CN111808583B - Composite plugging agent bridge plug plugging particles for drilling fluid - Google Patents
Composite plugging agent bridge plug plugging particles for drilling fluid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
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- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/10—Nanoparticle-containing well treatment fluids
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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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Abstract
The invention discloses a composite plugging agent bridge plug plugging particle for drilling fluid, which comprises the following raw materials: the plugging particles have the properties of high elasticity, corrosion resistance, salt resistance and high temperature resistance, and can ensure good adaptability to well wall cracks of different shapes; the vinyl acetate-ethylene copolymer emulsion stays at the cracks to form a film which is positioned on the surface of the rock and does not penetrate into the depth of the rock, the effect of the blocking film is weakened as long as the over-balanced pressure is eliminated, once reverse pressure exists, the blocking film is eliminated, the reservoir stratum cannot be permanently blocked and damaged, and the technical problems of leakage, sticking, collapse and oil layer damage which are easily caused when a plurality of pressure systems or pressure failure strata are drilled in a long open hole in the prior art can be well solved.
Description
Technical Field
The invention belongs to the technical field of plugging agents, and particularly relates to a composite plugging agent bridge plug plugging particle for drilling fluid.
Background
In the process of drilling, drilling fluid filtrate easily enters the stratum through tiny pores under the action of pressure difference, and the propagation of hydraulic pressure in the tiny cracks causes the cracks to develop, so that the stability of the well wall is poor, and well drilling accidents such as well wall collapse and the like are caused seriously.
The instability of the well wall can cause a series of underground complex conditions such as leakage spraying, collapse, clamping, inclination and the like. Further, the drilling period is prolonged, the drilling cost is increased, the drilling speed is reduced, and the economic benefit of oil and gas exploration and development is seriously influenced. The method for solving the instability of the hard and brittle shale well wall is to utilize the drilling fluid to add a plugging material, reduce the change amount of the horizontal stress of the well Jian Tongyan, prevent the pore pressure from transmitting and prolong the collapse period. At present, asphalt materials are mainly used as plugging materials for oil-based drilling fluids, the softening point of asphalt is required to be matched with the stratum, the softening point is difficult to determine in the actual operation process, and asphalt colloid influences the rheological property of the drilling fluid and affects the drilling speed to a certain extent.
The existing plugging agent has the following problems that 1, the plugging material has large particle size and poor matching property with the micro-pore and the micro-crack of a special shale stratum; 2. the compatibility with the oil-based drilling fluid is poor, and the quality of a filter cake of the oil-based drilling fluid cannot be effectively improved.
Disclosure of Invention
The invention aims to provide a composite plugging agent bridge plug plugging particle for drilling fluid.
The technical problems to be solved by the invention are as follows:
the composite plugging agent for drilling fluid is mainly used for plugging large pore passages, multiple pores and fractured loss in the drilling process, and is one of the most commonly used drilling fluid treating agents. Can effectively block different permeable stratums, namely has the effects of broad-spectrum leakage prevention and storage layer protection. The plugging effect of the traditional drilling fluid mainly depends on the matching degree of particle distribution and the pore throat size of the stratum, and the application range is narrow.
The purpose of the invention can be realized by the following technical scheme:
the composite plugging agent bridge plug plugging particles for the drilling fluid comprise the following raw materials in parts by weight: 30-50 parts of room-temperature vulcanized silicone rubber, 5-10 parts of modified carbon spheres, 10-15 parts of modified wood powder, 0.05-0.1 part of cross-linking agent, 0.02-0.04 part of vulcanizing agent, 3-8 parts of hard filler, 2-5 parts of dispersing agent and 20-30 parts of vinyl acetate-ethylene copolymer emulsion;
the preparation method of the composite plugging agent bridge plug plugging particles for the drilling fluid comprises the following steps:
firstly, dispersing a hard filler in room-temperature vulcanized silicone crude rubber, and stirring at a rotating speed of 300-500r/min for 2-4h to obtain a viscous mixture A;
secondly, adding a cross-linking agent and a vulcanizing agent into the viscous mixture A, reacting for 12-36h at the temperature of 20-50 ℃ and the rotating speed of 200-300r/min, then heating to 70-120 ℃ for reacting for 3-12h, and then cooling to room temperature to obtain a mixture B;
thirdly, adding a dispersing agent into the mixture B, stirring at the rotating speed of 300-500r/min, adding vinyl acetate-ethylene copolymer emulsion, and stirring for 3-5 hours to obtain a mixture C;
and fourthly, transferring the mixture C into a granulator for cutting granulation, cooling and drying, and mixing the mixture C with the modified carbon balls and the modified wood powder for 3-6 hours at a rotating speed of 150-300r/min to obtain the composite plugging agent bridge plug plugging particles for the drilling fluid.
