CN118027916A - Mesoporous silica grafted perfluoro ester nano plugging agent and oil-based drilling fluid - Google Patents
Mesoporous silica grafted perfluoro ester nano plugging agent and oil-based drilling fluid Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 66
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 58
- -1 perfluoro ester Chemical class 0.000 title claims abstract description 55
- 238000005553 drilling Methods 0.000 title claims abstract description 48
- 239000012530 fluid Substances 0.000 title claims abstract description 45
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 8
- 229940126062 Compound A Drugs 0.000 claims description 8
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 229930185605 Bisphenol Natural products 0.000 claims description 7
- 239000003995 emulsifying agent Substances 0.000 claims description 7
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- 239000010428 baryte Substances 0.000 claims description 6
- 229910052601 baryte Inorganic materials 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000002689 soil Substances 0.000 claims description 5
- WEERVPDNCOGWJF-UHFFFAOYSA-N 1,4-bis(ethenyl)benzene Chemical group C=CC1=CC=C(C=C)C=C1 WEERVPDNCOGWJF-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- 235000012255 calcium oxide Nutrition 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- RGKUSPKMWIGVLG-UHFFFAOYSA-N n'-(2-aminoethyl)ethane-1,2-diamine;trimethoxy(propyl)silane Chemical compound NCCNCCN.CCC[Si](OC)(OC)OC RGKUSPKMWIGVLG-UHFFFAOYSA-N 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 239000000080 wetting agent Substances 0.000 claims description 4
- FQHLOOOXLDQLPF-UHFFFAOYSA-N 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,11,11,12,12,12-henicosafluorododecyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F FQHLOOOXLDQLPF-UHFFFAOYSA-N 0.000 claims description 3
- AMFGWXWBFGVCKG-UHFFFAOYSA-N Panavia opaque Chemical compound C1=CC(OCC(O)COC(=O)C(=C)C)=CC=C1C(C)(C)C1=CC=C(OCC(O)COC(=O)C(C)=C)C=C1 AMFGWXWBFGVCKG-UHFFFAOYSA-N 0.000 claims description 3
- 239000002199 base oil Substances 0.000 claims description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 19
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
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- 150000002148 esters Chemical class 0.000 description 3
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 238000000227 grinding Methods 0.000 description 1
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- 239000008267 milk Substances 0.000 description 1
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- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical class O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The invention discloses a mesoporous silica grafted perfluoro ester nano plugging agent and an oil-based drilling fluid, and belongs to the technical field of oil and gas field drilling. The mesoporous silica grafted perfluoro ester nanometer plugging agent provided by the invention has the particle size of 90.1-325.8 nm. The plugging agent can be directly added into oil-based drilling fluid, and has little influence on rheological property of the drilling fluid. Compared with the drilling fluid without the plugging agent, the plugging performance of the drilling fluid added with the mesoporous silica grafted perfluoro ester nano plugging agent is obviously improved, the plugging rate of the oil-based drilling fluid is increased along with the increase of the addition amount of the plugging agent, and when the addition amount is 2%, the plugging rate reaches 95.30%. The synthesis method of the plugging agent is stable and reliable, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of drilling of oil and gas fields, in particular to a mesoporous silica grafted perfluoro ester nano plugging agent and an oil-based drilling fluid.
Background
Shale gas is a natural gas resource which is reserved in shale layers and can be mined, and the shale gas in China has huge recoverable reserves. However, in the drilling process at home and abroad, the problem of well wall collapse is frequently encountered due to extremely poor mechanical properties of shale gas stratum. According to statistical analysis of hundreds of wells in Chuan, shale formations in the well account for 70% of the total formation, while over 90% of the well wall collapse events occur on shale formations. Shale formations have special pore structures, which are of the ultra-low porosity and low permeability type, mostly nanoscale pore throats. In order to ensure the economic development of shale gas, horizontal well drilling has become a main shale gas development mode, and meanwhile, the shale gas well can be developed by adopting oil-based drilling fluid, so that the damage to a shale layer can be reduced, but the problem of well wall collapse still occurs in the actual production process. The root cause of this problem is the "hydraulic fracturing action", i.e., the entry of drilling fluid or filtrate into the pore gap, causing it to open while greatly reducing the friction between the fracture faces, resulting in a significant increase in collapse pressure. Therefore, development of nanoscale plugging materials is urgently needed to improve the plugging property of drilling fluid, reduce the entry of the drilling fluid into stratum, avoid well wall collapse and improve the oil and gas exploitation efficiency.
