocculation agent solution, again the amphiprotic polyacrylamide solution that carries inorganic particle is mixed with described flocculation agent solution, owing to thering is a large amount of exposed negatively charged ion in amphiprotic polyacrylamide solution, and in flocculation agent solution, contain a large amount of positively charged ions, two kinds of solution one contact, positively charged ion can be combined by ionic linkage with negatively charged ion, and moment completes reaction, generates compound shutoff system.The preparation method of the compound shutoff system of macropore of the present invention, have advantages of be swift in response, easy construction.
Embodiment
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.
Embodiment 1
The compound shutoff system of macropore described in the present embodiment, the amphiprotic polyacrylamide solution that the concentration that comprises 1kg is 0.2wt%, cationic polyacrylamide solution that the concentration of 1kg is 0.2wt% and the particle diameter of 0.03kg are 100 object activated Calcium carbonates.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 3000mg/L, under 680r/min stirring velocity, stir after 30min, stirring velocity is dropped to 420r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 2h.
(2) to the activated Calcium carbonate that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 680r/min, stir 15min, stir, obtain mixing solutions;
(3) cationic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 3000mg/L, under the stirring velocity of 380r/min, stir 30min, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions and described flocculation agent solution shake under the concussion speed of 50 times/min, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 2
The compound shutoff system of macropore described in the present embodiment, the amphiprotic polyacrylamide solution that the concentration that comprises 1.5kg is 0.3wt%, Dodecyl trimethyl ammonium chloride solution that the concentration of 1kg is 1wt% and the particle diameter of 0.075kg are 120 object activated Calcium carbonates.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 5000mg/L, under 680r/min stirring velocity, stir after 30min, stirring velocity is dropped to 420r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 2h.
(2) to the activated Calcium carbonate that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 680r/min, stir 15min, stir, obtain mixing solutions;
(3) Dodecyl trimethyl ammonium chloride of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 5000mg/L, under the stirring velocity of 380r/min, stir 10min, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions and described flocculation agent solution shake under the concussion speed of 90 times/min, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 3
The compound shutoff system of macropore described in the present embodiment, the amphiprotic polyacrylamide solution that the concentration that comprises 2kg is 0.35wt%, dodecyl benzyl dimethyl ammonium chloride solution that the concentration of 1kg is 2.5wt% and the particle diameter of 0.12kg are 150 object flyash.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 10000mg/L, under 700r/min stirring velocity, stir after 30min, stirring velocity is dropped to 400r/min, after continuing to stir 1.8h, obtain the amphiprotic polyacrylamide solution mixing;
(2) to the flyash that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 700r/min, stir 15min, stir, obtain mixing solutions;
(3) dodecyl benzyl dimethyl ammonium chloride of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 10000mg/L, under the stirring velocity of 400r/min, stir 10min, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions and described flocculation agent solution shake under the concussion speed of 50 times/min, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 4
The compound shutoff system of macropore described in the present embodiment, the amphiprotic polyacrylamide solution that the concentration that comprises 2.5kg is 0.4wt%, cation-modified Mierocrystalline cellulose that the concentration of 1kg is 0.3wt% and the particle diameter of 0.175kg are 170 object activated Calcium carbonates.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 15000mg/L, under 720r/min stirring velocity, stir after 30min, stirring velocity is dropped to 380r/min, continue to obtain after stirring 2h the amphiprotic polyacrylamide solution mixing;
(2) to the activated Calcium carbonate that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 720r/min, stir 15min, stir, obtain mixing solutions;
(3) the cation-modified Mierocrystalline cellulose of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 15000mg/L, under the stirring velocity of 380r/min, stir 2h, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions and described flocculation agent solution shake under the concussion speed of 60 times/min, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 5
The compound shutoff system of macropore described in the present embodiment, the amphiprotic polyacrylamide solution that the concentration that comprises 3kg is 0.5wt%, cationic modified starch solution that the concentration of 1kg is 0.5wt% and the particle diameter of 0.24kg are 200 object activated Calcium carbonates.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 20000mg/L, under 680r/min stirring velocity, stir after 30min, stirring velocity is dropped to 420r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 2h.
