CN114605969B - Plugging material, plugging type oil-based drilling fluid and preparation method thereof - Google Patents

Plugging material, plugging type oil-based drilling fluid and preparation method thereof Download PDF

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CN114605969B
CN114605969B CN202210254756.3A CN202210254756A CN114605969B CN 114605969 B CN114605969 B CN 114605969B CN 202210254756 A CN202210254756 A CN 202210254756A CN 114605969 B CN114605969 B CN 114605969B
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drilling fluid
plugging
oil
based drilling
plugging material
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CN114605969A (en
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林凌
古晗
马丽华
胡正文
邓小刚
罗平亚
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Southwest Petroleum University
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02Well-drilling compositions
    • C09K8/03Specific additives for general use in well-drilling compositions
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02Well-drilling compositions
    • C09K8/32Non-aqueous well-drilling compositions, e.g. oil-based

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Abstract

The invention discloses a plugging material and a plugging type oil-based drilling fluid and a preparation method thereof. The plugging material is prepared by adopting a mode of compounding a rigid plugging material and a deformable material, so that the problem of compatibility with oil-based drilling fluid is solved, the emulsion stability of the drilling fluid is maintained, good plugging performance is achieved, economic loss is reduced, and a set of high-temperature-resistant 150 ℃ and high-density 1.3-1.5 g/cm are formed 3 The plugging type oil-based drilling fluid system can effectively solve the underground complex conditions such as lost circulation, blowout, sticking and the like in the drilling process.

Description

Plugging material, plugging type oil-based drilling fluid and preparation method thereof
Technical Field
The invention relates to the technical field of petrochemical industry, in particular to a plugging material, a plugging type oil-based drilling fluid and a preparation method thereof.
Background
Drilling is a hidden underground engineering, faces complex and changeable stratum, has a large amount of ambiguity, randomness and unpredictability, and lost circulation is a underground complex condition that drilling fluid leaks into the stratum in drilling construction, and has the phenomena of lowered liquid level of a mud tank, reduced wellhead return amount and even lost return, lost a large amount of drilling fluid and plugging materials due to lost circulation, consumed a large amount of time for interrupting drilling operation, affected geological logging, induced other complex accidents and damaged oil and gas layers. The stratum drilled in the drilling process, such as shale, sandy or silty shale, and the like, may be unstable in the well wall, after filtrate of drilling fluid enters the shale, clay particles absorb water and expand to generate expansion pressure, so that the stress of the well wall rock is unbalanced, and when the yield strength of the rock is exceeded, the pressure is released in a well collapse mode.
At present, the oil-based drilling fluid is widely applied to drilling construction of unconventional oil and gas resource development of domestic tight oil and tight gas, shale oil and gas horizontal wells and the like. However, when lost circulation occurs in the oil-based drilling fluid drilling process, great economic loss can be caused due to high cost of the oil-based drilling fluid; the common water-based drilling fluid plugging material is generally a hydrophilic water-absorbing expansion material, has no good compatibility with an oil-based drilling fluid system, generally damages the emulsion stability of the oil-based drilling fluid system, and cannot exert good leakage-proof plugging effect in the oil-based drilling fluid system; meanwhile, the special lubricating property and rheological property of the oil-based drilling fluid are easy to cause difficult bridging of the plugging material and larger pressure fluctuation in a shaft, the plugging layer is easy to be reversely flushed, and the common plugging material cannot play a role in leakage prevention and plugging in the oil-based drilling fluid; thus, plugging problems with oil-based drilling fluid systems are a primary problem in drilling.
Disclosure of Invention
The invention aims to solve the defects in the prior art, provides a plugging material, a plugging oil-based drilling fluid and a preparation method thereof, solves the problem of compatibility with the oil-based drilling fluid by adopting a mode of compounding a rigid plugging material and a deformable material to prepare the plugging material, maintains the emulsion stability of the drilling fluid, has good plugging performance, reduces economic loss, and forms a set of high-temperature resistant 150 ℃ and the density of 1.3-1.5 g/cm 3 The plugging type oil-based drilling fluid system can effectively solve the underground complex conditions such as lost circulation, blowout, sticking and the like in the drilling process.
The invention first provides a plugging material, which consists of a rigid plugging material and a deformable material.
Preferably, the rigid blocking material is a carbon dot.
Preferably, the deformable material is an oxidized asphalt.
