CN113416523B - Oil-based gelling plugging agent - Google Patents
Oil-based gelling plugging agent Download PDFInfo
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- CN113416523B CN113416523B CN202110695966.1A CN202110695966A CN113416523B CN 113416523 B CN113416523 B CN 113416523B CN 202110695966 A CN202110695966 A CN 202110695966A CN 113416523 B CN113416523 B CN 113416523B
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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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- 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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Abstract
The application provides an oil-based gelling plugging agent, which comprises bentonite, expandable graphite, crystalline flake graphite, sodium ethoxide and a microcapsule composite material, wherein chlorinated paraffin-70 is used as a wall material, and benzoic acid and oil absorption fibers are used as core materials. The volume of the expandable graphite is expanded by utilizing the high temperature at the bottom of the well, so that the liquid phase in the leakage passage is adsorbed, and effective leaking stoppage ingredients in the liquid phase are promoted to enter the leakage passage. Meanwhile, the core material in the microcapsule composite material is released in the leakage passage due to the high temperature at the bottom of the well, the leakage passage is filled by the volume expansion of the oil absorption fiber in the core material, the viscosity of the bentonite is increased by changing the polarity and alkalinity of a liquid phase system due to benzoic acid in the core material, a viscous substance is formed in the leakage passage, the flow resistance in the passage is increased, the volume expanded oil absorption fiber and the expandable graphite are convenient to accumulate in the leakage passage, meanwhile, the fitting degree of a plug and a well wall is improved, and the single plugging success rate is improved.
Description
Technical Field
The application relates to the technical field of petroleum drilling, in particular to an oil-based gelling plugging agent.
Background
The oil-based drilling fluid takes oil as a dispersion medium, has better lubricating property and high temperature resistance compared with water-based drilling fluid, is an important medium means for drilling high-temperature deep wells, large-inclination directional wells, horizontal wells and complex stratums at present, and is widely used as a stuck freeing fluid, a perforation completion fluid, a workover fluid and a core flooding fluid. However, due to the strong lubricating property of the oil-based drilling fluid, the oil-based drilling fluid is easier to enter weak rock faces, and hydraulic fracture is generated, so that leakage is caused. Meanwhile, the surface of the well wall of the leakage passage is oleophilic, so that the flow resistance is reduced, and the plugging difficulty of the leakage passage is increased. Therefore, the oil-based drilling fluid is more prone to leakage than the water-based drilling fluid, and in addition, the oil-based drilling fluid is higher in cost, and the plugging agent matched with the oil-based drilling fluid is the key for improving the use efficiency of the oil-based drilling fluid.
The existing plugging agent for the oil-based drilling fluid is used for plugging a leakage passage in an expansion filling mode, and the plugging effect is highly dependent on the distribution density and volume change of an expansion material in the leakage passage, so the use of the plugging agent is dependent on the detection and analysis of the leakage passage. However, the detection work difficulty of the underground condition is large, the analysis of the stratum structure is only estimation, and the stratum structure is difficult to completely meet the actual condition, so that the success rate of single plugging is not high.
Disclosure of Invention
The application aims to provide an oil-based gelling plugging agent for solving the technical problem that the single plugging effect of the existing oil-based gelling plugging agent is poor.
The oil-based gelling plugging agent provided by the application comprises the following mixed components in parts by volume:
5 to 15 parts of bentonite;
20-40 parts of expandable graphite;
15-20 parts of crystalline flake graphite;
1.5 to 2.5 portions of sodium ethoxide;
30-50 parts of a microcapsule composite material; the microcapsule composite material is prepared by embedding chlorinated paraffin-70 serving as a wall material and benzoic acid and oil absorption fiber serving as a composite core material.
The components of the oil-based gelling plugging agent disclosed by the application are stable under the conditions of normal temperature and water resistance,
has both particles and powder, and the components are gray black as a whole due to the higher proportion of expandable graphite and crystalline flake graphite in the components.
