CN112430455A - Nano plugging agent and preparation method and application thereof - Google Patents
Nano plugging agent and preparation method and application thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices, or the like
- E21B33/138—Plastering the borehole wall; Injecting into the formation
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- C09K2208/10—Nanoparticle-containing well treatment fluids
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/18—Bridging agents, i.e. particles for temporarily filling the pores of a formation; Graded salts
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/34—Lubricant additives
Abstract
The invention provides a nano plugging agent and a preparation method and application thereof, wherein the nano plugging agent comprises the following components in parts by weight: white oil: 500-600 parts; graphene: 5 parts of a mixture; modifying agent: 5 parts of a mixture; nano calcium carbonate: 300-350 parts; nano silicon dioxide: 30-50 parts; a stabilizer: 20-40 parts. The nano plugging agent provided by the invention has a wide particle size distribution range, and can meet the plugging requirements of nano-pores of different shale strata in the drilling process.
Description
Technical Field
The invention relates to the technical field of petroleum drilling, in particular to a nano plugging agent and a preparation method and application thereof.
Background
In the drilling construction of a shale gas horizontal well, the problem of instability of a shale stratum well wall is solved firstly, the good plugging performance of the drilling fluid is one of main factors for ensuring the stability of the well wall, and the plugging agent matched with the stratum is the key of the good plugging capability of the drilling fluid. For the microcracks and pores of the shale stratum, the majority of microcracks and pores belong to the micro-nanometer level, the pores are extremely tiny, and the conventional micron-sized plugging agent has the particle size distribution limited in the micron level due to the large particle size, so that the ideal plugging effect cannot be achieved due to the mismatch of the particle size distribution and the nanometer-sized pore size of the shale stratum.
Disclosure of Invention
In view of the above, the main objective of the present invention is to provide a nano plugging agent, a preparation method and an application thereof, and to solve the technical problem of stably dispersing graphene and other nano materials in a base oil in a nano scale to achieve a good plugging property; the nano plugging agent has the technical characteristics that the particle size distribution can be adjusted according to the pore size of the shale stratum, so that the plugging and anti-collapse requirements of different stratums are met.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a nano plugging agent, which comprises the following components in parts by weight:
white oil: 500-600 parts;
graphene: 5 parts of a mixture;
modifying agent: 5 parts of a mixture;
nano calcium carbonate: 300-350 parts;
nano silicon dioxide: 30-50 parts;
a stabilizer: 20-40 parts.
The object of the present invention and the technical problems can be further achieved by the following technical measures.
Preferably, in the nano blocking agent, the white oil is light white oil W1-90, W1-100 or W1-110.
Preferably, in the nano plugging agent, the graphene is a nano material, and the particle size of the graphene is 10-100 nm.
Preferably, in the nano blocking agent, the modifier is n-dodecyltriethoxysilane or sodium oleate or sodium alkylsulfonamide acetate.
Preferably, in the nano blocking agent, the particle size of the nano calcium carbonate is 100-1000 nm.
Preferably, in the nano blocking agent, the nano silica has a particle size of 5-50 nm.
Preferably, in the nano plugging agent, the stabilizer is calcium stearate.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The preparation method of the nano plugging agent for the drilling fluid provided by the invention comprises the following steps:
1) adding a modifier into the white oil, uniformly dispersing, then adding graphene into the white oil, and uniformly dispersing to obtain a graphene mother liquor;
2) adding a stabilizer into the graphene mother liquor obtained in the step 1), uniformly dispersing, then sequentially adding nano calcium carbonate and nano silicon dioxide, and uniformly dispersing.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The invention provides an application of a nano plugging agent in drilling fluid plugging.
Preferably, the aforementioned application comprises the following steps: and adding the nano plugging agent into the drilling fluid, and uniformly stirring.
Preferably, in the aforementioned application, the drilling fluid is an oil-based drilling fluid or a water-based drilling fluid.