Preferably, the mass ratio of the rigid plugging material to the deformable material is 1:1-1:2.2.
Preferably, the preparation method of the plugging material comprises the following steps: continuously stirring the deformable material under the heating condition, adding the rigid plugging material for mixing, cooling, solidifying and crushing to obtain the composite material.
More preferably, the heating condition is 120 to 130 ℃.
The invention also provides a plugging type oil-based drilling fluid, which comprises the plugging material.
Preferably, the plugging type oil-based drilling fluid comprises the following components:
oil phase: water phase= (85-95): (5-15);
and the following components, based on 100mL of total volume of the oil phase and the water phase:
2.5 to 5g of main emulsifying agent,
1.2 to 3.5g of auxiliary emulsifier,
1.8 to 2.8g of organic soil,
3-4 g of filtrate reducer,
2.9 to 3.8g of alkalinity regulator,
0.2-2g of plugging material,
and a weighting agent determined based on the density of the drilling fluid.
More preferably, the plugging material is 1-2g.
Preferably, the oil phase is diesel oil or white oil.
Preferably, the water phase is a 20% calcium chloride water solution by mass fraction.
Preferably, the main emulsifier is one or more selected from calcium stearate, petroleum ferric sulfonate, calcium naphthenate and naphthenic acid amide.
Preferably, the secondary emulsifier is Span-80 (the main component is sorbitan monooleate) and/or polyoxypropylene stearate.
Preferably, the filtrate reducer is modified lignite resin.
Preferably, the organic soil is oleophilic clay formed by bentonite after being treated by quaternary ammonium salt surfactant.
More preferably, the quaternary ammonium salt is dodecyl trimethyl ammonium bromide and/or dodecyl dimethyl benzyl ammonium chloride.
Preferably, the alkalinity regulator is calcium oxide.
Preferably, the plugging material consists of a rigid plugging material and a deformable material in a mass ratio of 1:1-1:2.2.
More preferably, the rigid blocking material is a carbon dot.
More preferably, the deformable material is asphalt oxide.
Preferably, the weighting agent is calcium carbonate and/or barite.
Preferably, the adding amount of the weighting agent is used for adjusting the density of the drilling fluid to 1.3-1.5 g/cm 3
Preferably, the pH of the plugging oil-based drilling fluid is 8-9, the density of the system is 1.3-1.5 g/cm < 3 >, and the temperature resistance is 150 ℃.
The invention also provides a preparation method of the plugging type oil-based drilling fluid, which comprises the following steps:
sequentially adding organic soil, a main emulsifier, a secondary emulsifier and an alkalinity regulator into the oil phase, and stirring and mixing to obtain a mixture A;
adding a water phase into the mixture A under the stirring condition to obtain a mixture B;
and sequentially adding the filtrate reducer, the plugging material and the weighting agent into the mixture B under the stirring condition, wherein the obtained mixed liquid is the plugging type oil-based drilling fluid system.
Preferably, in the preparation method, each component is stirred for 5min after being added, and then the next component is added, wherein the stirring speed is 12000r/min.
The beneficial effects of the invention are as follows:
1. the invention adopts the combination of the rigid plugging material and the deformable material to obtain the plugging material, and aims at the unconventional tight reservoir layer with micro-cracks less than 20nm, the deformable material can make up the defects of the rigid plugging material, the rigid plugging material performs plugging bridging, a stressed frame is provided for other plugging agents, the deformable material strengthens the plugging effect, the wall protection effect and the seepage prevention effect are both achieved, the plugging effect is strengthened, the plugging effect is achieved by the cooperation of the rigid plugging material and the deformable material, the plugging material has better compatibility with an oil-based drilling fluid system, and the rheological property of the oil-based drilling fluid is less influenced.
2. The drilling fluid of the invention has the temperature resistance of 150 ℃ and the density of 1.3-1.5 g/cm 3 The plugging type oil-based drilling fluid has the advantages that the main emulsifying agent can reduce the surface energy, enhance the system stability, the filtrate reducer is adsorbed on the surface of organic soil and combined with other solid particles, the filtrate reducer reduces the filtrate loss, the leakage of water into the stratum is avoided, the alkalinity regulator maintains the pH of the system, the efficiency of the emulsifying agent is improved, the plugging material can form better compatibility with the oil-based drilling fluid system, the emulsion stability of the drilling fluid is ensured, and the weighting agent regulates the density of the drilling fluid to meet the requirement of the drilling fluid; the components are matched with each other, so that the drilling fluid has stronger plugging performance, can stabilize the well wall, prevent collapse, has good protection performance on oil and gas layers, particularly water-sensitive stratum, can cope with the easily collapsed stratum of shale, thick salt paste layers of deep wells, complex stratum and the like, is suitable for drilling deep wells and large inclined wells, and can effectively solve the underground complex condition encountered in the drilling process.