CN114196384B discloses a nano plugging material for drilling fluid, the plugging agent uses carbon modified nano silicon dioxide as matrix, the carbon material is distributed on the outer surface of the matrix, and the highest plugging rate is 85% when the adding amount is 1% under different adding amounts. CN113355069B discloses a modified nano silica plugging agent and oil-based drilling fluid, the final plugging rate is only 83.64%, and the mesoporous silica adopted in the invention has a larger specific surface, is more beneficial to grafting reaction in modification, and can reach more than 85% when the addition amount is 1.0%. CN113292973B discloses a high-temperature resistant silica grafted tertiary amine nano plugging agent and water-based drilling fluid, the product of which is hydrophilic and is not suitable for being used in oil-based drilling fluid. Mesoporous silica is a material with better strength, thermal stability and high specific area, and the mesoporous silica is used as a plugging material, so that the plugging agent can be ensured to keep the shape undamaged in deep wells and ultra-deep wells. Meanwhile, the modified and grafted shale-oriented plastic composite material has a flexible shell, can be better attached to the inner wall of a pore in a stratum, can better block the nano-pore in the shale stratum, and can maintain the stability of a well wall.
Disclosure of Invention
Aiming at the problem that the conventional plugging agent cannot effectively plug nano cracks in shale to cause the collapse of a well wall, the invention provides the mesoporous silica grafted perfluoro ester nano plugging agent, which has the characteristics of nanoscale particle size, external flexibility and internal rigidity, and the external flexible shell can generate partial deformation under the pressure of fluid and the reaction force of the inner wall of a pore throat, so that the external flexible shell is more attached to the inner wall of the pore, and the nanoscale cracks in a shale stratum are effectively plugged, thereby achieving the purpose of stabilizing the well wall. And a novel nano plugging oil-based drilling fluid applicable to shale formations is developed, so that the problem of well wall stability can be solved.
In order to achieve the above purpose, the technical scheme of the invention is as follows: the mesoporous silica grafted perfluoro ester nano plugging agent and the oil-based drilling fluid are characterized in that the mesoporous silica grafted perfluoro ester nano plugging agent is prepared by the following steps:
S1, adding 6.00-9.00 g mesoporous silica into 140-180 mL of toluene, performing ultrasonic dispersion for 15-30 min, adjusting the pH value to 4-5 by using hydrochloric acid, adding 150-225 mL of amino-containing silane coupling agent with the concentration of 14%, performing ultrasonic dispersion for 15-30 min, reacting for 5.0-6.0 h at 70-80 ℃, performing reduced pressure distillation for 1.5-2.0 h after the reaction is finished, washing for 3 times by using ethanol, and performing vacuum drying for 22.0-24.0 h at 60-65 ℃ to obtain a compound A;
S2, adding 16.25-24.37 g of the compound A obtained in the step S1 into 200-240 mL of methanol, adding 0.15-0.30 mol of bisphenol compound containing olefinic bonds, heating to 50-55 ℃ under the protection of nitrogen, reacting for 20.0-24.0 h, centrifuging after the reaction is finished, washing 3 times by using methanol, vacuum drying for 22.0-24.0 h at 60-65 ℃, adding 0.05-0.10 mol of dried product into 200-250 mL of toluene, performing ultrasonic dispersion for 15-30 min, slowly adding 0.15-0.30 mol of sulfone compound containing olefinic bonds, introducing nitrogen for 0.5-1.0 h, heating to 60-65 ℃, reacting for 42.0-48.0 h, performing reduced pressure distillation for 1.5-2.0 h, washing 3 times by using ethanol, and vacuum drying for 22.0-24.0 h at 60-65 ℃ to obtain a compound B;
S3, adding 83.80-128.11 g of the compound B obtained in the step S2 into 300-360 mL of toluene, adding 0.09-0.18 mol of perfluoro ester compound containing olefinic bonds and vinyl benzene cross-linking agent, heating to 60-65 ℃, performing ultrasonic dispersion for 15-30 min, adding 0.001-0.002 mol of catalyst potassium persulfate to react for 42.0-48.0 h, performing reduced pressure distillation for 1.5-2.0 h, washing with ethanol for 3 times after the reaction is finished, and performing vacuum drying at 60-65 ℃ for 22.0-24.0 h to obtain the mesoporous silica grafted perfluoro ester nano plugging agent;
The average particle diameter of the mesoporous silica in the step S1 is in the range of 40-55 nm.