By the technical scheme, the nano plugging agent and the preparation method and application thereof provided by the invention have the following advantages:
1) the nano plugging agent provided by the invention has a wide particle size distribution range, and can meet the plugging requirements of nano-pore gaps of different shale strata in the drilling process;
2) the nano plugging agent provided by the invention has strong plugging capability, and a rock core (the permeability is less than 0.1) is obtained under the condition that the addition amount of 2% (mass-volume ratio, based on the volume of drilling fluid)10-3μm2) The plugging rate is more than 80 percent, and the plugging rate of the nano filter membrane (100nm, 220nm and 450nm) is more than 95 percent; 2 percent (mass volume ratio, based on the volume of the drilling fluid) of the plugging agent is added into the oil-based drilling fluid, and the HTHP filtration loss reduction rate is more than 30 percent;
3) according to the nano blocking agent provided by the invention, 1.5% of mass-volume ratio is added into the oil-based drilling fluid, based on the volume of the drilling fluid), the AV, PV, YP and initial and final cut change rates of the drilling fluid are all less than 10%, the ES change rate is less than 12%, and meanwhile, the lubricity of the drilling fluid can be improved, and the improvement amplitude is more than 20%.
4) The nano plugging agent provided by the invention has good oil solubility and can be uniformly dispersed in the oil-based drilling fluid; the emulsifier is added, so that the drilling fluid can be uniformly dispersed in the water-based drilling fluid;
5) the nano blocking agent provided by the invention is an off-white fluid, the content of heavy metal is in the range specified by the industry standard SY/T6787-2010, and the nano blocking agent has biotoxicity EC50Greater than 2.5X 104mg/L, non-toxic and environment-friendly;
6) the nano plugging agent provided by the invention has good stability, and the centrifugal sedimentation time is more than 450min under the condition of the rotation speed of 4000rpm so as to ensure that no layering and no precipitation exist for more than one year.
7) The nano plugging agent provided by the invention is suitable for complex wells with high anti-collapse requirements, such as shale gas wells and the like.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to a nano blocking agent, a preparation method and applications thereof, and specific embodiments, features and properties thereof according to the present invention with reference to the preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The following materials and reagents are commercially available unless otherwise specified.
The invention provides a nano plugging agent, which comprises the following components in parts by weight:
white oil: 500-600 parts;
graphene: 5 parts of a mixture;
modifying agent: 5 parts of a mixture;
nano calcium carbonate: 300-350 parts;
nano silicon dioxide: 30-50 parts;
a stabilizer: 20-40 parts.
In specific implementation, the white oil can be light white oil W1-90 or W1-100 or W1-110, preferably light white oil W1-100, because when the nano blocking agent is prepared, on one hand, the low kinematic viscosity of W1-100 is favorable for preparation, and on the other hand, the nano blocking agent has better compatibility with oil-based drilling fluid.
In specific implementation, the graphene is a nano-grade material, and the particle size of the graphene is adjustable within the range of 10-100nm so as to meet the broad-spectrum plugging requirement; the material is fully utilized as the thinnest two-dimensional material, and can easily enter the nano-scale pore gaps of the stratum to realize effective plugging; the plugging agent has an ultrahigh specific surface area, so that a good plugging effect can be achieved under the condition of small addition amount; in addition, the plugging particle sizes required by different stratums are different, and the particle sizes can be adjusted according to the plugging requirements of different stratums.
In specific implementation, the modifier can be n-dodecyl triethoxysilane or sodium oleate or sodium alkyl sulfonamide acetate, and is preferably n-dodecyl triethoxysilane, so that the property of graphene mutual attraction can be better changed after preference is given, and the agglomeration of nanoparticles is prevented.
In specific implementation, the particle size of the nano calcium carbonate is adjustable within the range of 100-1000nm so as to meet the requirement of broad-spectrum plugging. When stratum pores and cracks are plugged, coarse-particle nano calcium carbonate is firstly bridged, and then fine-particle nano calcium carbonate is used for filling smaller pores formed by bridging of the coarse-particle nano calcium carbonate, so that a better plugging effect is achieved.
In specific implementation, the nano silicon dioxide is adjustable in the range of 5-50nm in particle size so as to meet the broad-spectrum plugging requirement. When stratum pores and cracks are plugged, the nano-silica assists the fine-particle nano-calcium carbonate to play a filling role so as to further improve the plugging effect.
In specific implementation, the stabilizer is calcium stearate, so that the surface wettability (mutual attraction property) of the graphene, the nano calcium carbonate and the nano silicon dioxide can be changed, the uniform dispersion capability of the graphene, the nano calcium carbonate and the nano silicon dioxide in the continuous phase is promoted, and finally the graphene, the nano calcium carbonate and the nano silicon dioxide are uniformly dispersed in the white oil.