The bentonite can be well dispersed in a polar and alkaline liquid phase system, and the viscosity of the bentonite is gradually increased along with the reduction of the polarity and the alkalinity of the liquid phase system. In the application, the bentonite changes viscosity through polarity and alkalinity regulation and control of a liquid phase system (formed by mixing the bentonite with well slurry/base fluid), and is used for forming a viscous substance in a leakage channel and increasing the fluid resistance in the leakage channel.
In the application, the expandable graphite can expand under the action of underground high temperature to change the internal pore diameter and adsorb liquid phase and small particulate matters, and is mainly used for quickly adsorbing the liquid phase in a leakage passage, so that the viscosity of bentonite is further improved; meanwhile, the method has the function of filling cracks by volume expansion and promotes the formation of leakage channel plugs.
In the application, the flake graphite promotes other components to enter the leakage passage through the lubricating property of the flake graphite.
During the mixing process of the sodium ethoxide and well slurry or base fluid, the polarity and the alkalinity of a liquid phase system are simultaneously increased. Meanwhile, after meeting water in the well slurry/base liquid, the sodium ethoxide can quickly react to obtain ethanol and sodium hydroxide, so that the polarity of a liquid phase system is further increased, and the bentonite can be well dispersed in the liquid phase system.
In the application, the wall material of the microcapsule composite material is chlorinated paraffin-70, is solid at normal temperature, and begins to soften and melt at the temperature of 100 ℃. After the liquid phase system is injected into the underground, the high temperature of the stratum of the leakage channel melts the wall material, so that the capsule wall is broken, and the core material is released to enter the leakage channel. The oil absorption fiber in the core material absorbs the oil phase in the leakage passage, so that the oil phase is expanded to fill the leakage passage.
Meanwhile, after entering the liquid phase system, benzoic acid in the core material is subjected to neutralization reaction with sodium ethoxide/sodium hydroxide, so that the polarity of the liquid phase system is reduced, and the alkalinity of the original strong alkaline liquid phase system is suddenly reduced. The polarity and alkalinity of the liquid phase system are changed, so that the viscosity of the bentonite is increased. In the leakage passage, viscous bentonite wraps the volume-expanded oil absorption fiber and the expandable graphite to form a plug.
The volume of the expandable graphite is expanded by utilizing the high temperature at the bottom of the well, so that the liquid phase in the leakage passage is adsorbed, and effective leaking stoppage ingredients in the liquid phase are promoted to enter the leakage passage. Meanwhile, the core material in the microcapsule composite material is released in the leakage passage due to the high temperature at the bottom of the well, the leakage passage is filled by the volume expansion of the oil absorption fiber in the core material, the viscosity of the bentonite is increased by changing the polarity and alkalinity of a liquid phase system through benzoic acid in the core material, a viscous substance is formed in the leakage passage, the flow resistance in the passage is increased, the volume expanded oil absorption fiber and the expandable graphite are convenient to accumulate in the leakage passage, and finally a plugging plug with viscous characteristics is formed in the leakage passage. The viscosity of the plug increases the plugging effect of the leakage channel well wall, and is beneficial to improving the success rate of single plugging.
In the present application, sodium bentonite with higher thermal stability and viscosity is preferably adopted as bentonite to match the formation temperature of the underground leakage passage.
In the application, the expandable graphite adopts a mark of which the expansion volume is more than or equal to 200mL/g in GB 10698-89, which is beneficial to improving the expansion adsorption effect of the expandable graphite, improving the efficiency of guiding effective plugging components to enter a leakage passage and promoting the rapid change of the viscosity of bentonite. The particle size of the expandable graphite is preferably 40 to 80 meshes, the volume change rate is large, and the cost is low.
In the application, the particle size of the crystalline flake graphite is 400 to 600 meshes.