(2) to the activated Calcium carbonate that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 690r/min, stir 15min, stir, obtain mixing solutions;
(3) cationic modified starch of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 20000mg/L, under the stirring velocity of 400r/min, stir 1h, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions and described flocculation agent solution shake under the concussion speed of 70 times/min, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 6
The compound shutoff system of macropore described in the present embodiment, the cationic modified starch that the cation-modified guanidine that glue that the amphiprotic polyacrylamide solution that the concentration that comprises 1.2kg is 0.25wt%, the concentration of 0.5kg are 0.4wt%, the concentration of 0.5kg are 0.4wt% and the particle diameter of 0.06kg are 100～200 object calcium carbonate.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 25000mg/L, under 700r/min stirring velocity, stir after 30min, stirring velocity is dropped to 400r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 1.8h;
(2) to the calcium carbonate that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 710r/min, stir 15min, stir, obtain mixing solutions;
(3) your glue of cation-modified guanidine of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 25000mg/L, under the stirring velocity of 420r/min, stir 30min, stir, obtain the first flocculation agent solution; The cationic modified starch of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 25000mg/L, under the stirring velocity of 380r/min, stir 2h, stir, obtain the second flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the first flocculation agent solution, the second flocculation agent solution in described step (3), described mixing solutions and described the first flocculation agent solution and the second flocculation agent solution shake under the concussion speed of 80 times/min, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 7
The compound shutoff system of macropore described in the present embodiment, the Dodecyl trimethyl ammonium chloride that the octadecyl dimethyl hydroxyethyl ammonium nitrate that the amphiprotic polyacrylamide solution that the concentration that comprises 1.8kg is 0.45wt%, the concentration of 0.5kg are 4wt%, the concentration of 0.5kg are 4wt% and the particle diameter of 0.099kg are 200 object silicon powders.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 30000mg/L, under 720r/min stirring velocity, stir after 30min, stirring velocity is dropped to 380r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 2h;
(2) to the silicon powder that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 680r/min, stir 15min, stir, obtain mixing solutions;
(3) the octadecyl dimethyl hydroxyethyl ammonium nitrate of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 30000mg/L, under the stirring velocity of 420r/min, stir 10min, stir, obtain the first flocculation agent solution; The Dodecyl trimethyl ammonium chloride of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 30000mg/L, under the stirring velocity of 420r/min, stir 10min, stir, obtain the second flocculation agent solution
(4) mixing solutions in described step (2) is mixed with the first flocculation agent solution, the second flocculation agent solution in described step (3), described mixing solutions and described the first flocculation agent solution and the second flocculation agent solution, under the concussion speed of 100 times/min, shake, make its short mix evenly and generate rapidly compound shutoff system.
Embodiment 8
The compound shutoff system of macropore described in the present embodiment, the amphiprotic polyacrylamide solution that the concentration that comprises 1.2kg is 0.45wt%, octadecyl dimethyl hydroxyethyl ammonium nitrate that the concentration of 1.2kg is 4wt% and the particle diameter of 0.1kg are 245 object activated Calcium carbonates.
The preparation method of the compound shutoff system of macropore described in the present embodiment comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 22000mg/L, under 720r/min stirring velocity, stir after 30min, stirring velocity is dropped to 420r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 2h;
(2) to the activated Calcium carbonate that adds the specified particle diameter of specified quantitative in the amphiprotic polyacrylamide solution in described step (1), under the stirring velocity of 720r/min, stir 15min, stir, obtain mixing solutions;
(3) cationic polyacrylamide of specified quantitative is slowly added in the oilfield injection water that the salinity of specified quantitative is 22000mg/L, under the stirring velocity of 420r/min, stir 1.5h, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), under the concussion speed of 100 times/min, shake, make its short mix evenly and generate rapidly compound shutoff system.
Performance measurement evaluation Example
(1) quantitative measurement evaluation Example
Adopt CT3 matter structure instrument to carry out intensity test to the compound shutoff system preparing in above-mentioned all embodiment 1～8, test result is in table 1.