The invention also provides a preparation method of the nano plugging agent, which comprises the following steps:
1) adding a modifier into the white oil, uniformly dispersing, then adding graphene into the white oil, and uniformly dispersing to obtain a graphene mother liquor;
by utilizing oxygen-containing functional groups such as hydroxyl, carboxyl and the like existing in the functionalized graphene nanosheets and taking n-dodecyl triethoxysilane with long-chain alkyl as a modifier, the functionalized graphene nanosheets are grafted with the long-chain alkyl in a chemical bonding manner to change the suspension stability of the functionalized graphene nanosheets in the white oil, and the required graphene mother liquor is prepared through the previous steps;
2) adding a stabilizer into the graphene mother liquor obtained in the step 1), uniformly dispersing, then sequentially adding nano calcium carbonate and nano silicon dioxide, and performing ultrasonic wave or microwave oscillation dispersion or ultrahigh-speed stirring and shearing to ensure that the nano calcium carbonate and the nano silicon dioxide are uniformly dispersed so as to obtain the required nano plugging agent.
The nano plugging agent is prepared by a fractional step method so that the graphene can be better dispersed in the white oil; if all the raw materials are mixed and dispersed together, a problem of uneven dispersion may occur.
The invention also provides an application of the nano plugging agent in drilling fluid plugging, which specifically comprises the following steps: and adding the nano plugging agent into the drilling fluid, and uniformly stirring.
The present invention is further illustrated by the following specific examples, which are not to be construed as limiting the invention thereto.
Example 1
The embodiment provides a preparation method of a nano plugging agent for drilling fluid, which comprises the following steps:
1) taking 600g of light white oil W1-100, adding 5g of n-dodecyl triethoxysilane modifier, performing ultrasonic oscillation dispersion (frequency of 50KHz), performing oscillation dispersion for 30 minutes, adding 5g of graphene, and continuing oscillation for 20 minutes to obtain graphene mother liquor;
2) adding 40g of stabilizer into the prepared graphene mother liquor, oscillating and dispersing by using ultrasonic waves (the frequency is 50KHz), adding 350g of nano calcium carbonate and 50g of nano silicon dioxide after oscillating and dispersing for 30 minutes, and continuously oscillating for 20 minutes to prepare the nano plugging agent (1050 g); the nano plugging agent comprises the following components in parts by weight: white oil: 600 parts of water; graphene: 5 parts of a mixture; modifying agent: 5 parts of a mixture; nano calcium carbonate: 350 parts of (a); nano silicon dioxide: 50 parts of a mixture; a stabilizer: 40 parts of the components.
The drilling fluid nano plugging agent prepared in the example 1 is subjected to laser particle size analysis, and the particle size distribution condition is as follows: d10 is less than 100nm, D50 is less than 313nm, D90 is less than 952nm, and the particle size distribution range meets the set requirements (D10 is less than 100nm, D50 is less than 500nm, and D90 is less than 1000nm, which are determined according to the fracture width and pore throat size distribution condition of the drilling stratum).
The nano plugging agent for the drilling fluid prepared in the example 1 is added into a white oil-based drilling fluid system, and the compatibility with the drilling fluid and the high-temperature and high-pressure water loss reduction condition are evaluated, wherein the specific formula of the drilling fluid system is as follows:
formula 1: w1-100 white oil (164.5g) + organic soil (6g, available from Kyodo GmbH) + Primary emulsifier (6.5g, available from Kyodo GmbH) + Secondary emulsifier (12.5g, available from Kyodo GmbH GnO) CaO (2(20g) + Water (60g) + fluid loss additive (25g, from Chengdu Daidao Limited company) + barite 4.3(680g, from Sichuan Haoyo company)
And (2) formula: formula 1+ 1% (mass volume ratio) nano plugging agent
And (3) formula: formula 1+ 1.5% (mass volume ratio) nano plugging agent
And (4) formula: formula 1+ 2% (mass volume ratio) nano plugging agent
The drilling fluids prepared according to the formulas 1 to 4 were hot rolled at 130 ℃ for 16h and then tested for various properties. The experimental data of the rheological property, the fluid loss, the lubricity and the like are shown in table 1, wherein rho is density, AV is apparent viscosity, PV is plastic viscosity, YP is dynamic shear force, G10 '/10' is static shear force, FLHTHPKf is viscosity coefficient for high temperature and high pressure water loss.
The drilling fluid performance determination method is carried out according to the following petroleum industry standards: the oil and gas industry drilling fluid field tests a second part of oil-based drilling fluid, GB/T16783.2-2012. Wherein the rheological test temperature is 65 ℃. + -. 2 ℃ and the HTHP test temperature is 130 ℃. + -. 2 ℃.