Further, the dispersant is span 80 or tween 80.
Further, the hard filler is a mixture consisting of nanoscale silica, nanoscale calcium carbonate, 400-mesh calcium carbonate and 800-mesh calcium carbonate, and the mass ratio of the nanoscale silica to the nanoscale calcium carbonate to the 400-mesh calcium carbonate to the 800-mesh calcium carbonate is 5-8:3-5:1:2-4.
Further, the cross-linking agent is one or a mixture of two of tetraethoxysilane and poly tetraethoxysilane mixed in any proportion.
Further, the vulcanizing agent is dibutyltin dilaurate or stannous octoate.
Further, the preparation method of the modified carbon sphere comprises the following steps:
s1, adding 100-200 parts by weight of natural starch into 300-400 parts by weight of deionized water, carrying out ultrasonic treatment for 2-4h at 800W to obtain a transparent solution, carrying out hydrothermal reaction on the transparent solution at 130-150 ℃ for 4-6h to obtain a brown solution, and carrying out freeze drying on the brown solution to obtain hydrophilic powder;
s2, adding 100-150 parts by weight of sodium metaaluminate into a reaction kettle, then adding dilute sulfuric acid into the sodium metaaluminate, adjusting the pH =4 of the solution, adding 10-20 parts by weight of urea and 5-10 parts by weight of hexadecyl trimethyl ammonium bromide into the solution, stirring for 4-6h at the rotating speed of 200-300r/min, then adding the carbon spheres in the S1 into the reaction kettle, heating to 90-100 ℃, stirring for 2-3h at the rotating speed of 100-150r/min, preserving heat for 3-5h, then cooling to room temperature, adjusting the pH =7 of the mixture, and drying to obtain the modified carbon spheres.
Further, the preparation method of the modified wood flour comprises the following steps:
s11, preparing graded cork particles, namely taking 20-30 parts by weight of 30-50 mesh cork particles, 20-30 parts by weight of 60-80 mesh cork particles and 30-50 parts by weight of 100-120 mesh cork particles, and stirring and mixing for 2-4h at the rotating speed of 600-800r/min by using a stirrer to obtain the graded cork particles;
s12, mixing the graded cork granule obtained in the step S11 with the enzymolysis liquid according to the mass ratio of 1: mixing 50-100 parts of the raw materials, adding the mixture into a beaker, moving the beaker into a digital display speed measurement constant temperature magnetic stirrer, and performing constant temperature enzymolysis for 4-6 hours at the temperature of 30-40 ℃ and the rotating speed of 300-500 r/min;
s13, filtering the mixture in the step S12, wherein the mesh number of a filter screen is 150 meshes, washing the obtained filter cake for 3-5 times by using deionized water, transferring the washed filter cake into an oven, and drying the filter cake to constant weight at the temperature of 105-110 ℃ to obtain dry cork wood powder particles;
s14, taking 40-60 parts by weight of isocyanate, 20-30 parts by weight of ethyl orthosilicate and 10-20 parts by weight of dry cork wood powder particles, mixing, performing ultrasonic immersion for 40-60min under the condition that the ultrasonic frequency is 45-55kHz, filtering to obtain filter residue, washing the filter residue 3-5 times with absolute ethyl alcohol, and drying to constant weight to obtain the modified wood powder.
Further, the enzymolysis liquid is prepared from pectinase and deionized water according to a mass ratio of 1: 100-150.