In the application, the components are powder and are easy to absorb moisture, and the sodium ethoxide is easy to react with water, so that the mixing of the components is divided into two stages. The first stage is to premix and dry the components except sodium ethoxide. In the premixed component, the wall material of the microcapsule composite material is melted at about 100 ℃, so that the premixed component is dried at a low temperature. The heat pump type fluidized bed adopted in the application has the relative humidity of inlet air flow not higher than 20%, the inlet air temperature of 60-65 ℃ and the outlet air temperature of 30-35 ℃. The second stage is to mix sodium ethoxide into the pre-mixed components after the first stage drying. Preferably, the temperature of the mixing environment is controlled to be not higher than 40 ℃ and the relative humidity is controlled to be not higher than 5%, and the packaging is carried out after the mixing is finished, so that the application is effectively isolated from the external environment. In this application, adopt trinity wrapping bag to provide the confined environment of water proof, oxygen isolation for the material.
In the present application, the microcapsule composite material is prepared by the following steps:
s1, mixing the following components in parts by volume: (25 to 35): (50-80) taking benzoic acid, oil absorption fiber and chlorinated paraffin-70 for later use;
s2, heating the chlorinated paraffin in the step S1 to the temperature of-70 to 100 to 120 ℃ to obtain a liquid wall material;
s3, keeping the temperature of the liquid wall material obtained in the step S2 within 95-115 ℃, and putting the benzoic acid and the oil absorption fiber obtained in the step S1 into the liquid wall material for homogenization to prepare an emulsion;
and S4, carrying out spray drying treatment on the emulsion obtained in the step S3, and screening powder particles.
Wherein the content of the first and second substances,
in the step S1, the oil fiber comprises polyolefin fiber and wood fiber which are mixed according to the volume part ratio of (5-8) 1. The polyolefin fiber can specifically adsorb the oil phase, and has excellent adsorption efficiency and expansion rate. The wood fiber has strong surface adhesion, and is beneficial to promoting the gathering of the polyolefin fiber at the crack well wall of the perspective channel so as to improve the plugging effect; meanwhile, the wood fiber has the capacity of adsorbing an oil phase and a water phase, can be used as a filter medium of a liquid phase system, and reduces the complex components in the lost liquid phase system;
in the step S3, as the core material comprises two components, in order to ensure the mixing effect of the core material during embedding, the oil-absorbing fiber and benzoic acid are premixed, dried and crushed before feeding, and mixed powder with the particle size of 150 to 200 mu m is screened;
in step S4, the particle size of the powder particles obtained by screening is 300 to 500 μm. The leaking stoppage effect of the application depends on the process of controlling the release of the core material in the microcapsule composite material at high temperature in the well, so that the core material must be fully embedded. The quality of the components of the microcapsule composite material is ensured by selecting the particle sizes of the core material powder and the embedded particles;
and S4, adopting a low-temperature spray drying method, wherein the feeding speed is 30 to 55ml/min, and the spray drying temperature is 20 to 35 ℃.
According to the prediction of the underground stratum structure, the addition amount of the composite fluid system in the well slurry/base fluid is adjusted to form the composite fluid system for use while drilling. The addition amount of 1 to 3 percent can be used for treating low pressure and small permeability leakage. Can also be compounded with bridging substances to perform bridge plug plugging.
Drawings
In order to more clearly illustrate the technical solutions in the present application or the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a result of normal temperature leak stoppage experiment using the oil-based gelling leak stopper prepared in example 1 in example 4.
Fig. 2 is a result of high temperature leak stoppage experiment using the oil-based gelling leak stopper prepared in example 1 in example 4.
FIG. 3 is a graph showing the results of fluidity tests of example 4 using the oil-based gelling plugging agent prepared in example 1 at different temperatures.
Fig. 4 is a result of water invasion and oil invasion experiments performed by the oil-based gelling plugging agent prepared in example 1 in example 4.
Fig. 5 is a graph showing the results of the thickening experiment performed in example 4 using the oil-based gelling plugging agent prepared in example 1.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the embodiments of the present application. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
Embodiments of the present application will be described in detail below with reference to the accompanying drawings.