TABLE 1 evaluation of the Nano plugging Agents in the white oil based System
As can be seen from the data in the table 1, the nano plugging agent added in the formula 2-4 in an amount of 1-2% (mass to volume ratio) in the embodiment 1 of the invention has small influence on the rheological property and the emulsion stability of the white oil-based drilling fluid system, and the variation amplitude is less than 12%; meanwhile, the filter loss reducing effect is good, and when the addition of the nano plugging agent reaches 2 percent (mass-volume ratio), the HTHP filter loss reduction rate is more than 30 percent; from the viscosity coefficient representing the lubricity, the viscosity coefficient of the drilling fluid can be reduced after the nano plugging agent is added, and the lubricity of the drilling fluid is improved.
The solid phase in the oil-based drilling fluid is mostly micron-scale particles, and the traditional anti-collapse plugging agent is lack of nano-scale particles and cannot well plug nano-scale microcracks. The nano plugging agent disclosed by the embodiment 1 of the invention is matched with a nano pore gap of a shale stratum, and can be well embedded into a nano microcrack to form a compact plugging layer, so that on one hand, the invasion of a liquid phase (caused by self-absorption and pressure difference driving) to the deep part of the shale is prevented, on the other hand, the transmission of pressure to the inside of the crack is blocked, the pressure difference acts on the surface of the shale, the collapse pressure of the shale stratum is reduced, the strength and the integrity of a shale well wall are maintained, and the effects of plugging and anti-collapse are achieved.
A core plugging property evaluation experiment was performed on the nano plugging agent described in example 1, and the experimental results are shown in table 2.
Table 2 evaluation experiment data of core plugging property
Remarking: the confining pressure is 5MPa, and the plugging time is 120 min.
As can be seen from the data in Table 2, the nano plugging agent with the mass volume ratio of 1 percent (based on the volume of the drilling fluid) is added into the white oil, so that the plugging capability of the rock core can be greatly improved, and the improvement rate reaches 70.6 percent; the improvement rate is 82.9 percent when the addition amount reaches 2 percent (mass volume ratio, based on the volume of the drilling fluid); this shows that the nano plugging agent of embodiment 1 of the present invention is matched with the nano-pore gaps of the shale formation, and can be well embedded into the nano-micropores and the micro-cracks to form a compact plugging layer, thereby achieving the purpose of improving the plugging rate.
The evaluation experiment of the plugging property of the filter membrane was carried out on the nano plugging agent described in example 1, and the experimental results are shown in table 3.
TABLE 3 evaluation of filter plugging Properties
As can be seen from the data in Table 3, the addition of 2% (mass to volume ratio, based on the volume of the drilling fluid) of the nano plugging agent into the white oil can greatly improve the plugging capability of the nano filter membrane: the plugging rate of 100nm, 220nm and 450nm filter membranes can reach more than 98 percent. This shows that the nano plugging agent of embodiment 1 of the present invention is matched with the nano-pore gaps of the shale formation, and can be well embedded into the nano-micropores and the micro-cracks to form a compact plugging layer, thereby achieving the purpose of increasing the plugging rate.
The nano plugging agent described in example 1 was subjected to heavy metal content detection, and the experimental results are shown in table 4.
Table 4 heavy metal content test results of the nano blocking agent described in example 1
| Detecting items | Detection standard | Standard value | Unit of | Example 1 |
| Total chromium | SY/T 6788-2010 | ≤1000 | mg/kg | ≤1000 |
| Total mercury | SY/T 6788-2010 | ≤15 | mg/kg | ≤15 |
| Total lead | SY/T 6788-2010 | ≤1000 | mg/kg | ≤1000 |
| Total cadmium | SY/T 6788-2010 | ≤20 | mg/kg | ≤20 |
| Total arsenic | SY/T 6788-2010 | ≤75 | mg/kg | ≤75 |
According to the biotoxicity index and the detection method in the technical requirement of environmental protection of oilfield chemical agents (SY/T6788-2010), the biotoxicity experiment is carried out on the nano plugging agent for the drilling fluid in the example 1, and the result is shown in Table 5.
TABLE 5 Biotoxicity index and results for water-soluble oilfield chemicals
The data in table 5 show that: the heavy metal content of the nano plugging agent in the embodiment 1 of the invention is in the industry standard range; EC of the NanoBlocker described in example 150More than 25000mg/L, and the biotoxicity level is non-toxic, which indicates that the nano plugging agent is environment-friendly.