Further, the isocyanate is one of diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate or phorone diisocyanate or a mixture of several diisocyanates in any proportion.
The invention has the beneficial effects that:
1. the modified carbon spheres prepared by the method have wide raw material sources, have micron-sized dimensions, are internally rigid, have elasticity on the outside, and can easily enter micropores or microcracks to play a role in bridging and plugging.
2. According to the invention, the graded cork particles are prepared, and then the graded cork particles are subjected to enzymolysis modification treatment, so that isocyanate and ethyl orthosilicate are inserted into pores inside the cork particles, when the cork particle water-absorbing agent is used, the cork particles have excellent elasticity and gradually absorb water, water molecules enter the cork particles to contact with the isocyanate and the ethyl orthosilicate after water absorption, wherein the isocyanate quickly reacts after water contact to generate carbon dioxide gas and amine substances, so that the cork particles expand, the water-leaking pores are extruded, the pores are blocked, the ethyl orthosilicate can also perform hydrolysis reaction with water to generate polysilicic acid, the polysilicic acid is adsorbed on the inner wall of a plant cell membrane, and a supporting structure is formed on the inner wall of the plant cell membrane, so that on one hand, the carbon dioxide is prevented from escaping, the cork cells are maintained in an expanded and extruded state, on the other hand, the excellent mechanical property of the cork cell membrane is ensured, and the cork cell membrane is prevented from being broken.
3. The composite plugging agent bridge plug plugging particles for drilling fluid are added with multi-particle level hard fillers, and the multi-particle level hard fillers are fused with room temperature silicon sulfide raw rubber, so that the hard fillers are wrapped with a layer of room temperature silicon sulfide raw rubber, and the room temperature silicon sulfide raw rubber has the properties of high elasticity, corrosion resistance, high temperature resistance and the like, is matched with the salt resistance and high temperature resistance of the fillers such as nano-scale silicon dioxide, nano-scale calcium carbonate and the like, and is added with modified carbon balls and modified wood flour with different particle sizes, so that the elasticity of the plugging particles can ensure that the plugging particles have good adaptability to well wall cracks with different shapes. The vinyl acetate-ethylene copolymer emulsion stays at the cracks to form a film which is positioned on the surface of the rock and does not penetrate into the depth of the rock, the action of the blocking film is weakened as long as the over-balanced pressure is eliminated, once the blocking film has reverse pressure, the blocking film can be eliminated without generating permanent blocking to damage a reservoir stratum, the leakage pressure and the fracture force gradient can be improved, the safety density window is equivalently expanded, and the technical problems of leakage, drill sticking, collapse and oil layer damage which are easily caused when a plurality of pressure systems or pressure failure strata are drilled with long naked eyes in the prior art can be better solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The composite plugging agent bridge plug plugging particles for the drilling fluid comprise the following raw materials in parts by weight: 30 parts of room-temperature vulcanized silicone crude rubber, 5 parts of modified carbon spheres, 10 parts of modified wood powder, 0.05 part of cross-linking agent, 0.02 part of vulcanizing agent, 3 parts of hard filler, 2 parts of dispersing agent and 20 parts of vinyl acetate-ethylene copolymer emulsion;
the preparation method of the composite plugging agent bridge plug plugging particles for the drilling fluid comprises the following steps:
firstly, dispersing a hard filler in room-temperature vulcanized silicone rubber, and stirring at a rotating speed of 300r/min for 2 hours to obtain a viscous mixture A;
secondly, adding a cross-linking agent and a vulcanizing agent into the viscous mixture A, reacting for 12 hours at the temperature of 20 ℃ and the rotating speed of 200r/min, then heating to 70 ℃ for reacting for 3 hours, and then cooling to room temperature to obtain a mixture B;
thirdly, adding a dispersing agent into the mixture B, stirring at the rotating speed of 300r/min, adding vinyl acetate-ethylene copolymer emulsion, and stirring for 3 hours to obtain a mixture C;
and fourthly, transferring the mixture C into a granulator for cutting granulation, cooling and drying, and mixing the mixture C with the modified carbon balls and the modified wood powder for 3 hours at a rotating speed of 150r/min to obtain the composite plugging agent bridge plug plugging particles for the drilling fluid.