The mesoporous silica grafted perfluoro ester nano plugging agent is a plugging agent for oil-based drilling fluid.
The bisphenol compound containing the olefinic bond is one of bisphenol alpha dimethacrylate and bisphenol A glycerol dimethacrylate; the silane coupling agent containing amino is diethylenetriamine propyl trimethoxy silane; the sulfone compound containing the diene bond is 1,1' -sulfonyl bis [4- (2-propylene) oxybenzene ]; the perfluoro ester compound containing olefinic bond is one of 2- (perfluoro decyl) ethyl methacrylate and 2-perfluoro decyl ethyl acrylate; the divinylbenzene-type cross-linking agent is p-divinylbenzene.
The oil-based drilling fluid of claim 3, wherein: 70 to 80 parts by weight of base oil 3# white oil, 20.0 to 30.0 parts by weight of CaCl 2 brine with the concentration of 25%, 3.0 to 4.0 parts by weight of main emulsifier HW Pmul-1,2.0 to 2.5 parts by weight of auxiliary emulsifier HW Smul-1,3.0 to 5.0 parts by weight of organic soil HW-Gel-3,2.0 to 4.0 parts by weight of wetting agent HW-Wet-1,2.0 to 3.5 parts by weight of quicklime, 3.0 to 4.0 parts by weight of filtrate reducer HWLC-1,2.0 to 5.0 parts by weight of superfine calcium carbonate, and 0.5 to 2.0 parts by weight of mesoporous silica grafted perfluorinated ester nanometer plugging agent and a plurality of parts by weight of barite.
The density of the oil-based drilling fluid is regulated to be 1.0-2.2 g/cm 3 by barite.
The invention has the following beneficial effects:
1. the synthesis method of the invention is simple, stable and reliable, and the source of the compound needed by synthesis is sufficient, and the invention is easy to produce.
2. The shale blocking agent provided by the invention has stable performance, good high-temperature resistance and excellent blocking performance, and can meet the drilling requirements of various complex well conditions.
3. The shale plugging agent provided by the invention has the particle size of 90.1-325.8 nm, has the characteristic of external softness and internal rigidity after modification, and can generate partial deformation under the pressure of fluid and the reaction force of the inner wall of the pore throat, so that the shale plugging agent is more attached to the inner wall of the pore, and can better plug the nano-pore seams in the shale stratum.
Drawings
FIG. 1 is a graph showing the particle size distribution of mesoporous silica grafted perfluoro ester nano plugging agent of example 1;
FIG. 2 is a graph showing the particle size distribution of mesoporous silica grafted perfluoroester nanosealing agents of example 2.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In this example, unless otherwise specified, the parts are parts by weight.
1. Synthesizing the mesoporous silica grafted perfluoro ester nanometer plugging agent:
Example 1:
S1, adding 6.00g of mesoporous silica into 140mL of toluene, performing ultrasonic dispersion for 20min, adjusting the pH value to 5 by using hydrochloric acid, adding 150mL of diethylenetriamine propyl trimethoxy silane with the concentration of 14%, performing ultrasonic dispersion for 20min, reacting for 5.0h at 70 ℃, performing reduced pressure distillation for 2.0h after the reaction is finished, washing for 3 times by using ethanol, and performing vacuum drying at 60 ℃ for 24.0h to obtain a compound A;
S2, adding 16.25g of the compound A obtained in the step S1 into 200-240 mL of methanol, adding 54.66g of bisphenol alpha dimethacrylate, heating to 50 ℃ under the protection of nitrogen, reacting for 24.0h, centrifugally separating, washing 3 times by using methanol, vacuum drying at 60 ℃ for 24.0h, taking 70.61g of dried product, adding into 200mL of toluene, ultrasonically dispersing for 20min, introducing nitrogen for 1.0h, slowly adding 39.81g of 1,1' -sulfonyl bis [4- (2-propylene) oxybenzene ], heating to 60-65 ℃, reacting for 48.0h, decompressing and distilling for 2.0h, washing 3 times by using ethanol, and vacuum drying at 60 ℃ for 24.0h to obtain the compound B;
S3, adding 83.80g of the compound B obtained in the step S2 into 300mL of toluene, adding 55.63g of 2-perfluorodecyl ethyl acrylate and 11.70g of p-divinylbenzene, heating to 60 ℃, performing ultrasonic dispersion for 20min, adding 0.27g of catalyst potassium persulfate to react for 48.0h, performing reduced pressure distillation for 2.0h, washing with ethanol for 3 times after the reaction is finished, and performing vacuum drying at 60 ℃ for 24.0h to obtain the mesoporous silica grafted perfluor ester nano plugging agent;
example 2:
S1, adding 6.00g of mesoporous silica into 160mL of toluene, performing ultrasonic dispersion for 30min, adjusting the pH value to 4 by using hydrochloric acid, adding 150mL of diethylenetriamine propyl trimethoxy silane with the concentration of 14%, performing ultrasonic dispersion for 30min, reacting for 5.0h at 80 ℃, performing reduced pressure distillation for 2.0h after the reaction is finished, washing with ethanol for 3 times, and performing vacuum drying at 65 ℃ for 22.0h to obtain a compound A.