Example 1
The oil-based gelling plugging agent provided by the embodiment comprises the following mixed components in parts by volume:
5 to 8 parts of sodium bentonite;
500-I to 25 parts of expandable graphite KP;
15-20 parts of 400-mesh flake graphite;
1.5 to 2.5 portions of sodium ethoxide;
30-40 parts of a microcapsule composite material;
wherein, the first and the second end of the pipe are connected with each other,
the microcapsule composite material is prepared by the following steps:
s1, taking benzoic acid, oil absorption fiber and chlorinated paraffin-70 according to the volume part ratio of 1; wherein the oil absorption fiber comprises polyolefin fiber and wood fiber which are mixed in a volume part ratio of 5;
s2, sequentially premixing, drying and crushing the benzoic acid and the oil absorption fiber in the step S1 by adopting existing mixing, drying and crushing equipment, and screening powder with the particle size of 150 to 200 micrometers for later use;
s3, heating the chlorinated paraffin in the step S1 to the temperature of-70-100-120 ℃ to obtain a liquid wall material, and keeping the liquid wall material at the constant temperature of 95-115 ℃ by adopting the existing equipment;
s4, putting the powder in the step S2 into the liquid wall material in the step S3, and homogenizing the powder at constant temperature by adopting the existing equipment to prepare an emulsion;
s5, processing the emulsion obtained in the step S4 by adopting a low-temperature spray drying process at the feeding speed of 30 to 55ml/min and the spray drying temperature of 20 to 35 ℃ to prepare powder particles;
s6, screening the powder particles obtained in the step S5 by adopting 35-mesh and 50-mesh screens, and collecting the powder particles with the particle size of about 300 to 500 microns.
After the components are prepared, the components except the sodium ethoxide are mixed and dried at low temperature (not higher than 70 ℃) by adopting the existing equipment. Then, sodium ethoxide is mixed in under a dry environment, and then the mixture is packaged.
Example 2
The oil-based gelling plugging agent provided by the embodiment comprises the following mixed components in parts by volume:
8 to 12 parts of sodium bentonite;
500-II to 20-30 parts of expandable graphite KP;
15-20 parts of 500-mesh crystalline flake graphite;
1.5 to 2.5 portions of sodium ethoxide;
40-50 parts of a microcapsule composite material;
wherein the content of the first and second substances,
the microcapsule composite material is prepared by the following steps:
s1, taking benzoic acid, oil absorption fiber and chlorinated paraffin-70 according to the volume part ratio of 1; wherein the oil absorption fiber comprises polyolefin fiber and wood fiber which are mixed according to the volume part ratio of 8;
s2, sequentially premixing, drying and crushing the benzoic acid and the oil absorption fiber in the step S1 by adopting existing mixing, drying and crushing equipment, and screening powder with the particle size of 150 to 200 micrometers for later use;
s3, heating the chlorinated paraffin in the step S1 to the temperature of-70-100-120 ℃ to obtain a liquid wall material, and keeping the liquid wall material at the constant temperature of 95-115 ℃ by adopting the existing equipment;
s4, putting the powder in the step S2 into the liquid wall material in the step S3, and homogenizing the powder at constant temperature by adopting the existing equipment to prepare an emulsion;
s5, processing the emulsion obtained in the step S4 by adopting a low-temperature spray drying process at the feeding speed of 30 to 55ml/min and the spray drying temperature of 20 to 35 ℃ to prepare powder particles;
s6, screening the powder particles obtained in the step S5 by adopting a 35-mesh screen and a 50-mesh screen, and collecting the powder particles with the particle size of about 300 to 500 micrometers.
After the components are prepared, the components except the sodium ethoxide are mixed and dried at low temperature (not higher than 70 ℃) by adopting the existing equipment. And then, mixing sodium ethoxide in a dry environment, and packaging.