The dispersant is span 80.
The hard filler is a mixture consisting of nanoscale silicon dioxide, nanoscale calcium carbonate, 400-mesh calcium carbonate and 800-mesh calcium carbonate, and the mass ratio of the nanoscale silicon dioxide to the nanoscale calcium carbonate to the 400-mesh calcium carbonate to the 800-mesh calcium carbonate is 5:3:1:2.
the cross-linking agent is tetraethoxysilane.
The vulcanizing agent is dibutyltin dilaurate.
The preparation method of the modified carbon sphere comprises the following steps:
s1, adding 100 parts by weight of natural starch into 300 parts by weight of deionized water, carrying out ultrasonic treatment for 2 hours at 800W to obtain a transparent solution, carrying out hydrothermal reaction on the transparent solution at the temperature of 130 ℃ for 4 hours to obtain a brown solution, and carrying out freeze drying on the brown solution to obtain hydrophilic powder;
s2, adding 100 parts by weight of sodium metaaluminate into a reaction kettle, then adding dilute sulfuric acid into the sodium metaaluminate, adjusting the pH =4 of the solution, adding 10 parts by weight of urea and 5 parts by weight of hexadecyl trimethyl ammonium bromide into the solution, stirring for 4 hours at the rotating speed of 200r/min, then adding the carbon spheres in the S1 into the reaction kettle, heating to 90 ℃, stirring for 2 hours at the rotating speed of 100r/min, then preserving heat for 3 hours, then cooling to room temperature, adjusting the pH =7 of the mixture, and drying to obtain the modified carbon spheres.
The preparation method of the modified wood powder comprises the following steps:
s11, preparing graded cork particles, namely taking 20 parts by weight of 30-mesh cork particles, 20 parts by weight of 60-mesh cork particles and 30 parts by weight of 100-mesh cork particles, and stirring and mixing for 2 hours at a rotating speed of 600r/min by using a stirrer to obtain the graded cork particles;
s12, mixing the graded cork granule obtained in the step S11 with the enzymolysis liquid according to the mass ratio of 1:50, mixing and adding into a beaker, moving the beaker into a digital display speed measurement constant temperature magnetic stirrer, and carrying out constant temperature enzymolysis for 4 hours at the temperature of 30 ℃ and the rotating speed of 300 r/min;
s13, filtering the mixture obtained in the S12, wherein the mesh number of a filter screen is 150 meshes, washing the obtained filter cake for 3 times by using deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight under the condition that the temperature is 105 ℃ to obtain dried cork wood powder particles;
s14, taking 40 parts by weight of isocyanate, 20 parts by weight of ethyl orthosilicate and 10 parts by weight of dry cork wood powder particles, mixing, carrying out ultrasonic immersion for 40min under the condition that the ultrasonic frequency is 45kHz, then filtering to obtain filter residue, washing the filter residue for 3 times by using absolute ethyl alcohol, and drying to constant weight to obtain the modified wood powder.
The enzymolysis liquid is prepared from pectinase and deionized water according to a mass ratio of 1:100, and preparing the product.
The isocyanate is diphenylmethane diisocyanate.