3. The plugging type oil-based drilling fluid prepared by the plugging material has good rheological property and good electrical stability, can meet the plugging technical requirement in the construction process of the oil-based drilling fluid, and obviously reduces the use cost of the oil-based drilling fluid; the high-temperature-resistant high-pressure water-sensitive stratum has good temperature resistance (150 ℃), good filtration performance, low high-temperature high-pressure filtration loss and good protection performance on the water-sensitive stratum.
Drawings
FIG. 1 is a TEM image of carbon dots prepared according to the invention
Detailed Description
The present invention will be described in further detail with reference to specific embodiments thereof in order to enable those skilled in the art to better understand the technical aspects of the invention.
The invention provides a plugging material, a plugging type oil-based drilling fluid and a preparation method thereof, wherein a nano plugging agent is prepared by adopting a mode of compounding a rigid plugging material and a deformable material, so that the problem of compatibility with the oil-based drilling fluid is solved, the emulsion stability of the drilling fluid is maintained, good plugging performance is achieved, and further the reduction is realizedEconomic loss, and forms a set of temperature resistant 150 ℃ and density of 1.3-1.5 g/cm 3 The plugging type oil-based drilling fluid system can effectively solve the underground complex conditions such as lost circulation, blowout, sticking and the like in the drilling process.
In particular, the present invention first provides a plugging material consisting of a rigid plugging material and a deformable material.
Furthermore, the rigid plugging material is a carbon dot, is composed of spherical-like carbon nano particles with the size below 10nm, is provided with sp2 hybridized carbon crystal nucleus at the center, and is composed of an sp3 hybridized amorphous carbon framework and a large number of functionalized surface groups at the periphery; the rigid plugging material has the advantages of good carbon point stability, low toxicity, wide raw material sources, simple preparation method and simple required equipment conditions. The carbon dot structure shown in fig. 1 can be obtained by using a preparation method common in the art.
In the invention, the preparation of carbon dots mainly comprises the following two methods:
the method comprises the following steps: firstly, dissolving 3g of citric acid and 6g of urea in 20mL of deionized water, and stirring until the citric acid and the urea are completely dissolved to form colorless and transparent solution; then placing the solution into a 650W microwave oven, heating deeply for 5 minutes, and gradually changing the solution from a colorless transparent state to brown in the heating process to finally obtain a dark brown solid; finally, redissolving the dark brown solid in 20mL of deionized water, stirring to fully dissolve the dark brown solid, and performing centrifugal purification treatment to obtain the aqueous solution of carbon dots.
The second method is as follows: preparing by a hydrothermal method: weighing 1.15g of citric acid, dissolving the citric acid in 20mL of deionized water, sufficiently dissolving the citric acid by ultrasonic treatment, transferring the prepared solution into a 30mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 4 hours at 200 ℃ in a muffle furnace, naturally cooling the reaction system to room temperature after the reaction is finished, and removing supernatant; then 1.5g of sulfanilic acid is weighed and added into the supernatant, the supernatant is fully dissolved by ultrasonic treatment, and then the solution is transferred into a hydrothermal reaction kettle to react for 5 hours at 135 ℃ in a muffle furnace; after the reaction is finished, naturally cooling the reaction system to room temperature again, removing supernatant, sequentially passing through water-based filter membranes of 0.45 and 0.22 mu m to finally obtain carbon dot solution, and finally obtaining carbon dots through freeze drying.
The deformable material of the invention is asphalt oxide. The preparation method comprises the following steps: adding asphalt powder (softening point 120 ℃) into a three-neck flask, adding potassium permanganate solution under magnetic stirring, heating until boiling reflux reaction is carried out for 40min until the potassium permanganate solution is removed, stopping the reaction, at the moment, a large amount of asphalt floats on the liquid surface, manganese dioxide is deposited on the water bottom, pouring into a beaker, adding water, pouring the upper solid into a Buchner funnel, carrying out suction filtration (taking care of not pouring the lower manganese dioxide), drying, and crushing to obtain the oxidized asphalt powder.