The quantitative measurement result of the compound shutoff system of table 1
| Embodiment numbering | Ultimate compression strength/N |
| 1 | 1000 |
| 2 | 1025 |
| 3 | 1285 |
| 4 | 1725 |
| 5 | 2025 |
| 6 | 1680 |
| 7 | 3100 |
| 8 | 3615 |
As shown in Table 1, more than the ultimate compression strength of the core simulating test that compound shutoff system of the present invention is carried out can reach 1000N, show that compound occluding body of the present invention system at high temperature, have very strong shutoff stability under high salinity, can guarantee effective macropore plugging in site operation, improve oil recovery factor.
(2) sealing ratiod test evaluation example
In the preparation process of the compound shutoff system of macropore of the present invention, because the amphiprotic polyacrylamide solution mixing with inorganic particle is in the time contacting with flocculation agent solution, can generate compound shutoff system moment, (two-fluid process refers to and uses two kinds of different working fluids two-fluid process on the compound oil field of its feature in conventional water plugging and profile controlling method, separate with spacer pad, alternately inject stratum, through being extrapolated in stratum after certain distance, there is chemical reaction and produce shutoff material in two kinds of working fluid contacts), therefore in carrying out shutoff process of the test, the rock core of the compound shutoff system simulated field reservoir condition to described in embodiment 1～8 adopt two-fluid process to carry out simulation test.
Adopt respectively the proportioning of the compound shutoff system described in embodiment 1～8 to carry out following simulation test, the temperature of simulation test is 60～80 ℃, the rock core test of simulated field reservoir condition is: get length 0.9m-1.1m, the rock core of diameter 0.03m-0.04m, water drive is surveyed its stifled front rate of permeation K to pressure-stabilisation
w0,---the flocculation agent solution of the certain concentration of injection specified quantitative---injection spacer pad 4ml---the injection amphiprotic polyacrylamide solution of certain concentration of specified quantitative and the mixing solutions of the inorganic particle of specified quantitative---injection spacer pad 4ml---the flocculation agent solution of the certain concentration of injection specified quantitative---follow-up water drive of injection spacer pad 4ml---the injection amphiprotic polyacrylamide solution of certain concentration of specified quantitative and mixing solutions of the inorganic particle of specified quantitative---that employing following steps are carried out shutoff test: water drive survey core permeability, until water drive to pressure-stabilisation, survey the stifled rear rate of permeation K of rock core
w1, and press formula
calculate reservoir core plugging rate.Experimental result is in table 2.
In order to further illustrate the concrete grammar of above-mentioned simulation test, the present invention further, be elaborated with the method that adopts the compound shutoff system proportioning described in embodiment 2 to carry out simulation test, other embodiment all adopts the simulation test identical with the method to test, specific as follows:
Get length 1.1m, the rock core of diameter 0.04m, is 70 ℃ in temperature, and water drive is surveyed its stifled front rate of permeation K to pressure-stabilisation
w0=14.6 μ m
2,---the Dodecyl trimethyl ammonium chloride solution 0.04PV (wherein PV refers to rock pore volume) that implantation concentration is 1wt%------the amphiprotic polyacrylamide solution that the concentration of injecting 1.5kg is 0.3wt% is the mixing solutions 0.06PV of 120 object activated Calcium carbonates with the particle diameter of 0.075kg------the flocculation agent solution 0.04PV that implantation concentration is 1wt%------the amphiprotic polyacrylamide solution that the concentration of injection 1.5kg is 0.3wt% and the particle diameter of 0.075kg are the mixing solutions 0.06PV of 120 object activated Calcium carbonates---the follow-up water drive 3PV that injects spacer pad 4ml that injects spacer pad 4ml that injects spacer pad 4ml that adopts following steps to carry out shutoff test: water drive is surveyed core permeability, until water drive to pressure-stabilisation, survey the stifled rear rate of permeation K of rock core
w1=0.9928 μ m
2, and press formula
calculate reservoir core plugging rate, experimental result is in table 2.
Need to be to above-mentioned simulation test with further illustrating, due to the density of flocculation agent solution and the density of described amphiprotic polyacrylamide solution basic identical, so, in simulation test, adopt volume ratio to replace the mass ratio in embodiment to carry out core simulating test.In addition for above-mentioned simulation test, all carry out core simulating test three times by the proportioning in each embodiment, get the mean value of its test result as final testing result.