S2, adding 16.25g of the compound A obtained in the step S1 into 240mL of methanol, adding 76.89g of bisphenol A glycerol dimethacrylate, heating to 50 ℃ under the protection of nitrogen, reacting for 24.0h, centrifugally separating, washing 3 times by using methanol, vacuum drying at 65 ℃ for 22.0h, taking 99.16g of dried product, adding into 250mL of toluene, ultrasonically dispersing for 30min, introducing nitrogen for 1.0h, slowly adding 39.81g of 1,1' -sulfonyl bis [4- (2-propylene) oxybenzene ], heating to 65 ℃, reacting for 48.0h, decompressing and distilling for 2.0h after the reaction is finished, washing 3 times by using ethanol, and vacuum drying at 65 ℃ for 22.0h to obtain the compound B.
S3, adding 128.11g of the compound B obtained in the step S2 into 360mL of toluene, adding 52.90g of 2- (perfluorodecyl) ethyl methacrylate and 11.70g of p-divinylbenzene, heating to 60-65 ℃, performing ultrasonic dispersion for 30min, adding 0.27g of catalyst potassium persulfate to react for 48.0h, performing reduced pressure distillation for 2.0h, washing with ethanol for 3 times after the reaction is finished, performing vacuum drying at 65 ℃ for 22.0h, and grinding a dried sample to obtain the mesoporous silica grafted perfluoro ester nano plugging agent.
2. Preparing oil-based drilling fluid:
Directly weighing 4.0 parts of a main emulsifier HW Pmul-1, 2.5 parts of auxiliary milk HW Smul-1 and 4.0 parts of a wetting agent HW-Wet-1 in a high stirring cup; 320mL of 3# white oil is measured and introduced into a high stirring cup, and stirred for 20min; weighing 20.0g of organic soil HW-Gel-3 by using cellophane, and adding 5.0 parts of organic soil HW-Gel-3 into a high stirring cup under a high stirring state, and stirring for 20min; weighing 80mL of CaCl 2 water solution with the concentration of 25%, adding the water solution into a high stirring cup, and stirring for 20min; slowly adding 3.5 parts of quicklime into a high stirring cup under a high stirring state, and stirring for 20min; slowly adding 4.0 parts of filtrate reducer HWLC-1 into a high stirring cup under a high stirring state, and stirring for 20min; slowly adding 4.5 parts of superfine calcium carbonate into a high stirring cup under a high stirring state, and stirring for 20min; under the high stirring state, 207 parts of barite with the density of 4.2g/cm 3 is slowly added into a high stirring cup, and stirring is continued for 30min, so as to prepare the drilling fluid base slurry with the density of 1.95g/cm 3.
Performance testing
To further illustrate the effectiveness of the mesoporous silica grafted perfluoro ester nano plugging agent and oil-based drilling fluids of the present invention, performance tests were performed on the modified tin dioxide strongly adsorbed plugging agents and oil-based drilling fluids of examples 1 and 2.
1. Particle size test of mesoporous silica grafted perfluoro ester nano plugging agent
The particle size of the mesoporous silica grafted perfluoro ester nano plugging agent prepared in the embodiment 1 is shown in a graph 1, the particle size range of the mesoporous silica grafted perfluoro ester nano plugging agent prepared in the embodiment 2 is shown in a graph 2, the particle size range of the mesoporous silica grafted perfluoro ester nano plugging agent prepared in the embodiment 2 is 92.6-325.8 nm, and the particle size range of the mesoporous silica grafted perfluoro ester nano plugging agent is 90.1-325.8 nm as can be seen from the graph 1 and the graph 2, so that the mesoporous silica grafted perfluoro ester nano plugging agent meets the nano plugging requirement.