Example 2
The composite plugging agent bridge plug plugging particles for the drilling fluid comprise the following raw materials in parts by weight: 40 parts of room temperature vulcanized silicone crude rubber, 6 parts of modified carbon spheres, 13 parts of modified wood powder, 0.08 part of cross-linking agent, 0.03 part of vulcanizing agent, 5 parts of hard filler, 4 parts of dispersing agent and 25 parts of vinyl acetate-ethylene copolymer emulsion;
the preparation method of the composite plugging agent bridge plug plugging particles for the drilling fluid comprises the following steps:
firstly, dispersing a hard filler in room-temperature vulcanized silicone rubber, and stirring at a rotating speed of 400r/min for 2-4h to obtain a viscous mixture A;
secondly, adding a cross-linking agent and a vulcanizing agent into the viscous mixture A, reacting for 18 hours at the temperature of 30 ℃ and the rotating speed of 250r/min, then heating to 90 ℃ for reaction for 10 hours, and then cooling to room temperature to obtain a mixture B;
thirdly, adding a dispersing agent into the mixture B, stirring at the rotating speed of 400r/min, adding vinyl acetate-ethylene copolymer emulsion, and stirring for 4 hours to obtain a mixture C;
and fourthly, transferring the mixture C into a granulator for cutting granulation, cooling and drying, and mixing the mixture C with the modified carbon balls and the modified wood powder for 5 hours at a rotating speed of 200r/min to obtain the composite plugging agent bridge plug plugging particles for the drilling fluid.
The dispersant is span 80.
The hard filler is a mixture consisting of nanoscale silicon dioxide, nanoscale calcium carbonate, 400-mesh calcium carbonate and 800-mesh calcium carbonate, and the mass ratio of the nanoscale silicon dioxide to the nanoscale calcium carbonate to the 400-mesh calcium carbonate to the 800-mesh calcium carbonate is 4:4:1:3.
the cross-linking agent is one or a mixture of two of tetraethoxysilane and poly tetraethoxysilane mixed in any proportion.
The vulcanizing agent is dibutyltin dilaurate or stannous octoate.
The preparation method of the modified carbon sphere comprises the following steps:
s1, adding 150 parts by weight of natural starch into 350 parts by weight of deionized water, carrying out ultrasonic treatment for 3 hours at 800W to obtain a transparent solution, carrying out hydrothermal reaction on the transparent solution at the temperature of 140 ℃ for 5 hours to obtain a brown solution, and carrying out freeze drying on the brown solution to obtain hydrophilic powder;
s2, adding 130 parts by weight of sodium metaaluminate into the reaction kettle, then adding dilute sulfuric acid into the sodium metaaluminate, adjusting the pH =4 of the solution, adding 15 parts by weight of urea and 8 parts by weight of hexadecyl trimethyl ammonium bromide into the solution, stirring for 5 hours at the rotating speed of 250r/min, then adding the carbon spheres in the S1 into the reaction kettle, heating to 95 ℃, stirring for 2.5 hours at the rotating speed of 130r/min, then preserving heat for 4 hours, then cooling to room temperature, adjusting the pH =7 of the mixture, and drying to obtain the modified carbon spheres.
The preparation method of the modified wood powder comprises the following steps:
s11, preparing graded cork particles, namely taking 25 parts by weight of 40-mesh cork particles, 25 parts by weight of 70-mesh cork particles and 40 parts by weight of 110-mesh cork particles, and stirring and mixing for 3 hours at a rotating speed of 700r/min by using a stirrer to obtain the graded cork particles;
s12, mixing the graded cork granule obtained in the step S11 with the enzymolysis liquid according to the mass ratio of 1:60, mixing and adding into a beaker, moving the beaker into a digital display speed measurement constant-temperature magnetic stirrer, and carrying out constant-temperature enzymolysis for 5 hours at the temperature of 35 ℃ and the rotating speed of 400 r/min;
s13, filtering the mixture obtained in the S12, wherein the mesh number of a filter screen is 150 meshes, washing the obtained filter cake for 4 times by using deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight under the condition that the temperature is 108 ℃ to obtain dried cork wood powder particles;
s14, taking 50 parts by weight of isocyanate, 25 parts by weight of ethyl orthosilicate and 15 parts by weight of dry cork wood powder particles, mixing, carrying out ultrasonic immersion for 50min under the condition that the ultrasonic frequency is 50kHz, then filtering to obtain filter residue, washing the filter residue for 4 times by using absolute ethyl alcohol, and drying to constant weight to obtain the modified wood powder.
The enzymolysis liquid is prepared from pectinase and deionized water according to the mass ratio of 1:120, and (3).
The isocyanate is diphenylmethane diisocyanate.