Example 2
The embodiment provides a preparation method of a nano plugging agent for drilling fluid, which comprises the following steps:
1) taking 500g of light white oil W1-90, adding 5g of sodium oleate modifier, performing ultrasonic oscillation dispersion (frequency of 50KHz), adding 5g of graphene after performing oscillation dispersion for 30 minutes, and continuing to perform oscillation for 20 minutes to obtain graphene mother liquor;
2) adding 20g of stabilizer into the prepared graphene mother liquor, oscillating and dispersing by using ultrasonic waves (the frequency is 50KHz), adding 300g of nano calcium carbonate and 30g of nano silicon dioxide after oscillating and dispersing for 30 minutes, and continuously oscillating for 20 minutes to prepare the nano plugging agent (860 g); the nano plugging agent comprises the following components in parts by weight: white oil: 500 parts; graphene: 5 parts of a mixture; modifying agent: 5 parts of a mixture; nano calcium carbonate: 300 parts of (A); nano silicon dioxide: 30 parts of (1); a stabilizer: and 20 parts.
The drilling fluid nano plugging agent prepared in the example 2 is subjected to laser particle size analysis, and the particle size distribution condition is as follows: d10 is less than 100nm, D50 is less than 350nm, D90 is less than 976nm, and the particle size distribution range meets the set requirements (D10 is less than 100nm, D50 is less than 500nm, D90 is less than 1000nm, which is determined according to the fracture width and pore throat size distribution condition of the drilling stratum).
The nano plugging agent for the drilling fluid prepared in the example 2 is added into a white oil-based drilling fluid system, and the compatibility with the drilling fluid and the high-temperature and high-pressure water loss reduction condition are evaluated, wherein the specific formula of the drilling fluid system is as follows:
formula 1: w1-100 white oil (164.5g), organic soil (6g, available from Kyodo Dow Co., Ltd.) + primary milk (6.5g, available from Kyodo Co., Ltd.) + secondary milk (12.5g, available from Kyodo Co., Ltd.) + CaO (15g) + CaCl2(20g) + water (60g) + filtrate reducer (25g, available from Kyodo Co., Ltd.) + barite 4.3(680g, available from Sichuan Haowu Co., Ltd.);
and (2) formula: 1+ 1% (mass volume ratio) of nano plugging agent is prepared;
and (3) formula: the formula is 1 plus 1.5 percent (mass volume ratio) of the nano plugging agent;
and (4) formula: the formula is 1+ 2% (mass volume ratio) of the nano plugging agent;
the drilling fluids prepared according to the formulas 1 to 4 were hot rolled at 130 ℃ for 16h and then tested for various properties. The experimental data of rheological property, fluid loss, lubricity and other properties are shown in Table 6, wherein ρ is density, AV is apparent viscosity, PV is plastic viscosity, YP is dynamic shear force, G10 '/10' is static shear force, FL isHTHPKf is viscosity coefficient for high temperature and high pressure water loss.
The drilling fluid performance determination method is carried out according to the following petroleum industry standards: the oil and gas industry drilling fluid field tests a second part of oil-based drilling fluid, GB/T16783.2-2012. Wherein the rheological test temperature is 65 ℃. + -. 2 ℃ and the HTHP test temperature is 130 ℃. + -. 2 ℃.
TABLE 6 evaluation test data of nano plugging agent in white oil-based system
As can be seen from the data in Table 6, the nano plugging agent of the embodiment 2 has small influence on the rheological property and the emulsion stability of the white oil-based drilling fluid system when the nano plugging agent of the formula 2-4 is added into the formula 1-2% (mass to volume ratio, based on the volume of the drilling fluid), and the variation amplitude is less than 12%; meanwhile, the filter loss reducing effect is good, and when the addition of the nano plugging agent reaches 2 percent (mass-volume ratio, based on the volume of the drilling fluid), the HTHP filter loss reduction rate is more than 30 percent; from the viscosity coefficient representing the lubricity, the viscosity coefficient of the drilling fluid can be reduced after the nano plugging agent is added, and the lubricity of the drilling fluid is improved.