2. Drilling fluid rheology and high temperature high pressure fluid loss (HTHP) testing
The prepared oil-based drilling fluid (base slurry) is added with mesoporous silica grafted perfluoro ester nano plugging agents in example 1 and example 2 with different addition amounts (calculated according to weight fraction), and the mixture is aged for 16 hours at 160 ℃, and the performance parameters of the oil-based drilling fluid are measured, and the results are shown in table 1.
As can be seen from Table 1, when the addition of the mesoporous silica grafted perfluoro ester nano plugging agent is less than 1.0%, the apparent viscosity and the plastic viscosity of the oil-based drilling fluid slowly increase along with the increase of the addition of the mesoporous silica grafted perfluoro ester nano plugging agent, the dynamic shear force is between 4.5 Pa and 6.0Pa, and the demulsification voltage of the oil-based drilling fluid slightly increases, which indicates that the compatibility of the mesoporous silica grafted perfluoro ester nano plugging agent and the oil-based drilling fluid is better, and the rheological property of the oil-based drilling fluid is less affected. The high-temperature high-pressure filtration loss (HTHP) is reduced along with the increase of the addition of the plugging agent, the high-temperature high-pressure filtration loss is obviously reduced when the addition of the plugging agent is 0.5% -1.0%, and when the addition of the plugging agent exceeds 1.0%, the HTHP change is not obvious, which indicates that the optimal addition of the mesoporous silica grafted perfluoro ester nano plugging agent is 1.0%.
Table 1 oil-based drilling fluid performance tables for different loadings of mesoporous silica grafted perfluoro ester nano plugging agent
Note that: the HTHP temperature was 160℃and the differential pressure was 3.5MPa.
3. Drilling fluid plugging performance test
And simulating a stratum nano-fracture stratum by using the outcrop core, measuring the average flow of a drilling fluid system in the outcrop core, and calculating the permeability K=Q mu L/(A delta P) of the outcrop core before and after the mesoporous silica grafted perfluoro ester nano-plugging agent is added by a Darcy formula, so that the plugging rate of the mesoporous silica grafted perfluoro ester nano-plugging agent on the outcrop core is calculated, and the plugging performance of the outcrop core is evaluated. The blocking rate was (initial permeability-permeability after blocking)/initial permeability×100%.
And the permeability of the outcrop core is tested by using clear water, and the outcrop core with the same permeability is selected to reduce experimental errors. The mesoporous silica grafted perfluoro ester nano plugging agents synthesized in the example 1 and the example 2 with different mass fractions are respectively added into the base slurry, and the influence of the mesoporous silica grafted perfluoro ester nano plugging agent on the permeability of the outcrop core is shown in the table 2.
From table 2, it can be seen that the mesoporous silica grafted perfluoro ester nano plugging agent is used as a nano plugging agent, and can effectively reduce the permeability of the outcrop core and improve the plugging rate. As the addition of the mesoporous silica grafted perfluoro ester nano plugging agent is increased, the permeability is obviously reduced, but when the addition exceeds 1.0%, the permeability is slowly reduced, and the plugging rate change is not obvious, which shows that the optimal addition of the mesoporous silica grafted perfluoro ester nano plugging agent is 1.0%, the plugging effect is excellent, and when the addition of the mesoporous silica grafted perfluoro ester nano plugging agent is 1.0%, the plugging rates measured by the outcrop cores of the embodiment 1 and the embodiment 2 are 91.47% and 91.94%.
TABLE 2 outcrop core permeability data for different addition amounts of mesoporous silica grafted perfluor ester nano plugging agent
In conclusion, the preparation method of the mesoporous silica grafted perfluoro ester nano plugging agent is stable and reliable, and the prepared compound plugging agent has good plugging property, rheological property, oil solubility and dispersibility and excellent well wall stabilizing effect. The plugging agent can achieve excellent plugging effect only by a small amount, and is an effective way for solving the problems of well wall stability and drilling fluid leakage.
The present invention is not limited to the above-mentioned embodiments, but is not limited to the above-mentioned embodiments, and any simple modification, equivalent changes and modification made to the above-mentioned embodiments according to the technical matters of the present invention can be made by those skilled in the art without departing from the scope of the present invention.