In the invention, the mass ratio of the rigid plugging material to the deformable material is 1:1-1:2.2.
In the field, compared with a conventional reservoir, an unconventional tight reservoir has strong heterogeneity, small pores and throats, a nano-scale pore system is taken as a main part, micro-millimeter pores are locally developed, pore throat structures with different microscale are complex and various, and pore types are various, including intra-grain pores in organic matters, intra-grain pores in minerals, inter-grain pores between minerals and organic matters or between mineral particles and mineral particles, and micro-cracks.
The invention adopts carbon dots as rigid plugging materials, and oxidized asphalt as deformable materials, and aims at unconventional tight reservoirs with microcracks of less than 20nm, and a novel nano plugging agent is prepared by adopting a mode of compounding the carbon dots and the oxidized asphalt, so that the deformability of the prepared oxidized asphalt compensates the defect of plugging the carbon dots, the rigid plugging materials carry out plugging bridging, a stress frame is provided for other plugging agents, the deformable materials strengthen the plugging effect, the wall protection effect and the seepage prevention effect are realized, and the plugging effect is realized by the cooperation of the carbon dots and the oxidized asphalt. The plugging material has better compatibility with an oil-based drilling fluid system, and has smaller influence on rheological property of the oil-based drilling fluid.
Specifically, the preparation method of the plugging material comprises the following steps: weighing oxidized asphalt in a beaker, heating and stirring at 120-130 ℃ until the asphalt is softened, slowly adding carbon points according to the mass ratio, stirring for 4-6 hours, fully and uniformly mixing, cooling to room temperature for solidification, and crushing to obtain the plugging material.
The invention also provides a plugging type oil-based drilling fluid, which comprises the plugging material.
Further, the plugging type oil-based drilling fluid comprises the following components:
oil phase: water phase= (85-95): (5-15);
and the following components, based on 100mL of total volume of the oil phase and the water phase:
2.5 to 5g of main emulsifying agent,
1.2 to 3.5g of auxiliary emulsifier,
1.8 to 2.8g of organic soil,
3-4 g of filtrate reducer,
2.9 to 3.8g of alkalinity regulator,
0.2-2g of plugging material,
and a weighting agent determined based on the density of the drilling fluid.
The drilling fluid of the invention has the temperature resistance of 150 ℃ and the density of 1.3-1.5 g/cm 3 The plugging type oil-based drilling fluid system has strong plugging performance, can stabilize a well wall, prevents collapse, has good protection performance on oil and gas layers, particularly water-sensitive stratum, is mainly used for coping with the stratum which is easy to collapse of shale, a thick salt paste layer of a deep well, a complex stratum and the like, is suitable for drilling of the deep well and a large inclined well, and can effectively solve the underground complex condition encountered in the drilling process.
The oil phase is diesel oil or white oil.
The water phase is 5-15% calcium chloride water solution by mass fraction. Can improve the ion concentration of the water phase and the water in the tissue drilling fluid permeates into the stratum.
The main emulsifier is one or more selected from calcium stearate, petroleum ferric sulfonate, calcium naphthenate and naphthenic acid amide; the secondary emulsifier is Span-80 (the main component is sorbitan monooleate) and/or polyoxypropylene stearate. The emulsifier has the function of forming an adsorption film with certain strength on an oil/water interface, and preventing coalescence and combination during collision of liquid drops; and the interfacial tension is reduced, so that the surface energy of the emulsifying system is reduced, and the stability is enhanced.
The filtrate reducer is modified lignite resin. The filtrate reducer can be adsorbed on the surfaces of clay particles, ionizes a large number of negative groups, improves the thickness of hydration films, and forms a thin filter cake in cooperation with other solid particles in the system, so that the filtrate reducer reduces the filtrate loss and avoids water leakage into the stratum.
The organic soil is oleophylic clay formed by bentonite after being treated by quaternary ammonium salt surfactant; still further, the quaternary ammonium salt is dodecyl trimethyl ammonium bromide and/or dodecyl dimethyl benzyl ammonium chloride. The organic soil is a lipophilic colloid and has the functions of improving viscosity, forming a filter cake, reducing the filtration loss and enhancing the stability of emulsion.
The alkalinity regulator is calcium oxide. Maintaining pH, preventing drill corrosion, improving emulsifier efficacy while preventing CO 2 And H 2 S and other acid gases to the drilling fluid.