The solid phase in the oil-based drilling fluid is mostly micron-scale particles, and the traditional anti-collapse plugging agent is lack of nano-scale particles and cannot well plug nano-scale microcracks. The nano plugging agent in embodiment 2 of the invention is matched with the nano pore gaps of the shale stratum, and can be well embedded into the nano microcracks to form a compact plugging layer, so that on one hand, the invasion of a liquid phase (caused by self-absorption and pressure difference driving) to the deep part of the shale is prevented, on the other hand, the transmission of pressure to the inside of the cracks is blocked, the pressure difference acts on the surface of the shale, the collapse pressure of the shale stratum is reduced, the strength and the integrity of a shale well wall are maintained, and the effects of plugging and anti-collapse are achieved.
The nano plugging agent described in example 2 was subjected to a core plugging property evaluation experiment, and the experimental results are shown in table 7.
Table 7 evaluation experiment data of core plugging property
Remarking: the confining pressure is 5MPa, and the plugging time is 120 min.
As can be seen from the data in Table 7, the nano plugging agent with the mass volume ratio of 1 percent (based on the volume of the drilling fluid) is added into the white oil, so that the plugging capability of the rock core can be greatly improved, and the improvement rate reaches 73.6 percent; when the addition amount reaches 2 percent (mass-volume ratio, based on the volume of the drilling fluid), the improvement rate is 81.3 percent; this shows that the nano plugging agent of embodiment 2 of the present invention can be well embedded into nano micropores and micro cracks to form a compact plugging layer by matching with the nano pore gaps of the shale formation, so as to achieve the purpose of increasing the plugging rate.
The evaluation experiment of the plugging property of the filter membrane was performed on the nano plugging agent described in example 2, and the experimental results are shown in table 8.
TABLE 8 evaluation of filter plugging Properties
It can be seen from the data in table 8 that 2% (mass to volume ratio, based on the volume of the drilling fluid) of the nano plugging agent is added to the white oil, so that the plugging capability of the nano filter membrane can be greatly improved: the plugging rate of 100nm, 220nm and 450nm filter membranes can reach more than 98 percent. This shows that the nano plugging agent of embodiment 2 of the present invention is matched with the nano-pore gaps of the shale formation, and can be well embedded into the nano-micropores and the micro-cracks to form a compact plugging layer, thereby achieving the purpose of increasing the plugging rate.
The nano plugging agent described in example 2 was subjected to heavy metal content detection, and the experimental results are shown in table 9.
Table 9 heavy metal content test results of the nano blocking agent described in example 2
| Detecting items | Detection standard | Standard value | Unit of | Example 2 |
| Total chromium | SY/T 6788-2010 | ≤1000 | mg/kg | ≤1000 |
| Total mercury | SY/T 6788-2010 | ≤15 | mg/kg | ≤15 |
| Total lead | SY/T 6788-2010 | ≤1000 | mg/kg | ≤1000 |
| Total cadmium | SY/T 6788-2010 | ≤20 | mg/kg | ≤20 |
| Total arsenic | SY/T 6788-2010 | ≤75 | mg/kg | ≤75 |
According to the biotoxicity index and the detection method in the technical requirement of environmental protection of oilfield chemical agents (SY/T6788-2010), the biotoxicity experiment is carried out on the nano plugging agent for the drilling fluid in the example 2, and the results are shown in Table 10.
TABLE 10 Biotoxicity index and results for water-soluble oilfield chemicals
The data in table 10 indicates that: the heavy metal content of the nano plugging agent in the embodiment 2 of the invention is in the industry standard range; EC of the NanoBlocker described in example 250More than 25000mg/L, and the biotoxicity level is non-toxic, which indicates that the nano plugging agent is environment-friendly.
Example 3
The embodiment provides a preparation method of a nano plugging agent for drilling fluid, which comprises the following steps:
1) taking 550g of light white oil W1-110, adding 5g of sodium alkylsulfonamide modifier, performing ultrasonic oscillation dispersion (frequency of 50KHz), adding 5g of graphene after performing oscillation dispersion for 30 minutes, and continuing to perform oscillation for 20 minutes to obtain graphene mother liquor;
2) adding 30g of stabilizer into the prepared graphene mother liquor, performing ultrasonic oscillation dispersion (frequency of 50KHz), adding 325g of nano calcium carbonate and 40g of nano silicon dioxide after performing oscillation dispersion for 30 minutes, and continuing to oscillate for 20 minutes to prepare the nano plugging agent (955 g); the nano plugging agent comprises the following components in parts by weight: white oil: 550 parts of a mixture; graphene: 5 parts of a mixture; modifying agent: 5 parts of a mixture; nano calcium carbonate: 300 parts of (A); nano silicon dioxide: 40 parts of a mixture; a stabilizer: 30 parts of.