Claims (5)
1. The mesoporous silica grafted perfluoro ester nano plugging agent and the oil-based drilling fluid are characterized in that the mesoporous silica grafted perfluoro ester nano plugging agent is prepared by the following steps:
S1, adding 6.00-9.00 g mesoporous silica into 140-180 mL of toluene, performing ultrasonic dispersion for 15-30 min, adjusting the pH value to 4-5 by using hydrochloric acid, adding 150-225 mL of amino-containing silane coupling agent with the concentration of 14%, performing ultrasonic dispersion for 15-30 min, reacting for 5.0-6.0 h at 70-80 ℃, performing reduced pressure distillation for 1.5-2.0 h after the reaction is finished, washing for 3 times by using ethanol, and performing vacuum drying for 22.0-24.0 h at 60-65 ℃ to obtain a compound A;
S2, adding 16.25-24.37 g of the compound A obtained in the step S1 into 200-240 mL of methanol, adding 0.15-0.30 mol of bisphenol compound containing olefinic bonds, heating to 50-55 ℃ under the protection of nitrogen, reacting for 20.0-24.0 h, centrifuging after the reaction is finished, washing 3 times by using methanol, vacuum drying for 22.0-24.0 h at 60-65 ℃, adding 0.05-0.10 mol of dried product into 200-250 mL of toluene, performing ultrasonic dispersion for 15-30 min, slowly adding 0.15-0.30 mol of sulfone compound containing olefinic bonds, introducing nitrogen for 0.5-1.0 h, heating to 60-65 ℃, reacting for 42.0-48.0 h, performing reduced pressure distillation for 1.5-2.0 h, washing 3 times by using ethanol, and vacuum drying for 22.0-24.0 h at 60-65 ℃ to obtain a compound B;
S3, adding 83.80-128.11 g of the compound B obtained in the step S2 into 300-360 mL of toluene, adding 0.09-0.18 mol of perfluoro ester compound containing olefinic bonds and vinyl benzene cross-linking agent, heating to 60-65 ℃, performing ultrasonic dispersion for 15-30 min, adding 0.001-0.002 mol of catalyst potassium persulfate to react for 42.0-48.0 h, performing reduced pressure distillation for 1.5-2.0 h, washing with ethanol for 3 times after the reaction is finished, and performing vacuum drying at 60-65 ℃ for 22.0-24.0 h to obtain the mesoporous silica grafted perfluoro ester nano plugging agent;
Wherein the bisphenol compound containing olefinic bond is one of bisphenol alpha dimethacrylate and bisphenol A glycerol dimethacrylate; the silane coupling agent containing amino is diethylenetriamine propyl trimethoxy silane; the sulfone compound containing the diene bond is 1,1' -sulfonyl bis [4- (2-propylene) oxybenzene ]; the perfluoro ester compound containing olefinic bond is one of 2- (perfluoro decyl) ethyl methacrylate and 2-perfluoro decyl ethyl acrylate; the divinylbenzene-type cross-linking agent is p-divinylbenzene.
2. The mesoporous silica grafted perfluoro ester nano plugging agent according to claim 1, wherein the particle size of the nano silica in the step S1 is 40-55 nm.
3. The mesoporous silica grafted perfluoro ester nano plugging agent and oil-based drilling fluid according to claim 1, wherein the drilling fluid comprises the following components: base oil 3# white oil, caCl 2 brine with the concentration of 25%, a main emulsifier HW Pmul-1, an auxiliary emulsifier HW Smul-1, organic soil HW-Gel-3, a wetting agent HW-Wet-1, quicklime, superfine calcium carbonate, a filtrate reducer HWLC-1, a mesoporous silica grafted perfluoro ester nano plugging agent and barite.
4. The oil-based drilling fluid of claim 4, wherein: 70-80 parts of base oil 3# white oil, 20-30 parts of CaCl 2 brine with the concentration of 25%, 3.0-4.0 parts of main emulsifier HW Pmul-1, 2.0-2.5 parts of auxiliary emulsifier HW Smul-1,3.0-5.0 parts of organic soil HW-Gel-3,2.0-4.0 parts of wetting agent HW-Wet-1, 2.0-3.5 parts of quicklime, 3.0-4.0 parts of filtrate reducer HWLC-1, 2.0-5.0 parts of superfine calcium carbonate, 0.5-2.0 parts of mesoporous silica grafted perfluoro ester nano plugging agent and a plurality of parts of barite.
5. The oil-based drilling fluid according to claim 4, wherein the oil-based drilling fluid has a density adjusted to 1.0-2.2 g/cm 3 with barite.
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