Wherein, the plugging material consists of a rigid plugging material and a deformable material with the mass ratio of 1:1-1:2.2; further, the rigid plugging material is carbon dots; the deformable material is an oxidized asphalt.
The weighting agent is calcium carbonate and/or barite; the adding amount of the weighting agent is used for adjusting the density of the drilling fluid to 1.3-1.5 g/cm 3
The pH value of the plugging type oil-based drilling fluid is 8-9, and the system density is 1.3-1.5 g/cm 3 The temperature resistance was 150 ℃.
The invention also provides a preparation method of the plugging type oil-based drilling fluid, which comprises the following steps:
sequentially adding organic soil, a main emulsifier, a secondary emulsifier and an alkalinity regulator into the oil phase, and stirring and mixing to obtain a mixture A;
adding a water phase into the mixture A under the stirring condition to obtain a mixture B;
and sequentially adding the filtrate reducer, the plugging material and the weighting agent into the mixture B under the stirring condition, wherein the obtained mixed liquid is the plugging type oil-based drilling fluid system.
In the preparation method, each component is stirred for 5min after being added, and then the next component is added, wherein the stirring speed is 12000r/min.
The plugging type oil-based drilling fluid prepared by the plugging material has good rheological property and good electrical stability, can meet the plugging technical requirement in the construction process of the oil-based drilling fluid, and obviously reduces the use cost of the oil-based drilling fluid; the high-temperature-resistant high-pressure water-sensitive stratum has good temperature resistance (150 ℃), good filtration performance, low high-temperature high-pressure filtration loss and good protection performance on the water-sensitive stratum.
The drilling fluid can effectively reduce the increase of pore pressure of the well wall caused by the invasion of filtrate in the drilling process, prevent the occurrence of instability of the well wall, and the novel plugging material can enter micropores and microcracks to form compact plugging effect.
The foregoing is a detailed description of the invention and the following examples of the invention.
(1) Detection of routine Properties
Rheological property test and pressure loss test of drilling fluid at normal temperature the drilling fluid is detected according to the national standard GB/T16783.1-2014 detection method. Detecting parameters: AV (apparent viscosity), PV (plastic viscosity), YP (dynamic shear force), GEL (static shear force), FLHTHP (high temperature high pressure fluid loss).
(2) Drilling fluid temperature resistance test
The temperature resistance test of the drilling fluid is a high-temperature high-pressure filtration test and a high-temperature hot rolling aging test. According to the national standard GB/T16783.1-2014 detection method, the drilling fluid is detected.
The high-temperature hot rolling aging experimental process comprises the following steps: taking out after ageing at 150 ℃/16h by hot rolling, and measuring the related performance of the drilling fluid at 30 ℃ after stirring at a high speed for 10 min.
(3) Determination of rheological properties of drilling fluids:
(1) The national standard drilling fluid is adopted for field test in GB/T16783.1 2006:
(2) The drilling fluid rheological property test temperature is 30℃:
(3) Aging at 150deg.C for 16h, and measuring high temperature and high pressure filtration loss at 180deg.C under 3.5MPa.
Example 1
Preparation of carbon dots: dissolving 3g of citric acid and 6g of urea in 20mL of deionized water, and stirring until the citric acid and the urea are completely dissolved to form colorless and transparent solution; then placing the solution into a 650W microwave oven, heating deeply for 5 minutes, and gradually changing the solution from a colorless transparent state to brown in the heating process to finally obtain a dark brown solid; finally, redissolving the dark brown solid in 20mL of deionized water, stirring to fully dissolve the dark brown solid, and performing centrifugal purification treatment to obtain an aqueous solution of carbon dots, wherein FIG. 1 is a TEM image of the carbon dots of the invention.
Preparation of oxidized asphalt: adding asphalt powder (softening point 120 ℃) into a three-neck flask, adding potassium permanganate solution under magnetic stirring, heating until boiling reflux reaction is carried out for 40min until the potassium permanganate solution is removed, and stopping the reaction; at this time, a large amount of asphalt floats on the liquid surface, manganese dioxide is sunk on the water bottom, the mixture is poured into a beaker, water is added, the upper layer solid is poured into a Buchner funnel, suction filtration (taking care that the lower layer manganese dioxide is not poured), drying and crushing are carried out, and oxidized asphalt powder is obtained.