The drilling fluid nano plugging agent prepared in the example 3 is subjected to laser particle size analysis, and the particle size distribution condition is as follows: d10 is less than 100nm, D50 is less than 321nm, D90 is less than 940nm, and the particle size distribution range meets the set requirements (D10 is less than 100nm, D50 is less than 500nm, and D90 is less than 1000nm, which are determined according to the fracture width and pore throat size distribution condition of the drilling stratum).
The nano plugging agent prepared in the example 3 is added into a white oil-based drilling fluid system, and the compatibility with the drilling fluid and the high-temperature and high-pressure water loss reduction condition are evaluated, wherein the specific formula of the drilling fluid system is as follows:
formula 1: w1-100 white oil (164.5g) + organic soil (6g, available from GYUDADY CO., LTD.) + Primary milk (6.5g, available from GYUDADY CO., LTD.) + Secondary milk (12.5g, available from GYUDADY CO., LTD.) + CaO (15g) + CaCl2(20g) + Water (60g) + fluid loss additive (25g, from Chengdu Daidao Limited company) + barite 4.3(680g, from Sichuan Haoyo company)
And (2) formula: 1+ 1% (mass volume ratio) of nano plugging agent is prepared;
and (3) formula: the formula is 1 plus 1.5 percent (mass volume ratio) of the nano plugging agent;
and (4) formula: the formula is 1+ 2% (mass volume ratio) of the nano plugging agent;
the drilling fluids prepared according to the formulas 1 to 4 were hot rolled at 130 ℃ for 16h and then tested for various properties. The experimental data of rheological property, fluid loss and lubricity are shown in Table 11, wherein ρ is density, AV is apparent viscosity, PV is plastic viscosity, YP is dynamic shear force, G10 '/10' is static shear force, FLHTHPKf is viscosity coefficient for high temperature and high pressure water loss.
The drilling fluid performance determination method is carried out according to the following petroleum industry standards: the oil and gas industry drilling fluid field tests a second part of oil-based drilling fluid, GB/T16783.2-2012. Wherein the rheological test temperature is 65 ℃. + -. 2 ℃ and the HTHP test temperature is 130 ℃. + -. 2 ℃.
TABLE 11 evaluation test data of nano plugging agent in white oil based system
As can be seen from the data in Table 11, the nano plugging agent of example 3 of the present invention added to formulations 2 to 4 in an amount of 1 to 2% (mass to volume ratio, based on the volume of the drilling fluid) has little influence on the rheological property and the emulsion stability of the white oil-based drilling fluid system, and the variation range is less than 12%; meanwhile, the filter loss reducing effect is good, and when the addition of the nano plugging agent reaches 2 percent (mass-volume ratio, based on the volume of the drilling fluid), the HTHP filter loss reduction rate is more than 30 percent; from the viscosity coefficient representing the lubricity, the viscosity coefficient of the drilling fluid can be reduced after the nano plugging agent is added, and the lubricity of the drilling fluid is improved.
The solid phase in the oil-based drilling fluid is mostly micron-scale particles, and the traditional anti-collapse plugging agent is lack of nano-scale particles and cannot well plug nano-scale microcracks. The nano plugging agent in embodiment 3 of the invention is matched with the nano pore gaps of the shale stratum, and can be well embedded into the nano microcracks to form a compact plugging layer, so that on one hand, the invasion of a liquid phase (caused by self-absorption and pressure difference driving) to the deep part of the shale is prevented, on the other hand, the transmission of pressure to the inside of the cracks is blocked, the pressure difference acts on the surface of the shale, the collapse pressure of the shale stratum is reduced, the strength and the integrity of a shale well wall are maintained, and the effects of plugging and anti-collapse are achieved.
A core plugging property evaluation experiment was performed on the nano plugging agent described in example 3, and the experimental results are shown in table 12.
TABLE 12 evaluation test data of core plugging property
Remarking: the confining pressure is 5MPa, and the plugging time is 120 min.
As can be seen from the data in Table 12, the nano plugging agent with the mass volume ratio of 1 percent (based on the volume of the drilling fluid) is added into the white oil, so that the plugging capability of the rock core can be greatly improved, and the improvement rate reaches 75 percent; when the addition amount reaches 2 percent (mass-volume ratio, based on the volume of the drilling fluid), the improvement rate is 84.7 percent; this shows that the nano plugging agent of embodiment 3 of the present invention can be well embedded into nano micropores and micro cracks to form a compact plugging layer by matching with the nano pore gaps of the shale formation, so as to achieve the purpose of increasing the plugging rate.