Example 3
The purpose of the invention can be realized by the following technical scheme:
the composite plugging agent bridge plug plugging particles for the drilling fluid comprise the following raw materials in parts by weight: 50 parts of room-temperature vulcanized silicone raw rubber, 10 parts of modified carbon spheres, 15 parts of modified wood powder, 0.1 part of cross-linking agent, 0.04 part of vulcanizing agent, 8 parts of hard filler, 5 parts of dispersing agent and 30 parts of vinyl acetate-ethylene copolymer emulsion;
the preparation method of the composite plugging agent bridge plug plugging particles for the drilling fluid comprises the following steps:
firstly, dispersing a hard filler in room-temperature vulcanized silicone rubber, and stirring at a rotating speed of 500r/min for 4 hours to obtain a viscous mixture A;
secondly, adding a cross-linking agent and a vulcanizing agent into the viscous mixture A, reacting for 36 hours at the temperature of 50 ℃ and the rotating speed of 300r/min, then heating to 120 ℃ for reacting for 12 hours, and then cooling to room temperature to obtain a mixture B;
thirdly, adding a dispersing agent into the mixture B, stirring at the rotating speed of 500r/min, adding the vinyl acetate-ethylene copolymer emulsion, and stirring for 5 hours to obtain a mixture C;
and fourthly, transferring the mixture C into a granulator for cutting granulation, cooling and drying, and mixing the mixture C with the modified carbon balls and the modified wood powder for 6 hours at the rotating speed of 300r/min to obtain the composite plugging agent bridge plug plugging particles for the drilling fluid.
The dispersant is span 80.
The hard filler is a mixture consisting of nanoscale silicon dioxide, nanoscale calcium carbonate, 400-mesh calcium carbonate and 800-mesh calcium carbonate, and the mass ratio of the nanoscale silicon dioxide to the nanoscale calcium carbonate to the 400-mesh calcium carbonate to the 800-mesh calcium carbonate is 8:5:1:4.
the cross-linking agent is tetraethoxysilane.
The vulcanizing agent is dibutyltin dilaurate or stannous octoate.
The preparation method of the modified carbon spheres comprises the following steps:
s1, adding 200 parts by weight of natural starch into 400 parts by weight of deionized water, carrying out ultrasonic treatment for 4 hours at 800W to obtain a transparent solution, carrying out hydrothermal reaction on the transparent solution at the temperature of 150 ℃ for 6 hours to obtain a brown solution, and carrying out freeze drying on the brown solution to obtain hydrophilic powder;
s2, adding 150 parts by weight of sodium metaaluminate into a reaction kettle, then adding dilute sulfuric acid into the sodium metaaluminate, adjusting the pH of the solution to be =4, adding 20 parts by weight of urea and 10 parts by weight of hexadecyl trimethyl ammonium bromide into the solution, stirring for 6 hours at the rotation speed of 300r/min, then adding the carbon spheres in the S1 into the reaction kettle, heating to 100 ℃, stirring for 3 hours at the rotation speed of 150r/min, then keeping the temperature for 5 hours, then cooling to the room temperature, adjusting the pH of the mixture to be =7, and drying to obtain the modified carbon spheres.
The preparation method of the modified wood powder comprises the following steps:
s11, preparing graded cork particles, namely taking 30 parts by weight of 50-mesh cork particles, 30 parts by weight of 80-mesh cork particles and 50 parts by weight of 120-mesh cork particles, and stirring and mixing for 4 hours at a rotating speed of 800r/min by using a stirrer to obtain the graded cork particles;
s12, mixing the graded cork granules obtained in the S11 with the enzymolysis liquid according to the mass ratio of 1:100, mixing and adding into a beaker, moving the beaker into a digital display speed measurement constant temperature magnetic stirrer, and carrying out constant temperature enzymolysis for 6 hours at the temperature of 40 ℃ and the rotating speed of 500 r/min;
s13, filtering the mixture in the step S12, wherein the mesh number of a filter screen is 150 meshes, washing the obtained filter cake for 5 times by using deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight at the temperature of 110 ℃ to obtain dry cork powder particles;
s14, taking 60 parts by weight of isocyanate, 30 parts by weight of ethyl orthosilicate and 20 parts by weight of dry cork wood powder particles, mixing, carrying out ultrasonic immersion for 60min under the condition that the ultrasonic frequency is 55kHz, then filtering to obtain filter residue, washing the filter residue for 5 times by using absolute ethyl alcohol, and drying to constant weight to obtain the modified cork wood powder.