Preparation of plugging material: weighing oxidized asphalt in a beaker, heating and stirring at 120-130 ℃ until the asphalt is softened, adding carbon point powder according to the mass ratio of carbon point to oxidized asphalt of 1:1, stirring for 4-6 hours, fully and uniformly mixing, cooling to room temperature for solidification, and crushing to obtain the plugging material.
The plugging type oil-based drilling fluid comprises the following components:
85mL of oil phase (diesel oil) and 15mL of water phase (20 Wt% calcium chloride aqueous solution) are mixed to form 100mL of water-in-oil, 2.5g of main emulsifier (calcium stearate) +1.2g of auxiliary emulsifier (Span-80) +3.0g of filtrate reducer (modified lignite resin) +2.0g of organic soil (lipophilic clay formed after treatment by dodecyl trimethyl ammonium bromide) +3.0g of alkalinity regulator (calcium oxide) +weighting agent (barite) are added, the density of a drilling fluid system is 1.30g/cm < 3 >, and the addition amount of plugging materials is 0g, 0.2g, 0.4g, 0.6g, 0.8g, 1g, 1.5g and 2g respectively.
The preparation of the plugging type oil-based drilling fluid comprises the following steps:
sequentially adding organic soil, a main emulsifier, an auxiliary emulsifier and an alkalinity regulator into the oil phase, and stirring and mixing to obtain a mixture A; adding a water phase into the mixture A under the stirring condition to obtain a mixture B; sequentially adding a filtrate reducer, a plugging material and a weighting agent into the mixture B under the stirring condition, wherein the obtained mixed liquid is a plugging type oil-based drilling fluid system; after each component is added, the mixture is stirred for 5min, and then the next component is added, wherein the stirring speed is 12000r/min.
After the plugging oil-based drilling fluid is subjected to hot rolling at 150 ℃ for 16 hours, the influence of the addition amount of the plugging material on the performance of the drilling fluid is evaluated, and the result is shown in Table 1.
Table 1 evaluation of plugging material addition amount on drilling fluid properties
As shown in Table 1, with the increase of the addition amount of the plugging material, the rheological property and the electrical stability of the oil-based drilling fluid system are not greatly changed, which indicates that the system is stable, but the high-temperature high-pressure fluid loss is greatly reduced, which indicates that carbon points in the plugging material are used as the plugging bridge of the rigid plugging material, a stress frame is provided for the deformable material asphalt oxide, the plugging effect is strengthened by the carbon points and the plugging material, the fluid loss is reduced, the transfer of filtrate to the stratum is reduced, and the plugging material and the oil-based drilling fluid have good compatibility.
Example 2
The preparation of carbon dots, the preparation of oxidized asphalt and the preparation of the plugging material are the same as in example 1.
The plugging type oil-based drilling fluid comprises the following components:
85mL of the oil phase (diesel oil) and 15mL of the water phase (20 Wt% aqueous calcium chloride solution) were mixed to form 100mL of water-in-oil, and 2.5g of the main emulsifier (iron petroleum sulfonate) +1.2g of the auxiliary emulsifier (polyoxypropylene)Ethylene stearate) +3.0g filtrate reducer (modified lignite resin) +1.8g organic clay (lipophilic clay formed after treatment with dodecyldimethylbenzyl ammonium chloride) +2.9g alkalinity regulator (calcium oxide) +1.0g plugging material+15 g weighting agent (calcium carbonate), to adjust the drilling fluid density to 1.30g/cm 3
The preparation method of the plugging type oil-based drilling fluid in this embodiment is the same as that in embodiment 1.
The properties of the resulting plugged oil-based drilling fluids are shown in Table 2:
table 2 properties of plugged oil-based drilling fluid systems
Example 3
The preparation of carbon dots, the preparation of oxidized asphalt and the preparation of the plugging material are the same as in example 1, except that the mass ratio of carbon dots to oxidized asphalt in the preparation of the plugging material in this example is 1:1.5.
The plugging type oil-based drilling fluid comprises the following components:
95mL of oil phase (diesel oil) and 5mL of aqueous phase (20 Wt% calcium chloride aqueous solution) were mixed to form 100mL of water-in-oil, 5.0g of main emulsifier (calcium naphthenate) +3.5g of auxiliary emulsifier (Span-80) +4.0g of filtrate reducer (modified lignite resin) +2.8g of organic clay (lipophilic clay formed after treatment with dodecyl trimethyl ammonium bromide) +3.8g of alkalinity regulator (calcium oxide) +2.0g of plugging material+21 g of weighting agent (barite) were added, and the drilling fluid density was adjusted to 1.50g/cm 3
The preparation method of the plugging type oil-based drilling fluid in this embodiment is the same as that in embodiment 1.