The evaluation test of the plugging property of the filter membrane was performed on the nano plugging agent described in example 3, and the test results are shown in table 13.
TABLE 13 evaluation of Filter Membrane plugging Properties
It can be seen from the data in table 13 that 2% (mass to volume ratio, based on the volume of the drilling fluid) of the nano plugging agent is added to the white oil, so that the plugging capability of the nano filter membrane can be greatly improved: the plugging rate of 100nm, 220nm and 450nm filter membranes can reach more than 98 percent. This shows that the nano plugging agent of embodiment 3 of the present invention is matched with the nano-pore gaps of the shale formation, and can be well embedded into the nano-micropores and the micro-cracks to form a compact plugging layer, thereby achieving the purpose of increasing the plugging rate.
The nano plugging agent described in example 3 was subjected to heavy metal content detection, and the experimental results are shown in table 14.
Table 14 heavy metal content test results of the nano blocking agent described in example 2
According to the biotoxicity index and the detection method in the technical requirement of environmental protection of oilfield chemical agents (SY/T6788-2010), the biotoxicity experiment is carried out on the nano blocking agent described in the example 3, and the results are shown in Table 15.
TABLE 15 Biotoxicity indices and results for water-soluble oilfield chemicals
The data in table 15 indicate that: the heavy metal content of the nano plugging agent in the embodiment 3 of the invention is in the industry standard range; EC of the NanoBlocker described in example 350More than 25000mg/L, and the biotoxicity level is non-toxic, which indicates that the nano plugging agent is environment-friendly.
The nano plugging agent prepared by a fractional step method is selected and combined with the graphene and the nano inorganic mineral particles according to the microstructure and the scale distribution condition of shale stratum pore gaps, so that the wide particle size distribution range (D10 is less than 100nm, D50 is less than 500nm, D90 is less than 1000nm), the various particle forms and the adjustable particle size distribution and distribution range are ensured, nano-sized pores and cracks in a shale well wall can be effectively plugged, the invasion of drilling fluid filtrate to the stratum is reduced, the damage effect of the hydraulic wedging effect on the shale around the well is weakened, the well wall is further stabilized, and collapse is prevented.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The recitation of numerical ranges herein includes all numbers subsumed within that range and includes any two numbers subsumed within that range. Different values of the same index appearing in all embodiments of the invention can be combined arbitrarily to form a range value.
The features of the invention claimed and/or described in the specification may be combined, and are not limited to the combinations set forth in the claims by the recitations therein. The technical solutions obtained by combining the technical features in the claims and/or the specification also belong to the scope of the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (10)
1. The nano plugging agent is characterized by comprising the following components in parts by weight:
white oil: 500-600 parts;
graphene: 5 parts of a mixture;
modifying agent: 5 parts of a mixture;
nano calcium carbonate: 300-350 parts;
nano silicon dioxide: 30-50 parts;
a stabilizer: 20-40 parts.
2. The nano plugging agent of claim 1, wherein the white oil is light white oil W1-90 or W1-100 or W1-110.
3. The nano plugging agent of claim 1, wherein the graphene is a nano-scale material with a particle size of 10-100 nm.
4. The nano blocking agent according to claim 1, wherein the modifier is n-dodecyltriethoxysilane or sodium oleate or sodium alkylsulfonamide acetate.
5. The nano plugging agent of claim 1, wherein the nano calcium carbonate has a particle size of 100-1000 nm.
6. The nano plugging agent of claim 1, wherein the nano silica has a particle size of 5 to 50 nm.
7. The nano-blocking agent according to claim 1, wherein the stabilizer is calcium stearate.
8. A method for preparing the nano plugging agent according to any one of claims 1 to 7, which comprises the following steps:
1) adding a modifier into the white oil, uniformly dispersing, then adding graphene into the white oil, and uniformly dispersing to obtain a graphene mother liquor;
2) adding a stabilizer into the graphene mother liquor obtained in the step 1), uniformly dispersing, then sequentially adding nano calcium carbonate and nano silicon dioxide, and uniformly dispersing.
9. Use of the nano plugging agent according to any one of claims 1 to 7 in plugging of drilling fluids.
10. Use according to claim 9, characterized in that it comprises the following steps: and adding the nano plugging agent into the drilling fluid, and uniformly stirring.
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