Through respectively above-described embodiment 1～8 being undertaken after simulation test by the rock core test method of above-mentioned simulated field reservoir condition, the sealing ratiod of testing rock core, result is as shown in table 2:
Table 2 core simulating test sealing ratiod test result
| Embodiment numbering | Kwo/μm 2 | Kw1/μm 2 | 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, adopt the sealing ratiod of the core simulating test that compound shutoff system of the present invention carries out can reach more than 90%, result shows, compound occluding body of the present invention ties up to has very strong sealing characteristics under high temperature, high salinity, can guarantee effective macropore plugging in site operation, improve oil recovery factor.
Obviously, above-described embodiment is only for example is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments, and the apparent variation of being extended out thus or variation are still among the protection domain in the invention claim.
Claims (10)
1. the compound shutoff system of macropore, is characterized in that, comprises that concentration is amphiprotic polyacrylamide solution, flocculation agent solution and the inorganic particle of 0.2～0.5wt%;
Wherein, described flocculation agent solution is that concentration is the cation type polymer solution of 0.2～0.5wt% or the cats product solution that concentration is 1～4wt%.
2. the compound shutoff system of macropore according to claim 1, it is characterized in that, the cation type polymer in described cation type polymer solution is any one or a few in your glue of cationic modified starch, cationic polyacrylamide, cation-modified Mierocrystalline cellulose or cation-modified guanidine; Cats product in described cats product solution is quaternary ammonium salt cationic surfactant.
3. the compound shutoff system of macropore according to claim 2, it is characterized in that, described quaternary ammonium salt cationic surfactant is any one or a few in Dodecyl trimethyl ammonium chloride, dodecyl benzyl dimethyl ammonium chloride, octadecyl dimethyl hydroxyethyl ammonium nitrate.
4. according to the compound shutoff system of the arbitrary described macropore of claim 1～3, it is characterized in that, the cation type polymer in described flocculation agent solution or the cationic degree of cats product are 20%-25%.
5. according to the compound shutoff system of the arbitrary described macropore of claim 1～4, it is characterized in that, the addition of described inorganic particle accounts for 3～8wt% of described amphiprotic polyacrylamide solution total mass.
6. according to the compound shutoff system of the arbitrary described macropore of claim 1～5, it is characterized in that, the particle diameter of described inorganic particle is 100 order～200 orders.
7. according to the compound shutoff system of the arbitrary described macropore of claim 1～6, it is characterized in that, in mass, described amphiprotic polyacrylamide solution is 1:1～3:1 with the addition ratio of described flocculation agent solution.
8. the preparation method of the compound shutoff system of the arbitrary described macropore of claim 1～7, comprises the steps:
(1) amphiprotic polyacrylamide of specified quantitative is slowly added to the water, stirs, obtain amphiprotic polyacrylamide solution;
(2) to the inorganic particle that adds specified quantitative in the amphiprotic polyacrylamide solution in described step (1), stir, obtain mixing solutions;
(3) cation type polymer of specified quantitative or cats product are slowly added to the water, stir, obtain flocculation agent solution;
(4) mixing solutions in described step (2) is mixed with the flocculation agent solution in described step (3), described mixing solutions contacts and generates compound shutoff system with described flocculation agent solution.
9. preparation method according to claim 8, it is characterized in that, in described step (1), amphiprotic polyacrylamide and water stir after 30min under 680-720r/min stirring velocity, stirring velocity is dropped to 380-420r/min, continue to stir the amphiprotic polyacrylamide solution that obtains mixing after 1.5-2h.
According to claim 8 or claim 9, preparation method, is characterized in that, in described step (2), described amphiprotic polyacrylamide solution and inorganic particle stir 15min under the stirring velocity of 680～720r/min, the mixing solutions that obtains mixing.
Preparation method according to claim 8 or claim 9, it is characterized in that, in described step (3), described cats product and water stir 10min under the stirring velocity of 380-420r/min, or described cation type polymer and water stir 30min-2h, the flocculation agent solution that obtains mixing under the stirring velocity of 380-420r/min.
10. according to Claim 8～9 arbitrary described preparation methods, it is characterized in that, in described step (4), described mixing solutions and described flocculation agent solution are shaken under the concussion speed of 50～100 times/min, make its short mix evenly and complete reaction, obtain compound shutoff system.
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