The properties of the resulting plugged oil-based drilling fluids are shown in Table 3:
table 3 properties of a blocked oil-based drilling fluid system
Example 4
The preparation of carbon dots, the preparation of oxidized asphalt and the preparation of the plugging material are the same as in example 1.
The plugging type oil-based drilling fluid comprises the following components:
90mL of oil phase (diesel oil) and 10mL of aqueous phase (20 Wt% calcium chloride aqueous solution) are mixed to form 100mL of water-in-oil, 3.0g of main emulsifier (naphthenic acid amide) +2.0g of auxiliary emulsifier (Span-80) +3.5g of filtrate reducer (modified lignite resin) +2.0g of organic clay (lipophilic clay formed after treatment by dodecyl dimethyl benzyl ammonium chloride) +3.0g of alkalinity regulator (calcium oxide) +1.5g of plugging material+21 g of weighting agent (barite) are added, and the drilling fluid density is adjusted to 1.50g/cm 3
The preparation method of the plugging type oil-based drilling fluid in this embodiment is the same as that in embodiment 1.
The properties of the resulting plugged oil-based drilling fluids are shown in Table 4:
table 4 properties of a blocked oil-based drilling fluid system
Example 5
The preparation of carbon dots, the preparation of oxidized asphalt and the preparation of the plugging material are the same as in example 1, except that the mass ratio of carbon dots to oxidized asphalt in the preparation of the plugging material in this example is 1:2.
The plugging type oil-based drilling fluid comprises the following components:
85mL of oil phase (diesel oil) and 15mL of water phase (20 Wt% calcium chloride aqueous solution) were mixed to form 100mL of water-in-oil, and 4.0g of main emulsifier (calcium stearate) +2.5g of secondary emulsifier (Span-80) +3.0g of filtrate reducer (modified lignite resin) +2.5g of organic clay (lipophilic clay formed after treatment with dodecyldimethylbenzyl ammonium chloride) +3.5g of alkalinity regulator (calcium oxide) +1.7g of plugging material+18 g of weighting agent (barite) were added to adjust the drilling fluid density to 1.40g/cm3.
The preparation method of the plugging type oil-based drilling fluid in this embodiment is the same as that in embodiment 1.
The properties of the resulting plugged oil-based drilling fluid are shown in Table 5:
table 5 properties of the blocked oil-based drilling fluid system
Example 6
The preparation of carbon dots, the preparation of oxidized asphalt and the preparation of the plugging material are the same as in example 1, except that the mass ratio of carbon dots to oxidized asphalt in the preparation of the plugging material in this example is 1:2.2.
The plugging type oil-based drilling fluid comprises the following components:
90mL of oil phase (diesel oil) and 10mL of aqueous phase (20 wt% calcium chloride aqueous solution) were mixed to form 100mL of water-in-oil, and 4.5g of main emulsifier (iron petroleum sulfonate) +3.0g of secondary emulsifier (polyoxypropylene stearate) +3.5g of filtrate reducer (modified lignite resin) +2.0g of organic clay (lipophilic clay formed after treatment with dodecyltrimethylammonium bromide) +3.0g of alkalinity regulator (calcium oxide) +2.0g of plugging material+21 g of weighting agent (barite) were added to adjust the drilling fluid density to 1.50g/cm3.
The preparation method of the plugging type oil-based drilling fluid in this embodiment is the same as that in embodiment 1.
The properties of the resulting plugged oil-based drilling fluids are shown in Table 6:
table 6 properties of plugged oil-based drilling fluid systems
As can be seen from examples 2-6, the plugging type oil-based drilling fluid obtained by the invention has good rheological property, moderate viscosity and shear force after being aged at a high temperature of 150 ℃, and the demulsification voltage is more than 600V, and the minimum high-temperature high-pressure filtration loss is 2.2mL. By adding the novel plugging material into the oil-based drilling fluid system, a set of leakage-proof strong plugging oil-based drilling fluid system is formed, so that plugging can be effectively carried out, and the high-temperature high-pressure water loss of the oil-based drilling fluid system is reduced.