Example 3
The oil-based gelling plugging agent provided by the embodiment comprises the following mixed components in parts by volume:
10 to 15 parts of sodium bentonite;
300-I to 40 parts of expandable graphite KP;
15 parts of 600-mesh crystalline flake graphite;
1.5 to 2.5 portions of sodium ethoxide;
40-45 parts of a microcapsule composite material;
wherein the content of the first and second substances,
the microcapsule composite material is prepared by the following steps:
s1, taking benzoic acid, oil absorption fiber and chlorinated paraffin-70 according to the volume part ratio of 1; wherein the oil absorption fiber comprises polyolefin fiber and wood fiber which are mixed according to the volume part ratio of 6;
s2, sequentially premixing, drying and crushing the benzoic acid and the oil absorption fiber in the step S1 by adopting existing mixing, drying and crushing equipment, and screening powder with the particle size of 150-200 mu m for later use;
s3, heating the chlorinated paraffin in the step S1 at a temperature of between 70 and 100 to 120 ℃ to obtain a liquid wall material, and keeping the liquid wall material at a constant temperature of between 95 and 115 ℃ by adopting the existing equipment;
s4, putting the powder in the step S2 into the liquid wall material in the step S3, and homogenizing the powder at constant temperature by adopting the existing equipment to prepare an emulsion;
s5, processing the emulsion obtained in the step S4 by adopting a low-temperature spray drying process at the feeding speed of 30 to 55ml/min and the spray drying temperature of 20 to 35 ℃ to prepare powder particles;
s6, screening the powder particles obtained in the step S5 by adopting 35-mesh and 50-mesh screens, and collecting the powder particles with the particle size of about 300 to 500 microns.
Mixing the above components at low temperature (not higher than 70 deg.C) with existing equipment, and drying. And then, mixing sodium ethoxide in a dry environment, and packaging.
Example 4
In this example, the oil-based gelling plugging agent obtained in example 1 was mixed with an oil-based emulsion in an amount of 1.5% to prepare a plugging slurry, and the following experiments were performed.
(1) Normal temperature plugging experiment
A20-to 40-mesh sand bed is adopted, the pressure is 0.7MPa, and the experimental time is 30min, and the result is shown in figure 1. And (3) determining the result by adopting an FA non-permeability filtration apparatus, wherein the FA leakage is zero, and the FA invasion depth is 3cm.
(2) High temperature plugging experiment
In the high-temperature plugging experiment, the plugging slurry is aged for 16h at 150 ℃, and the result is shown in figure 2, the aged plugging solution is in a jelly shape, and a glass rod can be vertically inserted without falling.
(3) Fluidity test
The fluidity of the plugging slurry at different temperatures was measured by a fluidity tester, and the results are shown in fig. 3.
In FIG. 3, the fluidity and rheological properties of the plugging slurry at room temperature, 110 deg.C (16 h), and 140 deg.C (16 h) are shown from left to right. As can be seen from the figure, the fluidity at room temperature was 20.5cm; after aging for 16h at 110 ℃, the material has no fluidity and the fluidity is 8.5; after aging for 16h at 140 ℃, the product has no fluidity and the fluidity is 6.5.
(4) Water invasion and oil invasion experiment
Plugging slurry formed by aging at 140 ℃ in a fluidity experiment is manufactured into a regular shape and is respectively soaked in clean water and diesel oil, and the result is shown in figure 4.
In fig. 4, the results of the water invasion experiment and the oil invasion experiment are shown from left to right, respectively. The conglomerate made of the plugging slurry does not scatter in water; after soaking in diesel oil for 3h, the scattered powder is gradually increased. The application shows that the water invasion resistance is excellent, and the oil invasion resistance is good.
(5) Thickening experiment
A self-made cylinder (with the inner diameter of 3cm and the height of 27cm, the mass of 151.24g and bottom sinking in the plugging slurry at 55 ℃) is adopted to simulate a static shear tester to test the static shear force of the plugging slurry at 140 ℃ for different times. The result shows that the plugging slurry finishes thickening when the shear force is kept unchanged for about 7 to 8 hours at the temperature of 140 ℃.