The enzymolysis liquid is prepared from pectinase and deionized water according to a mass ratio of 1:150, and preparing the medicament.
The isocyanate is diphenylmethane diisocyanate.
Comparative example 1
Modified carbon spheres in the raw materials of the example 1 are removed, and the rest of the preparation process is unchanged.
Comparative example 2
The modified wood flour was removed from the feed of example 2 and the remainder of the preparation was unchanged.
Comparative example 3
The comparative example is a common plugging agent for drilling fluid in the market.
The plugging agents of the embodiments 1-3 and the comparative examples 1-3 are subjected to performance tests, the rheological property, the API filtration loss and the high-temperature and high-pressure filtration loss are determined according to the method specified in the national standard GB/T16783.1-2006, and the test results are shown in the following table 1.
1. Sample preparation
Blank sample: the drilling fluid takes 5# white oil and organic bentonite as base slurry, wherein the mass fraction of the organic bentonite is 2%.
Test samples 1 to 6: taking 6 parts of 400mL blank drilling fluid, respectively adding the plugging agents of examples 1-3 and comparative examples 1-3 into the blank drilling fluid, wherein the addition amount of the plugging agent is 2% of the mass of the blank drilling fluid, and respectively preparing a sample 1, a sample 2, a sample 3, a sample 4, a sample 5 and a sample 6.
2. Test method
After the test object was stirred at a high speed for 20 minutes, the rheological properties (apparent viscosity, plastic viscosity, and dynamic shear force) and the API fluid loss were measured at 65 ℃.
And then, putting the test object into an aging tank, hot rolling for 16 hours at 200 ℃, cooling to room temperature, transferring into a stirring tank, stirring at high speed for 5 minutes, and measuring the rheological property, the API (application program interface) fluid loss and the high-temperature high-pressure fluid loss (HTHP. FL) at 65 ℃, wherein the test temperature of the high-temperature high-pressure fluid loss is 200 ℃, and the pressure difference is 3.5MPa.
TABLE 1 tables of the results of the performance tests of the plugging agents of examples 1 to 3 and comparative examples 1 to 3
As can be seen from the above table, the drilling fluid rheological property, the API filtration loss and the high-temperature and high-pressure filtration loss of the plugging agent provided in the examples 1 to 3 are superior to those of the comparative examples 1 to 3, which shows that the plugging particles of the present invention can ensure good adaptability to well wall fractures of different shapes.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. The composite plugging agent bridge plug plugging particles for the drilling fluid are characterized by comprising the following raw materials in parts by weight: 30-50 parts of room temperature vulcanized silicone raw rubber, 5-10 parts of modified carbon spheres, 10-15 parts of modified wood powder, 0.05-0.1 part of cross-linking agent, 0.02-0.04 part of vulcanizing agent, 3-8 parts of hard filler, 2-5 parts of dispersing agent and 20-30 parts of vinyl acetate-ethylene copolymer emulsion;
the preparation method of the composite plugging agent bridge plug plugging particles for the drilling fluid comprises the following steps:
firstly, dispersing a hard filler in room-temperature vulcanized silicone crude rubber, and stirring at a rotating speed of 300-500r/min for 2-4h to obtain a viscous mixture A;
secondly, adding a cross-linking agent and a vulcanizing agent into the viscous mixture A, reacting for 12-36h at the temperature of 20-50 ℃ and the rotating speed of 200-300r/min, then heating to 70-120 ℃ for reacting for 3-12h, and then cooling to room temperature to obtain a mixture B;
thirdly, adding a dispersing agent into the mixture B, stirring at the rotating speed of 300-500r/min, adding vinyl acetate-ethylene copolymer emulsion, and stirring for 3-5 hours to obtain a mixture C;