Example 7
The only difference from example 1 is that the carbon dots are prepared by hydrothermal method:
weighing 1.15g of citric acid, dissolving the citric acid in 20mL of deionized water, sufficiently dissolving the citric acid by ultrasonic treatment, transferring the prepared solution into a 30mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 4 hours at 200 ℃ in a muffle furnace, naturally cooling the reaction system to room temperature after the reaction is finished, and removing supernatant; then 1.5g of sulfanilic acid is weighed and added into the supernatant, the sulfanilic acid is fully dissolved by ultrasonic, and the solution is transferred into a hydrothermal reaction kettle to react for 5 hours at 135 ℃ in a muffle furnace. After the reaction is finished, naturally cooling the reaction system to room temperature again, removing supernatant, sequentially passing through water-based filter membranes of 0.45 and 0.22 mu m to finally obtain carbon dot solution, and finally obtaining carbon dots through freeze drying.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.

Claims (6)

1. A plugging material, characterized in that: the plugging material consists of a rigid plugging material and a deformable material; the rigid plugging material is carbon dots; the deformable material is oxidized asphalt; the mass ratio of the carbon dots to the oxidized asphalt is 1:1.5; continuously stirring the deformable material under the heating condition, adding the rigid plugging material for mixing, cooling, solidifying and crushing to obtain the plugging material;
the carbon dots are prepared by any one of the following methods:
firstly, dissolving 3g of citric acid and 6g of urea in 20mL of deionized water, and stirring until the citric acid and the urea are completely dissolved to form colorless and transparent solution; then placing the solution into a 650W microwave oven, heating deeply for 5 minutes, and gradually changing the solution from a colorless transparent state to brown in the heating process to finally obtain a dark brown solid; finally, redissolving the dark brown solid in 20mL of deionized water, stirring to fully dissolve the dark brown solid, performing centrifugal purification treatment to obtain an aqueous solution of carbon dots, and performing freeze drying to obtain the carbon dots;
or weighing 1.15g of citric acid, dissolving the citric acid in 20mL of deionized water, fully dissolving the citric acid by ultrasonic treatment, transferring the prepared solution into a 30mL hydrothermal reaction kettle with a polytetrafluoroethylene lining, reacting for 4 hours at 200 ℃ in a muffle furnace, naturally cooling the reaction system to room temperature after the reaction is finished, and removing supernatant; then 1.5g of sulfanilic acid is weighed and added into the supernatant, the supernatant is fully dissolved by ultrasonic treatment, and then the solution is transferred into a hydrothermal reaction kettle to react for 5 hours at 135 ℃ in a muffle furnace; after the reaction is finished, naturally cooling the reaction system to room temperature again, removing supernatant, sequentially passing through water-based filter membranes of 0.45 and 0.22 mu m to obtain a carbon dot solution, and finally obtaining carbon dots through freeze drying.
2. The utility model provides a shutoff formula oil-based drilling fluid which characterized in that: comprising the plugging material of claim 1.
3. The plugged oil-based drilling fluid of claim 2, wherein: the plugging type oil-based drilling fluid comprises the following components:
oil phase: aqueous phase= (85-95): (5-15);
and the following components, based on 100mL of total volume of the oil phase and the water phase:
2.5 to 5g of main emulsifying agent,
1.2 to 3.5g of auxiliary emulsifier,
1.8 to 2.8g of organic soil, 3 to 4g of filtrate reducer,
2.9 to 3.8g of alkalinity regulator,
0.2-2g of plugging material,
and a weighting agent determined based on the density of the drilling fluid.
4. The plugged oil-based drilling fluid of claim 3, wherein: the plugging material is 1-2g.
5. The plugged oil-based drilling fluid of claim 3, whereinIn the following steps: the pH of the plugging oil-based drilling fluid is 8-9, and the system density is 1.3-1.5 g/cm 3 The temperature is resistant to 150 ℃.
6. A method of preparing the plugged oil-based drilling fluid of claim 3, comprising the steps of:
sequentially adding organic soil, a main emulsifier, a secondary emulsifier and an alkalinity regulator into the oil phase, and stirring and mixing to obtain a mixture A;
adding a water phase into the mixture A under the stirring condition to obtain a mixture B;
and sequentially adding the filtrate reducer, the plugging material and the weighting agent into the mixture B under the stirring condition, wherein the obtained mixed liquid is the plugging type oil-based drilling fluid system.
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