The pressure thickening test of the plugging slurry by using a DFC-071013 type pressure thickening instrument showed that the results are shown in FIG. 5. The leakage-stopping slurry has good fluidity at 65 ℃ and the consistency is lower than 20BC, so that the safety of ground slurry preparation can be ensured; the well still has better fluidity at 110 ℃, the consistency is lower than 36BC, and the safety of the well entering temperature rise process is ensured; the plugging slurry is quickly thickened at 140 ℃ and loses fluidity, which shows that the plugging slurry can be quickly gelled at the excitation temperature of a leaking layer to finish plugging.
Claims (8)
1. The oil-based gelling plugging agent is characterized by comprising the following mixed components in parts by volume:
5 to 15 parts of bentonite;
20-40 parts of expandable graphite;
15-20 parts of crystalline flake graphite;
1.5 to 2.5 portions of sodium ethoxide;
30-50 parts of a microcapsule composite material;
wherein, the first and the second end of the pipe are connected with each other,
the expandable graphite is of a mark with an expansion volume of more than or equal to 200mL/g in GB 10698-89, and the particle size is 40-80 meshes;
the particle size of the flake graphite is 400 to 600 meshes;
the microcapsule composite material is prepared by the following steps:
s1, taking benzoic acid, oil absorption fiber and chlorinated paraffin-70 for later use according to the volume ratio of 1 (25 to 35) to 50 to 80;
s2, heating the chlorinated paraffin in the step S1 to the temperature of-70 to 100 to 120 ℃ to obtain a liquid wall material;
s3, keeping the temperature of the liquid wall material obtained in the step S2 within 95-115 ℃, and putting the benzoic acid and the oil absorption fiber obtained in the step S1 into the liquid wall material for homogenization to prepare an emulsion;
s4, carrying out spray drying treatment on the emulsion obtained in the step S3, and screening powder particles with the particle size of 300-500 mu m.
2. The oil-based gelling plugging agent according to claim 1, wherein sodium bentonite is used as the bentonite.
3. The oil-based gelling plugging agent as claimed in claim 1, wherein the bentonite, the expandable graphite, the flake graphite and the microcapsule composite material are premixed and then dried in a heat pump fluidized bed to reduce the water content to not more than 3%.
4. The oil-based gelling plugging agent as claimed in claim 3, wherein the air inlet temperature of the heat pump type fluidized bed is 60 to 65 ℃, the air outlet temperature is 30 to 35 ℃, and the relative humidity of the air inlet flow is not higher than 20%.
5. The oil-based gelling plugging agent according to claim 3, wherein a dry premix of the bentonite, the expandable graphite, the flake graphite and the microcapsule composite material is uniformly mixed with the sodium ethoxide, and then is hermetically packaged by a three-in-one packaging bag.
6. The oil-based gelling plugging agent as claimed in claim 1, wherein in step S1, the oil absorbing fiber comprises polyolefin fiber and wood fiber mixed in a volume ratio of (5 to 8): 1.
7. The oil-based gelling plugging agent according to claim 6,
in the step S3, the oil absorption fiber and the benzoic acid are premixed, dried and crushed in sequence before feeding, so that the particle size of the mixture is 150 to 200 mu m;
in the step S4, the particle size of the powder particles obtained by screening is 300 to 500 mu m.
8. The oil-based gelling plugging agent as claimed in claim 6, wherein the step S4 is performed by a low-temperature spray drying method, the feeding rate is 30 to 55ml/min, and the spray drying temperature is 20 to 35 ℃.
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| CN112592700B (en) * | 2020-12-22 | 2022-04-29 | 广州江盐化工有限公司 | Oil-based drilling fluid based on chlorinated paraffin and preparation method and application thereof |
| CN116081617A (en) * | 2023-01-16 | 2023-05-09 | 中国石油大学(华东) | Ultra-deep oil and gas reservoir wet phase expandable modified graphite water control system and preparation method and application thereof |
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