fourthly, transferring the mixture C into a granulator for cutting granulation, cooling and drying, and mixing the mixture C with modified carbon balls and modified wood powder for 3-6 hours at a rotating speed of 150-300r/min to obtain the composite plugging agent bridge plug plugging particles for the drilling fluid;
the preparation method of the modified carbon sphere comprises the following steps:
s1, adding 100-200 parts by weight of natural starch into 300-400 parts by weight of deionized water, carrying out ultrasonic treatment for 2-4h at 800W to obtain a transparent solution, carrying out hydrothermal reaction on the transparent solution at 130-150 ℃ for 4-6h to obtain a brown solution, and carrying out freeze drying on the brown solution to obtain hydrophilic powder;
s2, adding 100-150 parts by weight of sodium metaaluminate into a reaction kettle, then adding dilute sulfuric acid into the sodium metaaluminate, adjusting the pH of the solution to be =4, adding 10-20 parts by weight of urea and 5-10 parts by weight of hexadecyl trimethyl ammonium bromide into the solution, stirring for 4-6h at the rotating speed of 200-300r/min, then adding the hydrophilic powder in the S1 into the reaction kettle, heating to 90-100 ℃, stirring for 2-3h at the rotating speed of 100-150r/min, then preserving heat for 3-5h, then cooling to room temperature, adjusting the pH of the mixture to be =7, and drying to obtain a modified carbon ball;
the preparation method of the modified wood powder comprises the following steps:
s11, taking the following raw materials, namely 20-30 parts of cork particles with 30-50 meshes, 20-30 parts of cork particles with 60-80 meshes and 30-50 parts of cork particles with 100-120 meshes, and stirring and mixing for 2-4 hours at a rotating speed of 600-800r/min by using a stirrer to obtain graded cork particles;
s12, mixing the graded cork granule obtained in the step S11 with the enzymolysis liquid according to the mass ratio of 1: mixing 50-100 parts of the raw materials, adding the mixture into a beaker, moving the beaker into a digital display speed measurement constant temperature magnetic stirrer, and performing constant temperature enzymolysis for 4-6 hours at the temperature of 30-40 ℃ and the rotating speed of 300-500 r/min;
s13, filtering the mixture obtained in the S12, wherein the mesh number of a filter screen is 150 meshes, washing the obtained filter cake with deionized water for 3-5 times, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight at 105-110 ℃ to obtain dry cork wood powder particles;
s14, taking 40-60 parts by weight of diphenylmethane diisocyanate, 20-30 parts by weight of ethyl orthosilicate and 10-20 parts by weight of dry cork wood powder particles, mixing, carrying out ultrasonic immersion for 40-60min under the condition that the ultrasonic frequency is 45-55kHz, filtering to obtain filter residue, washing the filter residue with absolute ethyl alcohol for 3-5 times, and drying to constant weight to obtain the modified wood powder.
2. The composite plugging agent bridge plug plugging particle for drilling fluid as claimed in claim 1, wherein the hard filler is a mixture of nanoscale silica, nanoscale calcium carbonate, 400-mesh calcium carbonate and 800-mesh calcium carbonate, and the mass ratio of the nanoscale silica to the nanoscale calcium carbonate to the 400-mesh calcium carbonate to the 800-mesh calcium carbonate is 5-8:3-5:1:2-4.
3. The composite plugging agent bridge plug plugging particle for drilling fluid as claimed in claim 1, wherein the dispersant is span 80 or tween 80.
4. The composite plugging agent bridge plug plugging particle for drilling fluid as claimed in claim 1, wherein the cross-linking agent is one or a mixture of tetraethoxysilane and polyethyltetraethoxysilane mixed at any ratio.
5. The composite plugging agent bridge plugging particles for drilling fluid as claimed in claim 1, wherein the vulcanizing agent is dibutyltin dilaurate or stannous octoate.
6. The composite plugging agent bridge plug plugging particle for drilling fluid as claimed in claim 1, wherein the enzymatic hydrolysate is pectinase and deionized water in a mass ratio of 1: 100-150.
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